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Sample records for znfe2o4 spinel revealed

  1. Evaluation of Antioxidant and Cytotoxicity Activities of Copper Ferrite (CuFe2O4 and Zinc Ferrite (ZnFe2O4 Nanoparticles Synthesized by Sol-Gel Self-Combustion Method

    Directory of Open Access Journals (Sweden)

    Samikannu Kanagesan

    2016-08-01

    Full Text Available Spinel copper ferrite (CuFe2O4 and zinc ferrite (ZnFe2O4 nanoparticles were synthesized using a sol-gel self-combustion technique. The structural, functional, morphological and magnetic properties of the samples were investigated by Fourier transform infrared spectroscopy (FTIR, X-ray diffraction (XRD, Transmission electron microscopy (TEM and vibrating sample magnetometry (VSM. XRD patterns conform to the copper ferrite and zinc ferrite formation, and the average particle sizes were calculated by using a transmission electron microscope, the measured particle sizes being 56 nm for CuFe2O4 and 68 nm for ZnFe2O4. Both spinel ferrite nanoparticles exhibit ferromagnetic behavior with saturation magnetization of 31 emug−1 for copper ferrite (50.63 Am2/Kg and 28.8 Am2/Kg for zinc ferrite. Both synthesized ferrite nanoparticles were equally effective in scavenging 2,2-diphenyl-1-picrylhydrazyl hydrate (DPPH free radicals. ZnFe2O4 and CuFe2O4 nanoparticles showed 30.57% ± 1.0% and 28.69% ± 1.14% scavenging activity at 125 µg/mL concentrations. In vitro cytotoxicity study revealed higher concentrations (>125 µg/mL of ZnFe2O4 and CuFe2O4 with increased toxicity against MCF-7 cells, but were found to be non-toxic at lower concentrations suggesting their biocompatibility.

  2. Formation of the ZnFe2O4 phase in an electric arc furnace off-gas treatment system.

    Science.gov (United States)

    Suetens, T; Guo, M; Van Acker, K; Blanpain, B

    2015-04-28

    To better understand the phenomena of ZnFe2O4 spinel formation in electric arc furnace dust, the dust was characterized with particle size analysis, X-ray fluorescence (XRF), electron backscatter diffraction (EBSD), and electron probe micro-analysis (EPMA). Different ZnFe2O4 formation reaction extents were observed for iron oxide particles with different particle sizes. ZnO particles were present as both individual particles and aggregated on the surface of larger particles. Also, the slag particles found in the off-gas were shown not to react with the zinc vapor. After confirming the presence of a ZnFe2O4 formation reaction, the thermodynamic feasibility of in-process separation - a new electric arc furnace dust treatment technology - was reevaluated. The large air intake and the presence of iron oxide particles in the off-gas were included into the thermodynamic calculations. The formation of the stable ZnFe2O4 spinel phase was shown to be thermodynamically favorable in current electric arc furnace off-gas ducts conditions even before reaching the post combustion chamber. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Formation of the ZnFe2O4 phase in an electric arc furnace off-gas treatment system

    International Nuclear Information System (INIS)

    Suetens, T.; Guo, M.; Van Acker, K.; Blanpain, B.

    2015-01-01

    Highlights: • EAF dust was characterized with particle size analysis, XRF, and EPMA. • Slag particles showed no sign of reaction with Zn vapor. • Fe 2 O 3 particles showed different degrees of reaction based on their size. • The thermodynamic stability of Zn vapor in EAF off-gas ducts was reevaluated. • In presence of Fe 2 O 3 , Zn vapor reacts to form ZnFe 2 O 4 and ZnO. - Abstract: To better understand the phenomena of ZnFe 2 O 4 spinel formation in electric arc furnace dust, the dust was characterized with particle size analysis, X-ray fluorescence (XRF), electron backscatter diffraction (EBSD), and electron probe micro-analysis (EPMA). Different ZnFe 2 O 4 formation reaction extents were observed for iron oxide particles with different particle sizes. ZnO particles were present as both individual particles and aggregated on the surface of larger particles. Also, the slag particles found in the off-gas were shown not to react with the zinc vapor. After confirming the presence of a ZnFe 2 O 4 formation reaction, the thermodynamic feasibility of in-process separation – a new electric arc furnace dust treatment technology – was reevaluated. The large air intake and the presence of iron oxide particles in the off-gas were included into the thermodynamic calculations. The formation of the stable ZnFe 2 O 4 spinel phase was shown to be thermodynamically favorable in current electric arc furnace off-gas ducts conditions even before reaching the post combustion chamber

  4. ZnFe2O4 nanoparticles for potential application in radiosensitization

    International Nuclear Information System (INIS)

    Hidayatullah, M; Nurhasanah, I; Budi, W S

    2016-01-01

    Radiosensitizer is a material that can increase the effects of radiation in radiotherapy application. Various materials with high effective atomic number have been developed as a radiosensitizer, such as metal, iron oxide and quantum dot. In this study, ZnFe 2 O 4 nanoparticles are included in iron oxide class were synthesized by precipitation method from the solution of zinc nitrate and ferrite nitrate and followed by calcination at 700° C for 3 hours. The XRD pattern shows that most of the observed peaks can be indexed to the cubic phase of ZnFe 2 O 4 with a lattice parameter of 8.424 Å. SEM image reveals that nanoparticles are the sphere-like shape with size in the range 84-107 nm. The ability of ZnFe 2 O 4 nanoparticles as radiosensitizer was examined by loading those nanoparticles into Escherichia coli cell culture which irradiated with photon energy of 6 MV at a dose of 2 Gy. ZnFe 2 O 4 nanoparticles showed ability to increase the absorbed dose by 0.5 to 1.0 cGy/g. In addition, the presence of 1 g/L ZnFe 2 O 4 nanoparticles resulted in an increase radiation effect by 6.3% higher than if exposed to radiation only. These results indicated that ZnFe 2 O 4 nanoparticles can be used as the radiosensitizer for increasing radiation effect in radiotherapy. (paper)

  5. Size dependent electrical and magnetic properties of ZnFe2O4 nanoparticles synthesized by the combustion method: Comparison between aspartic acid and glycine as fuels

    International Nuclear Information System (INIS)

    Shanmugavani, A.; Kalai Selvan, R.; Layek, Samar; Sanjeeviraja, C.

    2014-01-01

    Using two different fuels such as aspartic acid and glycine, the spinel zinc ferrite nanoparticles were synthesized by the combustion method at different pH values. The thermochemical calculations for both the fuel assisted materials and its adiabatic flame temperature were calculated. The X-ray diffraction (XRD) pattern revealed the formation of single phase ZnFe 2 O 4 with high crystallinity. The characteristic functional groups of Fe3O and Zn3O were identified through FTIR analysis. Uniform size distribution of spherical particle in the average size range of 35–100 nm was inferred from SEM images. The room temperature DC conductivities of ZnFe 2 O 4 particles prepared by using aspartic and glycine are in the order of 10 −7 and 10 −8 respectively. The dielectric spectral analysis inferred that the obtained dielectric constant is high at low frequency and decreases with increase in frequency. This dielectric behavior is in accordance with the Maxwell–Wagner interfacial polarization. VSM and Mössbauer analysis revealed that the prepared material exhibits paramagnetic behavior and Fe 3+ state of iron content in ZnFe 2 O 4 at room temperature. - Highlights: • For the first time aspartic acid is used as a fuel to synthesize ZnFe 2 O 4 nanoparticles. • Theoretical adiabatic flame temperature for the formation of ZnFe 2 O 4 is calculated. • Individual spherical shape particles are achieved by combustion synthesis. • Enhanced room temperature conductivity for aspartic acid assisted particles are revealed. • Size dependent electrical and magnetic properties are demonstrated

  6. Study of solid state interactions in the systems ZnFe2O4 - CaO, ZnFe2O4 - MgO and zinc cake with CaO and MgO

    Directory of Open Access Journals (Sweden)

    Peltekov A.B.

    2013-01-01

    Full Text Available The solid state interactions of CaO and MgO with synthetic and industrial ZnFe2O4 (in zinc cake have been studied using chemical, XRD analysis and Mössbauer spectroscopy. The exchange reactions in the systems ZnFe2O4 - CaO and ZnFe2O4 - MgO have been investigated in the range of 850-1200ºC and duration up to 180 min. It has been established that Ca2+ and Mg2+ ions exchange Zn2+ in ferrite partially and the solubility of zinc in a 7% sulfuric acid solution increases. The possibilities for utilization of the obtained results in zinc hydrometallurgy have been discussed.

  7. Structural, optical and magnetic studies of CuFe2O4, MgFe2O4 and ZnFe2O4 nanoparticles prepared by hydrothermal/solvothermal method

    Science.gov (United States)

    Kurian, Jessyamma; Mathew, M. Jacob

    2018-04-01

    In this paper we report the structural, optical and magnetic studies of three spinel ferrites namely CuFe2O4, MgFe2O4 and ZnFe2O4 prepared in an autoclave under the same physical conditions but with two different liquid medium and different surfactant. We use water as the medium and trisodium citrate as the surfactant for one method (Hydrothermal method) and ethylene glycol as the medium and poly ethylene glycol as the surfactant for the second method (solvothermal method). The phase identification and structural characterization are done using XRD and morphological studies are carried out by TEM. Cubical and porous spherical morphologies are obtained for hydrothermal and solvothermal process respectively without any impurity phase. The optical studies are carried out using FTIR and UV-Vis reflectance spectra. In order to elucidate the nonlinear optical behaviour of the prepared nanomaterial, open aperture z-scan technique is used. From the fitted z-scan curves nonlinear absorption coefficient and the saturation intensity are determined. The magnetic characterization of the samples is performed at room temperature using vibrating sample magnetometer measurements. The M-H curves obtained are fitted using theoretical equation and the different components of magnetization are determined. Nanoparticles with high saturation magnetization are obtained for MgFe2O4 and ZnFe2O4 prepared under solvothermal reaction. The magnetic hyperfine parameters and the cation distribution of the prepared materials are determined using room temperature Mössbauer spectroscopy. The fitted spectra reveal the difference in the magnetic hyperfine parameters owing to the change in size and morphology.

  8. Nanocrystalline spinel ferrite (MFe2O4, M = Ni, Co, Mn, Mg, Zn) powders prepared by a simple aloe vera plant-extracted solution hydrothermal route

    International Nuclear Information System (INIS)

    Phumying, Santi; Labuayai, Sarawuth; Swatsitang, Ekaphan; Amornkitbamrung, Vittaya; Maensiri, Santi

    2013-01-01

    Graphical abstract: This figure shows the specific magnetization curves of the as-prepared MFe 2 O 4 (M = Ni, Co, Mn, Mg, Zn) powders obtained from room temperature VSM measurement. These curves are typical for a soft magnetic material and indicate hysteresis ferromagnetism in the field ranges of ±500 Oe, ±1000 Oe, and ±2000 Oe for the CoFe 2 O 4 , MgFe 2 O 4 and MnFe 2 O 4 respectively, whereas the samples of NiFe 2 O 4 and ZnFe 2 O 4 show a superparamagnetic behavior. Highlights: ► Nanocrystalline MFe 2 O 4 powders were synthesized by a novel hydrothermal method. ► Metal acetylacetonates and aloe vera plant-extracted solution are used. ► This biosynthetic route is very simple and provides high-yield oxide nanomaterials. ► XRD and TEM results indicate that the prepared samples have only spinel structure. ► The maximum M s of 68.9 emu/g at 10 kOe were observed for the samples of MnFe 2 O 4 . - Abstract: Nanocrystalline spinel ferrite MFe 2 O 4 (M = Ni, Co, Mn, Mg, Zn) powders were synthesized by a novel hydrothermal method using Fe(acac) 3 , M(acac) 3 (M = Ni, Co, Mn, Mg, Zn) and aloe vera plant extracted solution. The X-ray diffraction and selected-area electron diffraction results indicate that the synthesized nanocrystalline have only spinel structure without the presence of other phase impurities. The crystal structure and morphology of the spinel ferrite powders, as revealed by TEM, show that the NiFe 2 O 4 and CoFe 2 O 4 samples contain nanoparticles, whereas the MnFe 2 O 4 and MgFe 2 O 4 samples consist of many nanoplatelets and nanoparticles. Interestingly, the ZnFe 2 O 4 sample contains plate-like structure of networked nanocrystalline particles. Room temperature magnetization results show a ferromagnetic behavior of the CoFe 2 O 4 , MnFe 2 O 4 and MgFe 2 O 4 samples, whereas the samples of NiFe 2 O 4 and ZnFe 2 O 4 exhibit a superparamagnetic behavior

  9. Inverse spinel ZnFe2O4 nanoparticles synthesized by ion implantation and post-annealing: An investigation using X-ray spectroscopy and magneto-transport

    International Nuclear Information System (INIS)

    Zhou Shengqiang; Potzger, K.; Buerger, D.; Kuepper, K.; Helm, M.; Fassbender, J.; Schmidt, H.

    2009-01-01

    Noncrystalline ZnFe 2 O 4 has been investigated intensively due to the drastic difference in cation distribution compared with bulk materials. We previously synthesized ZnFe 2 O 4 nanoparticles by ion implantation and post-annealing [S. Zhou, K. Potzger, H. Reuther, G. Talut, F. Eichhorn, J. von Borany, W. Skorupa, M. Helm, J. Fassbender, J. Phys. D - Appl. Phys. 40 (2007) 964]. These ZnFe 2 O 4 nanocrystals are crystallographically oriented inside the ZnO matrix and show a hysteretic behavior upon magnetization reversal at 5 K. Their magnetic properties are explained by assuming that Fe 3+ ions partially occupy tetrahedral sites. In this paper an X-ray spectroscopic and magneto-transport investigation on ZnFe 2 O 4 nanocrystals in a ZnO matrix will be presented. The occupation of Fe 3+ at tetrahedral sites has been directly proved. A positive magnetoresistance (MR) effect is observed and is attributed to ordinary MR.

  10. Magnetically separable core–shell ZnFe_2O_4@ZnO nanoparticles for visible light photodegradation of methyl orange

    International Nuclear Information System (INIS)

    Kulkarni, Suresh D.; Kumbar, Sagar; Menon, Samvit G.; Choudhari, K.S.; Santhosh, C.

    2016-01-01

    Highlights: • Phase pure, magnetic ZnFe_2O_4@ZnO nanoparticles synthesized with excellent yield. • ZnFe_2O_4@ZnO displayed higher UV photocatalytic efficiency than ZnO nanoparticles. • First report on visible light photodegradation of methyl orange by ZnFe_2O_4@ZnO. • Excellent reusability of ZnFe_2O_4@ZnO nanoparticles observed for azo dye removal. - Abstract: Visible light photodegradation of aqueous methyl orange using magnetically separable core–shell ZnFe_2O_4@ZnO nanoparticles is reported. A combination of low temperature (190 °C) microwave synthesis and hydrothermal method were used to prepare phase pure material with excellent yield (95%). The magnetic separability, surface area of 41 m"2/g and visible light absorption make ZnFe_2O_4@ZnO nanoparticles a good solar photocatalyst. ZnFe_2O_4@ZnO displayed greater UV photocatalytic efficiency than ZnO owing to the generation of large number of electron-hole pairs. Visible light photodegradation of MO using ZnFe_2O_4@ZnO nanoparticles is reported for the first time. Higher first order rate constants under both UV and visible light for core-shell nanoparticles suggested their superiority over its individual oxides. The ZnFe_2O_4@ZnO showed excellent reusability with high photocatalytic efficiencies suggesting its suitability for solar photocatalytic applications.

  11. Synthesis of ZnFe2O4/SiO2 composites derived from a diatomite template.

    Science.gov (United States)

    Liu, Zhaoting; Fan, Tongxiang; Zhou, Han; Zhang, Di; Gong, Xiaolu; Guo, Qixin; Ogawa, Hiroshi

    2007-03-01

    A novel porous ZnFe2O4/SiO2 composite product has been generated with a template-directed assembly method from porous diatomite under different synthesis conditions, such as precursor concentrations (metallic nitrates), calcination temperature and diatomite type. The phase composition and morphology of all the materials were examined by x-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). The results indicated that an inherited hierarchical porous structure from the diatomite template can be obtained, and the synthesis conditions were found to have clear effects on the formation of the ZnFe2O4/SiO2 composite. The ideal composite of ZnFe2O4/SiO2 can be obtained through optimization of diatomite template type, precursor solution and calcination temperature. Furthermore, the adsorption abilities of two types of diatomites were analyzed in detail using FTIR spectra and nitrogen adsorption measurements etc, which proved that A-diatomite (Shengzhou-diatomite) is better than B-diatomite (Changbai-diatomite) on the aspect of adsorbing Zn and Fe ions, and of forming the ZnFe2O4.

  12. ZnFe2O4 Containing Nanoparticles: Synthesis and Magnetic Properties

    Directory of Open Access Journals (Sweden)

    Zālīte Ilmārs

    2017-05-01

    Full Text Available Solid solutions of Co1−xZnxFe2O4 and Ni1−xZnxFe2O4 (0 < x < 1 nanoparticles were synthesized by sol-gel self-propagating combustion method. The obtained single cubic phase product has a specific surface area 25 m2∙g−1 to 33 m2∙g−1 and crystallite size 25 nm to 40 nm. Lattice parameters change linearly from 8.371 A (CoFe2O4 and 8.337 A (NiFe2O4 to 8.431 A (ZnFe2O4. The saturation magnetization (Ms changes non-linearly from 60.8 emu∙g−1 (CoFe2O4, respectively, from 35.6 emu∙g−1 (NiFe2O4 to 3.3 emu∙g−1 (ZnFe2O4 reaching maximal value 76.1 emu∙g−1 for Co0.8Zn0.2Fe2O4 and 64.9 emu∙g−1 – for Ni0.6Zn0.4Fe2O4.

  13. Nonstoichiometric Zn Ferrite and ZnFe2O4/Fe2O3 Composite Spheres: Preparation, Magnetic Properties, and Chromium Removal

    Science.gov (United States)

    Hang, Chun-Liang; Yang, Li-Xia; Sun, Chang-Mei; Liang, Ying

    2018-03-01

    Monodisperse and porous nonstoichiometric Zn ferrite can be prepared by a solvothermal method. Such non-Zn ferrite was used to be the precursor for synthesis of ZnFe2O4/Fe2O3 composite via calcination at 600°C for 3 h in air. X-ray powder diffractometer (XRD) and Energy Dispersive Spectrometer (EDS) proved the nonstoichiometry of Zn ferrite synthesized by solvothermal method and the formation of ZnFe2O4/Fe2O3 composite via calcination. TEM image showed that non-Zn ferrite spheres with wormlike nanopore structure were made of primary nanocrystals. BET surface area of non-Zn ferrite was much higher than that of ZnFe2O4/Fe2O3 composite. Saturation magnetization of non-Zn ferrites was significantly higher than that of ZnFe2O4/Fe2O3 composites. Calcination of non-Zn ferrite resulted in the formation of large amount of non-magnetic Fe2O3,which caused a low magnetization of composite. Because of higher BET surface area and higher saturation magnetization, non-Zn ferrite presented better Cr6+ adsorption property than ZnFe2O4/Fe2O3 composites.

  14. Synthesis of ZnFe2O4/ZnO nanocomposites immobilized on graphene with enhanced photocatalytic activity under solar light irradiation

    International Nuclear Information System (INIS)

    Sun, Lin; Shao, Rong; Tang, Lanqin; Chen, Zhidong

    2013-01-01

    Highlights: ► ZnFe 2 O 4 /ZnO nanocomposites immobilized on graphene were successfully prepared. ► The photocatalyst exhibited excellent reactivity under solar light irradiation. ► The photocatalysts could be recycled by external magnetic field conveniently. ► The photocatalytic mechanism of the novel material was proposed in detail. -- Abstract: Magnetically recyclable ZnFe 2 O 4 /ZnO nanocomposites immobilized on different content of graphene with favorable photocatalytic activity under solar light irradiation were successfully prepared on the basis of an ultrasound aided solution method. The molar ratio of ZnFe 2 O 4 to ZnO and the content of graphene could be controlled by adjusting the amount of zinc salts and graphene oxide dispersions. The most excellent photocatalytic activity under solar light irradiation was displayed when the molar ratio of ZnFe 2 O 4 to ZnO was 0.1 and the weight ratio of graphene to ZnFe 2 O 4 /ZnO was 0.04. Furthermore, the presence of magnetical ZnFe 2 O 4 will facilitate the recycling process of photocatalyst nanoparticles

  15. Synthesis and properties of ZnFe2O4 replica with biological hierarchical structure

    International Nuclear Information System (INIS)

    Liu, Hongyan; Guo, Yiping; Zhang, Yangyang; Wu, Fen; Liu, Yun; Zhang, Di

    2013-01-01

    Highlights: • ZFO replica with hierarchical structure was synthesized from butterfly wings. • Biotemplate has a significant impact on the properties of ZFO material. • Our method opens up new avenues for the synthesis of spinel ferrites. -- Abstract: ZnFe 2 O 4 replica with biological hierarchical structure was synthesized from Papilio paris by a sol–gel method followed by calcination. The crystallographic structure and morphology of the obtained samples were characterized by X-ray diffraction, field-emission scanning electron microscope, and transmittance electron microscope. The results showed that the hierarchical structures were retained in the ZFO replica of spinel structure. The magnetic behavior of such novel products was measured by a vibrating sample magnetometer. A superparamagnetism-like behavior was observed due to nanostructuration size effects. In addition, the ZFO replica with “quasi-honeycomb-like structure” showed a much higher specific capacitance of 279.4 F g −1 at 10 mV s −1 in comparison with ZFO powder of 137.3 F g −1 , attributing to the significantly increased surface area. These results demonstrated that ZFO replica is a promising candidate for novel magnetic devices and supercapacitors

  16. Magnetic structure evolution in mechanically milled nanostructured ZnFe2O4 particles

    DEFF Research Database (Denmark)

    Jiang, Jianzhong; Wynn, P.; Mørup, Steen

    1999-01-01

    Nanostructured partially-inverted ZnFe2O4 particles have been prepared from bulk ZnFe2O4 by high-energy ball milling in an open container. The grain size reduction, cation site distributions, and the evolution of magnetic structures have been studied by x-ray diffraction with Rietveld structure...... refinements, transmission electron microscopy, and Mossbauer spectroscopy. It is found that a change of magnetic structure from an antiferromagnetic to a ferrimagnetic (or ferromagnetic) structure occurs in the milled samples. This change is correlated with the redistribution of the cations, Zn and Fe...

  17. An excellent performance anode of ZnFe2O4/flake graphite composite for lithium ion battery

    International Nuclear Information System (INIS)

    Yao, Lingmin; Hou, Xianhua; Hu, Shejun; Tang, Xiaoqin; Liu, Xiang; Ru, Qiang

    2014-01-01

    Highlights: • ZnFe 2 O 4 /flake graphite composite was synthesized by hydrothermal method. • The ZnFe 2 O 4 /flake graphite anode demonstrated high initial coulombic efficiency of 87.7%. • The initial discharge /charge capacity was 848 mA h g −1 and 744 mA h g −1 . • The high capacity retention of 98% was obtained for the ZnFe 2 O 4 /flake graphite anode. -- Abstract: An approach of hydrothermal reaction for lithium ion battery was adopted, by which ZnFe 2 O 4 /flake graphite composites with excellent performance could be prepared as anode materials for lithium ion batteries. With nano-sized ZnFe 2 O 4 particles coating on the electrochemical active matrix of flake graphite, the special composites allowed improved electronic conductivity and constructed an expressway for the transport of charges and lithium ions. Thus the ZnFe 2 O 4 /flake graphite anode became a compromise between capacity and cycle ability. The initial discharge–charge capacity was 848 mA h g −1 and 744 mA h g −1 at a constant current density of 100 mA g −1 , respectively. As high as 87.7% of the initial coulombic efficiency was obtained. Additionally, the charge capacity maintained constantly in the range of 720–735 mA h g −1 in following cycles. And a high reversible charge capacity of 730 mA h g −1 could be attained after 100 cycles, with the reversible capacity retention of 98%

  18. First report on synthesis of ZnFe_2O_4 thin film using successive ionic layer adsorption and reaction: Approach towards solid-state symmetric supercapacitor device

    International Nuclear Information System (INIS)

    Raut, Shrikant S.; Sankapal, Babasaheb R.

    2016-01-01

    Highlights: • First report on synthesis of ZnFe_2O_4 thin film using SILAR method. • ZnFe_2O_4 electrode yields the specific capacitance of 471 Fg"−"1 at a scan rate of 5 mV s"−"1 in 1 M NaOH aqueous solution. • Solid-state symmetric supercapacitor device based on ZnFe_2O_4 sandwiched in polyvinyl alcohol (PVA)–LiClO_4 gel electrolyte exhibits voltage windows of 1.0 V. • ZnFe_2O_4-SSS supercapacitor device shows good energy and power density with long cycle life. - Abstract: ZnFe_2O_4 thin film has been synthesized by a simple and low cost successive ionic layer adsorption and reaction (SILAR) method without the use of surfactant or template. The nanoplate composed of nanoparticles with porous surface morphology has been revealed which is beneficial towards supercapacitor application. Formed ZnFe_2O_4 thin film has been tested as an electrode material for supercapacitor through electrochemical analysis. First attempt for SILAR synthesized ZnFe_2O_4 thin film exhibited a specific capacitance of 471 Fg"−"1 at a scan rate of 5 mVs"−"1 in 1 M NaOH aqueous solution. Further, ZnFe_2O_4 solid-state symmetric (SSS) supercapacitor device demonstrated voltage window of 1.0 V with specific capacitance of 32 Fg"−"1, energy density of 4.47 Whkg"−"1 and power density of 277 Wkg"−"1 at 1 Ag"−"1 current density. Such high performance capacitive behavior indicates ZnFe_2O_4 thin film is promising and low cost electrode material towards energy storage devices for various portable electronic systems.

  19. Graphene–palladium nanowires based electrochemical sensor using ZnFe2O4–graphene quantum dots as an effective peroxidase mimic

    International Nuclear Information System (INIS)

    Liu, Weiyan; Yang, Hongmei; Ma, Chao; Ding, Ya-nan; Ge, Shenguang; Yu, Jinghua; Yan, Mei

    2014-01-01

    Highlights: • The nanohybrid ZnFe 2 O 4 /GQDs was developed by assembling the GQDs on the ZnFe 2 O 4 through a photo-Fenton reaction. • The ZnFe 2 O 4 /GQDs exhibited higher peroxidase-like activity and better stability than each individual and HRP. • An electrochemical sensor was fabricated using ZnFe 2 O 4 /GQDs nanohybrid as a mimic enzymatic to detect DNA. • Graphene and Pd nanowires were modified on the glassy carbon electrode, which improved the electronic transfer rate. - Abstract: We proposed an electrochemical DNA sensor by using peroxidase-like magnetic ZnFe 2 O 4 –graphene quantum dots (ZnFe 2 O 4 /GQDs) nanohybrid as a mimic enzymatic label. Aminated graphene and Pd nanowires were successively modified on glassy carbon electrode, which improved the electronic transfer rate as well as increased the amount of immobilized capture ssDNA (S1). The nanohybrid ZnFe 2 O 4 /GQDs was prepared by assembling the GQDs on the surface of ZnFe 2 O 4 through a photo-Fenton reaction, which was not only used as a mimic enzyme but also as a carrier to label complementary ssDNA (S3). By synergistically integrating highly catalytically activity of nano-sized GQDs and ZnFe 2 O 4 , the nanohybrid possessed highly-efficient peroxidase-like catalytic activity which could produce a large current toward the reduction of H 2 O 2 for signal amplification. Thionine was used as an excellent electron mediator. Compared with traditional enzyme labels, the mimic enzyme ZnFe 2 O 4 /GQDs exhibited many advantages such as environment friendly and better stability. Under the optimal conditions, the approach provided a wide linear range from 10 −16 to 5 × 10 −9 M and low detection limit of 6.2 × 10 −17 M. The remarkable high catalytic capability could allow the nanohybrid to replace conventional peroxidase-based assay systems. The new, robust and convenient assay systems can be widely utilized for the identification of other target molecules

  20. Porous Hierarchical Nitrogen-doped Carbon Coated ZnFe_2O_4 Composites as High Performance Anode Materials for Lithium Ion Batteries

    International Nuclear Information System (INIS)

    Yue, Hongyun; Wang, Qiuxian; Shi, Zhenpu; Ma, Chao; Ding, Yanmin; Huo, Ningning; Zhang, Jun; Yang, Shuting

    2015-01-01

    Porous hierarchical and nitrogen-doped carbon coated ZnFe_2O_4 (ZnFe_2O_4@NC) was obtained by combustion method and unique carbon coating technology. Gum Arabic was firstly introduced in the carbon coating process as an additive, which played an important role to control the uniformity of carbon coating layer. The nitrogen-doped carbon layer was obtained through the pyrolysis of glycine. The elemental composition and content of the nitrogen-doped carbon in composites were characterized by X-ray photoelectron spectroscopy (XPS), energy dispersive spectroscopy (EDS) and thermal gravimetric analysis (TGA). The galvanostatic charge/discharge cycling was used to test the electrochemical performance of ZnFe_2O_4@NC and pure ZnFe_2O_4. The sub-micro size ZnFe_2O_4@NC with unique porous structure showed an excellent electrochemical performance as an anode material, which was higher than that of pure ZnFe_2O_4. ZnFe_2O_4@NC could maintain the specific discharge capacity of 1477 mAh g"−"1 at 0.1 A g"−"1 after 100 cycles and 705 mAh g"−"1 at 1 A g"−"1 after 1000 cycles, respectively.

  1. Solvothermal Synthesis of Hierarchical Colloidal Nanocrystal Assemblies of ZnFe2O4 and Their Application in Water Treatment

    Directory of Open Access Journals (Sweden)

    Peizhi Guo

    2016-09-01

    Full Text Available Hierarchical colloidal nanocrystal assemblies (CNAs of ZnFe2O4 have been synthesized controllably by a solvothermal method. Hollow ZnFe2O4 spheres can be formed with the volume ratios of ethylene glycol to ethanol of 1:4 in the starting systems, while solid ZnFe2O4 CNAs are obtained by adjusting the volume proportion of ethylene glycol to ethanol from 1:2 to 2:1. Magnetometric measurement data showed that the ZnFe2O4 CNAs obtained with the volume ratios of 1:2 and 1:1 exhibited weak ferromagnetic behavior with high saturation magnetization values of 60.4 and 60.3 emu·g−1, respectively. However, hollow spheres showed a saturation magnetization value of 52.0 emu·g−1, but the highest coercivity among all the samples. It was found that hollow spheres displayed the best ability to adsorb Congo red dye among all the CNAs. The formation mechanisms of ZnFe2O4 CNAs, as well as the relationship between their structure, crystallite size, and properties were discussed based on the experimental results.

  2. Synthesis and characterization of magnetic diphase ZnFe2O4/γ-Fe2O3 electrospun fibers

    International Nuclear Information System (INIS)

    Arias, M.; Pantojas, V.M.; Perales, O.; Otano, W.

    2011-01-01

    Magnetic nanofibers of ZnFe 2 O 4 /γ-Fe 2 O 3 composite were synthesized by electrospinning from a sol-gel solution containing a molar ratio (Fe/Zn) of 3. The effects of the calcination temperature on phase composition, particle size and magnetic properties have been investigated. Zinc ferrite fibers were obtained by calcinating the electrospun fibers in air from 300 to 800 deg. C and characterized by thermogravimetric analyses, Fourier transformed infrared spectroscopy, X-ray photoemission spectroscopy, X-ray diffraction, vibration sample magnetometry and magnetic force microscopy. The resulting fibers, with diameters ranging from 90 to 150 nm, were ferrimagnetic with high saturation magnetization as compared to bulk. An increase in the calcination temperature resulted in an increase in particle size and saturation magnetization. The observed increase in saturation magnetization was most likely due to the formation and growth of ZnFe 2 O 4 /γ-Fe 2 O 3 diphase crystals. The highest saturation magnetization (45 emu/g) was obtained for fibers calcined at 800 deg. C. - Research highlights: → Nanofibers were produced by electrospinning from a sol-gel. → ZnFe 2 O 4 /γ-Fe 2 O 3 formed after cacination in air from 300 to 800 deg. C. → Fibers were ferrimagnetic with high saturation magnetization. → Crystallite particle size and saturation magnetization increase with temperature. → Magnetic domains with sizes similar to topographical grains were observed.

  3. Graphene-palladium nanowires based electrochemical sensor using ZnFe2O4-graphene quantum dots as an effective peroxidase mimic.

    Science.gov (United States)

    Liu, Weiyan; Yang, Hongmei; Ma, Chao; Ding, Ya-nan; Ge, Shenguang; Yu, Jinghua; Yan, Mei

    2014-12-10

    We proposed an electrochemical DNA sensor by using peroxidase-like magnetic ZnFe2O4-graphene quantum dots (ZnFe2O4/GQDs) nanohybrid as a mimic enzymatic label. Aminated graphene and Pd nanowires were successively modified on glassy carbon electrode, which improved the electronic transfer rate as well as increased the amount of immobilized capture ssDNA (S1). The nanohybrid ZnFe2O4/GQDs was prepared by assembling the GQDs on the surface of ZnFe2O4 through a photo-Fenton reaction, which was not only used as a mimic enzyme but also as a carrier to label complementary ssDNA (S3). By synergistically integrating highly catalytically activity of nano-sized GQDs and ZnFe2O4, the nanohybrid possessed highly-efficient peroxidase-like catalytic activity which could produce a large current toward the reduction of H2O2 for signal amplification. Thionine was used as an excellent electron mediator. Compared with traditional enzyme labels, the mimic enzyme ZnFe2O4/GQDs exhibited many advantages such as environment friendly and better stability. Under the optimal conditions, the approach provided a wide linear range from 10(-16) to 5×10(-9) M and low detection limit of 6.2×10(-17) M. The remarkable high catalytic capability could allow the nanohybrid to replace conventional peroxidase-based assay systems. The new, robust and convenient assay systems can be widely utilized for the identification of other target molecules. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Experimental and ab initio study of the hyperfine parameters of ZnFe {sub 2}O{sub 4} with defects

    Energy Technology Data Exchange (ETDEWEB)

    Quintero, J. Melo; Salcedo Rodríguez, K. L.; Pasquevich, G. A.; Zélis, P. Mendoza; Stewart, S. J., E-mail: stewart@fisica.unlp.edu.ar; Rodríguez Torres, C. E.; Errico, L. A. [Universidad Nacional de La Plata, IFLP-CCT- La Plata-CONICET and Departamento de Física, Facultad de Ciencias Exactas, C. C. 67 (Argentina)

    2016-12-15

    We present a combined Mössbauer and ab initio study on the influence of oxygen-vacancies on the hyperfine and magnetic properties of the ZnFe {sub 2}O{sub 4} spinel ferrite. Samples with different degree of oxygen-vacancies were obtained from zinc ferrite powder that was thermally treated at different temperatures up to 650 {sup ∘}C under vacuum.Theoretical calculations of the hyperfine parameters, magnetic moments and magnetic alignment have been carried out considering different defects such as oxygen vacancies and cation inversion. We show how theoretical and experimental approaches are complementary to characterize the local structure around Fe atoms and interpret the observed changes in the hyperfine parameters as the level of defects increases.

  5. Visible light photocatalytic activities of ZnFe_2O_4/ZnO nanoparticles for the degradation of organic pollutants

    International Nuclear Information System (INIS)

    Rameshbabu, R.; Kumar, Niraj; Karthigeyan, A.; Neppolian, B.

    2016-01-01

    ZnFe_2O_4/ZnO nanoparticles have been synthesized by co-precipitation method using polyvinyl alcohol (PVA) as surfactant. The phase formation of synthesized products was systematically investigated from powder X-ray diffraction. Cubic ZnFe_2O_4 and hexagonal ZnO were identified in accordance with different molar concentrations of Fe"3"+ ions. The morphology and functionality were analyzed using field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and Fourier transform infrared (FTIR) spectroscopy. The optical properties and change in the band gap from UV to visible region upon increasing molar concentration of Fe"3"+ ions were analyzed from diffuse reflectance spectra (DRS). Superparamagnetic property was observed for synthesized ZnFe_2O_4/ZnO nanoparticles using vibrating sample magnetometer (VSM). The methylene blue and methyl orange were taken as model dyes to illustrate the photocatalytic activity of synthesized products under visible light irradiation. Maximum degradation of 99% for methyl orange (MO) was achieved by the use of 13 nm sized ZnFe_2O_4/ZnO nanoparticles as catalyst and a minutely less activity was observed for the methylene blue (MB) degradation (98%), when the photocatalytic processes were carried out for 5 h and 6 h, respectively. - Highlights: • Co-precipitation method is proposed to synthesize magnetic nanoparticles. • Modifications in the molar concentration lead to the shift in absorption edge. • Superparamagnetic property is demonstrated for the nanoparticles. • Two dye pollutants are utilized to demonstrate the photocatalytic activity.

  6. Some Spinel Oxide Compounds as Reducing Gas Sensors

    Directory of Open Access Journals (Sweden)

    Nicolae Rezlescu

    2007-04-01

    Full Text Available Four spinel ferrites, MFe2O4 (M = Cu, Cd, Zn and Ni, having various grain sizes (100 – 700 nm were prepared by sol-gel-selfcombustion and their sensing properties to reducing gases were investigated. The gas sensing characteristics were obtained by measuring the sensitivity as a function of various controlling factors, like operating temperature, composition and concentration of the gas, and finally the response time. The sensitivity of four ferrites to reducing gases like acetone, ethanol and LPG was been compared. It was revealed that CuFe2O4 is the most sensitive to LPG and ZnFe2O4 can be used as a sensor to selectively detect ethanol vapors in air. The strong interaction between ethanol and porous ZnFe2O4 can explain the selective sensitivity to ethanol and negligible sensitivity to the other reducing gases.

  7. In-situ synthesized ZnFe2O4 firmly anchored to the surface of MWCNTs as a long-life anode material with high lithium storage performance

    Science.gov (United States)

    Yang, Tianbo; Zhang, Wanxi; Li, Linlin; Jin, Bo; Jin, Enmei; Jeong, Sangmoon; Jiang, Qing

    2017-12-01

    Because of two different metal cations in the crystal structures, binary transition metal oxides possess a lot of unique properties. ZnFe2O4 emerges from these transition metal oxides on account of its high theoretical capacity (1072 mAh g-1). One-dimensional multi-walled carbon nanotubes (MWCNTs) would be a desirable conductive additive for ZnFe2O4, thereby improving the electrochemical performance of ZnFe2O4. In this work, we prepare ZnFe2O4/MWCNTs by solvothermal method with further heat-treatment. ZnFe2O4 nanoparticles are firmly anchored to the surface of MWCNTs. ZnFe2O4/MWCNTs nanocomposite displays high specific capacity (1278 mAh g-1 at a current density of 200 mA g-1 after 200 cycles, and 565 mAh g-1 at a current density of 1500 mA g-1 after 500 cycles), and good rate performance (367 mAh g-1 even at a current density of 6000 mAh g-1 after 80 cycles). The superior electrochemical performance may promote ZnFe2O4 to be a promising alternative anode in lithium-ion batteries.

  8. Enhanced photocatalytic performances and magnetic recovery capacity of visible-light-driven Z-scheme ZnFe2O4/AgBr/Ag photocatalyst

    Science.gov (United States)

    He, Jie; Cheng, Yahui; Wang, Tianzhao; Feng, Deqiang; Zheng, Lingcheng; Shao, Dawei; Wang, Weichao; Wang, Weihua; Lu, Feng; Dong, Hong; Zheng, Rongkun; Liu, Hui

    2018-05-01

    High efficiency, high stability and easy recovery are three key factors for practical photocatalysts. Z-scheme heterostructure is one of the most promising photocatalytic systems to meet all above requirements. However, efficient Z-scheme photocatalysts which could absorb visible light are still few and difficult to implement at present. In this work, the composite photocatalysts ZnFe2O4/AgBr/Ag were prepared through a two-step method. A ∼92% photodegradation rate on methyl orange was observed within 30 min under visible light, which is much better than that of individual ZnFe2O4 or AgBr/Ag. The stability was also greatly improved compared with AgBr/Ag. The increased performance is resulted from the suitable band alignment of ZnFe2O4 and AgBr, and it is defined as Z-scheme mechanism which was demonstrated by detecting active species and electrochemical impedance spectroscopy. Besides, ZnFe2O4/AgBr/Ag is ferromagnetic and can be recycled by magnet. These results show that ZnFe2O4/AgBr/Ag is a potential magnetically recyclable photocatalyst which can be driven by visible light.

  9. Magnetic and bioactivity evaluation of ferrimagnetic ZnFe2O4 containing glass ceramics for the hyperthermia treatment of cancer

    International Nuclear Information System (INIS)

    Shah, Saqlain A.; Hashmi, M.U.; Alam, S.; Shamim, A.

    2010-01-01

    Glass ceramics of the composition xZnO.25Fe 2 O 3 .(40-x)SiO 2 .25CaO.7P 2 O 5 .3Na 2 O were prepared by the melt-quench method using oxy-acetylene flame. Glass-powder compacts were sintered at 1100 deg. C for 3 h and then rapidly cooled at -10 deg. C. X-ray diffraction (XRD) revealed 3 prominent crystalline phases: ZnFe 2 O 4 , CaSiO 3 and Ca 10 (PO 4 ) 6 (OH) 2 . Vibrating sample magnetometer (VSM) data at 10 KOe and 500 Oe showed that saturation magnetization, coercivity and hence hysteresis area increased with the increase in ZnO content. Nano-sized ZnFe 2 O 4 crystallites were of pseudo-single domain structure and thus coercivity increased with the increase in crystallite size. ZnFe 2 O 4 exhibited ferrimagnetism due to the random distribution of Zn 2+ and Fe 3+ cations at tetrahedral A sites and octahedral B sites. This inversion/random distribution of cations was probably due to the surface effects of nano-ZnFe 2 O 4 and rapid cooling of the material from 1100 deg. C (thus preserving the high temperature state of the random distribution of cations). Calorimetric measurements were carried out using magnetic induction furnace at 500 Oe magnetic field and 400 KHz frequency. The data showed that maximum specific power loss and temperature increase after 2 min were 26 W/g and 37 deg. C, respectively for the sample containing 10% ZnO. The samples were immersed in simulated body fluid (SBF) for 3 weeks. Scanning electron microscope (SEM), energy dispersive spectroscopy (EDX) and XRD results confirmed the growth of precipitated hydroxyapatite phase after immersion in SBF, suggesting that the ferrimagnetic glass ceramics were bioactive and could bond to the living tissues in physiological environment.

  10. Magnetic and bioactivity evaluation of ferrimagnetic ZnFe 2O 4 containing glass ceramics for the hyperthermia treatment of cancer

    Science.gov (United States)

    Shah, Saqlain A.; Hashmi, M. U.; Alam, S.; Shamim, A.

    2010-02-01

    Glass ceramics of the composition xZnO·25Fe 2O 3·(40- x)SiO 2·25CaO·7P 2O 5·3Na 2O were prepared by the melt-quench method using oxy-acetylene flame. Glass-powder compacts were sintered at 1100 °C for 3 h and then rapidly cooled at -10 °C. X-ray diffraction (XRD) revealed 3 prominent crystalline phases: ZnFe 2O 4, CaSiO 3 and Ca 10(PO 4) 6(OH) 2. Vibrating sample magnetometer (VSM) data at 10 KOe and 500 Oe showed that saturation magnetization, coercivity and hence hysteresis area increased with the increase in ZnO content. Nano-sized ZnFe 2O 4 crystallites were of pseudo-single domain structure and thus coercivity increased with the increase in crystallite size. ZnFe 2O 4 exhibited ferrimagnetism due to the random distribution of Zn 2+ and Fe 3+ cations at tetrahedral A sites and octahedral B sites. This inversion/random distribution of cations was probably due to the surface effects of nano-ZnFe 2O 4 and rapid cooling of the material from 1100 °C (thus preserving the high temperature state of the random distribution of cations). Calorimetric measurements were carried out using magnetic induction furnace at 500 Oe magnetic field and 400 KHz frequency. The data showed that maximum specific power loss and temperature increase after 2 min were 26 W/g and 37 °C, respectively for the sample containing 10% ZnO. The samples were immersed in simulated body fluid (SBF) for 3 weeks. Scanning electron microscope (SEM), energy dispersive spectroscopy (EDX) and XRD results confirmed the growth of precipitated hydroxyapatite phase after immersion in SBF, suggesting that the ferrimagnetic glass ceramics were bioactive and could bond to the living tissues in physiological environment.

  11. Influence of Zn/Fe Molar Ratio on Optical and Magnetic Properties of ZnO and ZnFe2O4 Nanocrystal as Calcined Products of Layered Double Hydroxides

    Directory of Open Access Journals (Sweden)

    Abdullah Ahmed Ali Ahmed

    2014-01-01

    Full Text Available The coprecipitation method has been used to synthesize layered double hydroxide (Zn-Fe-LDH nanostructure at different Zn2+/Fe3+ molar ratios. The structural properties of samples were studied using powder X-ray diffraction (PXRD. LDH samples were calcined at 600°C to produce mixed oxides (ZnO and ZnFe2O4. The crystallite size of mixed oxide was found in the nanometer scale (18.1 nm for ZnFe2O4 and 43.3 nm for ZnO. The photocatalytic activity of the calcination products was investigated using ultraviolet-visible-near infrared (UV-VIS-NIR diffuse reflectance spectroscopy. The magnetic properties of calcined LDHs were investigated using a vibrating sample magnetometer (VSM. The calcined samples showed a paramagnetic behavior for all Zn2+/Fe3+ molar ratios. The effect of molar ratio on magnetic susceptibility of the calcined samples was also studied.

  12. Facile and efficient one-pot solvothermal and microwave-assisted synthesis of stable colloidal solutions of MFe2O4 spinel magnetic nanoparticles

    International Nuclear Information System (INIS)

    Solano, Eduardo; Perez-Mirabet, Leonardo; Martinez-Julian, Fernando; Guzmán, Roger; Arbiol, Jordi; Puig, Teresa; Obradors, Xavier; Yañez, Ramón; Pomar, Alberto; Ricart, Susagna; Ros, Josep

    2012-01-01

    Well-defined synthesis conditions of high quality MFe 2 O 4 (M = Mn, Fe, Co, Ni, Zn, and Cu) spinel ferrite magnetic nanoparticles, with diameters below 10 nm, have been described based on facile and efficient one-pot solvothermal or microwave-assisted heating procedures. Both methods are reproducible and scalable and allow forming concentrated stable colloidal solutions in polar solvents, but microwave-assisted heating allows reducing 15 times the required annealing time and leads to an enhanced monodispersity of the nanoparticles. Non-agglomerated nanoparticles dispersions have been achieved using a simple one-pot approach where a single compound, triethyleneglycol, behaves at the same time as solvent and capping ligand. A narrow nanoparticle size distribution and high quality crystallinity have been achieved through selected nucleation and growth conditions. High resolution transmission electron microscopy images and electron energy loss spectroscopy analysis confirm the expected structure and composition and show that similar crystal faceting has been formed in both synthetic approaches. The spinel nanoparticles behave as ferrimagnets with a high saturation magnetization and are superparamagnetic at room temperature. The influence of synthesis route on phase purity and unconventional magnetic properties is discussed in some particular cases such as CuFe 2 O 4 , CoFe 2 O 4 , and ZnFe 2 O 4 .

  13. Defect kinetics in spinels: Long-time simulations of MgAl2O4, MgGa2O4, and MgIn2O4

    International Nuclear Information System (INIS)

    Uberuaga, B. P.; Voter, A. F.; Sickafus, K. E.; Bacorisen, D.; Smith, Roger; Ball, J. A.; Grimes, R. W.

    2007-01-01

    Building upon work in which we examined defect production and stability in spinels, we now turn to defect kinetics. Using temperature accelerated dynamics (TAD), we characterize the kinetics of defects in three spinel oxides: magnesium aluminate MgAl 2 O 4 , magnesium gallate MgGa 2 O 4 , and magnesium indate MgIn 2 O 4 . These materials have varying tendencies to disorder on the cation sublattices. In order to understand chemical composition effects, we first examine defect kinetics in perfectly ordered, or normal, spinels, focusing on point defects on each sublattice. We then examine the role that cation disorder has on defect mobility. Using TAD, we find that disorder creates local environments which strongly trap point defects, effectively reducing their mobility. We explore the consequences of this trapping via kinetic Monte Carlo (KMC) simulations on the oxygen vacancy (V O ) in MgGa 2 O 4 , finding that V O mobility is directly related to the degree of inversion in the system

  14. Magnetic properties of ZnFe2O4 nanoparticles produced by a low-temperature solid-state reaction method

    International Nuclear Information System (INIS)

    Li Fashen; Wang Haibo; Wang Li; Wang Jianbo

    2007-01-01

    ZnFe 2 O 4 nanoparticles with average grain size ranging from 40 to 60 nm behaving superparamagnetic at room temperature have been produced using a low-temperature solid-state reaction (LTSSR) method without ball-milling process. Abnormal magnetic properties such as S-shape hysteresis loops and non-zero magnetic moments were observed. ZnFe 2 O 4 nanoparticles were also synthesized using a NaOH coprecipitation method and a PVA sol-gel method to study the relationship between the preparation processes and the magnetic properties. Spin-glass behavior was observed in the low temperature solid-state reaction produced Zn ferrite in the zero-field cooled (ZFC) measurement. Our work proves that the various preparation methods will to some extent determine the properties of magnetic nanoparticles

  15. Magnetic and catalytic properties of inverse spinel CuFe{sub 2}O{sub 4} nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Anandan, S., E-mail: sanand@nitt.edu [Nanomaterials and Solar Energy Conversion Lab, Department of Chemistry, National Institute of Technology, Trichy 620 015 (India); Department of Environmental Engineering and Science, Feng Chia University, Taichung 407, Taiwan (China); Selvamani, T.; Prasad, G. Guru [Nanomaterials and Solar Energy Conversion Lab, Department of Chemistry, National Institute of Technology, Trichy 620 015 (India); Asiri, A.M. [The Center of Excellence for Advanced Materials Research, King Abdulaziz University, P.O. Box 80203, Jeddah 21413 (Saudi Arabia); Wu, J.J., E-mail: jjwu@fcu.edu.tw [Department of Environmental Engineering and Science, Feng Chia University, Taichung 407, Taiwan (China)

    2017-06-15

    Highlights: • Copper ferrite (CuFe{sub 2}O{sub 4}) nanoparticles were synthesized via citrate-nitrate combustion method. • Spectroscopic information’s have found that CuFe{sub 2}O{sub 4} nanoparticles as an inverse spinel structure. • Magnetic study exhibits CuFe{sub 2}O{sub 4} nanoparticles have ferromagnetic behavior. • CuFe{sub 2}O{sub 4} nanoparticles employed for photocatalytic decolourisation of methylene blue under visible light irradiation. - Abstract: In this research, inverse spinel copper ferrite nanoparticles (CuFe{sub 2}O{sub 4} NPs) were synthesized via citrate-nitrate combustion method. The crystal structure, particle size, morphology and magnetic studies were investigated using various instrumental tools to illustrate the formation of the inverse spinel structure. Mossbauer spectrometry identified Fe is located both in the tetrahedral and octahedral site in the ratio (40:60) and the observed magnetic parameters values such as saturation magnetization (M{sub s} = 20.62 emu g{sup −1}), remnant magnetization (M{sub r} = 11.66 emu g{sup −1}) and coercivity (H{sub c} = 63.1 mTesla) revealed that the synthesized CuFe{sub 2}O{sub 4} NPs have a typical ferromagnetic behaviour. Also tested CuFe{sub 2}O{sub 4} nanoparticles as a photocatalyst for the decolourisation of methylene blue (MB) in the presence of peroxydisulphate as the oxidant.

  16. Folic acid-functionalized magnetic ZnFe2O4 hollow microsphere core/mesoporous silica shell composite particles: synthesis and application in drug release.

    Science.gov (United States)

    Yang, Dandan; Wei, Kaiwei; Liu, Qi; Yang, Yong; Guo, Xue; Rong, Hongren; Cheng, Mei-Ling; Wang, Guoxiu

    2013-07-01

    A drug delivery system was designed by deliberately combining the useful functions into one entity, which was composed of magnetic ZnFe2O4 hollow microsphere as the core, and mesoporous silica with folic acid molecules as the outer shell. Amine groups coated magnetic ZnFe2O4 hollow microsphere core/mesoporous silica shell (MZHM-MSS-NH2) composite particles were first synthesized by a one-pot direct co-condensation method. Subsequently a novel kind of folic acid-functionalized magnetic ZnFe2O4 hollow microsphere core/mesoporous silica shell (MZHM-MSS-NHFA) composite particles were synthesized by conjugating folic acid as targeted molecule to MZHM-MSS-NH2. Ibuprofen, a well-known antiphlogistic drug, was used as a model drug to assess the loading and releasing behavior of the composite microspheres. The results show that the MZHM-MSS-NHFA system has the higher capacity of drug storage and good sustained drug-release property. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. Synthesis, Characterization, and Sensor Applications of Spinel ZnCo2O4 Nanoparticles

    Directory of Open Access Journals (Sweden)

    Juan Pablo Morán-Lázaro

    2016-12-01

    Full Text Available Spinel ZnCo2O4 nanoparticles were synthesized by means of the microwave-assisted colloidal method. A solution containing ethanol, Co-nitrate, Zn-nitrate, and dodecylamine was stirred for 24 h and evaporated by a microwave oven. The resulting solid material was dried at 200 °C and subsequently calcined at 500 °C for 5 h. The samples were characterized by scanning electron microscopy (SEM, transmission electron microscopy (TEM, X-ray diffraction (XRD, and Raman spectroscopy, confirming the formation of spinel ZnCo2O4 nanoparticles with average sizes between 49 and 75 nm. It was found that the average particle size decreased when the dodecylamine concentration increased. Pellets containing ZnCo2O4 nanoparticles were fabricated and tested as sensors in carbon monoxide (CO and propane (C3H8 gases at different concentrations and temperatures. Sensor performance tests revealed an extremely high response to 300 ppm of CO at an operating temperature of 200 °C.

  18. Facial synthesis of carbon-coated ZnFe2O4/graphene and their enhanced lithium storage properties

    Science.gov (United States)

    Yao, Libing; Su, Qingmei; Xiao, Yanling; Huang, Min; Li, Haojie; Deng, Huihui; Du, Gaohui

    2017-07-01

    Carbon-coated ZnFe2O4 spheres with sizes of 110-180 nm anchored on graphene nanosheets (ZF@C/G) are successfully prepared and applied as anode materials for lithium ion batteries (LIBs). The obtained ZF@C/G presents an initial discharge capacity of 1235 mAh g-1 and maintains a reversible capacity of 775 mAh g-1 after 150 cycles at a current density of 500 mA g-1. After being tested at 2 A g-1 for 700 cycles, the capacity still retains 617 mAh g-1. The enhanced electrochemical performances can be attributed to the synergetic role of graphene and uniform carbon coating ( 3-6 nm), which can inhibit the volume expansion, prevent the pulverization/aggregation upon prolonged cycling, and facilitate the electron transfer between carbon-coated ZnFe2O4 spheres. The electrochemical results suggest that the synthesized ZF@C/G nanostructures are promising electrode materials for high-performance lithium ion batteries. [Figure not available: see fulltext.

  19. Single-crystalline MgAl2O4 spinel nanotubes using a reactive and removable MgO nanowire template

    International Nuclear Information System (INIS)

    Fan Hongjin; Knez, Mato; Scholz, Roland; Nielsch, Kornelius; Pippel, Eckhard; Hesse, Dietrich; Goesele, Ulrich; Zacharias, Margit

    2006-01-01

    Using MgO nanowires as a reactive template, we fabricated for the first time single-crystal MgAl 2 O 4 spinel nanotubes through an interfacial solid-state reaction of MgO-Al 2 O 3 core-shell nanowires. Single-crystal MgO nanowires are coated with a conformal thin layer of amorphous Al 2 O 3 via atomic layer deposition. Subsequent annealing at 700 deg. C activates the interfacial reaction between MgO and Al 2 O 3 , transforming the alumina shell into a spinel shell. Finally, after etching away the remaining MgO core in ammonia sulfuric solution, MgAl 2 O 4 spinel nanotubes are obtained. As a transition from conventional planar spinel layers via thin-film interface reactions, our result might open a window for the fabrication of a wide variety of MgO-based spinel one-dimensional nanostructures

  20. Znx-1CuxMn2O4 spinels; synthesis, structural characterization and electrical evaluation

    International Nuclear Information System (INIS)

    Mendez M, F.; Lima, E.; Bosch, P.; Pfeiffer, H.; Gonzalez, F.

    2010-01-01

    This work presents the structural characterization and electrical evaluation of Zn x-1 Cu x Mn 2 O 4 spinels, which are materials presented as secondary phases into the vari stor ceramic systems. Samples were analyzed by X-ray diffraction, solid-state nuclear magnetic resonance, infrared spectroscopy, scanning electron microscopy and impedance spectroscopy. Although, the addition of copper to the ZnMn 2 O 4 spinel did not produce morphological changes, the structure and electrical behaviors changed considerably. Structurally, copper addition induced the formation of partial inverse spinels, and its addition increases significantly the electrical conductivity. Therefore, the formation of Zn x-1 Cu x Mn 2 O 4 spinels, as secondary phases into the vari stor materials, may compromise significantly the vari stor efficiency. (Author)

  1. Effect of metal cation ratio on chemical properties of ZnFe2O4/AC composite and adsorption of organic contaminant

    Science.gov (United States)

    Meilia, Demara; Misbah Khunur, Mochamad; Setianingsih, Tutik

    2018-01-01

    Porous woody char is biochar prepared through pyrolisis. The biochar can be used as adsorbent. In this research, ZnFe2O4/AC composite was synthesized through imregnation of the woody biochar with ZnFe2O4 to study effect of mol ratio of Fe(III) and Zn(II) toward their physicochemistry and adsorption of drug wastewater. Paracetamol was used as adsorbate model. This research was conducted in several steps, including activation of the woody biochar using KOH activator at temperatur 500 °C for 15 min to produce the activated carbon, fungsionalization of the carbon using H2SO4 oxidator (6M) at temperature of 80 °C for 3 h, impregnation of the oxidized activated carbon with Zn-Fe-LDH (Layered Double Hydroxide) at various mol ratio of Fe(III) and Zn(III), including 1:2, 1:3 and 1:4 using NaOH solution (5M) for coprecipitation, and calcination of Zn-Fe-LDH/AC at 950 °C for 5 min to produce ZnFe2O4/AC. FTIR diffraction characterization indicated existence of M-O (M = Zn(II), Fe(III)) and OH functional groups. FTIR spectra showed increasing of bands connected to -OH by increasing of the ratio till the ratio was achieved at 1:4, then decreased again. The ratio mol showed effect on the adsorption of paracetamol. Profile of adsorption value was fit with changing of functional groups. The highest adsorption was achieved at the ratio of 1:4. After calcination it gave the adsorption value of 17,66 mg/g.

  2. Spinels as cathodes for the electrochemical reduction of O2 and NO

    DEFF Research Database (Denmark)

    Simonsen, Vibe Louise Ernlund; Find, D.; Lilliedal, M.

    2007-01-01

    the largest difference in activity between reduction of oxygen and the reduction of nitric oxide, the activity being highest for the reduction of nitric oxide. The material is probably not stable when polarised cathodically. However it seems that the electrode material can be regenerated upon oxidation. NiFe2......Spinels were synthesised and investigated as electro-catalyst for the electrochemical reduction of oxygen and nitric oxide using cyclic voltammetry and cone shaped electrodes. The following four spinels were investigated; CoFe2O4, NiFe2O4, CuFe2O4 and Co3O4. The composition CuFe2O4 revealed......O4 is also more active for the reduction of nitric oxide than for the reduction of oxygen, whereas the cobalt containing spinels have a higher activity for the reduction of oxygen than for the reduction of nitric oxide....

  3. MgAl2O4 spinel refractory as containment liner for high-temperature alkali salt containing environments

    Science.gov (United States)

    Peascoe-Meisner, Roberta A [Knoxville, TN; Keiser, James R [Oak Ridge, TN; Hemric, James G [Knoxville, TN; Hubbard, Camden R [Oak Ridge, TN; Gorog, J Peter [Kent, WA; Gupta, Amul [Jamestown, NY

    2008-10-21

    A method includes containing a high-temperature alkali salt containing environment using a refractory containment liner containing MgAl.sub.2O.sub.4 spinel. A method, includes forming a refractory brick containing MgAl.sub.2O.sub.4 spinel having an exterior chill zone defined by substantially columnar crystallization and an interior zone defined by substantially equiaxed crystallization; and removing at least a portion of the exterior chill zone from the refractory brick containing MgAl.sub.2O.sub.4 spinel by scalping the refractory brick containing MgAl.sub.2O.sub.4 spinel to define at least one outer surface having an area of substantially equiaxed crystallization. A product of manufacture includes a refractory brick containing MgAl.sub.2O.sub.4 spinel including an interior zone defined by substantially equiaxed crystallization; and at least one outer surface having an area of substantially equiaxed crystallization.

  4. Structural relaxation and colour in the spinel-magnesiochromite (MgAl2O4-MgCr2O4) and gahnite-zincochromite (ZnAl2O4-ZnCr2O4) solid solution series

    Science.gov (United States)

    Hålenius, U.; Andreozzi, G. B.; Skogby, H.

    2009-04-01

    Recent studies on binary mineral solid solution series utilising synchrotron based x-ray absorption spectroscopies have indicated strong structural relaxation. For instance, it has been suggested that the real Cr-O bond distances remain nearly constant (relaxation parameter (ɛ) of 0.85, where ɛ=1 equals full relaxation) over the entire compositional range of the MgAl2O4-MgCr2O4 series (Juhin et al. 2007). In the present study we have measured room temperature optical absorption spectra of synthetic single crystals of the ZnAl2-2xCr2xO4 (0.03?x?1) and MgAl2-2xCr2xO4(0.02?x?1) series with the aim to explore the real architecture of the structure and in particular the Cr-O distance as function of composition. Our crystals were synthesized by means of flux-growth methods under atmospheric pressure and temperature profiles resulting in an estimated cation ordering temperature of ca 850 °C. Crystals close to the spinel (sensu stricto) and gahnite end-member compositions were faintly red in colour. With increasing Cr-content the crystals become more intensely red-coloured and at the higher Cr-contents there is a distinct shift towards a dark greenish colouration. These colour changes are reflected in the measured optical spectra by the position and intensity of the two spin-allowed electronic d-d transitions in octahedrally coordinated Cr3+ at ca 18000 (4A2g -4T2g (4F) transition) and 25000 cm-1(4A2g -4T1g (4F) transition). The energy of the first transition (?1-band) is ca 1200 cm-1 lower in magnesiochromite than in weakly Cr-doped spinel (x=0.02) and ca 1400 cm-1 lower in zincochromite than in gahnite with the lowest Cr-content (x=0.03). Concomitantly the energy of the second transition (?2-band) decreases with increasing Cr-content in both series by ca. 1800 cm-1. From the position of the ?1-band, a decrease in crystal field splitting, 10Dq, for six-coordinated Cr3+ with increasing Cr-content in the MgAl2-2xCr2xO4 and ZnAl2-2xCr2xO4 series of 6.5 and 7

  5. Novel ternary composites: Preparation, performance and application of ZnFe2O4/TiO2/polyaniline

    Science.gov (United States)

    Li, Juanbi; Xiao, Qiushi; Li, Liangchao; Shen, Junhai; Hu, Diqiong

    2015-03-01

    A series of ZnFe2O4/TiO2/polyaniline ternary composites with excellent photocatalytic activity were successfully synthesized by chemical method. The phase composition, morphology, conductivity, electrical and magnetic performances of the as-samples were characterized by means of modern measurement technology. And the photocatalytic degradation activity tests for the samples were estimated using rhodamine B (RhB) and methyl orange (MO) as targeted pollutants. The results indicated that there existed some interactions between each component in the ternary composites, and the electrical conductivities and photocatalytic degradation activities of the ternary composites were improved due to the coating of polyaniline. Moreover, when the mass fraction of aniline was up to 50%, the ternary composite exhibited a great decontaminating (including photocatalytic degradation and adsorption) activity of on both MO and RhB and displayed an excellent reusability.

  6. Cr diffusion in MgAl2O4 synthetic spinels: preliminary results

    Science.gov (United States)

    Freda, C.; Celata, B.; Andreozzi, G.; Perinelli, C.; Misiti, V.

    2012-04-01

    Chromian spinel is an accessory phase common in crustal and mantle rocks, including peridotites, gabbros and basalts. Spinel, it has been identified as one of the most effective, sensible, and versatile petrogenetic indicator in mafic and ultramafic rock systems due to the strict interdependence between its physico-chemical properties (chemical composition, cation configuration etc.) and genetic conditions (temperature, pressure, and chemical characteristics of the system). In particular, studies on intra- and inter-crystalline Mg-Fe2+, Cr-Al exchange demonstrated the close relationship between spinel composition and both degree of partial melting and equilibrium temperature of spinel-peridotites. Moreover, studies focused on the chemical zoning of Mg-Fe2+ and/or Cr-Al components in spinel have been used, combined with a diffusion model, to provide quantitative information on peridotites and gabbros pressure-temperature paths and on deformation mechanisms. Although these potentials, most of the experimental studies have been performed on spinels hosting a limited content of divalent iron (sensu stricto, MgAl2O4), whereas the scarce studies on Cr-Al inter-diffusion coefficient have been performed at 3-7 GPa as pressure boundary condition. In order to contribute to the understanding of processes occurring in the lithospheric mantle, we have initiated an experimental research project aiming at determining the Cr-Al inter-diffusion in spinel at 2 GPa pressure and temperature ranging from 1100 to 1250 °C. The experiments were performed in a end-loaded piston cylinder by using a 19 mm assembly and graphite-Pt double capsules. As starting materials we used synthetic Mg-Al spinel (200-300 μm in size) and Cr2O3 powder. Microanalyses of experimental charge were performed on polished carbon-coated mounts by electronic microprobe. Line elemental analyses were made perpendicular to the contact surface between Cr2O3 powder and spinel, at interval of 2 μm. By processing these

  7. EPR, mu-Raman and Crystallographic properties of spinel type ZnCr{sub 2}O{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Vargas-Hernandez, C; Almanza, O; Jurado, J F, E-mail: cvargash@unal.edu.c [Universidad Nacional de Colombia, Manizales-Colombia Laboratorio de Propiedades Opticas de Materiales-POM (Colombia)

    2009-05-01

    Structural, vibrational and electron paramagnetic resonance (EPR) analysis for compound ZnCr{sub 2}O{sub 4} are shown in this work. These types of materials are used in technological applications as humidity sensors and piezoelectric devices. The compound was obtained by mean of solid state reaction technique from binary precursors ZnO and Cr{sub 2}O{sub 3}. After three thermal treatments the sample structure was monitoring using X ray diffraction (XRD), the spinel cubic phase has been indexed within O{sup 7}{sub h}(Fd3m) spatial group. It is observed normal spinel phase. Micro-Raman analysis revealed bands for normal vibration modes of Zn and Cr atoms in tetrahedral and octahedral environments formed by oxygen atoms at approximately 400 and 900 cm{sup -1}, respectively. Bands around 941 cm{sup -1} are associated possibly to vacancies in the tetrahedral and octahedral sites due to interaction between Zn and Cr ions. EPR signal from 150 to 300 K isothermals indicates a transition between inverse spinel to normal spinel type in a central field around 3350 G. A signal at approximately 3400 G corresponding to the C'r{sup +3} in tetrahedral sites is observed near the central field.

  8. Luminescence of Cr{sup 3+} ions in ZnAl{sub 2}O{sub 4} and MgAl{sub 2}O{sub 4} spinels: correlation between experimental spectroscopic studies and crystal field calculations

    Energy Technology Data Exchange (ETDEWEB)

    Brik, M.G., E-mail: mikhail.brik@ut.ee [College of Sciences, Chongqing University of Posts and Telecommunications, Chongqing 400065 (China); Institute of Physics, University of Tartu, W. Ostwald Str. 1, Tartu 50411 (Estonia); Institute of Physics, Jan Dlugosz University, Al. Armii Krajowej 13/15, Czestochowa PL-42200 (Poland); Papan, J.; Jovanović, D.J. [University of Belgrade, Vinča Institute of Nuclear Sciences, P.O. Box 522, Belgrade 11001 (Serbia); Dramićanin, M.D., E-mail: dramican@vinca.rs [University of Belgrade, Vinča Institute of Nuclear Sciences, P.O. Box 522, Belgrade 11001 (Serbia)

    2016-09-15

    Details of preparation, spectroscopic and structural studies along with crystal field calculations for two Cr{sup 3+} doped spinels MgAl{sub 2}O{sub 4} and ZnAl{sub 2}O{sub 4} are given in the present paper. Both compounds show efficient red emission at about 685 nm, which is due to the {sup 2}E{sub g} → {sup 4}A{sub 2g} spin-forbidden transition of Cr{sup 3+} ions located at the sites with D{sub 3d} local symmetry. Analysis of structure of the CrO{sub 6} clusters was performed; comparison of the crystal field effects in both compounds revealed that the low-symmetry splitting of the orbital triplet states is more pronounced in ZnAl{sub 2}O{sub 4}. Both compounds show potential for applications as red-emitting phosphors. - Highlights: • Cr{sup 3+}-doped MgAl{sub 2}O{sub 4} and ZnAl{sub 2}O{sub 4} spinels were synthesized. • Excitation/emission spectra were recorded and analyzed. • Symmetry properties of the Cr-sites were analyzed. • Cr{sup 3+} energy levels in trigonal crystal field were calculated. • Cr{sup 3+}-doped MgAl{sub 2}O{sub 4} and ZnAl{sub 2}O{sub 4} spinels can be used as red phosphors.

  9. Mechanistic insights into the interaction between energetic oxygen ions and nanosized ZnFe2O4: XAS-XMCD investigations.

    Science.gov (United States)

    Singh, Jitendra Pal; Kaur, Baljeet; Sharma, Aditya; Kim, So Hee; Gautam, Sanjeev; Srivastava, Ramesh Chandra; Goyal, Navdeep; Lim, Weol Cheol; Lin, H-J; Chen, J M; Asokan, K; Kanjilal, D; Won, Sung Ok; Lee, Ik-Jae; Chae, Keun Hwa

    2018-04-20

    The interactions of energetic ions with multi-cation compounds and their consequences in terms of changes in the local electronic structure, which may facilitate intriguing hybridization between O 2p and metal d orbitals and magnetic ordering, are the subject of debate and require a deep understanding of energy transfer processes and magnetic exchange mechanisms. In this study, nanocrystals of ZnFe2O4 were exposed to O7+ ions with an energy of 100 MeV to understand, qualitatively and quantitatively, the metal-ligand field interactions, cation migration and magnetic exchange interactions by employing X-ray absorption fine structure measurements and X-ray magnetic circular dichroism to get deeper mechanistic insights. Nanosized zinc ferrite nanoparticles (NPs) with a size of ∼16 nm synthesized in the cubic spinel phase exhibited deterioration of the crystalline phase when 100 MeV O7+ ions passed through them. However, the size of these NPs remained almost the same. The behaviour of crystal deterioration is associated with the confinement of heat in this interaction. The energy confined inside the nanoparticles promotes cation redistribution as well as the modification of the local electronic structure. Prior to this interaction, almost 42% of Zn2+ ions occupied AO4 tetrahedra; however, this value increased to 63% after the interaction. An inverse effect was observed for metal ion occupancies in BO6 octahedra. The L-edge spectra of Fe and Zn reveal that the spin and valence states of the metal ions were not affected by this interaction. This effect is also supported by K-edge measurements for Fe and Zn. The t2g/eg intensity ratio in the O K-edge spectra decreased after this interaction, which is associated with detachment of Zn2+ ions from the lattice. The extent of hybridization, as estimated from the ratio of the post-edge to the pre-edge region of the O K-edge spectra, decreased after this interaction. The metal-oxygen and metal-metal bond lengths were modified

  10. Enhanced nonlinear optical absorption and optical limiting properties of superparamagnetic spinel zinc ferrite decorated reduced graphene oxide nanostructures

    International Nuclear Information System (INIS)

    Saravanan, M.; Sabari Girisun, T.C.

    2017-01-01

    Highlights: • Nanospindle and nanosphere ZnFe_2O_4 were decorated upon GO by hydrothermal method. • All the samples show superparamagnetism with almost zero coercivity and remanence. • The observed nonlinearity arises due to effective two photon absorption process. • Tuning of NLO behavior with variation in amount of ZnFe_2O_4 upon GO were achieved. • ZnFe_2O_4-(15 wt%)GO show higher NLO coefficients and superior limiting actions. - Abstract: Nonlinear absorption and optical limiting properties of ZnFe_2O_4-rGO magnetic nanostructures was investigated by the Z-scan technique using Q-switched Nd:YAG laser (5 ns, 532 nm, 10 Hz) as an excitation source. Excited state absorption was the dominant process responsible for the observed nonlinearity in ZnFe_2O_4 decorated rGO which arises due to photo-generated charge carriers in the conduction band of zinc ferrite and increases in defects at the surface of rGO due to the incorporation of ZnFe_2O_4. The magnitude of the nonlinear absorption co-efficient was found to be in the order of 10"−"1"0 m/W. A noteworthy enhancement in the third-order NLO properties in ZnFe_2O_4-(15 wt%) rGO with those of individual counter parts and well known graphene composites was reported. Role of induced defects states (sp"3) arising from the functionalization of rGO in the enhancement of NLO response was explained through Raman studies. Earlier incorporation and distribution of ZnFe_2O_4 upon GO through one-step hydrothermal method was analyzed by XRD and FTIR. Formation of (nanospheres/nanospindles) ZnFe_2O_4 along with reduction of graphene oxide was confirmed through TEM analysis. VSM studies showed zinc ferrite decorated rGO posseses superparamagnetic behavior. The tuning of nonlinear optical and magnetic behavior with variation in the content of spinel ferrites upon reduced graphene oxide provides an easy way to attain tunable properties which are exceedingly required in both optoelectronics and photothermal therapy

  11. Comparative Study of Optical and Magneto-Optical Properties of Normal, Disordered and Inverse Spinel Type Oxides

    OpenAIRE

    Zviagin, Vitaly; Richter, Peter; Böntgen, Tammo; Lorenz, Michael; Ziese, Michael; Zahn, Dietrich R. T.; Salvan, Georgeta; Grundmann, Marius; Schmidt-Grund, Rüdiger

    2015-01-01

    Co$_3$O$_4$, ZnFe$_2$O$_4$, CoFe$_2$O$_4$, ZnCo$_2$O$_4$, and Fe$_3$O$_4$ thin films were fabricated by pulsed laser deposition at high and low temperatures resulting in crystalline single-phase normal, inverse, as well as disordered spinel oxide thin films with smooth surface morphology. The dielectric function, determined by spectroscopic ellipsometry in a wide spectral range from 0.5 eV to 8.5 eV, is compared with the magneto-optical response of the dielectric tensor, investigated by magne...

  12. Performance Investigation of Automobile Radiator Operated with ZnFe2O4 Nano Fluid based Coolant

    Directory of Open Access Journals (Sweden)

    Tripathi Ajay

    2015-01-01

    Full Text Available The cooling system of an Automobile plays an important role in its performance, consists of two main parts, known as radiator and fan. Improving thermal efficiency of engine leads to increase the engine's performance, decline the fuel consumption and decrease the pollution emissions. Water and ethylene glycol as conventional coolants have been widely used in radiators of an automotive industry for many years. These heat transfer fluids offer low thermal conductivity. With the advancement of nanotechnology, the new generation of heat transfer fluids called, “nanofluids” have been developed and researchers found that these fluids offer higher thermal conductivity compared to that of conventional coolants. This study focused on the preparation of Zinc based nanofluids (ZnFe2O4 using chemical co-precipitation method and its application in an automotive cooling system along with mixture of ethylene glycol and water (50:50. Relevant input data, nanofluids properties and empirical correlations were obtained from literatures to investigate the heat transfer enhancement of an automotive car radiator operated with nano fluid-based coolants. It was observed that, overall heat transfer coefficient and heat transfer rate in engine cooling system increased with the usage of nanofluids (with ethylene glycol the base-fluid compared to ethylene glycol (i.e. base-fluid alone. It is observed that, about 78% of heat transfer enhancement could be achieved with the addition of 1% ZnFe2O4 particles in a base fluid at the Reynolds number of 84.4x103 and 39.5x103 for air and coolant respectively

  13. Synthesis of visible light active Gd3+-substituted ZnFe2O4 nanoparticles for photocatalytic and antibacterial activities

    Science.gov (United States)

    Patil, S. B.; Bhojya Naik, H. S.; Nagaraju, G.; Viswanath, R.; Rashmi, S. K.

    2017-08-01

    In the present analysis, we study the assembly of a low-cost and visible light active ZnFe2-xGdxO4 ( x = 0 , 0.3, 0.5 and 0.7) nanoparticles (NPs) photocatalyst. The synthesized samples were characterized by several physicochemical techniques, such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), UV-Visible absorption spectroscopy (UV-Vis), scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM). The phase transition from cubic to orthorhombic was confirmed by XRD patterns. The increase in the concentration of Gd3+ substitution in ZnFe2O4 NPs enhances the redshift of absorption in the visible region of UV-Vis absorption spectra and reduces the band gap. In the photo-Fenton-type reaction, the gadolinium-substituted zinc ferrite (ZGF) NPs exhibit a significant catalytic activity for the degradation of methylene blue (99% in 90 minutes) under visible light (500W xenon lamp) with respect to bare samples (95% in 240 minutes) and they also show an excellent reusability nature. These materials were also screened for antibacterial activity against Gram-negative bacteria strains ( Pseudomonas aeruginosa and Escherichia coli).

  14. Photoelectrochemical enhancement of ZnO/BiVO4/ZnFe2O4/rare earth oxide hetero-nanostructures

    Science.gov (United States)

    She, Xuefeng; Zhang, Zhuo; Baek, Minki; Yong, Kijung

    2018-01-01

    Over the decades, researchers have made great efforts to turn the world into a cleaner place through efficient recycling of industrial waste and developing of green energy. Here we demonstrate a prototype heterostructure photoelectrochemical (PEC) cell fabricated using recycled industrial waste. ZnFe2O4 (ZFO) nanorod (NR) clusters were synthesized on the BiVO4@ZnO hetero-nanostructures using recycled rare earth oxide (REO) slags as Fe source. The NR-based PEC cell exhibited a significantly enhanced photon to hydrogen conversion efficiency over the entire UV and visible spectrum. Further study demonstrates that the photo-carrier separation and migration processes can be facilitated by the cascade band alignment of the heterostructure and the clustered nanostructure network. In addition, the life-time of the photo-carriers can be enhanced by the REO passivation layer, leading to a further increased PEC performance. Our results present a novel approach for high efficiency PEC cells, and offer great promises to the efficient recycling of industrial waste for clean renewable energy applications.

  15. Synthesis of high-surface-area spinel-type MgAl2O4 nanoparticles ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 40; Issue 1. Synthesis of high-surface-area spinel-type MgAl 2 O 4 nanoparticles by [Al(sal) 2 (H 2 O) 2 ] 2 [Mg(dipic) 2 ] and [Mg(H 2 O) 6 ][Al(ox) 2 (H 2 O) 2 ] 2 ·5H 2 O: influence of inorganic precursor type. Volume 40 Issue 1 February 2017 pp 45-53 ...

  16. Studying magnetic structure of Bi doped Co2MnO4 cubic spinel by neutron diffraction

    International Nuclear Information System (INIS)

    Rajeevan, N.E.; Kaushik, S.D.; Kumar, Ravi

    2016-01-01

    In present work, we studied effect of Bi doped spinel Bi x Co 2-x MnO 4 (x = 0, 0.05, 0.10, 0.15 and 0.20) samples on their crystal as well as magnetic structure by employing neutron diffraction of wavelength 1.48 A using focusing crystal diffractometer of UGC-DAECSR Mumbai Centre at Dhruva, Trombay, Mumbai, India. The analysis of the neutron diffraction using Fullprof program reveals that crystal structure due to Bi doping remains intact and all the samples have been formed in the cubic spinel structure with Fd3m (space group no. 227). The lattice parameter shows the positive thermal expansion upon Bi doping across the temperature range. In order to understand the implication on the spin structure and magnetism in the detail, temperature dependent neutron diffraction study is carried out on some of the samples (x = 0, 0.1) in the series. The ND pattern of x = 0.1 at 2.9K is shown. The experimental finding in terms of modified magnetic structure upon Bi doping are discussed which are understood in terms of variation in the ferroelectric properties, bond lengths and their effect on the CoO 6 polyhedra. Furthermore, Bi substitution in Co 2 MnO 4 spinel brings in the balance of structural distortion, which affects both ferrimagnetism and ferroelectricity

  17. Structural, optical and dielectric properties of transition metal (MFe2O4; M = Co, Ni and Zn) nanoferrites

    Science.gov (United States)

    Chand, Prakash; Vaish, Swapnil; Kumar, Praveen

    2017-11-01

    In the present work, transition metal spinel ferrite (MFe2O4; M = Co, Ni, Zn) nanostructures synthesized by chemical co-precipitation method. XRD analysis confirms the formation of cubic spinel-type structure with space group Fd3m and the average crystallite size calculated by Scherrer's formula found to be in 9-14 nm range. Scanning electron microscopy was used to study surface morphology of the samples. Moreover, Raman and PL spectra also confirm the formation of the cubic structure. The Raman spectra measured on cobalt, nickel and zinc ferrite revealed a larger number of phonon bands than expected for the cubic spinel structure. The calculated optical energy band gaps, obtained by Tauc's relation from UV-Vis absorption spectra are found to be as 2.44, 3.54 and 3.25 eV for CoFe2O4, NiFe2O4&ZnFe2O, respectively. The analysis of the complex impedance spectra of all ferrites samples shows the presence of one semicircular arc at all selected temperatures, signifying a key role of the grain boundary contribution. The dielectric constants (ε ‧) were measured in the frequency range from 10 Hz to 5 MHz at different temperatures and is found to be decreased suddenly with an increase in frequency and maintain a steady state or constant at higher frequencies for all the three samples. The AC conductivity is found to be increased with frequency and temperature of all the three samples which is explained on the basis of Koop's phenomenological theory.

  18. Effect of cutting edge radius on surface roughness in diamond tool turning of transparent MgAl2O4 spinel ceramic

    Science.gov (United States)

    Yue, Xiaobin; Xu, Min; Du, Wenhao; Chu, Chong

    2017-09-01

    Transparent magnesium aluminate spinel (MgAl2O4) ceramic is one of an important optical materials. However, due to its pronounced hardness and brittleness, the optical machining of this material is very difficult. Diamond turning has advantages over the grinding process in flexibility and material removal rate. However, there is a lack of research that could support the use of diamond turning technology in the machining of MgAl2O4 spinel ceramic. Using brittle-ductile transition theory of brittle material machining, this work provides critical information that may help to realize ductile-regime turning of MgAl2O4 spinel ceramic. A characterization method of determination the cutting edge radius is introduced here. Suitable diamond tools were measured for sharpness and then chosen from a large number of candidate tools. The influence of rounded cutting edges on surface roughness of the MgAl2O4 spinel ceramic is also investigated. These results indicate that surface quality of MgAl2O4 spinel is relate to the radius of diamond tool's cutting edge, cutting speed, and feed rate. Sharp diamond tools (small radius of cutting edge) facilitated ductile-regime turning of MgAl2O4 spinel and shows great potential to reduce surface roughness and produce smoother final surface.

  19. Structural, electronic and magnetic properties of partially inverse spinel CoFe2O4: a first-principles study

    International Nuclear Information System (INIS)

    Hou, Y H; Liu, Z W; Yu, H Y; Zhong, X C; Qiu, W Q; Zeng, D C; Wen, L S; Zhao, Y J

    2010-01-01

    Partially inverse spinel CoFe 2 O 4 , which may be prepared through various heat treatments, differs remarkably from the ideal inverse spinel in many properties. The structure of partially inverse spinel CoFe 2 O 4 as well as its electronic and magnetic properties through a systemic theoretical calculation of (Co 1-x Fe x ) Tet (Co x Fe 2-x ) Oct O 4 (x = 0, 0.25, 0.5, 0.75 and 1.0) have been investigated by the generalized gradient approximation (GGA) + U approach. It is found that the Co and Fe ions prefer their high spin configurations with higher spin moments at octahedral sites in all the studied cases, in line with experimental observations. The Co ions at the octahedral sites favour being far away from each other in the partial inverse spinels, which also show half metallicity at certain inversion degrees.

  20. Direct observation of cation distributions of ideal inverse spinel CoFe2O4 nanofibres and correlated magnetic properties

    KAUST Repository

    Zeng, Xue

    2017-04-25

    Low-dimensional spinel ferrites have recently attracted increasing attention because their tunable magnetic properties make them attractive candidates as spin-filtering tunnel barriers in spintronic devices and as magnetic components in artificial multiferroic heterostructures. Although we know that the distribution of cations (Fe3+ and Co2+) in a spinel structure governs its magnetic properties, their distribution in the so-called ideal inverse spinel structure of a ferrite, CoFe2O4, has not yet been imaged with sub-ångstrom resolution. In this work, we fill this gap in evidence by reporting a direct observation of the distribution of cations in an ideal inverse spinel structure of CoFe2O4 nanofibres using aberration-corrected transmission electron microscopy (TEM). The ordering of Co2+ and Fe3+ at the octahedral sites imaged along either [001], [011] or [-112] orientation was identified as 1 : 1, in accordance with the ideal inverse spinel structure. The saturation magnetisation calculated based on the crystal structure as determined from the TEM image is in good agreement with that measured experimentally on the spinel CoFe2O4 nanofibres, further confirming results from TEM.

  1. High-pressure phase of the cubic spinel NiMn2O4

    DEFF Research Database (Denmark)

    Åsbrink, S.; Waskowska, A.; Olsen, J. Staun

    1998-01-01

    experimental uncertainty, there is no volume change at the transition. The cia ratio of the tetragonal spinel is almost independent of pressure and equal to 0.91. The phase transition is attributed to the Jahn-Teller-type distortion and the ionic configurationcan be assumed as (Mn3+)(tetr)[Ni2+Mn3+](oct......It has been observed that the fee spinel NiMn2O4 transforms to a tetragonal structure at about 12 GPa. The tetragonal phase does not revert to the cubic phase upon decompression and its unit-cell constants at ambient pressure are a(0)=8.65(8) and c(0)=7.88(15) Angstrom (distorted fee). Within thr......). The bulk modulus of the cubic phase is 206(4) GPa....

  2. Molecular dynamics simulations of spinels: LiMn2O4 and Li4Mn5O12 at high temperatures

    International Nuclear Information System (INIS)

    Ledwaba, R S; Matshaba, M G; Ngoepe, P E

    2015-01-01

    Energy storage technologies are critical in addressing the global challenge of clean sustainable energy. Spinel lithium manganates have attracted attention due to their electrochemical properties and also as promising cathode materials for lithium-ion batteries. The current study focused on the effects of high temperatures on the materials, in order to understand the sustainability in cases where the battery heats up to high temperature and analysis of lithium diffusion aids in terms of intercalation host compatibility. It is also essential to understand the high temperature behaviour and lithium ion host capability of these materials in order to perform the armorphization and recrystalization of spinel nano-architectures. Molecular dynamics simulations carried out to predict high temperature behaviour of the spinel systems. The NVE ensemble was employed, in the range 300 - 3000K. The melting temperature, lithium-ion diffusion and structural behaviour were monitored in both supercell systems. LiMn 2 O 4 indicated a diffusion rate that increased rapidly above 1500K, just before melting (∼1700K) and reached its maximum diffusion at 2.756 × 10 -7 cm 2 s -1 before it decreased. Li 4 Mn 5 O 12 indicated an exponential increase above 700K reaching 8.303 × 10 −7 cm 2 s −1 at 2000K and allowing lithium intercalation even above its melting point of around 1300K. This indicated better structural stability of Li 4 Mn 5 O 12 and capability to host lithium ions at very high temperatures (up to 3000 K) compared to LiMn 2 O 4 . (paper)

  3. Structural, dielectric and gas sensing behavior of Mn substituted spinel MFe2O4 (M=Zn, Cu, Ni, and Co) ferrite nanoparticles

    Science.gov (United States)

    Ranjith Kumar, E.; Siva Prasada Reddy, P.; Sarala Devi, G.; Sathiyaraj, S.

    2016-01-01

    Spinel ferrite (MnZnFe2O4, MnCuFe2O4, MnNiFe2O4 and MnCoFe2O4) nanoparticles have been prepared by evaporation method. The annealing temperature plays an important role on changing particle size of the spinel ferrite nanoparticles was found out by X-ray diffraction and transmission electron microscopy. The role of manganese substitution in the spinel ferrite nanoparticles were also analyzed for different annealing temperature. The substitution of Mn also creates a vital change in dielectric properties have been measured in the frequency range of 100 kHz to 5 MHz. These spinel ferrites are decomposed to α-Fe2O3 after annealing above 550 °C in air. Through the characterization of the prepared powder, the effect of annealing temperature, chemical composition and preparation technique on the microstructure, particle size and dielectric properties of the Mn substituted spinel ferrite nanoparticles are discussed. Furthermore, Conductance response of Mn substituted MFe2O4 ferrite nanoparticles were measured by exposing the materials to reducing gas like liquefied petroleum gas (LPG).

  4. Characterization of Li4Ti5O12 and LiMn2O4 spinel materials treated with aqueous acidic solutions

    NARCIS (Netherlands)

    Simon, D.R.

    2007-01-01

    In this thesis an investigation of two spinel materials, Li4Ti5O12 and LiMn2O4 used for Li-ion battery applications is performed interms of formation and reactivity towards acidic solutions. Subsequent characterizations such as structural, magnetic, chemical, and electrochemical characterizations

  5. In-situ synchrotron PXRD study of spinel LiMn2O4 nanocrystal formation

    DEFF Research Database (Denmark)

    Birgisson, Steinar; Jensen, Kirsten Marie Ørnsbjerg; Christiansen, Troels Lindahl

    Many solvothermal reactions have a great potential for environmentally friendly and easily scalable way for producing nanocrystalline materials on an industrial scale. Here we study hydrothermal formation of spinel LiMn2O4 which is a well-known cathode material for Li-ion batteries. The LiMn2O4...... nanoparticles are formed by reducing KMnO4 in an aqueous solution containing Li-ions. The reducing agent is an alcohol (here ethanol) and the reaction takes place under high pressure and temperature. The LiMn2O4 nanocrystals are unstable towards further reduction to Mn3O4 nanocrystals. Possible reaction route...

  6. Zn{sub x-1}Cu{sub x}Mn{sub 2}O{sub 4} spinels; synthesis, structural characterization and electrical evaluation

    Energy Technology Data Exchange (ETDEWEB)

    Mendez M, F.; Lima, E.; Bosch, P.; Pfeiffer, H. [UNAM, Instituto de Investigaciones en Materiales, Circuito Exterior, Ciudad Universitaria, 04510 Mexico D. F. (Mexico); Gonzalez, F., E-mail: pfeiffer@iim.unam.m [Universidad Autonoma Metropolitana, Unidad Iztapalapa, Av. San Rafael Atlixco No. 186, Col. Vicentina, 09340 Mexico D. F. (Mexico)

    2010-07-01

    This work presents the structural characterization and electrical evaluation of Zn{sub x-1}Cu{sub x}Mn{sub 2}O{sub 4} spinels, which are materials presented as secondary phases into the vari stor ceramic systems. Samples were analyzed by X-ray diffraction, solid-state nuclear magnetic resonance, infrared spectroscopy, scanning electron microscopy and impedance spectroscopy. Although, the addition of copper to the ZnMn{sub 2}O{sub 4} spinel did not produce morphological changes, the structure and electrical behaviors changed considerably. Structurally, copper addition induced the formation of partial inverse spinels, and its addition increases significantly the electrical conductivity. Therefore, the formation of Zn{sub x-1}Cu{sub x}Mn{sub 2}O{sub 4} spinels, as secondary phases into the vari stor materials, may compromise significantly the vari stor efficiency. (Author)

  7. Spinel LiMn 2 O 4 Nanorods as Lithium Ion Battery Cathodes

    KAUST Repository

    Kim, Do Kyung

    2008-11-12

    Spinel LiMn 2O 4 is a low-cost, environmentally friendly, and highly abundant material for Li-ion battery cathodes. Here, we report the hydrothermal synthesis of single-crystalline β-MnO 2 nanorods and their chemical conversion into free-standing single-crystalline LiMn 2O 4 nanorods using a simple solid-state reaction. The LiMn 2O 4 nanorods have an average diameter of 130 nm and length of 1.2 μm. Galvanostatic battery testing showed that LiMn 2O 4 nanorods have a high charge storage capacity at high power rates compared with commercially available powders. More than 85% of the initial charge storage capacity was maintained for over 100 cycles. The structural transformation studies showed that the Li ions intercalated into the cubic phase of the LiMn 2O 4 with a small change of lattice parameter, followed by the coexistence of two nearly identical cubic phases in the potential range of 3.5 to 4.3V. © 2008 American Chemical Society.

  8. Spinel LiMn 2 O 4 Nanorods as Lithium Ion Battery Cathodes

    KAUST Repository

    Kim, Do Kyung; Muralidharan, P.; Lee, Hyun-Wook; Ruffo, Riccardo; Yang, Yuan; Chan, Candace K.; Peng, Hailin; Huggins, Robert A.; Cui, Yi

    2008-01-01

    Spinel LiMn 2O 4 is a low-cost, environmentally friendly, and highly abundant material for Li-ion battery cathodes. Here, we report the hydrothermal synthesis of single-crystalline β-MnO 2 nanorods and their chemical conversion into free-standing single-crystalline LiMn 2O 4 nanorods using a simple solid-state reaction. The LiMn 2O 4 nanorods have an average diameter of 130 nm and length of 1.2 μm. Galvanostatic battery testing showed that LiMn 2O 4 nanorods have a high charge storage capacity at high power rates compared with commercially available powders. More than 85% of the initial charge storage capacity was maintained for over 100 cycles. The structural transformation studies showed that the Li ions intercalated into the cubic phase of the LiMn 2O 4 with a small change of lattice parameter, followed by the coexistence of two nearly identical cubic phases in the potential range of 3.5 to 4.3V. © 2008 American Chemical Society.

  9. Synthesis of high surface area spinel-type MgAl2O4 nanoparticles by

    Indian Academy of Sciences (India)

    68

    Spinel-type magnesium aluminate, MgAl2O4, is an effective refractory ceramic for ... such as good mechanical strength at high temperatures, high resistance to ... Materials. The starting chemicals with laboratory grade purity were provided ...

  10. Anomalous magnetoresistance in the spinel superconductor LiTi2O4.

    Science.gov (United States)

    Jin, K; He, G; Zhang, X; Maruyama, S; Yasui, S; Suchoski, R; Shin, J; Jiang, Y; Yu, H S; Yuan, J; Shan, L; Kusmartsev, F V; Greene, R L; Takeuchi, I

    2015-05-20

    LiTi2O4 is a unique compound in that it is the only known spinel oxide superconductor. The lack of high quality single crystals has thus far prevented systematic investigations of its transport properties. Here we report a careful study of transport and tunnelling spectroscopy in epitaxial LiTi2O4 thin films. An unusual magnetoresistance is observed which changes from nearly isotropic negative to prominently anisotropic positive as the temperature is decreased. We present evidence that shows that the negative magnetoresistance likely stems from the suppression of local spin fluctuations or spin-orbit scattering centres. The positive magnetoresistance suggests the presence of an orbital-related state, also supported by the fact that the superconducting energy gap decreases as a quadratic function of magnetic field. These observations indicate that the spin-orbital fluctuations play an important role in LiTi2O4 in a manner similar to high-temperature superconductors.

  11. Expansion during the formation of the magnesium aluminate spinel (MgAl(2)O(4)) from its basic oxide (MgO and Al(2)O(3)) powders

    Science.gov (United States)

    Duncan, Flavia Cunha

    The extraordinary expansion during the reaction sintering of the magnesium aluminate spinel (MgAl2O4) from its basic oxide (MgO and Al2O3) powders was studied. Experimental series of different size fractions of the reacting materials were formulated to produce the Mg-Al spinel. After batches were prepared, specimens were compacted and fired in air from 1200° to 1700°C for a fixed firing time. A separate set of specimens was fired as a function of time to determine the reaction kinetic parameters. Dimensional changes confirmed that extraordinary expansions of three to four times greater than the prediction from the reaction of solids occur. The solid-state reactions were monitored by X-ray diffraction. The activation energy of the spinel reaction formation was determined to be 280 +/- 20 kJ/mol. It is believed to be associated with the diffusivity of Mg 2+ in either magnesia or spinel during the development of the final spinel structure. New porosity developed in the compacts during the reaction formation of spinel. Scanning electron microscopy confirmed that the magnesia evaporated leaving behind porous magnesia grains, condensed on the alumina particles and reacted to form a shell of spinel. Hollow spinel particles resulted from the original particles of alumina. These porosities generated within the reacting materials influenced the expansions. Final volumetric expansion could potentially reach 56% as a result of the reaction of solids and the porosity generation within MgO and Al2O3. Models of a single alumina particle with and without development of internal porosity were developed. 3-D arrangements of particles showed additional porosity, influencing on the expansions. The decrease in porosity of some specimens fired at higher temperatures indicated that sintering and densification occur simultaneously with the reaction formation of spinel. The decrease in the interparticle porosity limits the full expansion of the particulates to levels lower than the

  12. IN-SITU SYNCHROTRON PXRD STUDY OF SPINEL TYPE LiMn2O4 NANOCRYSTAL FORMATION

    DEFF Research Database (Denmark)

    Birgisson, Steinar; Jensen, Kirsten Marie Ørnsbjerg; Christiansen, Troels Lindahl

    Many solvothermal reactions have a great potential for environmentally friendly and easily scalable way for producing nanocrystalline materials on an industrial scale. Here we study hydrothermal formation of spinel LiMn2O4 which is a well-known cathode material for Li-ion batteries. The LiMn2O4...... nanoparticles are formed by reducing KMnO4 in an aqueous solution containing Li-ions. The reducing agent is an alcohol (here ethanol) and the reaction takes place under high pressure and temperature. The LiMn2O4 nanocrystals are unstable towards further reduction to Mn3O4 nanocrystals. Proposed reaction route...

  13. Radiation-induced electrical conductivity in MgAl2O4 spinel

    International Nuclear Information System (INIS)

    Pells, G.P.

    1990-12-01

    The d.c. electrical conductivity of high purity, polycrystalline MgAl 2 O 4 spinel of 99.5% theoretical density has been measured during irradiation by 18 MeV protons at reactor relevant ionization dose rates. The radiation-induced conductivity (RIC) at 200 C varied in a slightly sub-linear manner with dose rate. At temperatures between 250-350 C the RIC varied in a complex manner with the dose rate dependence being itself dose rate dependent. At higher temperatures the RIC reverted to an essentially linear variation with dose rate. The complex dose rate dependence is ascribed to the magnesium vacancy concentration introduced by the small Al 2 O 3 excess (MgO:Al 2 O = 1:1.05) and the presence of anti-structure defects producing large concentrations of intrinsic electron and hole traps. There was no evidence that the accumulation of radiation damage influenced the details of radiation-induced conductivity and MgAl 2 O 4 retained reasonable insulating properties at the highest dose rate and temperature. (author)

  14. Direct observation of cation distributions of ideal inverse spinel CoFe2O4 nanofibres and correlated magnetic properties

    KAUST Repository

    Zeng, Xue; Zhang, Junwei; Zhu, Shimeng; Deng, Xia; Ma, Hongbin; Zhang, Junli; Zhang, Qiang; Li, Peng; Xue, Desheng; Mellors, Nigel J; Zhang, Xixiang; Peng, Yong

    2017-01-01

    multiferroic heterostructures. Although we know that the distribution of cations (Fe3+ and Co2+) in a spinel structure governs its magnetic properties, their distribution in the so-called ideal inverse spinel structure of a ferrite, CoFe2O4, has not yet been

  15. Effect of MgCl2 addition on the sintering behavior of MgAl2O4 spinel and formation of nano-particles

    Directory of Open Access Journals (Sweden)

    Mohammadi F.

    2014-01-01

    Full Text Available In this paper, the effect of MgCl2 addition on the sintering behavior of MgAl2O4 spinel produced via oxide mixture method was investigated. For this reason, the stoichiometric mixture of magnesite and calcined alumina as raw materials was calcined at 1100°C. The calcined mixture was milled, pressed and then, fired at 1300 and 1500°C after addition of various amounts of MgCl2. Besides, the physical properties, phase composition and microstructure of fired samples were investigated. The results showed that MgCl2 addition has great effect on the densification and particle size of spinel. Besides, MgCl2 addition increases the amount of spinel phase at all firing temperatures. Due to the decomposition of MgCl2 and then formation of ultra-fine MgO particles, the nano-sized spinel is formed on the surface of the larger spinel particles.

  16. Enhancement of Electrochemical Performance of LiMn2O4 Spinel Cathode Material by Synergetic Substitution with Ni and S

    Directory of Open Access Journals (Sweden)

    Monika Bakierska

    2016-05-01

    Full Text Available Nickel and sulfur doped lithium manganese spinels with a nominal composition of LiMn2−xNixO4–ySy (0.1 ≤ x ≤ 0.5 and y = 0.01 were synthesized by a xerogel-type sol-gel method followed by subsequent calcinations at 300 and 650 °C in air. The samples were investigated in terms of physicochemical properties using X-ray powder diffraction (XRD, transmission electron microscopy (EDS-TEM, N2 adsorption-desorption measurements (N2-BET, differential scanning calorimetry (DSC, and electrical conductivity studies (EC. Electrochemical characteristics of Li/Li+/LiMn2−xNixO4–ySy cells were examined by galvanostatic charge/discharge tests (CELL TEST, electrochemical impedance spectroscopy (EIS, and cyclic voltammetry (CV. The XRD showed that for samples calcined at 650 °C containing 0.1 and 0.2 mole of Ni single phase materials of Fd-3m group symmetry and nanoparticles size of around 50 nm were obtained. The energy dispersive X-ray spectroscopy (EDS mapping confirmed homogenous distribution of nickel and sulfur in the obtained spinel materials. Moreover, it was revealed that the adverse phase transition at around room temperature typical for the stoichiometric spinel was successfully suppressed by Ni and S substitution. Electrochemical results indicated that slight substitution of nickel (x = 0.1 and sulfur (y = 0.01 in the LiMn2O4 enhances the electrochemical performance along with the rate capability and capacity retention.

  17. Lithium-deficient Li YMn2O4 spinels (0.9 ≤ Y < 1): Lithium content, synthesis temperature, thermal behaviour and electrochemical properties

    International Nuclear Information System (INIS)

    Pascual, Laura; Perez-Revenga, M. Luz; Rojas, Rosa M.; Rojo, Jose M.; Amarilla, J. Manuel

    2006-01-01

    Lithium-deficient Li Y Mn 2 O 4 spinels (LD-Li Y Mn 2 O 4 ) with nominal composition (0.9 ≤ Y 2 O 3 and LiNO 3 at temperatures ranging from 700 deg. C to 850 deg. C. X-ray diffraction data show that LD-Li Y Mn 2 O 4 spinels are obtained as single phases in the range Y = 0.975-1 at 700 deg. C and 750 deg. C. Morphological characterization by transmission electron microscopy shows that the particle size of LD-Li Y Mn 2 O 4 spinels increases on decreasing the Li-content. The influence of the Li-content and the synthesis temperature on the thermal and electrochemical behaviours has been systematically studied. Thermal analysis studies indicate that the temperature of the first thermal effect in the differential thermal analysis (DTA)/thermogravimetric (TG) curves, T C1 , linearly increases on decreasing the Li-content. The electrochemical properties of LD-Li Y Mn 2 O 4 spinels, determined by galvanostatic cycling, notably change with the synthesis conditions. So, the first discharge capacity, Q disch. , at C rate increases on rising the Li-content and the synthesis temperature. The sample Li 0.975 Mn 2 O 4 synthesized at 700 deg. C has a Q disch. = 123 mAh g -1 and a capacity retention of 99.77% per cycle. This LD-Li Y Mn 2 O 4 sample had the best electrochemical characteristics of the series

  18. Ferrites nanoparticles MFe2O4 (M = Ni and Zn: hydrothermal synthesis and magnetic properties

    Directory of Open Access Journals (Sweden)

    Pérez Mazariego, J. L.

    2008-06-01

    Full Text Available MFe2O4 (M = Ni and Zn nanoparticles were prepared by the hydrothermal method. The obtained samples were characterized by X-ray and electron diffraction, Scanning and Transmission Electron Microscopy and Mössbauer spectroscopy. The transmission images show homogeneous shape and particle size ranging from 10 to 40 nm, depending on the nature of the M cation. Mössbauer spectroscopy yields to a ratio of occupancy between the A and B sites of 0.7 in the case of NiFe2O4 oxide. DC magnetization (2-300 K measurements reveal a superparamagnetic behaviour for the ZnFe2O4 sample with a blocking temperature of 20 K. By contrast, in the case of the NiFe2O4 ferrite the blocking temperature appears to be above 300 K and at lower temperature, it shows a ferrimagnetic behaviour arising from the superexchange interactions that take place in this inverse spinel. Mössbauer spectroscopy results confirm the bulk magnetic measurements.Se han preparado mediante el método hidrotermal nanopartículas de ferritas MFe2O4 (M = Ni, Zn. Las muestras obtenidas fueron caracterizadas mediante difracción de rayos X y electrones, microscopía electrónica de transmisión y barrido y espectroscopia Mössbauer. Las imágenes de transmisión muestran partículas de forma y tamaño homogéneo de 10 a 40 nm según la naturaleza del catión M. La espectroscopia Mössbauer revela una relación de ocupación entre los sitios A y B por los átomos de hierro de 0.7 en el caso del óxido NiFe2O4. Las medidas de magnetización DC (2 – 300 K muestran un comportamiento superparamagnético para la muestra ZnFe2O4 con una temperatura de bloqueo de 20 K. En el caso de las nanopartículas de NiFe2O4 la temperatura de bloqueo parece estar por encima de los 300 K mostrando por debajo de la misma, comportamiento ferrimagnético provocado por las interacciones de superintercambio que tienen lugar en esta espinela inversa. Los resultados de espectroscopia Mössbauer confirman los datos de las

  19. Heterostructured ZnFe2O4/Fe2TiO5/TiO2 Composite Nanotube Arrays with an Improved Photocatalysis Degradation Efficiency Under Simulated Sunlight Irradiation

    Science.gov (United States)

    Xiong, Kun; Wang, Kunzhou; Chen, Lin; Wang, Xinqing; Fan, Qingbo; Courtois, Jérémie; Liu, Yuliang; Tuo, Xianguo; Yan, Minhao

    2018-03-01

    To improve the visible light absorption and photocatalytic activity of titanium dioxide nanotube arrays (TONTAs), ZnFe2O4 (ZFO) nanocrystals were perfused into pristine TONTA pipelines using a novel bias voltage-assisted perfusion method. ZFO nanocrystals were well anchored on the inner walls of the pristine TONTAs when the ZFO suspensions (0.025 mg mL-1) were kept under a 60 V bias voltage for 1 h. After annealing at 750 °C for 2 h, the heterostructured ZFO/Fe2TiO5 (FTO)/TiO2 composite nanotube arrays were successfully obtained. Furthermore, Fe3+ was reduced to Fe2+ when solid solution reactions occurred at the interface of ZFO and the pristine TONTAs. Introducing ZFO significantly enhanced the visible light absorption of the ZFO/FTO/TONTAs relative to that of the annealed TONTAs. The coexistence of type I and staggered type II band alignment in the ZFO/FTO/TONTAs facilitated the separation of photogenerated electrons and holes, thereby improving the efficiency of the ZFO/FTO/TONTAs for photocatalytic degradation of methylene blue when irradiated with simulated sunlight. [Figure not available: see fulltext.

  20. Green Template-Free Synthesis of Hierarchical Shuttle-Shaped Mesoporous ZnFe2 O4 Microrods with Enhanced Lithium Storage for Advanced Li-Ion Batteries.

    Science.gov (United States)

    Hou, Linrui; Hua, Hui; Lian, Lin; Cao, Hui; Zhu, Siqi; Yuan, Changzhou

    2015-09-07

    Invited for the cover of this issue is Changzhou Yuan and co-workers at the Anhui University of Technology. The image depicts hierarchical shuttle-shaped mesoporous ZnFe2 O4 micro-rods, as a low-cost yet high-performance anode, for advanced next-generation Li-ion batteries. Read the full text of the article at 10.1002/chem.201501876. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Structural, dielectric and gas sensing behavior of Mn substituted spinel MFe{sub 2}O{sub 4} (M=Zn, Cu, Ni, and Co) ferrite nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Ranjith Kumar, E., E-mail: ranjueaswar@gmail.com [Department of Physics, Dr. NGP Institute of Technology, Coimbatore 641048, Tamil Nadu (India); Siva Prasada Reddy, P.; Sarala Devi, G. [Inorganic and Physical Chemistry Division, Indian Institute Chemical Technology, Hyderabad 500607 (India); Sathiyaraj, S. [Department of Chemistry, Dr. NGP Institute of Technology, Coimbatore 641048, Tamil Nadu (India)

    2016-01-15

    Spinel ferrite (MnZnFe{sub 2}O{sub 4}, MnCuFe{sub 2}O{sub 4}, MnNiFe{sub 2}O{sub 4} and MnCoFe{sub 2}O{sub 4}) nanoparticles have been prepared by evaporation method. The annealing temperature plays an important role on changing particle size of the spinel ferrite nanoparticles was found out by X-ray diffraction and transmission electron microscopy. The role of manganese substitution in the spinel ferrite nanoparticles were also analyzed for different annealing temperature. The substitution of Mn also creates a vital change in dielectric properties have been measured in the frequency range of 100 kHz to 5 MHz. These spinel ferrites are decomposed to α-Fe{sub 2}O{sub 3} after annealing above 550 °C in air. Through the characterization of the prepared powder, the effect of annealing temperature, chemical composition and preparation technique on the microstructure, particle size and dielectric properties of the Mn substituted spinel ferrite nanoparticles are discussed. Furthermore, Conductance response of Mn substituted MFe{sub 2}O{sub 4} ferrite nanoparticles were measured by exposing the materials to reducing gas like liquefied petroleum gas (LPG). - Highlights: • The egg white support to achieve sample with shorter reaction time. • Manganese plays a significant role in sensor response. • Nature of the ferrites was affected with increasing annealing temperature.

  2. Study of Mn dissolution from LiMn{sub 2}O{sub 4} spinel electrodes using rotating ring-disk collection experiments

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Li-Fang; Ou, Chin-Ching; Striebel, Kathryn A.; Chen, Jenn-Shing

    2003-07-01

    The goal of this research was to measure Mn dissolution from a thin porous spinel LiMn{sub 2}O{sub 4} electrode by rotating ring-disk collection experiments. The amount of Mn dissolution from the spinel LiMn{sub 2}O{sub 4} electrode under various conditions was detected by potential step chronoamperometry. The concentration of dissolved Mn was found to increase with increasing cycle numbers and elevated temperature. The dissolved Mn was not dependent on disk rotation speed, which indicated that the Mn dissolution from the disk was under reaction control. The in situ monitoring of Mn dissolution from the spinel was carried out under various conditions. The ring currents exhibited maxima corresponding to the end-of-charge (EOC) and end-of-discharge (EOD), with the largest peak at EOC. The results suggest that the dissolution of Mn from spinel LiMn{sub 2}O{sub 4} occurs during charge/discharge cycling, especially in a charged state (at >4.1 V) and in a discharged state (at <3.1 V). The largest peak at EOC demonstrated that Mn dissolution took place mainly at the top of charge. At elevated temperatures, the ring cathodic currents were larger due to the increase of Mn dissolution rate.

  3. Synthesis and characterization of mesoporous spinel NiCo2O4 using surfactant-assembled dispersion for asymmetric supercapacitors

    Science.gov (United States)

    Hsu, Chun-Tsung; Hu, Chi-Chang

    2013-11-01

    A simple and scalable process has been developed for synthesizing spinel NiCo2O4 nanocrystals through a thermal decomposition method. The introduction of hexadecyltrimethylammonium bromide (CTAB, (C16H33)N(CH3)3Br) into precursor solutions significantly enhances the homogeneity and porosity of spinel NiCo2O4. The porosity and high specific surface area of NiCo2O4 preserves the brilliant pseudo-capacitive performances due to providing smooth paths for electrolyte penetration and ion diffusion into inner active sites. Morphologies and microstructures of the active materials are examined by transmission electron microscopic (TEM) and X-ray diffraction (XRD) analyses. Thermogravimetric analysis (TGA) is used to evaluate the thermal properties of precursor solutions. The electrochemical performances of NiCo2O4 are systematically characterized by cyclic voltammetry and charge-discharge tests. Asymmetric supercapacitors are assembled with these brilliant binary oxides as the positive electrode and activated carbon as the negative electrode. The highly porous NiCo2O4 exhibits superior capacitive performances, i.e., high specific capacitance (764 F g-1 at 2 mV s-1) and long cycle life.

  4. Nanocrystalline spinel ferrite (MFe{sub 2}O{sub 4}, M = Ni, Co, Mn, Mg, Zn) powders prepared by a simple aloe vera plant-extracted solution hydrothermal route

    Energy Technology Data Exchange (ETDEWEB)

    Phumying, Santi; Labuayai, Sarawuth; Swatsitang, Ekaphan; Amornkitbamrung, Vittaya [Department of Physics, Faculty of Science, Khon Kaen University, Khon Kaen 40002 (Thailand); Integrated Nanotechnology Research Center (INRC), Khon Kaen University, Khon Kaen 40002 (Thailand); Maensiri, Santi, E-mail: santimaensiri@gmail.com [School of Physics, Institute of Science, Suranaree University of Technology, Nakhon Ratchasima 30000 (Thailand)

    2013-06-01

    Graphical abstract: This figure shows the specific magnetization curves of the as-prepared MFe{sub 2}O{sub 4} (M = Ni, Co, Mn, Mg, Zn) powders obtained from room temperature VSM measurement. These curves are typical for a soft magnetic material and indicate hysteresis ferromagnetism in the field ranges of ±500 Oe, ±1000 Oe, and ±2000 Oe for the CoFe{sub 2}O{sub 4}, MgFe{sub 2}O{sub 4} and MnFe{sub 2}O{sub 4} respectively, whereas the samples of NiFe{sub 2}O{sub 4} and ZnFe{sub 2}O{sub 4} show a superparamagnetic behavior. Highlights: ► Nanocrystalline MFe{sub 2}O{sub 4} powders were synthesized by a novel hydrothermal method. ► Metal acetylacetonates and aloe vera plant-extracted solution are used. ► This biosynthetic route is very simple and provides high-yield oxide nanomaterials. ► XRD and TEM results indicate that the prepared samples have only spinel structure. ► The maximum M{sub s} of 68.9 emu/g at 10 kOe were observed for the samples of MnFe{sub 2}O{sub 4}. - Abstract: Nanocrystalline spinel ferrite MFe{sub 2}O{sub 4} (M = Ni, Co, Mn, Mg, Zn) powders were synthesized by a novel hydrothermal method using Fe(acac){sub 3}, M(acac){sub 3} (M = Ni, Co, Mn, Mg, Zn) and aloe vera plant extracted solution. The X-ray diffraction and selected-area electron diffraction results indicate that the synthesized nanocrystalline have only spinel structure without the presence of other phase impurities. The crystal structure and morphology of the spinel ferrite powders, as revealed by TEM, show that the NiFe{sub 2}O{sub 4} and CoFe{sub 2}O{sub 4} samples contain nanoparticles, whereas the MnFe{sub 2}O{sub 4} and MgFe{sub 2}O{sub 4} samples consist of many nanoplatelets and nanoparticles. Interestingly, the ZnFe{sub 2}O{sub 4} sample contains plate-like structure of networked nanocrystalline particles. Room temperature magnetization results show a ferromagnetic behavior of the CoFe{sub 2}O{sub 4}, MnFe{sub 2}O{sub 4} and MgFe{sub 2}O{sub 4} samples, whereas the

  5. Nickel permanganate as a precursor in the synthesis of a NiMn2O4 spinel

    International Nuclear Information System (INIS)

    Schmidt, Jorge A.; Sagua, Aurora E.; Bazan, Julio C.; Prat, Maria R.; Braganza, Maria E.; Moran, Emilio

    2005-01-01

    The present study describes the preparation, characterization, and thermal decomposition of the compound Ni(MnO 4 ) 2 .xH 2 O, which was synthesized by a coprecipitation method at a low temperature. The role of this compound as a precursor in the synthesis of a Ni-Mn spinel was determined via X-ray, TG-DTA, electron diffraction, and EDAX measurements

  6. Reducing agent (NaBH4) dependent structure, morphology and magnetic properties of nickel ferrite (NiFe2O4) nanorods

    International Nuclear Information System (INIS)

    Saravanakumar, B.; Rani, B. Jansi; Ravi, G.; Thambidurai, M.; Yuvakkumar, R.

    2017-01-01

    Nickel ferrite (Ni-Fe 2 O 4 ) nanorods were synthesized employing a simple chemical reduction method. Reducing agent (NaBH 4 ) influence on structural, morphological and magnetic properties of NiFe 2 O 4 nanorods was investigated. XRD results clearly revealed the presence of inverse cubic spinel nickel ferrite structure characteristic peaks and confirmed the site inversion of inverse spinel structure of Fe 3+ tetrahedral A site and Ni 2+ octahedral B site. The observed Raman characteristic peak at 488 and 683 cm −1 were corresponded to E 1 g and A 1 g mode whereas A and B site respectively corresponded to tetrahedral and octahedral site of NiFe 2 O 4 inverse spinel structure. The obtained PL peaks at 530 and 542 nm were attributed to the emission spectra of Fe 3+ ions in site A of inverse spinel structure and Ni 2+ ions in site B of inverse spinel structure respectively. SEM result clearly revealed that increase in NaBH 4 concentration had remarkable impact on nanorods formation, nano-octahedron structure, homogeneity and regularity of Ni-Ferrites. VSM studies clearly revealed the soft ferromagnetic nature of NiFe 2 O 4 and increase in NaBH 4 concentration further induced raise in metal cations concentration in A- and B- site which might impact the resultant magnetization of ferrites. - Highlights: • Nano rod formation has been initiated while increase of NaBH 4 concentration. • Further increasing NaBH 4 concentration favors nano-octahedron formation. • VSM studies revealed soft ferromagnetic nature of NiFe 2 O 4 .

  7. The preparation of Zn-ferrite epitaxial thin film from epitaxial Fe3O4:ZnO multilayers by ion beam sputtering deposition

    International Nuclear Information System (INIS)

    Su, Hui-Chia; Dai, Jeng-Yi; Liao, Yen-Fa; Wu, Yu-Han; Huang, J.C.A.; Lee, Chih-Hao

    2010-01-01

    A new method to grow a well-ordered epitaxial ZnFe 2 O 4 thin film on Al 2 O 3 (0001) substrate is described in this work. The samples were made by annealing the ZnO/Fe 3 O 4 multilayer which was grown with low energy ion beam sputtering deposition. Both the Fe 3 O 4 and ZnO layers were found grown epitaxially at low temperature and an epitaxial ZnFe 2 O 4 thin film was formed after annealing at 1000 o C. X-ray diffraction shows the ZnFe 2 O 4 film is grown with an orientation of ZnFe 2 O 4 (111)//Al 2 O 3 (0001) and ZnFe 2 O 4 (1-10)//Al 2 O 3 (11-20). X-ray absorption spectroscopy studies show that Zn 2+ atoms replace the tetrahedral Fe 2+ atoms in Fe 3 O 4 during the annealing. The magnetic properties measured by vibrating sample magnetometer show that the saturation magnetization of ZnFe 2 O 4 grown from ZnO/Fe 3 O 4 multilayer reaches the bulk value after the annealing process.

  8. Thermoluminescent properties of Spinel-type oxides present in the Ternary system In2O3-TiO2-Mg O in air at 1350 degrees C

    International Nuclear Information System (INIS)

    Brown, F.; Hernandez P, T. C.; Alvarez M, V. E.; Cruz V, C.; Munoz, I. C.; Bernal, R.

    2015-10-01

    Full text: In the ternary system In 2 O 3 -TiO 2 -Mg O exists a solid solution Mg 2-x In 2x Ti 1-x O 4 (0≤ x ≤1) with spinel-type structure between MgIn 2 O 4 and Mg 2 TiO 4 (F. Brown et. al., 2000). In order to analyze their thermoluminescent (Tl) response, we obtained the spinel-type oxides with x= 0 (s1), 0.25 (s2), 0.5 (s3), 0.75 (s4), and 1 (s5) by a solid state reaction at 1350 degrees C in air. The X-ray patterns showed a spinel type structure for these compounds. The powders were exposed to beta particles from 90 Sr. The glow curve showed by s1 and s3 were hundreds of times more intense than s2, s4 and s5. At 50 Gy, s1 exhibits a main Tl maximum located at 200 degrees C, with two shoulders at 119 and 250 degrees C. The s3 oxide reveals a simple and wide glow curve at ≅195 degrees C with a Tl maximum located at 203 degrees C at 21.33 Gy. The peaks of the s1 and s3 oxide show a shift to lower temperatures and this increases its intensity as the irradiation dose increases. The lineal behavior observed for s1 and s3 were between 1.33-150 Gy and 10.66-341 Gy correspondingly, without evidence of saturation signal. After cycle 4, the s1 oxide has small variations in the relative sensitivity, with percentages below 1%. On the other hand, s3 reveals a relative sensitivity variation of 2.7%. Besides this, the standard deviation after ten consecutive irradiation-Tl readout cycles for s1 was 3.07 % and for s3 was 1%. The minimum detectable dose obtained were 0.5 Gy for s1 and 5.65 Gy for s3. These results suggest a possible application of Mg 1.5 InTi 0.5 O 4 in dosimetry. (Author)

  9. Synthesis and electrochemical characteristics of spinel LiMn2O4 via a precipitation spray-drying process

    International Nuclear Information System (INIS)

    Wu, H.M.; Tu, J.P.; Yuan, Y.F.; Li, Y.; Zhao, X.B.; Cao, G.S.

    2005-01-01

    Spinel LiMn 2 O 4 has been successfully synthesized using a precipitation spray-drying process. After the precursor was annealed at 750 deg. C for 10 h, the synthesized material was well-crystallized spinel particle, and exhibited uniform particle size distribution. From cyclic voltammetry results, there is an anomalous redox peaks (3.75/3.26 V). In the charge/discharge potential (versus Li) ranging from 3.2 to 4.5 V, it delivered a high initial discharge capacity of 123 mAh/g at a discharge rate of 60 μA/cm 2 (1/4 C rate). At a high discharge rate of 2.4 mA/cm 2 (10 C rate), the obtainable reversible capacity was 79 mAh/g. The simple procedure of precipitation spray-drying process is time and energy saving, and thus is promising for commercial application

  10. Microstructure, mechanical, thermal, EPR, and optical properties of MgAl2O4:Cr3+ spinel glass–ceramic nanocomposites

    International Nuclear Information System (INIS)

    Molla, A.R.; Kesavulu, C.R.; Chakradhar, R.P.S.; Tarafder, A.; Mohanty, S.K.; Rao, J.L.; Karmakar, B.; Biswas, S.K.

    2014-01-01

    Highlights: • E c of MgAl 2 O 4 spinel glass–ceramics has been found to be 250–270 kJ/mol. • TEM images show presence of cubic crystals of uniform size 10–15 nm in the GC. • HV ∼6.0 GPa, K c ∼ 5.0 MPa m 1/2 , flexural strength ∼100 MPa and E ∼ 55 GPa obtained. • Observed red emission of Cr 3+ ions due to spin-forbidden 2 E g → 4 A 2g transition. -- Abstract: The mechanical, thermal, and optical properties, along with the microstructure and electron paramagnetic resonance (EPR) spectra, have been studied for MgAl 2 O 4 :Cr 3+ spinel glass and glass–ceramics. The activation energy of the crystallization has been estimated from the differential scanning calorimetry (DSC) study using different models and is found to vary within 255–270 kJ/mol for the un-doped precursor glass. The microstructure of the glass–ceramics has been characterized using field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The TEM images demonstrate the presence of cubic crystals in the glass–ceramics of uniform size 10–15 nm. X-ray diffraction (XRD) and Fourier-transform infrared (FT-IR) spectroscopy reveal the presence of MgAl 2 O 4 spinel as the only crystalline phase, formed in the heat-treated glass–ceramics. The EPR spectrum of Cr 3+ doped glass sample exhibits a broad resonance signal with effective g = 1.97 whereas in glass–ceramic sample an additional weak resonance signal is observed at g = 3.83. The excitation spectrum exhibits two bands in the visible region. The emission spectrum exhibits an intense red emission at 690 nm which is characteristic of Cr 3+ ions caused by the spin-forbidden 2 E g → 4 A 2g transition. All the mechanical properties are found to have improved in the glass–ceramics when compared to glasses. A good combination of micro-hardness (∼6.0 GPa), high fracture toughness (∼5.0 MPa m 1/2 ), 3 point flexural strength (∼100 MPa) and elastic modulus (∼55 GPa) has been obtained

  11. Synthesis, characterization of spinels NiFe_2O_4 e CoFe_2O_4 and evaluation of performance in the trans esterification and esterification of cottonseed oil

    International Nuclear Information System (INIS)

    Dantas, J.; Silva, A.S.A.; Costa, A.C.F.M.; Freitas, N.L.

    2012-01-01

    The present study aimed synthesizes by combustion reaction and characterization of the spinel CoFe_2O_4 and NiFe_2O_4, and evaluation in the esterification and transesterification reaction of cottonseed oil for biodiesel. The samples were characterized by XRD, nitrogen adsorption/desorption (BET), SEM and transesterification e esterification reaction of the cottonseed oil for biodiesel. The results show that the synthesis was effective in achievement the CoFe_2O_4 and NiFe_2O_4 with surface area 23.75 and 18.18 m"2g"1. The results for esterification indicated that CoFe_2O_4 conversion 16.8 and 38.6%, however for transesterification reaction was observed that NiFe_2O_4 conversion 8.6 and 16.8% for ethanol and methanol, respectively. (author)

  12. Nature of the Electrochemical Properties of Sulphur Substituted LiMn2O4 Spinel Cathode Material Studied by Electrochemical Impedance Spectroscopy

    Directory of Open Access Journals (Sweden)

    Monika Bakierska

    2016-08-01

    Full Text Available In this work, nanostructured LiMn2O4 (LMO and LiMn2O3.99S0.01 (LMOS1 spinel cathode materials were comprehensively investigated in terms of electrochemical properties. For this purpose, electrochemical impedance spectroscopy (EIS measurements as a function of state of charge (SOC were conducted on a representative charge and discharge cycle. The changes in the electrochemical performance of the stoichiometric and sulphur-substituted lithium manganese oxide spinels were examined, and suggested explanations for the observed dependencies were given. A strong influence of sulphur introduction into the spinel structure on the chemical stability and electrochemical characteristic was observed. It was demonstrated that the significant improvement in coulombic efficiency and capacity retention of lithium cell with LMOS1 active material arises from a more stable solid electrolyte interphase (SEI layer. Based on EIS studies, the Li ion diffusion coefficients in the cathodes were estimated, and the influence of sulphur on Li+ diffusivity in the spinel structure was established. The obtained results support the assumption that sulphur substitution is an effective way to promote chemical stability and the electrochemical performance of LiMn2O4 cathode material.

  13. Structural Rietveld refinement and vibrational study of MgCr{sub x}Fe{sub 2−x}O{sub 4} spinel ferrites

    Energy Technology Data Exchange (ETDEWEB)

    Sabri, K. [Laboratoire des Sciences et technique de l’Environnement et de la Valorisation, département de Génie des Procédés, Université de Mostaganem, Mostaganem (Algeria); Rais, A., E-mail: amrais@yahoo.com [Laboratoire des Sciences et technique de l’Environnement et de la Valorisation, département de Génie des Procédés, Université de Mostaganem, Mostaganem (Algeria); Taibi, K. [Laboratoire de Science et Génie des Matériaux, USTHB, Alger, Algéria (Algeria); Moreau, M.; Ouddane, B. [Laboratory of LASIR Spectrochemistry, University of Science and Technology, 59650 Villeneuve d’Ascq (France); Addou, A. [Laboratoire des Sciences et technique de l’Environnement et de la Valorisation, département de Génie des Procédés, Université de Mostaganem, Mostaganem (Algeria)

    2016-11-15

    Spinel ferrites with the general formula MgCr{sub x}Fe{sub 2−x}O{sub 4} (0≤x≤1) were synthesized by the standard ceramic technique and characterized by X-ray diffraction. The XRD patterns confirmed that the mixed ferrite samples are in the cubic spinel structure which is further validated by Rietveld refinement in the space group Fd3m. The crystal structure and cell parameters were refined by Rietveld analysis. The vibrational study was achieved using Fourier Transform-InfraRed (FT-IR) and Raman spectroscopy. From FT-IR band frequencies, the force constants K{sub t} and K{sub o} , for tetrahedral (A) and octahedral (B) sites respectively, have been calculated and discussed with the trend of bond lengths obtained from Rietveld refinement. For all compositions, Raman spectra revealed the five active modes showing the vibration of O{sup 2−} ions at both the A-site and B-site ions. The frequencies trend with chromium content of both FT-IR and Raman spectra showed a shift toward higher values for all modes.

  14. Spontaneous electric polarization in the B-site magnetic spinel GeCu2O4

    Science.gov (United States)

    Yanda, Premakumar; Ghara, Somnath; Sundaresan, A.

    2018-04-01

    We report the observation of a spontaneous electric polarization at the antiferromagnetic ordering temperature (TN ∼ 33 K) of Cu2+ ions in the B-site magnetic spinel GeCu2O4, synthesized at high pressure and high temperature. This compound is known to crystallize in a tetragonal structure (space group I41/amd) due to Jahn-Teller distortion of Cu2+ ions and exhibit a collinear up-up-down-down (↑↑↓↓) antiferromagnetic spin configuration below TN. We found a clear dielectric anomaly at TN, where an electric polarization appears in the absence of applied magnetic field. The electric polarization is suppressed by applied magnetic fields, which demonstrates that the compound GeCu2O4 is a type-II multiferroic.

  15. Magnetic ordering in the spinel compound Li[Mn2?xLix]O4(x = 0,0.04)

    NARCIS (Netherlands)

    Gaddy, J.; Lamsal, J.; Petrovic, M.; Montfrooij, W.; Schmets, A.; Vojta, T.

    2009-01-01

    The two B-site ions Mn3+ and Mn4+ in the stoichiometric spinel structure LiMn2O4 form a complex, columnar ordered pattern below the charge-ordering transition at room temperature. On further cooling to below 66 K, the system develops long-range antiferromagnetic order. In contrast, whereas

  16. Ab initio investigation of the thermodynamics of cation distribution and of the electronic and magnetic structures in the LiMn2O4 spinel

    Science.gov (United States)

    Santos-Carballal, David; Ngoepe, Phuti E.; de Leeuw, Nora H.

    2018-02-01

    The spinel-structured lithium manganese oxide (LiMn2O4 ) is a material currently used as cathode for secondary lithium-ion batteries, but whose properties are not yet fully understood. Here, we report a computational investigation of the inversion thermodynamics and electronic behavior of LiMn2O4 derived from spin-polarized density functional theory calculations with a Hubbard Hamiltonian and long-range dispersion corrections (DFT+U-D3). Based on the analysis of the configurational free energy, we have elucidated a partially inverse equilibrium cation distribution for the LiMn2O4 spinel. This equilibrium degree of inversion is rationalized in terms of the crystal field stabilization effects and the difference between the size of the cations. We compare the atomic charges with the oxidation numbers for each degree of inversion. We found segregation of the Mn charge once these ions occupy the tetrahedral and octahedral sites of the spinel. We have obtained the atomic projections of the electronic band structure and density of states, showing that the normal LiMn2O4 has half-metallic properties, while the fully inverse spinel is an insulator. This material is in the ferrimagnetic state for the inverse and partially inverse cation arrangement. The optimized lattice and oxygen parameters, as well as the equilibrium degree of inversion, are in agreement with the available experimental data. The partial equilibrium degree of inversion is important in the interpretation of the lithium ion migration and surface properties of the LiMn2O4 spinel.

  17. ZnFe2O4-C/LiFePO4-CNT: A Novel High-Power Lithium-Ion Battery with Excellent Cycling Performance.

    Science.gov (United States)

    Varzi, Alberto; Bresser, Dominic; von Zamory, Jan; Müller, Franziska; Passerini, Stefano

    2014-07-15

    An innovative and environmentally friendly battery chemistry is proposed for high power applications. A carbon-coated ZnFe 2 O 4 nanoparticle-based anode and a LiFePO 4 -multiwalled carbon nanotube-based cathode, both aqueous processed with Na-carboxymethyl cellulose, are combined, for the first time, in a Li-ion full cell with exceptional electrochemical performance. Such novel battery shows remarkable rate capabilities, delivering 50% of its nominal capacity at currents corresponding to ≈20C (with respect to the limiting cathode). Furthermore, the pre-lithiation of the negative electrode offers the possibility of tuning the cell potential and, therefore, achieving remarkable gravimetric energy and power density values of 202 Wh kg -1 and 3.72 W kg -1 , respectively, in addition to grant a lithium reservoir. The high reversibility of the system enables sustaining more than 10 000 cycles at elevated C-rates (≈10C with respect to the LiFePO 4 cathode), while retaining up to 85% of its initial capacity.

  18. In-situ synchrotron PXRD study of spinel LiMn2O4 formation

    DEFF Research Database (Denmark)

    Birgisson, Steinar; Jensen, Kirsten Marie Ørnsbjerg; Christiansen, Troels Lindahl

    structural properties for the reaction being studied. Normally the reactions are started by heating and a constant temperature is kept throughout the experiment. In this study the hydrothermal reaction previously shown to produce spinel LiMn2O4 nanoparticles is studied in-situ to learn more about the phase......O4, depending on the initial concentration if Li-ions. An impurity phase, identified as Mn3O4, is also detected in different concentrations depending on reaction time and temperature. We have developed an experimental technique for in-situ measurements of solvothermal reactions under sub...... in the in-situ measurements it gives a unique opportunity to study reaction kinetics and thermodynamic quantities of the reactions. A temperature study of the reaction has been conducted to see how the formation rate and particle growth is affected by temperature while the precursor concentration is kept...

  19. Magnetic phase diagrams of the spinels AB2xGa2-2xO4 (A = Zn, Co; B = Al, Cr) systems

    International Nuclear Information System (INIS)

    Hamedoun, M.; Masrour, R.; Bouslykhane, K.; Hourmatallah, A.; Benzakour, N.

    2008-01-01

    The magnetic properties of the spinels CoAl 2x Ga 2-2x O 4 and ZnCr 2x Ga 2-2x O 4 systems in the range 0 ≤ x ≤ 1 have been studied by mean field theory and high-temperature series expansions. By using the first theory, we have evaluated the nearest neighbour and the next-neighbour super-exchange interaction J 1 (x) and J 2 (x), respectively, for the first systems in the range 0 ≤ x ≤ 1 and J 1 (x = 1), J 2 (x = 1) for the second system. The intra-planar and the inter-planar interactions are deduced. The corresponding classical exchange energy for magnetic structure is obtained for the first system. The second theory have been applied in the spinels CoAl 2x Ga 2-2x O 4 and ZnCr 2x Ga 2-2x O 4 systems, combined with the Pade approximants method, we have obtained the magnetic phase diagrams (T N versus dilution x) in the range 0 ≤ x ≤ 1. The obtained theoretical results are in agreement with experimental ones obtained by magnetic measurements and Moessbauer spectroscopy. The threshold percolation in the second system is x p ∼ 0.4. The critical exponents associated with the magnetic susceptibility (γ) and the correlation lengths (ν) are deduced in the range 0 ≤ x ≤ 1

  20. Enzyme mimics of spinel-type CoxNi1−xFe2O4 magnetic nanomaterial for eletroctrocatalytic oxidation of hydrogen peroxide

    International Nuclear Information System (INIS)

    Luo, Liqiang; Zhang, Yuting; Li, Fang; Si, Xiaojing; Ding, Yaping; Deng, Dongmei; Wang, Tianlin

    2013-01-01

    Graphical abstract: -- Highlights: •Spinel-type Co x Ni 1−x Fe 2 O 4 (x = 0, 0.2, 0.4, 0.5, 0.6, 0.8, 1.0) were synthesized. •Co x Ni 1−x Fe 2 O 4 were first employed as novel enzyme mimic sensing materials of H 2 O 2 . •Co 0.5 Ni 0.5 Fe 2 O 4 /CPE showed excellent electrocatalytic activity to H 2 O 2 . •Co 0.5 Ni 0.5 Fe 2 O 4 /CPE was successfully applied to determine H 2 O 2 in toothpastes. -- Abstract: A series of spinel-type Co x Ni 1−x Fe 2 O 4 (x = 0, 0.2, 0.4, 0.5, 0.6, 0.8, 1.0) magnetic nanomaterials were solvothermally synthesized as enzyme mimics for the eletroctrocatalytic oxidation of H 2 O 2 . X-ray diffraction and scanning electron microscope were employed to characterize the composition, structure and morphology of the material. The electrochemical properties of spinel-type Co x Ni 1−x Fe 2 O 4 with different (Co/Ni) molar ratio toward H 2 O 2 oxidation were investigated, and the results demonstrated that Co 0.5 Ni 0.5 Fe 2 O 4 modified carbon paste electrode (Co 0.5 Ni 0.5 Fe 2 O 4 /CPE) possessed the best electrocatalytic activity for H 2 O 2 oxidation. Under optimum conditions, the calibration curve for H 2 O 2 determination on Co 0.5 Ni 0.5 Fe 2 O 4 /CPE was linear in a wide range of 1.0 × 10 −8 –1.0 × 10 −3 M with low detection limit of 3.0 × 10 −9 M (S/N = 3). The proposed Co 0.5 Ni 0.5 Fe 2 O 4 /CPE was also applied to the determination of H 2 O 2 in commercial toothpastes with satisfactory results, indicating that Co x Ni 1−x Fe 2 O 4 is a promising hydrogen peroxidase mimics for the detection of H 2 O 2

  1. The performance of spinel bulk-like oxygen-deficient CoGa2O4 as an air-cathode catalyst in microbial fuel cell

    Science.gov (United States)

    Liu, Di; Mo, Xiaoping; Li, Kexun; Liu, Yi; Wang, Junjie; Yang, Tingting

    2017-08-01

    Nano spinel bulk-like CoGa2O4 prepared via a facile hydrothermal method is used as a high efficient electrochemical catalyst in activated carbon (AC) air-cathode microbial fuel cell (MFC). The maximum power density of the modified MFC is 1911 ± 49 mW m-2, 147% higher than the MFC of untreated AC cathode. Transmission electron microscope (TEM) and X-ray diffraction (XRD) exhibit the morphology and crystal structure of CoGa2O4. Rotating disk electrode (RDE) confirms the four-electron pathway at the cathode during the oxygen reduction reaction (ORR). Thermogravimetric analysis (TGA) and X-ray photoelectron spectroscopy (XPS) illustrate that the high rate oxygen vacancy exist in the CoGa2O4. The oxygen vacancy of CoGa2O4 plays an important role in catalytic activity. In a word, the prepared nano spinel bulk-like CoGa2O4 provides an alternative to the costly Pt in air-cathode for power output.

  2. Fabrication of MgAl2O4 spinel/niobium laminar composites by plasma spraying

    International Nuclear Information System (INIS)

    Boncoeur, M.; Lochet, N.; Miomandre, F.; Schnedecker, G.

    1994-01-01

    The feasibility of plasma spray manufacturing of laminar ceramic matrix composites made of alternate thin layers of a ceramic oxide and a metal is demonstrated with a composite made of 7 layers, each 0.2 mm thick, of MgAl 2 O 4 spinel and niobium. Microstructure and mechanical characteristics have been studied with both as-sprayed and heat-treated under vacuum at 1400 C conditions. It is shown that the as-sprayed composite is brittle but becomes pseudo-plastic after heat treatment. These laminar composites are very attractive for the manufacturing of large surface, few millimeter thick components. (from authors). 4 figs., 4 refs

  3. On stoichiometry and intermixing at the spinel/perovskite interface in CoFe2O4/BaTiO3 thin films.

    Science.gov (United States)

    Tileli, Vasiliki; Duchamp, Martial; Axelsson, Anna-Karin; Valant, Matjaz; Dunin-Borkowski, Rafal E; Alford, Neil McN

    2015-01-07

    The performance of complex oxide heterostructures depends primarily on the interfacial coupling of the two component structures. This interface character inherently varies with the synthesis method and conditions used since even small composition variations can alter the electronic, ferroelectric, or magnetic functional properties of the system. The focus of this article is placed on the interface character of a pulsed laser deposited CoFe2O4/BaTiO3 thin film. Using a range of state-of-the-art transmission electron microscopy methodologies, the roles of substrate morphology, interface stoichiometry, and cation intermixing are determined on the atomic level. The results reveal a surprisingly uneven BaTiO3 substrate surface formed after the film deposition and Fe atom incorporation in the top few monolayers inside the unit cell of the BaTiO3 crystal. Towards the CoFe2O4 side, a disordered region extending several nanometers from the interface was revealed and both Ba and Ti from the substrate were found to diffuse into the spinel layer. The analysis also shows that within this somehow incompatible composite interface, a different phase is formed corresponding to the compound Ba2Fe3Ti5O15, which belongs to the ilmenite crystal structure of FeTiO3 type. The results suggest a chemical activity between these two oxides, which could lead to the synthesis of complex engineered interfaces.

  4. Solid state opto-impedance of LiNiVO4 and LiMn2O4

    International Nuclear Information System (INIS)

    Kalyani, P; Sivasubramanian, S; Prabhu, S Naveen; Ragavendran, K; Kalaiselvi, N; Ranganathan, N G; Madhu, S; SundaraRaj, A; Manoharan, S P; Jagannathan, R

    2005-01-01

    Spinel type LiMn 2 O 4 and inverse spinel LiNiVO 4 systems serve as standard cathode materials or potential cathode systems for application in high energy density lithium-ion batteries. Upon photo-excitation using UV radiation of energy ∼5 eV, the LiNiVO 4 system shows significant modification in the solid state impedance pattern while the LiMn 2 O 4 system does not. This study has revealed a significant difference in the opto-impedance pattern for LiNiVO 4 with respect to LiMn 2 O 4 , which may be due to the different electronic processes involved. An attempt has been made to study this behaviour from the solid-state viewpoint

  5. Neutron diffraction study of magnetic structure in the diluted spinel ferrite Zn0.4Co0.6AlxFe2-xO4 (0.0≤x≤1.0)

    International Nuclear Information System (INIS)

    Zakaria, A.K.M.; Asgar, M.A.; Eriksson, S.G.; Ahmed, F.U.; Yunus, S.M.; Delaplane, R.

    2004-01-01

    The distributions of magnetic moments over the A and B sublattices in the spinel ferrite Zn 0.4 Co 0.6 Al x Fe 2-x O 4 and their ordering as functions of temperature and composition have been investigated by neutron diffraction. An increasing loss in B sublattice magnetization with increasing x causing gradual destabilization of the ferrimagnetic order has been revealed. The features observed in neutron results suggest several transitions for the system

  6. Formation of graphene-like 2D spinel MnCo2O4 and its lithium storage properties

    DEFF Research Database (Denmark)

    Huang, Guoyong; Guo, Xueyi; Cao, Xiao

    2017-01-01

    Two-dimensional (2D) materials fulfill the requirements for fast lithium storage due to the large exposed surface area and the open shortened path for Li insertion/extraction. Novel graphene-like 2D spinel MnCo2O4 powders have been synthesized, which inherit the morphology and structure of specia...

  7. Thermoluminescent properties of Spinel-type oxides present in the Ternary system In{sub 2}O{sub 3}-TiO{sub 2}-Mg O in air at 1350 degrees C

    Energy Technology Data Exchange (ETDEWEB)

    Brown, F.; Hernandez P, T. C.; Alvarez M, V. E.; Cruz V, C. [Universidad de Sonora, Departamento de Investigacion en Polimeros y Materiales, Apdo. Postal 130, 83000 Hermosillo, Sonora (Mexico); Munoz, I. C. [Universidad de Sonora, Departamento de Ciencias Quimico-Biologicas, Apdo. Postal 130, 83000 Hermosillo, Sonora (Mexico); Bernal, R., E-mail: imunoz@polimeros.uson.mx [Universidad de Sonora, Departamento de Investigacion en Fisica, Apdo. Postal 5-088, 83190 Hermosillo, Sonora (Mexico)

    2015-10-15

    Full text: In the ternary system In{sub 2}O{sub 3}-TiO{sub 2}-Mg O exists a solid solution Mg{sub 2-x}In{sub 2x}Ti{sub 1-x}O{sub 4} (0≤ x ≤1) with spinel-type structure between MgIn{sub 2}O{sub 4} and Mg{sub 2}TiO{sub 4} (F. Brown et. al., 2000). In order to analyze their thermoluminescent (Tl) response, we obtained the spinel-type oxides with x= 0 (s1), 0.25 (s2), 0.5 (s3), 0.75 (s4), and 1 (s5) by a solid state reaction at 1350 degrees C in air. The X-ray patterns showed a spinel type structure for these compounds. The powders were exposed to beta particles from {sup 90}Sr. The glow curve showed by s1 and s3 were hundreds of times more intense than s2, s4 and s5. At 50 Gy, s1 exhibits a main Tl maximum located at 200 degrees C, with two shoulders at 119 and 250 degrees C. The s3 oxide reveals a simple and wide glow curve at ≅195 degrees C with a Tl maximum located at 203 degrees C at 21.33 Gy. The peaks of the s1 and s3 oxide show a shift to lower temperatures and this increases its intensity as the irradiation dose increases. The lineal behavior observed for s1 and s3 were between 1.33-150 Gy and 10.66-341 Gy correspondingly, without evidence of saturation signal. After cycle 4, the s1 oxide has small variations in the relative sensitivity, with percentages below 1%. On the other hand, s3 reveals a relative sensitivity variation of 2.7%. Besides this, the standard deviation after ten consecutive irradiation-Tl readout cycles for s1 was 3.07 % and for s3 was 1%. The minimum detectable dose obtained were 0.5 Gy for s1 and 5.65 Gy for s3. These results suggest a possible application of Mg{sub 1.5}InTi{sub 0.5}O{sub 4} in dosimetry. (Author)

  8. Magnetic ordering and electrical resistivity in Co0.2Zn0.8Fe2O4 spinel oxide

    International Nuclear Information System (INIS)

    Bhowmik, R.N.; Ranganathan, R.; Ghosh, B.; Kumar, S.; Chattopadhyay, S.

    2008-01-01

    We report the magnetic, Moessbauer spectroscopy and resistivity measurements in order to understand the electronic behaviour of bulk Co 0.2 Zn 0.8 Fe 2 O 4 spinel oxide. The effect of magnetic order on electrical behaviour is observed from the resistivity measurements in the absence and presence of magnetic field. The analysis of Moessbauer spectra suggests the absence of Fe 2+ ions in the system, which implies that complete hopping of charge carriers between localized Fe 3+ /Co 2+ and Fe 2+ /Co 3+ pair of ions in B sublattice is not the favourable mechanism in Co 0.2 Zn 0.8 Fe 2 O 4 . We suggest that electrical behaviour of the present sample may be consistent with a model of fractional charge transfer via Fe B 3+ -O 2- -Co B 2+ superexchange path

  9. The role of reduced graphene oxide on the electrochemical activity of MFe2O4 (M = Fe, Co, Ni and Zn) nanohybrids

    Science.gov (United States)

    Suresh, Shravan; Prakash, Anand; Bahadur, D.

    2018-02-01

    In this work, a comparative study of electrochemical performance of reduced graphene oxide-ferrites (RGO-MFe2O4, M = Fe, Co, Ni, and Zn) nanohybrids synthesized by hydrothermal method was done. The structural morphology and investigation of other physical properties of nanohybrids confirm the cubic spinel phase of the MFe2O4, reduction of graphene oxide and the distribution of ferrite nanoparticles (NPs) on RGO nanosheets. The role of RGO on the electrochemical behavior of nanohybrids was understood by quantifying the charge storage capacitance and charging-discharging behavior in a 0.1 M Na2SO4 electrolyte. The specific capacitance values of pristine Fe3O4, CoFe2O4, NiFe2O4, and ZnFe2O4 are 128, 117, 15.2 and 9.1 F g-1 respectively whereas specific capacitance of RGO-Fe3O4, RGO-CoFe2O4, RGO-NiFe2O4 and RGO-ZnFe2O4 are 233, 200, 25 and 66.8 F g-1 respectively. Our investigation suggests that apart from specific surface area of nanohybrids other factors such as structural morphology determine interaction between nanohybrids and electrolyte ions which play critical role in elevating the performance of electrodes.

  10. Rietveld structure refinement and elastic properties of MgAlxCrxFe2-2xO4 spinel ferrites

    Science.gov (United States)

    Thummer, K. P.; Tanna, Ashish R.; Joshi, Hiren H.

    2017-05-01

    MgAlxCrxFe2-2xO4 (x = 0.1, 03 & 0.6) ferrites are synthesized by solid state reaction method. The Rietveld refinement of X-ray diffraction (XRD) data confirms the cubic spinel structure with Fd3m space group. The Fourier Transform Infrared Transmission Spectroscopy (FTIR) is employed to study elastic properties of present systems at 300K. The force constants for tetrahedral (A) and octahedral (B) sites of the spinel lattice are determined by infrared spectral and X-ray diffraction analysis. The elastic constants like bulk modulus, rigidity modulus, Young's modulus, Poisson's ratio and Debye temperature are determined. The vibrational frequency of both the interstitial sites increases as Al-Cr content increases hence the force constant and elastic moduli for all the samples are found to increase for the present ferrite system.

  11. Study of irradiation damages in MgAl{sub 2}O{sub 4} and ZnAl{sub 2}O{sub 4} spinels in the framework of nuclear waste transmutation; Dommages d'irradiation dans des ceramiques de structure spinelle MgAl{sub 2}O{sub 4} et ZnAl{sub 2}O{sub 4} application a la transmutation des dechets nucleaires

    Energy Technology Data Exchange (ETDEWEB)

    Thiriet-Dodane, C

    2002-07-01

    The transmutation of minor actinides in-reactor is one solution currently being studied for the long time management of nuclear waste. In the heterogeneous concept the radionuclides are incorporating in an inert ceramic matrix. The support material must be insensitive to radiation damage. Fission product damage is the main radiation damage source during the transmutation process and therefore it is of the utmost importance to study their effects. We irradiated spinels MgAl{sub 2}O{sub 4} (matrix of reference) and ZnAl{sub 2}O{sub 4} by fast ions (by example: {sup 86}Kr of approximately 400 MeV) simulating the fission products. Under these conditions, the damage is primarily due to the electronic energy losses (S{sub e}). One of the structural features of spinel AB{sub 2}O{sub 4} is that the two cations (A{sup 2+} and B{sup 3+}) can exchange their site. This phenomenon is quantified by the inversion parameter. We highlight by XRD in grazing incidence that the structural changes observed in MgAl{sub 2}O{sub 4} correspond to an order-disorder transition from the cation sub-networks and not to a phase shift as described in the literature. Using other techniques characterizing the space group (Raman spectroscopy) as well as the local order (NMR 27Al, spectroscopy of absorption X with the thresholds K of Al and Zn), we confirm this interpretation. Moreover, for a fluence of 10{sup 14} ions/cm{sup 2}, the loss of the order at long distance is observed thus meaning a beginning of amorphization of material. The ZnAl{sub 2}O{sub 4} spinel presents the same behaviour. For this last spinel, an evolution of the inversion parameter according to the stopping power 2 was highlighted after irradiation by ions {sup 86}Kr from approximately 20 MeV. We illustrate our study by the analysis of the results obtained in XRD of an irradiation out of composite fuel (MgAl{sub 2}O{sub 4} + UO{sub 2}) called THERMHET. (authors)

  12. Structure and electromagnetic properties of NiZn spinel ferrite with nano-sized ZnAl{sub 2}O{sub 4} additions

    Energy Technology Data Exchange (ETDEWEB)

    Zheng, Zongliang, E-mail: zzlma@163.com; Zhang, Huaiwu; Yang, Qinghui; Jia, Lijun

    2015-11-05

    In this study, nanocrystalline ZnAl{sub 2}O{sub 4} (ZA) (x = 0–20 wt%) were introduced into Ni{sub 0.4}Zn{sub 0.6}Fe{sub 2}O{sub 4} ferrite (NZ) by a solid-state reaction method combining a sol–gel auto-combustion method. The effects of ZA addition on the crystalline phase formation, microstructures, magnetic and dielectric properties were systematically investigated. X-ray diffraction and scanning electron microscope results reveal that the added ZA can fully solve into the NZ to form a ceramic with single-phase cubic spinel structure, and the grain size decreases obviously as x > 5 wt%. Meanwhile, the magnetic and dielectric properties exhibit significantly dependent on the ZA addition content. With the increasing addition level of ZA from 0 to 20 wt%, the initial permeability μ{sub i} is found increased initially and then decreased with the maximum 679 at x = 0.5 wt%. For the samples with x ≤ 5 wt%, permittivity ε′ is relatively higher at low frequencies (ε′ = 91–138 at 1 MHz) and dielectric loss tan δ{sub ε} shows distinct peak behavior. When x reaches 10 wt%, however, the ε′ and tan δ{sub ε} show very stable spectra from 1 MHz to 1 GHz. - Highlights: • Various amount of nanocrystalline ZnAl{sub 2}O{sub 4} (ZA) were introduced into NiZn ferrite. • NiZn ferrite can form single-phase spinel ceramic materials with ZA additives. • ZA has significant effects on magnetic and dielectric properties of the ceramics. • It provides a new method for fabricating NiZn ferrite with tunable properties.

  13. Sodium storage capability of spinel Li4Mn5O12

    International Nuclear Information System (INIS)

    Zhang, Jiaolong; Wang, Wenhui; Li, Yingshun; Yu, Denis Y.W.

    2015-01-01

    Highlights: • Electrochemical behavior of spinel Li 4 Mn 5 O 12 is examined in Na-ion battery. • A capacity of 120.7 mAh g −1 is obtained during the first sodiation process. • Na storage performance is found to be strongly dependent on particle size. • Ion-exchange between Li ions and Na ions occurs in Li 4 Mn 5 O 12 structure upon cycling. • Loss of crystallinity with cycling, leading to capacity fading. - Abstract: Spinel Li 4 Mn 5 O 12 , a well-known 3 V Li-ion battery (LIB) material with excellent cycling stability and good rate capability, is examined as Na-ion battery (NIB) cathode for the first time. Electrochemical studies clearly show that Na ions can be reversibly inserted into and extracted from the three-dimensional spinel structure. However, unlike in LIB, the available capacity in NIB is strongly dependent on the particle size and current rate due to the sluggish Na-ion transport in solid phase. Cycle performance of Li 4 Mn 5 O 12 in NIB is also inferior to that in LIB. Ex-situ X-ray diffraction study indicates a gradual loss of crystallinity with cycling, and that the crystal lattice undergoes an irreversible expansion during the initial 20 cycles. Inductively coupled plasma spectroscopy shows a decrease of Li/Mn ratio in Li 4 Mn 5 O 12 with cycling. The results suggest that Li ions are removed from the material during the charging process. The charge-discharge mechanism is also discussed in the paper.

  14. Reducing agent (NaBH{sub 4}) dependent structure, morphology and magnetic properties of nickel ferrite (NiFe{sub 2}O{sub 4}) nanorods

    Energy Technology Data Exchange (ETDEWEB)

    Saravanakumar, B.; Rani, B. Jansi; Ravi, G. [Nanomaterials Laboratory, Department of Physics, Alagappa University, Karaikudi 630 004, Tamil Nadu (India); Thambidurai, M. [Luminous Centre of Excellence for Semiconductor Lighting and Displays, School of Electrical & Electronic Engineering, The Photonics Institute (TPI), Nanyang Technological University, 50 Nanyang Avenue, 639798 (Singapore); Yuvakkumar, R., E-mail: yuvakkumar@gmail.com [Nanomaterials Laboratory, Department of Physics, Alagappa University, Karaikudi 630 004, Tamil Nadu (India)

    2017-04-15

    Nickel ferrite (Ni-Fe{sub 2}O{sub 4}) nanorods were synthesized employing a simple chemical reduction method. Reducing agent (NaBH{sub 4}) influence on structural, morphological and magnetic properties of NiFe{sub 2}O{sub 4} nanorods was investigated. XRD results clearly revealed the presence of inverse cubic spinel nickel ferrite structure characteristic peaks and confirmed the site inversion of inverse spinel structure of Fe{sup 3+} tetrahedral A site and Ni{sup 2+} octahedral B site. The observed Raman characteristic peak at 488 and 683 cm{sup −1} were corresponded to E{sub 1} {sub g} and A{sub 1} {sub g} mode whereas A and B site respectively corresponded to tetrahedral and octahedral site of NiFe{sub 2}O{sub 4} inverse spinel structure. The obtained PL peaks at 530 and 542 nm were attributed to the emission spectra of Fe{sup 3+} ions in site A of inverse spinel structure and Ni{sup 2+} ions in site B of inverse spinel structure respectively. SEM result clearly revealed that increase in NaBH{sub 4} concentration had remarkable impact on nanorods formation, nano-octahedron structure, homogeneity and regularity of Ni-Ferrites. VSM studies clearly revealed the soft ferromagnetic nature of NiFe{sub 2}O{sub 4} and increase in NaBH{sub 4} concentration further induced raise in metal cations concentration in A- and B- site which might impact the resultant magnetization of ferrites. - Highlights: • Nano rod formation has been initiated while increase of NaBH{sub 4} concentration. • Further increasing NaBH{sub 4} concentration favors nano-octahedron formation. • VSM studies revealed soft ferromagnetic nature of NiFe{sub 2}O{sub 4}.

  15. Unique atom hyper-kagome order in Na4Ir3O8 and in low-symmetry spinel modifications.

    Science.gov (United States)

    Talanov, V M; Shirokov, V B; Talanov, M V

    2015-05-01

    Group-theoretical and thermodynamic methods of the Landau theory of phase transitions are used to investigate the hyper-kagome atomic order in structures of ordered spinels and a spinel-like Na4Ir3O8 crystal. The formation of an atom hyper-kagome sublattice in Na4Ir3O8 is described theoretically on the basis of the archetype (hypothetical parent structure/phase) concept. The archetype structure of Na4Ir3O8 has a spinel-like structure (space group Fd\\bar 3m) and composition [Na1/2Ir3/2](16d)[Na3/2](16c)O(32e)4. The critical order parameter which induces hypothetical phase transition has been stated. It is shown that the derived structure of Na4Ir3O8 is formed as a result of the displacements of Na, Ir and O atoms, and ordering of Na, Ir and O atoms, ordering dxy, dxz, dyz orbitals as well. Ordering of all atoms takes place according to the type 1:3. Ir and Na atoms form an intriguing atom order: a network of corner-shared Ir triangles called a hyper-kagome lattice. The Ir atoms form nanoclusters which are named decagons. The existence of hyper-kagome lattices in six types of ordered spinel structures is predicted theoretically. The structure mechanisms of the formation of the predicted hyper-kagome atom order in some ordered spinel phases are established. For a number of cases typical diagrams of possible crystal phase states are built in the framework of the Landau theory of phase transitions. Thermodynamical conditions of hyper-kagome order formation are discussed by means of these diagrams. The proposed theory is in accordance with experimental data.

  16. DT fusion neutron irradiation of BNL--LASL superconductor wires, LASL YAG, Al2O3 and Spinel, LASL-IIT MgO, YAG, Al2O3 and Spinel, and NRL GeO2 crystals, December 28, 1977

    International Nuclear Information System (INIS)

    MacLean, S.C.

    1978-01-01

    The DT fusion neutron irradiation of eleven BNL-LAST superconductor wires, six NRL GeO 2 crystals, two YAG, two Spinel and two Al 2 O 3 crystals for LASL and four LASL high purity single crystals of MgO, YAG, Spinel and Al 2 O 3 is described. The sample position, beam-on time, and neutron dose record are given. The maximum fluence on any sample was 1.51 x 10 16 neutrons/cm 2

  17. The role of annealing temperature and bio template (egg white) on the structural, morphological and magnetic properties of manganese substituted MFe2O4 (M=Zn, Cu, Ni, Co) nanoparticles

    Science.gov (United States)

    Ranjith Kumar, E.; Jayaprakash, R.; Kumar, Sanjay

    2014-02-01

    Manganese substituted ferrites (ZnFe2O4, CuFe2O4, NiFe2O4 and CoFe2O4) have been prepared in the bio template medium by using a simple evaporation method. The annealing temperature plays an important position on changing particle size and morphology of the mixed ferrite nanoparticles were found out by X-ray diffraction, transmission electron microscopy and scanning electron microscopy methods. The role of manganese substitution in the mixed ferrite nanoparticles were also analyzed for different annealing temperature. The substitution of Mn also creates a vital change in magnetic properties which is studied by using vibrating sample magnetometer (VSM). These spinel ferrites are decomposed to α-Fe2O3 after annealing above 550 °C in air. However, α-Fe2O3 phase was slowly vanished after ferrites annealing above 900 °C. The effect of this secondary phase on the structural change and magnetic properties of the mixed ferrite nanoparticles is discussed.

  18. First-principle investigation on stability of Co-doped spinel λ-Mn4-xCoxO8

    Institute of Scientific and Technical Information of China (English)

    HUANG Ke-long; CHEN Chun-an; LIU Su-qin; LUO Qiong; LIU Zhi-guo

    2007-01-01

    The mechanism of stability of Co-doped spinel λ-MnO2 that is referred to as spinel LiχMn2O4 (χ=0) was studied by using the first-principle calculation method. The total energy and formation enthalpy can be decreased remarkably due to the Co substation,resulting in a more stable structure of λ-MnχCr2O4. The bond order and DOS analysis were given in detail to explain the nature of stability improvement. The calculated results show that as the content of Co dopant increases, the bond order of Mn-O becomes larger and the peak of density of states around Fermi level shifts toward lower energy. The charge density distribution illustrates that the Mn-O bonding is ionic and partially covalent, and the covalent Mn-O bonding becomes stronger with the increase of Co dopant content. The results confirm that the Co-doping will enhance the stability of λ-MnO2 and hence improve the electrochemistry performance of LiχMn2O4.

  19. Crystal growth and magnetic properties of spinel (Co,Mn)3O4

    Science.gov (United States)

    Kang, Sun Hee; Kim, Ill Won; Jeong, Yoon Hee; Koo, Tae Yeong

    2012-04-01

    Single crystals of cubic and tetragonal spinel Co3-xMnxO4 (x=1.0 and 1.5) were successfully grown using a solvent evaporation method with PbF2 flux. Single crystals in octahedral shape with a size of about 4 mm on edge were obtained from 100 cm3 Pt crucibles. Ferrimagnetic transitions were detected at 170 K and 160 K from the measurements of temperature dependent magnetization and specific heat of Co2MnO4 and Co1.5Mn1.5O4, respectively. Low temperature field-dependent magnetization curves give a strong indication of the non-collinear spin structure, offering an insulating Co3-xMnxO4 system as a possible candidate for examining the multiferroicity.

  20. Comparison effects and electron spin resonance studies of α-Fe2O4 spinel type ferrite nanoparticles.

    Science.gov (United States)

    Bayrakdar, H; Yalçın, O; Cengiz, U; Özüm, S; Anigi, E; Topel, O

    2014-11-11

    α-Fe2O4 spinel type ferrite nanoparticles have been synthesized by cetyltrimethylammonium bromide (CTAB) and ethylenediaminetetraacetic acid (EDTA) assisted hydrothermal route by using NaOH solution. Electron spin resonance (ESR/EPR) measurements of α-Fe2O4 nanoparticles have been performed by a conventional x-band spectrometer at room temperature. The comparison effect of nanoparticles prepared by using CTAB and EDTA in different α-doping on the structural and morphological properties have been investigated in detail. The effect of EDTA-assisted synthesis for α-Fe2O4 nanoparticles are refined, and thus the spectroscopic g-factor are detected by using ESR signals. These samples can be considered as great benefits for magnetic recording media, electromagnetic and drug delivery applications. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Nanoporous LiMn2O4 spinel prepared at low temperature as cathode material for aqueous supercapacitors

    Science.gov (United States)

    Wang, F. X.; Xiao, S. Y.; Gao, X. W.; Zhu, Y. S.; Zhang, H. P.; Wu, Y. P.; Holze, R.

    2013-11-01

    LiMn2O4 spinel was prepared by a hydrothermal method using α-MnO2 nanotubes as precursor at 180 °C, a temperature much lower than that in previously reported methods. It is nanoporous with a pore size of about 40-50 nm and a BET surface area of 9.76 m2 g-1. It exhibits a high specific capacitance of 189 F g-1 at 0.3 A g-1 as a cathode for an aqueous supercapacitor. Even at 12 A g-1, it still has a capacitance of 166 F g-1. After 1500 cycles, there is no evident capacity fading. The LiMn2O4 cathode can deliver an energy density of 31.9 Wh kg-1 at 3480 W kg-1 and even maintain 19.4 Wh kg-1 at about 5100 W kg-1 based on the mass of LiMn2O4.

  2. Optical and dielectric properties of neutron irradiated MgAl2O4 spinels

    International Nuclear Information System (INIS)

    Ibarra, A.

    1996-01-01

    The radiation effects on the optical and electrical properties of stoichiometric MgAl 2 O 4 spinel specimens irradiated in FFTF-MOTA at temperatures between 385 and 750 C to fluence ranging from 5.3 to 24.9 x 10 26 n m -2 (E>0.1 McV) are measured. In the optical properties a strong absorption in the ultraviolet range is observed together with a small band around 20 000 cm -1 (510 nm). Two strong luminescence emissions are also observed around 700 nm, with excitation spectra in the ultraviolet region. In the electrical properties a strong decrease of conductivity is observed in the temperature range from 0 to 500 C. Other techniques (like dielectric spectroscopy and EPR) have been used. (orig.)

  3. Solution-combustion synthesized aluminium-doped spinel (LiAl(subx)Mn(sub2-x)O(sub4) as a high-performance lithium-ion battery cathode material

    CSIR Research Space (South Africa)

    Kebede, MA

    2015-06-01

    Full Text Available High-performing (LiAl(subx)Mn(sub2-x)O(sub4) (x = 0, 0.125, 0.25, 0.375, and 0.5) spinel cathode materials for lithium-ion battery were developed using a solution combustion method. The as-synthesized cathode materials have spinel cubic structure...

  4. Mitigation of chromium poisoning of cathodes in solid oxide fuel cells employing CuMn1.8O4 spinel coating on metallic interconnect

    Science.gov (United States)

    Wang, Ruofan; Sun, Zhihao; Pal, Uday B.; Gopalan, Srikanth; Basu, Soumendra N.

    2018-02-01

    Chromium poisoning is one of the major reasons for cathode performance degradation in solid oxide fuel cells (SOFCs). To mitigate the effect of Cr-poisoning, a protective coating on the surface of interconnect for suppressing Cr vaporization is necessary. Among the various coating materials, Cu-Mn spinel coating is considered to be a potential candidate due to their good thermal compatibility, high stability and good electronic conductivity at high temperature. In this study, Crofer 22 H meshes with no protective coating, those with commercial CuMn2O4 spinel coating and the ones with lab-developed CuMn1.8O4 spinel coating were investigated. The lab-developed CuMn1.8O4 spinel coating were deposited on Crofer 22 H mesh by electrophoretic deposition and densified by a reduction and re-oxidation process. With these different Crofer 22 H meshes (bare, CuMn2O4-coated, and CuMn1.8O4-coated), anode-supported SOFCs with Sr-doped LaMnO3-based cathode were electrochemically tested at 800 °C for total durations of up to 288 h. Comparing the mitigating effects of the two types of Cu-Mn spinel coatings on Cr-poisoning, it was found that the performance of the denser lab-developed CuMn1.8O4 spinel coating was distinctly better, showing no degradation in the cell electrochemical performance and significantly less Cr deposition near the cathode/electrolyte interface after the test.

  5. Nanostructural origin of semiconductivity and large magnetoresistance in epitaxial NiCo2O4/Al2O3 thin films

    Science.gov (United States)

    Zhen, Congmian; Zhang, XiaoZhe; Wei, Wengang; Guo, Wenzhe; Pant, Ankit; Xu, Xiaoshan; Shen, Jian; Ma, Li; Hou, Denglu

    2018-04-01

    Despite low resistivity (~1 mΩ cm), metallic electrical transport has not been commonly observed in inverse spinel NiCo2O4, except in certain epitaxial thin films. Previous studies have stressed the effect of valence mixing and the degree of spinel inversion on the electrical conduction of NiCo2O4 films. In this work, we studied the effect of nanostructural disorder by comparing the NiCo2O4 epitaxial films grown on MgAl2O4 (1 1 1) and on Al2O3 (0 0 1) substrates. Although the optimal growth conditions are similar for the NiCo2O4 (1 1 1)/MgAl2O4 (1 1 1) and the NiCo2O4 (1 1 1)/Al2O3 (0 0 1) films, they show metallic and semiconducting electrical transport, respectively. Post-growth annealing decreases the resistivity of NiCo2O4 (1 1 1)/Al2O3 (0 0 1) films, but the annealed films are still semiconducting. While the semiconductivity and the large magnetoresistance in NiCo2O4 (1 1 1)/Al2O3 (0 0 1) films cannot be accounted for in terms of non-optimal valence mixing and spinel inversion, the presence of anti-phase boundaries between nano-sized crystallites, generated by the structural mismatch between NiCo2O4 and Al2O3, may explain all the experimental observations in this work. These results reveal nanostructural disorder as being another key factor for controlling the electrical transport of NiCo2O4, with potentially large magnetoresistance for spintronics applications.

  6. Optimization of reaction conditions in selective oxidation of styrene over fine crystallite spinel-type CaFe2O4 complex oxide catalyst

    International Nuclear Information System (INIS)

    Pardeshi, Satish K.; Pawar, Ravindra Y.

    2010-01-01

    The CaFe 2 O 4 spinel-type catalyst was synthesized by citrate gel method and well characterized by thermogravimetric analysis, atomic absorption spectroscopy, Fourier-transform infrared spectroscopy, X-ray diffraction and transmission electron microscopy. The crystallization temperature of the spinel particle prepared by citrate gel method was 600 o C which was lower than that of ferrite prepared by other methods. CaFe 2 O 4 catalysts prepared by citrate gel method show better activity for styrene oxidation in the presence of dilute H 2 O 2 (30%) as an oxidizing agent. In this reaction the oxidative cleavage of carbon-carbon double bond of styrene takes place selectively with 38 ± 2 mol% conversion. The major product of the reaction is benzaldehyde up to 91 ± 2 mol% and minor product phenyl acetaldehyde up to 9 ± 2 mol%, respectively. The products obtained in the styrene oxidation reaction were analyzed by gas chromatography and mass spectroscopy. The influence of the catalyst, reaction time, temperature, amount of catalyst, styrene/H 2 O 2 molar ratio and solvents on the conversion and product distribution were studied.

  7. A general approach for MFe2O4 (M = Zn, Co, Ni) nanorods and their high performance as anode materials for lithium ion batteries

    Science.gov (United States)

    Wang, Nana; Xu, Huayun; Chen, Liang; Gu, Xin; Yang, Jian; Qian, Yitai

    2014-02-01

    MFe2O4 (M = Zn, Co, Ni) nanorods are synthesized by a template-engaged reaction, with β-FeOOH nanorods as precursors which are prepared by a hydrothermal method. The final products are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and high-resolution transmission electron microscopy (HRTEM). The electrochemical properties of the MFe2O4 (M = Zn, Co, Ni) nanorods are tested as the anode materials for lithium ion batteries. The reversible capacities of 800, 625 and 520 mAh g-1 are obtained for CoFe2O4, ZnFe2O4 and NiFe2O4, respectively, at the high current density of 1000 mA g-1 even after 300 cycles. The superior lithium-storage performances of MFe2O4 (M = Zn, Co, Ni) nanorods can be attributed to the one-dimensional (1D) nanostructure, which can shorten the diffusion paths of lithium ions and relax the strain generated during electrochemical cycling. These results indicate that this method is an effective, simple and general way to prepare good electrochemical properties of 1D spinel Fe-based binary transition metal oxides. In addition, the impact of different reaction temperatures on the electrochemical properties of MFe2O4 nanorods is also investigated.

  8. Spinel Li2CoTi3O8 nanometer obtained for application as pigment

    International Nuclear Information System (INIS)

    Costa de Camara, M. S.; Alves Pimentel, L.; Longo, E.; Nobrega Azevedo, L. da; Araujo Melo, D. M. de

    2016-01-01

    Pigments are used in ceramics, cosmetics, inks, and other applications widely materials. To this must be single and easily reproducible. Moreover, the pigments obtained in the nanoscale are more stable, reproducible and highlight color in small amounts compared with those obtained in micrometer scale. The mixed oxides with spinel structures AB 2 O 4 have important applications, including: pigments, refractories, catalytic and electronic ceramics. In this context, the aim of this work was the preparation of powder Li 2 CoTi 3 O 8 spinel phase with nanometer particle size of the polymeric precursor method (Pechini) and characterization by means of thermal analysis (TG/DTA) X-ray diffraction (XRD), refined by the Rietveld method, BET, transmission electron microscopy (TEM), Raman and colorimetric coordinates. The pigment was obtained by heat treatment of 400 degree centigrade to 1000 degree centigrade after pyrolysis at 300 degree centigrade/1 h for removing the organic material. Li 2 CoTi 3 O 8 desired spinel phase was obtained from 500 degree centigrade, and presenting stability nanometer to about 1.300 degree centigrade. Spinel green phase introduced at temperatures in the range of 400 degree centigrade and 500 degree centigrade, and 600 degree centigrade at temperatures between blue and 1000 degree centigrade. (Author)

  9. 3D CNT macrostructure synthesis catalyzed by MgFe2O4 nanoparticles-A study of surface area and spinel inversion influence

    Science.gov (United States)

    Zampiva, Rúbia Young Sun; Kaufmann Junior, Claudir Gabriel; Pinto, Juliano Schorne; Panta, Priscila Chaves; Alves, Annelise Kopp; Bergmann, Carlos Pérez

    2017-11-01

    The MgFe2O4 spinel exhibits remarkable magnetic properties that open up numerous applications in biomedicine, the environment and catalysis. MgFe2O4 nanoparticles are excellent catalyst for carbon nanotube (CNT) production. In this work, we proposed to use MgFe2O4 nanopowder as a catalyst in the production of 3D macroscopic structures based on CNTs. The creation of these nanoengineered 3D architectures remains one of the most important challenges in nanotechnology. These systems have high potential as supercapacitors, catalytic electrodes, artificial muscles and in environmental applications. 3D macrostructures are formed due to an elevated density of CNTs. The quantity and quality of the CNTs are directly related to the catalyst properties. A heat treatment study was performed to produce the most effective catalyst. Factors such as superficial area, spinel inversion, crystallite size, degree of agglomeration and its correlation with van der Waals forces were examined. As result, the ideal catalyst properties for CNT production were determined and high-density 3D CNT macrostructures were produced successfully.

  10. Solid state opto-impedance of LiNiVO{sub 4} and LiMn{sub 2}O{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Kalyani, P; Sivasubramanian, S; Prabhu, S Naveen; Ragavendran, K; Kalaiselvi, N; Ranganathan, N G; Madhu, S; SundaraRaj, A; Manoharan, S P; Jagannathan, R [Central Electrochemical Research Institute, Karaikudi-630006, Tamil Nadu (India)

    2005-04-07

    Spinel type LiMn{sub 2}O{sub 4} and inverse spinel LiNiVO{sub 4} systems serve as standard cathode materials or potential cathode systems for application in high energy density lithium-ion batteries. Upon photo-excitation using UV radiation of energy {approx}5 eV, the LiNiVO{sub 4} system shows significant modification in the solid state impedance pattern while the LiMn{sub 2}O{sub 4} system does not. This study has revealed a significant difference in the opto-impedance pattern for LiNiVO{sub 4} with respect to LiMn{sub 2}O{sub 4}, which may be due to the different electronic processes involved. An attempt has been made to study this behaviour from the solid-state viewpoint.

  11. FC and ZFC magnetic properties of ferro-spinels (MFe2O4) prepared by solution-combustion method

    Science.gov (United States)

    Aravind, G.; Kumar, R. Vijaya; Nathaniyal, V.; Rambabu, T.; Ravinder, D.

    2017-07-01

    Magnetic ferro-spinels MFe2O4 (M= Co and Ni) prepared by citrate-gel solution combustion method using metal nitrates with low sintering temperature (500°C). From the XRD and TEM studies confirm that a nano crystalline nature of the prepared samples. Field Cooled (FC) and Zero Field Cooled (ZFC) magnetic studies of the prepared ferro-spinels are measured by using vibrating sample magnetometer (VSM). The resultant magnetization of the prepared samples as a function of an applied magnetic field 10 T was measured at two different temperatures 5 K and 310 K. Field Cooled (FC) and Zero Field Cooled (ZFC) magnetization measurements under an applied field of 100 Oe and 1000 Oe in the temperature range of 5-375 K were carried out, which shows the blocking temperature of these two samples at around 350 K.

  12. Atomic-deficient nanostructurization in water-sorption alumomagnesium spinel ceramics MgAl2O4

    Science.gov (United States)

    Ingram, A.

    2018-02-01

    Atomic-deficient nanostructurization in alumomagnesium MgAl2O4 ceramics sintered at 1100-1400 °C caused by water sorption are studied employing positron annihilation lifetime spectroscopy. Detected PAL spectra are reconstructed from unconstrained x4-term decomposition, and further transformed to x3-term form to be applicable for analysis with x3-x2-CDA (coupling decomposition algorithm). It is proved that water-immersion processes reduce positronium (Ps) decaying in large-size holes of ceramics (1.70-1.84 nm in radius) at the expense of enhanced trapping in tiny ( 0.2 nm in radius) Ps-traps. The water sorption is shown to be more pronounced in structurally imperfect ceramics sintered at T s = 1100-1200 °C due to irreversible transformations between constituting phases, while reversible physical-sorption processes are dominated in structurally uniform ceramics composed of main spinel phase.

  13. Study of the crystallographic and magnetic properties of cubic manganite spinels NiMn2O4

    International Nuclear Information System (INIS)

    Boucher, B.

    1969-01-01

    We study the variation of the crystallographic properties (inversion degree, position parameters and short range order) of the cubic spinel Mn ν Ni 1-ν [Mn 2ν Ni ν ]O 4 , as a function of the thermal treatment applied to the sample. ν lies between 0. 74 and 0. 93; the slower the sample is cooled the more inverse it is. We show, in a molecular field theory, that a system of three magnetic sublattices can afford a 'star' configuration. We establish the conditions of stability of such a structure and its evolution as a function of temperature is foreseen. Neutron diffraction measurements show that the magnetic structure of NiMn 2 O 4 at 4.2 K is a 'star' configuration and that with increasing temperature it becomes a collinear structure in agreement with the theory. Furthermore, we find an anomaly in the value of specific heat at the transition temperature between 'star' and collinear structures. (author) [fr

  14. Hydrogenation of carbon monoxide on Co/MgAl2O4 and Ce-Co/MgAl2O4 catalysts

    International Nuclear Information System (INIS)

    Kondoh, S.; Muraki, H.; Fujitani

    1986-01-01

    It is well known that various hydrocarbons are obtained by hydrogenation of CO on Fischer-Tropsch catalysts, the products depending on the catalyst components such as Co, Ni, Fe and Ru: and the reaction conditions, particularly, temperature, pressure, space velocity and H 2 /CO ratio. Further, both reactivity and selectivity of catalysts may be improved by suitable selection of support and an additive. The main program of the present work is to develop a catalyst for producing C 5 + liquid hydrocarbons, as an automobile fuel, by the Fischer-Tropsch synthesis. The authors have studied unique CO catalyst systems consisting of various supports - such as Al 2 O 3 (γ, β, α), MgAl 2 O 4 (alumina magnesia spinel), MgO and additives selected from the lanthanoid elements (LE). The composition of spinel-based supports was altered in a range from 28 mol % excess Al 2 O 3 to 28 mol % excess MgO. Particularly, they found that a MgAl 2 O 4 support with 15-18 mol % excess Al 2 O 3 is the most preferable for our purpose and CeO 2 as the additive for Co/spinel catalyst remarkably improves C 5 + yield. Further, it was confirmed that the catalytic activity of Co-base catalysts agree with the oxidation state of Co-oxides on Co and Co-Ce/spinel catalysts. The performance of Co-based catalysts for the production of higher hydrocarbons from syn-gas were described elsewhere. The items described in this report include (a) selection of supports, (b) selection of optimum reaction conditions for Co-Ce/spinel catalyst, (c) redox characteristics of Co-oxides on a spinel surface, and (d) experimental observation of TPD profiles, adsorption capacities and IR spectra relating to adsorbed CO

  15. Facile synthesis of spinel CuCr{sub 2}O{sub 4} nanoparticles and studies of their photocatalytic activity in degradation of some selected organic dyes

    Energy Technology Data Exchange (ETDEWEB)

    Paul, Bappi; Bhuyan, Bishal [Department of Chemistry, National Institute of Technology Silchar, Silchar, 788010, Assam (India); Purkayastha, Debraj Dhar, E-mail: debrajdp@yahoo.com [Department of Chemistry, National Institute of Technology Silchar, Silchar, 788010, Assam (India); Dhar, Siddhartha Sankar, E-mail: ssd_iitg@hotmail.com [Department of Chemistry, National Institute of Technology Silchar, Silchar, 788010, Assam (India); Behera, Satyananda [Department of Ceramic Engineering, National Institute of Technology Rourkela, Rourkela, 769008, Odisha (India)

    2015-11-05

    Copper chromite (CuCr{sub 2}O{sub 4}) spinel nanoparticle catalysts have been successfully synthesized employing urea assisted co-precipitation followed by calcination. The synthesized nanoparticles were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and N{sub 2} adsorption-desorption isotherm (BET). The XRD pattern revealed formation of tetragonal body-centered CuCr{sub 2}O{sub 4} and TEM image showed quasi-spherical particles of size 5–35 nm. The photocatalytic activity of CuCr{sub 2}O{sub 4} was evaluated in degradation of some organic dyes such as methylene blue (MB), methyl orange (MO), and rhodamine B (RhB), without and with the assistance of H{sub 2}O{sub 2} under solar irradiation. The CuCr{sub 2}O{sub 4} photocatalysts showed high activity in degradation of RhB (93.6%) and MO (92.3%), but low activity in degradation of MB (80.6%). The catalyst reusability was tested by conducting the degradation of RhB dye with the spent catalyst and it was observed that the catalyst did not show any significant loss in its activity even after five cycles. - Highlights: • CuCr{sub 2}O{sub 4} nanoparticles were synthesized by urea assisted co-precipitation followed by calcination. • The XRD pattern revealed formation of tetragonal body-centered CuCr{sub 2}O{sub 4}. • The TEM images showed the material to be quasi-spherical in shape with sizes 5–35 nm. • CuCr{sub 2}O{sub 4} nanoparticles exhibited pronounced photocatalytic activity.

  16. Influence of the preparation method on the morphology of templated NiCo{sub 2}O{sub 4} spinel

    Energy Technology Data Exchange (ETDEWEB)

    Cabo, Moises; Pellicer, Eva, E-mail: eva.pellicer.icn@uab.cat; Rossinyol, Emma; Solsona, Pau [Universitat Autonoma de Barcelona, Departament de Fisica, Facultat de Ciencies (Spain); Castell, Onofre [Universitat Autonoma de Barcelona, Servei de Microscopia, Facultat de Ciencies (Spain); Surinach, Santiago; Baro, Maria Dolors [Universitat Autonoma de Barcelona, Departament de Fisica, Facultat de Ciencies (Spain)

    2011-09-15

    The synthesis of NiCo{sub 2}O{sub 4} spinel by several nanocasting strategies (i.e., multi-step nanocasting, one-step nanocasting and soft-templating), in which nickel and cobalt nitrates are used as precursors and Pluronic P123 as surfactant, is explored. First, in the multi-step nanocasting, the effect of the impregnation method (evaporation, solid-liquid and two-solvent) of the SBA-15 silica template on the morphology of NiCo{sub 2}O{sub 4} replica is investigated. The evaporation method seems to be the best choice to obtain mesoporous NiCo{sub 2}O{sub 4} powder which, after calcination at 375 Degree-Sign C and subsequent template removal, displays the highest surface area (93.1 m{sup 2}/g). We have also checked the feasibility of the one-step nanoscating approach for the synthesis of ordered NiCo{sub 2}O{sub 4} arrays, though this methodology entails severe difficulties, mainly related to the different decomposition temperature of the nitrate precursors and the P123 surfactant. Finally, randomly oriented, aggregated NiCo{sub 2}O{sub 4} nanoparticles are obtained by means of P123 surfactant-assisted soft-templating approach.

  17. Magnetic properties of magnetic Co1-xMgxFe2O4 spinel by HTSE method

    International Nuclear Information System (INIS)

    Hamedoun, M.; Benyoussef, A.; Bousmina, M.

    2011-01-01

    Magnetic properties and exchange-coupling interactions of diluted magnetic spinels A 1-x A' x B 2 X 4 , where A and B are magnetic ions, namely Co 1-x Mg x Fe 2 O 4 , were investigated using the high-temperature series expansion method (HTSE) and the distribution method of magnetic cations in the range 0≤x≤1. The magnetic phase diagram and transition temperature versus dilution x were determined using the Pade approximants method along with HTSE. The critical exponent associated with the magnetic susceptibility γ was then deduced. The obtained results are in good agreement with experimental results and critical exponent values are consistent with those suggested by the universality hypothesis.

  18. Non-monotonic compositional dependence of isothermal bulk modulus of the (Mg1–xMnxCr2O4 spinel solid solutions, and its origin and implication

    Directory of Open Access Journals (Sweden)

    Xi Liu

    2016-12-01

    Full Text Available The compressibility of the spinel solid solutions, (Mg1−xMnxCr2O4 with x = 0.00 (0, 0.20 (0, 0.44 (2, 0.61 (2, 0.77 (2 and 1.00 (0, has been investigated by using a diamond-anvil cell coupled with synchrotron X-ray radiation up to ∼10 GPa (ambient T. The second-order Birch–Murnaghan equation of state was used to fit the PV data, yielding the following values for the isothermal bulk moduli (KT, 198.2 (36, 187.8 (87, 176.1 (32, 168.7 (52, 192.9 (61 and 199.2 (61 GPa, for the spinel solid solutions with x = 0.00 (0, 0.20 (0, 0.44 (2, 0.61 (2, 0.77 (2 and 1.00 (0, respectively (KT′ fixed as 4. The KT value of the MgCr2O4 spinel is in good agreement with existing experimental determinations and theoretical calculations. The correlation between the KT and x is not monotonic, with the KT values similar at both ends of the binary MgCr2O4MnCr2O4, but decreasing towards the middle. This non-monotonic correlation can be described by two equations, KT = −49.2 (11x + 198.0 (4 (x ≤ ∼0.6 and KT = 92 (41x + 115 (30 (x ≥ ∼0.6, and can be explained by the evolution of the average bond lengths of the tetrahedra and octahedra of the spinel solid solutions. Additionally, the relationship between the thermal expansion coefficient and composition is correspondingly reinterpreted, the continuous deformation of the oxygen array is demonstrated, and the evolution of the component polyhedra is discussed for this series of spinel solid solutions. Our results suggest that the correlation between the KT and composition of a solid solution series may be complicated, and great care should be paid while estimating the KT of some intermediate compositions from the KT of the end-members.

  19. Nitrogen-doped graphene aerogel-supported spinel CoMn2O4 nanoparticles as an efficient catalyst for oxygen reduction reaction

    Science.gov (United States)

    Liu, Yisi; Li, Jie; Li, Wenzhang; Li, Yaomin; Chen, Qiyuan; Zhan, Faqi

    2015-12-01

    Spinel CoMn2O4 (CMO) nanoparticles grown on three-dimensional (3D) nitrogen-doped graphene areogel (NGA) is prepared by a facile two-step hydrothermal method. The NGA not only possesses the intrinsic property of graphene, but also has abundant pore conformations for supporting spinel metal oxide nanoparticles, thus would be suitable as a good electrocatalysts' support for oxygen reduction reaction (ORR). The structure, morphology, porous properties, and chemical composition of CMO/NGA are investigated by X-ray diffraction (XRD) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy, nitrogen adsorption-desorption measurements, and X-ray photoelectron spectroscopy (XPS). The electrocatalytic activity of catalysts is discussed by cyclic voltammograms (CV), electrochemical impedance spectroscopy (EIS), and rotating disk electrode (RDE) measurements in O2-saturated 0.1 M KOH electrolyte. The CMO/NGA hybrid exhibits more positive onset potential and half-wave potential, faster charge transfer than that of CMO and NGA, and its electrocatalytic performance is comparable with the commercial 20 wt.% Pt/C. Furthermore, it mainly favors a direct 4e- reaction pathway, and has excellent ethanol tolerance and high durability, which is attributed to the unique 3D crumpled porous nanostructure of NGA with large specific area and fast electron transport, and the synergic covalent coupling between the CoMn2O4 nanoparticles and NGA.

  20. Synthesis and characterization of ZnGa2O4 particles prepared by solid state reaction

    International Nuclear Information System (INIS)

    Can, Musa Mutlu; Hassnain Jaffari, G.; Aksoy, Seda; Shah, S. Ismat; Fırat, Tezer

    2013-01-01

    Highlights: ► Synthesis of ZnGa 2 O 4 particles produced from metallic Zn and Ga particles. ► The structural comparison of spinel and partially inverse spinel structure in ZnGa 2 O 4 . ► The Ga atoms occupied 13% of tetrahedral site in ZnGa 2 O 4 . ► The band gap, calculated from climate point of UV–visible, was found as 4.6 ± 0.1 eV. ► The optical analyses were shown defective ZnO structure in ZnGa 2 O 4 . - Abstract: We employed solid state reaction technique to synthesize ZnGa 2 O 4 particles, produced in steps of mixing/milling the ingredients in H 2 O following thermal treating under 1200 °C. We compare spinel and partially inverse spinel structure in ZnGa 2 O 4 particles using Rietveld refinement. Crystal structure of ZnGa 2 O 4 particles was identified with two structural phases; normal spinel structure and partially inverse spinel structure using Rietveld refinement. It is found that the partially inverse spinel structures occupy nearly 13% and the rest is normal spinel structure. The obtained X-ray diffraction data show that lattice constant and the position of Oxygen atoms remain almost constant in both structures. The characterization of the particles was also improved using X-ray photoelectron spectroscopy and Fourier transforms infrared spectroscopy measurements. The optical analyses were done with UV–visible spectroscopy. The band gap, calculated from climate point of UV–visible data, was found as 4.6 ± 0.1 eV. Despite no unexpected compound (such as ZnO and Ga 2 O 3 ) in the structure, the optical analyses were shown defective ZnO structure in ZnGa 2 O 4 .

  1. 2D Kagome ordering in the 3D frustrated spinel Li2Mn2O4

    International Nuclear Information System (INIS)

    Wiebe, C R; Russo, P L; Savici, A T; Uemura, Y J; MacDougall, G J; Luke, G M; Kuchta, S; Greedan, J E

    2005-01-01

    Muon spin relaxation (μSR) experiments on the geometrically frustrated spinel oxide, Li 2 Mn 2 O 4 , show the development of spin correlations over a range of lengthscales with decreasing temperature. Increased relaxation below ∼150 K is consistent with the onset of spin correlations. Below 50 K, spin order, on a lengthscale which is long range for the μSR probe, appears abruptly in temperature, consistent with prior neutron diffraction results. The oscillations in the zero field asymmetry are analysed using a three frequency model. By locating the muon site, this is shown to be consistent with the unexpected 2Dq=√3x√3 structure on the Kagome planes proposed originally from neutron data. Longitudinal field data demonstrate that some spin dynamics persist even at 2 K. Thus, a very complex magnetic ground state, featuring the coexistence of long lengthscale 2D ordering and significant spin dynamics, is proposed. This is unusual considering the 3D topology of the Mn 3+ spins in this material

  2. Synthesis and magnetic properties of CoFe2O4 spinel ferrite nanoparticles doped with lanthanide ions

    International Nuclear Information System (INIS)

    Kahn, Myrtil L.; Zhang, Z. John

    2001-01-01

    Lanthanide ions have been doped into cobalt spinel ferrites using an oil-in-water micellar method to form CoLn 0.12 Fe 1.88 O 4 nanoparticles with Ln=Ce, Sm, Eu, Gd, Dy, or Er. Doping with lanthanide ions (Ln III ) modulates the magnetic properties of cobalt spinel ferrite nanoparticles. In particular cases of Gd 3+ or Dy 3+ ions, a dramatic increase in the blocking temperature and coercivity is observed. Indeed, the introduction of only 4% of Gd 3+ ions increases the blocking temperature ∼100 K and the coercivity 60%. Initial studies on the magnetic properties of these doped nanoparticles clearly demonstrate that the relationship between the modulation of magnetic properties and the nature of doped Ln III ions is interesting but very complex. [copyright] 2001 American Institute of Physics

  3. PROPERTIES OF ORGANIC COATINGS CONTAINING PIGMENTS WITH SURFACE MODIFIED WITH A LAYER OF ZnFe2O4

    Directory of Open Access Journals (Sweden)

    Kateřina Nechvílová

    2015-11-01

    Full Text Available This work is focussed on the properties of organic coatings containing pigments whose surface was chemically coated with zinc ferrite (ZnFe2O4 layer. Four silicate types with different particle shapes were selected as the cores: diatomite, talc, kaolin and wollastonite. The untreated particles exhibit a barrier effect. The aim of this project was to apply the surface treatment approach with a view to enhancing not only the model paint films’ anticorrosion properties but also their resistance to physico- mechanical tests pursuant to ISO standards (cupping, bending, impact, adhesion. Other parameters examined included: particle size and morphology, density of the modified pigment, oil consumption, pH, conductivity, and electrochemical properties of the paint film. A solvent-based epoxy-ester resin was used as the binder and also served as the reference material. The pigment volume concentration (PVC was 1% and 10%. During the last stage of the experiment, the paint films were exposed to a corrosive environment stimulating seaside conditions or conditions roads treated with rock salt. The accelerated cyclic corrosion test in a neutral salt mist atmosphere was conducted for 864 hours. The results served to ascertain a suitable environment for organic coatings.

  4. The role of particle size on the electrochemical properties at 25 and at 55 deg. C of the LiCr0.2Ni0.4Mn1.4O4 spinel as 5 V-cathode materials for lithium-ion batteries

    International Nuclear Information System (INIS)

    Aklalouch, Mohamed; Rojas, Rosa M.; Rojo, Jose Maria; Saadoune, Ismael; Amarilla, Jose Manuel

    2009-01-01

    The role of the particle size on the electrochemical properties at 25 and at 55 deg. C of the LiCr 0.2 Ni 0.4 Mn 1.4 O 4 spinel synthesized by combustion method has been determined. Samples with different particle size were obtained by heating the raw spinel from 700 to 1100 deg. C, for 1 h in air. X-ray diffraction patterns revealed that all the prepared materials are single-phase spinels. The main effect of the thermal treatment is the remarkable increase of the particles size from ∼60 to ∼3000 nm as determined by transmission electron microscopy. The electrochemical properties were determined at high discharge currents (1C rate) in two-electrode Li-cells. At 25 and at 55 deg. C, in spite of the great differences in particle size, the discharge capacity drained by all samples is similar (Q dch ∼ 135 mAh g -1 ). Instead, the cycling performances strongly change with the particle size. The spinels with Φ > 500 nm show better cycling stability at 25 and at 55 deg. C than those with Φ -1 ), and remarkable cycling performances (capacity retention after 250 cycles >96%) are very attractive materials as 5V-cathodes for high-energy Li-ion batteries.

  5. Attestation in self-propagating combustion approach of spinel AFe_2O_4 (A = Co, Mg and Mn) complexes bearing mixed oxidation states: Magnetostructural properties

    International Nuclear Information System (INIS)

    Bennet, J.; Tholkappiyan, R.; Vishista, K.; Jaya, N. Victor; Hamed, Fathalla

    2016-01-01

    Highlights: • Spinel type ferrite compounds AFe_2O_4 (A = Co, Mg and Mn) have been successfully prepared by self-propagating combustion method using glycine as fuel. • To investigate and confirms the presence of phases in the synthesized ferrite nanoparticles by XRD and FTIR analysis. • The formation of mixed oxidation state of cobalt (Co"2"+ and Co"3"+), iron (Fe"2"+ and Fe"3"+) and manganese (Mn"2"+ and Mn"3"+) ions were studied and confirmed from XPS analysis. • The magnetic properties of the synthesized ferrites were studied by VSM measurement. - Abstract: Spinel type nano-sized ferrite compounds AFe_2O_4 (A = Co, Mg and Mn) have been successfully prepared by self-propagating combustion method using glycine as fuel at 400 °C under air atmosphere for 4 h. The crystal structure, chemical composition, morphology and magnetic properties of the synthesized samples were characterized by X−ray diffraction, Fourier transform infrared spectroscopy, X−ray photoelectron spectroscopy, Energy dispersive X−ray, Scanning and Transmission electron microscopy and vibrating sample magnetometer. The chemical reaction and role of fuel on the nanoparticles formation were discussed. The XRD pattern of the synthesized samples shows the formation of pure phase with average crystallite size of 97, 57 and 98 nm from Scherrer formula and 86, 54 and 87 nm from Williamson and Hall (W–H) formula respectively. FTIR absorption spectra revealed that the presence of strong absorption peaks near 400–600 cm"−"1 corresponds to tetrahedral and octahedral complex of spinel ferrites. The relative concentrations of electronic states of elements such as cobalt (Co"2"+ and Co"3"+), iron (Fe"2"+ and Fe"3"+) and manganese (Mn"2"+ and Mn"3"+) oxidation states were studied from XPS and it is found that 55% of Fe ions are in Fe"2"+ state and the remaining is in Fe"3"+ state and thus the cationic distribution of Fe ions occurred in both tetrahedral and octahedral sites. SEM analysis

  6. Foamlike porous spinel Mn(x)Co(3-x)O4 material derived from Mn3[Co(CN)6]2⋅nH2O nanocubes: a highly efficient anode material for lithium batteries.

    Science.gov (United States)

    Hu, Lin; Zhang, Ping; Zhong, Hao; Zheng, Xinrui; Yan, Nan; Chen, Qianwang

    2012-11-19

    A new facile strategy has been designed to fabricate spinel Mn(x)Co(3-x)O(4) porous nanocubes, which involves a morphology-conserved and pyrolysis-induced transformation of Prussian Blue Analogue Mn(3)[Co(CN)(6)](2)⋅nH(2)O perfect nanocubes. Owing to the release of CO(2) and N(x)O(y) in the process of interdiffusion, this strategy can overcome to a large extent the disadvantage of the traditional ceramic route for synthesis of spinels, and Mn(x)Co(3-x)O(4) with foamlike porous nanostructure is effectively obtained. Importantly, when evaluated as an electrode material for lithium-ion batteries, the foamlike Mn(x)Co(3-x)O(4) porous nanocubes display high specific discharge capacity and excellent rate capability. The improved electrochemical performance is attributed to the beneficial features of the particular foamlike porous nanostructure and large surface area, which reduce the diffusion length for Li(+) ions and enhance the structural integrity with sufficient void space for buffering the volume variation during the Li(+) insertion/extraction. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Spin canting and magnetic transition in NixZn1-xFe2O4 (x=0.0, 0.5 and 1.0) nanoparticles

    Science.gov (United States)

    Rani, Stuti; Raghav, Dharmendra Singh; Yadav, Prashant; Varma, G. D.

    2018-04-01

    Nanoparticles of NixZn1-xFe2O4(x=0.0, 0.5 and 1.0) have been synthesized via co-precipitation method and studied thestructural and magnetic properties. Rietveld refinement of X ray diffraction data of as synthesized samples revealthat the samples have mixed spinel structure with space group Fd-3m. The lattice parameter of the samples decreases as doping concentration of Ni ions increases. Magnetic measurements show paramagnetic to ferrimagnetic transition at room temperature on Ni doping in ZnFe2O4 nanoparticles. The magnetic measurements also show spin canting in samples possibly due to their nanocrystalline nature. The spin canting angles have been calculated with the help of Yafet-Kittel (Y-K) model. Furthermore, the Law of approach (LA) fitting of M-H curves indicates that the samples are highly anisotropicin nature. The Arrot plots of as synthesized samples also indicate the paramagnetic to ferrimagnetic transition. The correlation between the structural and observed magnetic properties of NixZn1-xFe2O4(x=0.0, 0.5 and 1.0) nanocrystals will be described and discussed in this paper.

  8. Phase relations and Gibbs energies of spinel phases and solid solutions in the system Mg-Rh-O

    Energy Technology Data Exchange (ETDEWEB)

    Jacob, K.T., E-mail: katob@materials.iisc.ernet.in [Department of Materials Engineering, Indian Institute of Science, Bangalore 560 012 (India); Prusty, Debadutta [Department of Materials Engineering, Indian Institute of Science, Bangalore 560 012 (India); Kale, G.M. [Institute for Materials Research, University of Leeds, Leeds, LS2 9JT (United Kingdom)

    2012-02-05

    Highlights: Black-Right-Pointing-Pointer Refinement of phase diagram for the system Mg-Rh-O and thermodynamic data for spinel compounds MgRh{sub 2}O{sub 4} and Mg{sub 2}RhO{sub 4} is presented. Black-Right-Pointing-Pointer A solid-state electrochemical cell is used for thermodynamic measurement. Black-Right-Pointing-Pointer An advanced design of the solid-state electrochemical cell incorporating buffer electrodes is deployed to minimize polarization of working electrode. Black-Right-Pointing-Pointer Regular solution model for the spinel solid solution MgRh{sub 2}O{sub 4} - Mg{sub 2}RhO{sub 4} based on ideal mixing of cations on the octahedral site is proposed. Black-Right-Pointing-Pointer Factors responsible for stabilization of tetravalent rhodium in spinel compounds are identified. - Abstract: Pure stoichiometric MgRh{sub 2}O{sub 4} could not be prepared by solid state reaction from an equimolar mixture of MgO and Rh{sub 2}O{sub 3} in air. The spinel phase formed always contained excess of Mg and traces of Rh or Rh{sub 2}O{sub 3}. The spinel phase can be considered as a solid solution of Mg{sub 2}RhO{sub 4} in MgRh{sub 2}O{sub 4}. The compositions of the spinel solid solution in equilibrium with different phases in the ternary system Mg-Rh-O were determined by electron probe microanalysis. The oxygen potential established by the equilibrium between Rh + MgO + Mg{sub 1+x}Rh{sub 2-x}O{sub 4} was measured as a function of temperature using a solid-state cell incorporating yttria-stabilized zirconia as an electrolyte and pure oxygen at 0.1 MPa as the reference electrode. To avoid polarization of the working electrode during the measurements, an improved design of the cell with a buffer electrode was used. The standard Gibbs energies of formation of MgRh{sub 2}O{sub 4} and Mg{sub 2}RhO{sub 4} were deduced from the measured electromotive force (e.m.f.) by invoking a model for the spinel solid solution. The parameters of the model were optimized using the measured

  9. Structural changes of manganese spinel at elevated temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Li, Guohua; Iijima, Yukiko; Azuma, Hideto [Nishi Battery Laboratories, Sony Corporation, 4-16-1 Okata, Kanagawa 243-0021 Atsugi (Japan); Kudo, Yoshihiro [Technical Support Center, Sony Corporation, 4-16-1 Okata, Kanagawa 243-0021 Atsugi (Japan)

    2002-01-01

    A chemical synthesis route to Cr-doped and undoped Mn spinel was developed for the purpose of detailed structural analysis for elucidating the relationship between storage performance and structural changes at elevated temperatures. We identified a two-phase segregation in the lithium compositional range of 0.62}O{sub 4}, which is in the same region wherein severe degradation upon storage at elevated temperatures was observed for electrochemical cells. These two phases also coexist in Cr-doped spinel in the lithium compositional range of 0.4O{sub 4}. The investigation by X-ray diffraction (XRD) indicated that the crystallinity of the spinel decreased after storage at elevated temperatures. X-ray absorption fine structure (XAFS) analysis revealed that the Cr-doped samples showed less change in the local structure after storage than the undoped spinel samples. These results suggest that the Cr-doped spinel has higher structural stability at elevated temperatures than the undoped spinel.

  10. Synthesis, characterization and photocatalytic properties of spinel CuAl2O4 nanoparticles by a sonochemical method

    International Nuclear Information System (INIS)

    Lv Weizhong; Liu Bo; Qiu Qi; Wang Fang; Luo Zhongkuan; Zhang Peixin; Wei Shaohui

    2009-01-01

    Spinel copper aluminate (CuAl 2 O 4 ) nanoparticles were synthesized with the aid of sonication by a precursor approach. The precursors were prepared by sonicating an aqueous solution of copper nitrate, aluminium nitrate, and urea. Upon heating at 900 deg. C for 6 h, the precursor formed nanosized CuAl 2 O 4 particles with an average size of 17 nm and with a surface area of about 110 m 2 g -1 . The nanosized copper aluminate particles as well as the precursors were characterized by elemental analysis, powder X-ray diffraction, transmission electron microscopy (TEM) image with electron diffraction pattern, thermogravimetric analysis, differential scanning calorimeter (DSC), Fourier transform of infrared spectroscopy (FT-IR), and Brunauer-Emmett-Teller (BET) surface area measurements. The photocatalytic degradation was investigated using methyl orange under the irradiation of Hg lamp (λ > 400 nm). The resulting degradation rates of the methyl orange were measured to be as high as 98% in 2 h.

  11. Magnetic ordering and electrical resistivity in Co{sub 0.2}Zn{sub 0.8}Fe{sub 2}O{sub 4} spinel oxide

    Energy Technology Data Exchange (ETDEWEB)

    Bhowmik, R.N. [Experimental Condensed Matter Physics Division, Saha Institute of Nuclear Physics, 1/AF, Bidhannagar, Kolkata 700065 (India)], E-mail: rabindranath.bhowmik@saha.ac.in; Ranganathan, R. [Experimental Condensed Matter Physics Division, Saha Institute of Nuclear Physics, 1/AF, Bidhannagar, Kolkata 700065 (India); Ghosh, B.; Kumar, S. [Department of Physics, Jadavpur University, Kolkata 700 032 (India); Chattopadhyay, S. [Department of Physics, University of Calcutta, 92, A.P.C. Road, Kolkata 700009 (India)

    2008-05-29

    We report the magnetic, Moessbauer spectroscopy and resistivity measurements in order to understand the electronic behaviour of bulk Co{sub 0.2}Zn{sub 0.8}Fe{sub 2}O{sub 4} spinel oxide. The effect of magnetic order on electrical behaviour is observed from the resistivity measurements in the absence and presence of magnetic field. The analysis of Moessbauer spectra suggests the absence of Fe{sup 2+} ions in the system, which implies that complete hopping of charge carriers between localized Fe{sup 3+}/Co{sup 2+} and Fe{sup 2+}/Co{sup 3+} pair of ions in B sublattice is not the favourable mechanism in Co{sub 0.2}Zn{sub 0.8}Fe{sub 2}O{sub 4}. We suggest that electrical behaviour of the present sample may be consistent with a model of fractional charge transfer via Fe{sub B}{sup 3+}-O{sup 2-}-Co{sub B}{sup 2+} superexchange path.

  12. A new high-pressure phase of Fe2SiO4 and the relationship between spin and structural transitions

    Science.gov (United States)

    Yamanaka, T.; Kyono, A.; Nakamoto, Y.; Kharlamova, S. A.; Struzhkin, V. V.; Gramsch, S.; Mao, H.; Hemley, R. J.

    2013-12-01

    Structure transformation of Fe2SiO4 Angle-dispersive powder x-ray diffraction was carried out at beam line 16-BMD APS. Structure of a new high-pressure phase of I-Fe2SiO4 spinel was determined by Rietveld profile fitting of x-ray diffraction data up to 64GPa at ambient temperature. A structural transition from the cubic spinel to the new structure was observed at 34GPa. Diffraction patterns taken at 44.6GPa and 54.6GPa indicate a two-phase mixture of spinel and new high-pressure phase. Reversible transition from I-Fe2SiO4 to spinel was confirmed. Laser heating experiment at 1500K proved the decomposition of Fe2SiO4 spinel to two oxides of FeO and SiO2. Spin transition X-ray emission measurements of Fe2SiO4 were carried out up to 65GPa at ambient temperature at beam line 16-IDD APS. The spin transition exerts an influence to Fe2SiO4 spinel structure and triggers two distinct curves of the lattice constant in the spinel phase. Although the compression curve of the spinel is discontinuous at approximately 20 GPa, Fe Kβ emission measurements show that the transition from a high spin (HS) to an intermediate spin (IS) state begins at 17GPa in the spinel phase. The IS electronic state is gradually enhanced with pressure, which results in an isostructural phase transition. HS-to-LS transition of iron bearing spinels starts from 15.6GPa in Fe3O4 and 19.6GPa in Fe2TiO4. The transition is more capable due to Fe2+ in the octahedral site. The extremely shortened octahedral bonds result in a distortion of 6-fold cation site. New structure of Fe2SiO4 Monte Carlo method was applied to find candidates for the high-pressure phase using the diffraction intensities with fixed lattice constants determined by DICVOL. Rietveld profile fitting was then performed using the initial model. The new structure is a body centered orthorhombic phase (I-Fe2SiO4) with space group Imma and Z=4, with two crystallographically distinct FeO6 octahedra. Silicon exists in six-fold coordination in I-Fe2SiO

  13. Synthesis and magnetic properties of ferrites spinels Mg{sub x}Cu{sub 1-x}Fe{sub 2}O{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Mounkachi, O.; Hamedoun, M. [Institute of Nanomaterials and Nanotechnology, MAScIR, Rabat (Morocco); Belaiche, M. [Institute of Nanomaterials and Nanotechnology, MAScIR, Rabat (Morocco); Hassan II Academy of Science and Technology, Rabat (Morocco); Laboratoire de Magnetisme, Materiaux Magnetiques, Microonde et Ceramique, Ecole Normale Superieure, Universite Mohammed V-Agdal, B.P. 9235, Ocean, Rabat (Morocco); Benyoussef, A. [Institute of Nanomaterials and Nanotechnology, MAScIR, Rabat (Morocco); Hassan II Academy of Science and Technology, Rabat (Morocco); LMPHE, (URAC 12), Faculte des Sciences, Universite Mohammed V-Agdal, Rabat (Morocco); Masrour, R. [Laboratory of Materials, Process, Environment and Quality, Cady Ayad University, National School of Applied Sciences, Safi (Morocco); El Moussaoui, H. [Institute of Nanomaterials and Nanotechnology, MAScIR, Rabat (Morocco); LMPHE, (URAC 12), Faculte des Sciences, Universite Mohammed V-Agdal, Rabat (Morocco); Sajieddine, M., E-mail: hamedoun@hotmail.com [Faculte des Sciences et Techniques, Universite Moulay Slimane, Beni Mellal (Morocco)

    2012-01-01

    Polycrystalline Mg{sub 0.6}Cu{sub 0.4}Fe{sub 2}O{sub 4} ferrites have been prepared using solid-state reaction technique. Their structural and magnetic properties have been studied, using X-ray diffraction and magnetic measurements. Using mean field theory and high-temperature series expansions (HTSE), extrapolated with the pade approximants method, the magnetic properties of Mg{sub 1-x}Cu{sub x}Fe{sub 2}O{sub 4} have been studied. The nearest neighbor super-exchange interactions for intra-site and inter-site of the Mg{sub 1-x}Cu{sub x}Fe{sub 2}O{sub 4} ferrites spinels, in the range 0{<=}x{<=}1, have been computed using the probability approach, based on Moessbauer data. The Curie temperature T{sub c} is calculated as a function of Mg concentration. The obtained theoretical results are in good agreement with experimental ones obtained by magnetic measurements.

  14. Synthesis and electrochemical characterization of nano-CeO2-coated nanostructure LiMn2O4 cathode materials for rechargeable lithium batteries

    International Nuclear Information System (INIS)

    Arumugam, D.; Kalaignan, G. Paruthimal

    2010-01-01

    LiMn 2 O 4 spinel cathode materials were coated with 0.5, 1.0, and 1.5 wt.% CeO 2 by a polymeric process, followed by calcination at 850 o C for 6 h in air. The surface-coated LiMn 2 O 4 cathode materials were physically characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray photoelectron microscopy (XPS). XRD patterns of CeO 2 -coated LiMn 2 O 4 revealed that the coating did not affect the crystal structure or the Fd3m space group of the cathode materials compared to uncoated LiMn 2 O 4 . The surface morphology and particle agglomeration were investigated using SEM, TEM image showed a compact coating layer on the surface of the core materials that had average thickness of about 20 nm. The XPS data illustrated that the CeO 2 completely coated the surface of the LiMn 2 O 4 core cathode materials. The galvanostatic charge and discharge of the uncoated and CeO 2 -coated LiMn 2 O 4 cathode materials were measured in the potential range of 3.0-4.5 V (0.5 C rate) at 30 o C and 60 o C. Among them, the 1.0 wt.% of CeO 2 -coated spinel LiMn 2 O 4 cathode satisfies the structural stability, high reversible capacity and excellent electrochemical performances of rechargeable lithium batteries.

  15. The effect of bismuth on the structure, magnetic and electric properties of Co2MnO4 spinel multiferroic

    Science.gov (United States)

    Chouaya, H.; Smari, M.; Walha, I.; Dhahri, E.; Graça, M. P. F.; Valente, M. A.

    2018-04-01

    Mixed Co2Mn1-xBixO4 (x = 0, x = 0.05 and x = 0.1) samples were prepared by the sol-gel method using the citric acid route and characterized by various techniques. The X-ray diffraction (XRD) and Raman spectroscopic analyses confirmed the formation of inverse spinel cubic structure with Fd 3 ‾ m space group. The introduction of Bismuth (Bi) into Co2MnO4 did not modify the ferrimagnetic character of the parent compound Co2MnO4, whereas the field-cooled magnetizations MFC and the Curie temperature Tc decreased when increasing the Bi content. The electrical properties showed an activation energy (Ea) increase caused by the decrease of the double-exchange interaction following the substitution of Mn3+ by Bi3+. Eventually, the temperature coefficient of resistance (TCR) shows significant values for all samples can be investigated also as good candidates for bolometer applications.

  16. Recycling Spent Primary Cells for the Synthesis of Spinel ZnMn 2 O ...

    African Journals Online (AJOL)

    The mixture was then placed in a fireclay crucible and irradiated in a domestic microwave oven (Pioneer, Model PM-25 L, 2450 MHz, 1000 W) for 20 minutes and reaction products were separated and characterised. Spherical particles of spinel zinc manganese oxide (ZnMn2O4) were isolated after crushing the reduced ...

  17. Mg1-xZnxFe2O4 nanoparticles: Interplay between cation distribution and magnetic properties

    Directory of Open Access Journals (Sweden)

    S. Raghuvanshi

    2018-04-01

    Full Text Available Correlation between cationic distribution, magnetic properties of Mg1-xZnxFe2O4 (0.0 ≤ x ≤ 1.0 ferrite is demonstrated, hardly shown in literature. X-ray diffraction (XRD confirms the formation of cubic spinel nano ferrites with grain diameter between 40.8 to 55.4 nm. Energy dispersive spectroscopy (EDS confirms close agreement of Mg/Fe, Zn/Fe molar ratio, presence of all elements (Mg, Zn, Fe, O, formation of estimated ferrite composition. Zn addition (for Mg shows: i linear increase of lattice parameter aexp, accounted for replacement of an ion with higher ionic radius (Zn > Mg; ii presence of higher population of Fe3+ ions on B site, and unusual occurrence of Zn, Mg on A and B site leads to non-equilibrium cation distribution where we observe inverse to mixed structure, and is in contrast to reported literature where inverse to normal transition is reported; iii effect on A-A, A-B, B-B exchange interactions, affecting coercivity Hc, Ms. A new empirical relation is also obtained showing linear relation between saturation magnetization Ms – inversion parameter δ, oxygen parameter u4¯3m. Non-zero Y-K angle (αYK values implies Y-K type magnetic ordering in the studied samples.

  18. The effect of Y2O3 addition on thermal shock behavior of magnesium aluminate spinel

    Directory of Open Access Journals (Sweden)

    Pošarac Milica

    2009-01-01

    Full Text Available The effect of yttria additive on the thermal shock behavior of magnesium aluminate spinel has been investigated. As a starting material we used spinel (MgAl2O4 obtained by the modified glycine nitrate procedure (MGNP. Sintered products were characterized in terms of phase analysis, densities, thermal shock, monitoring the damaged surface area in the refractory specimen during thermal shock and ultrasonic determination of the Dynamic Young modulus of elasticity. It was found that a new phase between yttria and alumina is formed, which improved thermal shock properties of the spinel refractories. Also densification of samples is enhanced by yttria addition.

  19. Pengaruh Variasi Temperatur Hidrotermal Pada Sintesis Lithium Mangan Oksida (Limn2o4 Spinel Terhadap Efisiensi Adsorpsi Dan Desorpsi Ion Lithium Dari Lumpur Sidoarjo

    Directory of Open Access Journals (Sweden)

    Yusuf Kurniawan

    2014-09-01

    Full Text Available Perkembangan teknologi dalam bidang material menunjukkan perkembangan yang sangat pesat dalam beberapa tahun terakhir.Salah satu material yang sangat dibutuhkan dalam berbagai aplikasi adalah lithium. Lithium sendiri bisa didapatkan dari air laut brines dan geothermal fluid. Salah satunya adalah Lumpur Sidoarjo. Lithium Mangan Oksida Spinel digunakan sebagai material absorben karena murah, tidak beracun dan mudah didapatkan. Pada penelitian ini metode hidrotermal digunakan sebagai metode sintesis pada LiMn2O4 karena dapat dilakukan pada temperatur yang relatif rendah dan menghasilkan partikel yang lebih homogen. Metode hidrotermal dilakukan pada temperatur 160 oC, 180 oC dan 200 oC selama 24 jam. Pengujian XRD dilakukan untuk mengetahui struktur kristal. Pengujian SEM dilakukan untuk mengetahui morfologi material setelah proses hidrotermal. Pengujian BET dilakukan untuk mengetahui surface area. Setelah itu metode acid treatment dilakukan untuk proses adsorpsi dan desorpsi. Adsorpsi dilakukan dengan mencelupkan Lithium Mangan Oksida Spinel yang telah disintesis kedalam Lumpur Sidoarjo.Pengujian ICP dilakukan untuk mengetahui kandungan lithium yang terdapat pada Lumpur Sidoarjo sebelum dan sesudah adsorpsi untuk mengetahui jumlah lithium yang terserap.Pengujian desorpsi dilakukan dengan mencelupkan LiMn2O4 kedalam larutan HCL. Pada uji XRD menunjukkan bahwa LiMn2O4 berstruktur kristal cubic. Dari hasil uji SEM terlihat bahwa tidak banyak perbedaan morfologi pada ketiga variasi.Partikel cenderung membentuk aglomerasi. Pada hasil uji ICP menunjukkan bahwa LiMn2O4 dengan temperatur hidrotermal 160oC memiliki efisiensi adsorpsi paling tinggi dengan 6,775 ppm. Sementara untuk desorpsi yang paling tinggi adalah 200oC sebesar 0.081 ppm

  20. Oxygen vacancies at the spinel/perovskite γ-Al{sub 2}O{sub 3}/SrTiO{sub 3} heterointerface probed by resonant photoelectron spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Schuetz, Philipp; Pfaff, Florian; Zapf, Michael; Gabel, Judith; Dudy, Lenart; Berner, Goetz; Sing, Michael; Claessen, Ralph [Physikalisches Institut and Roentgen Center for Complex Material Systems (RCCM), Universitaet Wuerzburg (Germany); Chen, Yunzhong; Pryds, Nini [Department of Energy Conversion and Storage, Technical University of Denmark, Risoe (Denmark); Schlueter, Christoph; Lee, Tien-Lin [Diamond Light Source Ltd., Harwell Science and Innovation Campus, Didcot (United Kingdom)

    2016-07-01

    The spinel/perovskite heterointerface between the band insulators γ-Al{sub 2}O{sub 3} and SrTiO{sub 3} hosts a two-dimensional electron system (2DES) with exceptionally high electron mobility. Soft x-ray resonant photoelectron spectroscopy at the Ti L absorption edge is used to probe the Ti 3d derived interface states. Marked differences in the resonance behavior are found for the SrTiO{sub 3} valence band and the different interface states, which are observed in the band gap of SrTiO{sub 3}. A comparison to X-ray absorption spectra of Ti 3d{sup 0} and Ti 3d{sup 1} systems reveals the presence of different types of electronic states with Ti 3d character, i.e., oxygen vacancy induced, trapped in-gap states and itinerant states contributing to the 2DES. Exposure to low doses of oxygen during irradiation allows for the reversible manipulation of the oxygen stoichiometry, thus revealing the presence of an oxygen vacancy-induced state, which is characteristic for this spinel/perovskite interface.

  1. Surface enrichment of Pt in stable Pt-Ir nano-alloy particles on MgAl 2 O 4 spinel in oxidizing atmosphere

    Energy Technology Data Exchange (ETDEWEB)

    Li, Weizhen; Nie, Lei; Chen, Ying; Kovarik, Libor; Liu, Jun; Wang, Yong

    2017-04-01

    With the capability of MgAl2O4 spinel {111} nano-facets in stabilizing small Rh, Ir and Pt particles, bimetallic Ir-Pt catalysts on the same support were investigated, aiming at further lowering the catalyst cost by substituting expensive Pt with cheaper Ir in the bulk. Small Pt-Ir nano-alloy particles (< 2nm) were successfully stabilized on the spinel {111} nano-facets as expected. Interestingly, methanol oxidative dehydrogenation (ODH) rate on the surface Pt atoms increases with oxidizing aging but decreases upon reducing treatment, where Ir is almost inactive under the same reaction conditions. Up to three times enhancement in Pt exposure was achieved when the sample was oxidized at 800 °C in air for 1 week and subsequently reduced by H2 for 2 h, demonstrating successful surface enrichment of Pt on Pt-Ir nano-alloy particles. A dynamic stabilization mechanism involving wetting\

  2. Spinel-structured surface layers for facile Li ion transport and improved chemical stability of lithium manganese oxide spinel

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Hae Ri [Center for Energy Convergence Research, Korea Institute of Science Technology, Hwarang-ro 14-gil 5, Seongbuk-gu, Seoul 136-791 (Korea, Republic of); Department of Chemical and Biological Engineering, Korea University, 145, Anam-ro, Seongbuk-gu, Seoul 136-701 (Korea, Republic of); Seo, Hyo Ree; Lee, Boeun; Cho, Byung Won [Center for Energy Convergence Research, Korea Institute of Science Technology, Hwarang-ro 14-gil 5, Seongbuk-gu, Seoul 136-791 (Korea, Republic of); Lee, Kwan-Young [Department of Chemical and Biological Engineering, Korea University, 145, Anam-ro, Seongbuk-gu, Seoul 136-701 (Korea, Republic of); Oh, Si Hyoung, E-mail: sho74@kist.re.kr [Center for Energy Convergence Research, Korea Institute of Science Technology, Hwarang-ro 14-gil 5, Seongbuk-gu, Seoul 136-791 (Korea, Republic of)

    2017-01-15

    Graphical abstract: Strategically-designed spinel-structured nano-scale surface layer, LiM{sub x}Mn{sup IV}{sub 1−x}O{sub 4}, featuring a high Li{sup +} ion conductivity and a good chemical stability was applied on Al-doped LiMn{sub 2}O{sub 4} spinel for the drastic improvement of the electrochemical performance at the elevated temperature as a promising cathode material for lithium rechargeable batteries. - Highlights: • Spinel-structured surface layer with a high Li-ion conductivity and a good chemical stability was prepared. • Simple wet process was developed to apply nano-scale surface layer on aluminum doped lithium manganese oxide spinel. • The properties of nano-scale surface layer were characterized by analytical tools including GITT, HR-TEM and XAS. • Materials with surface coating layer exhibit an excellent electrochemical performance at the elevated temperature. - Abstract: Li-ion conducting spinel-structured oxide layer with a manganese oxidation state close to being tetravalent was prepared on aluminum-doped lithium manganese oxide spinel for improving the electrochemical performances at the elevated temperatures. This nanoscale surface layer provides a good ionic conduction path for lithium ion transport to the core and also serves as an excellent chemical barrier for protecting the high-capacity core material from manganese dissolution into the electrolyte. In this work, a simple wet process was employed to prepare thin LiAlMnO{sub 4} and LiMg{sub 0.5}Mn{sub 1.5}O{sub 4} layers on the surface of LiAl{sub 0.1}Mn{sub 1.9}O{sub 4}. X-ray absorption studies revealed an oxidation state close to tetravalent manganese on the surface layer of coated materials. Materials with these surface coating layers exhibited excellent capacity retentions superior to the bare material, without undermining the lithium ion transport characteristics and the high rate performances.

  3. Electrochemical properties of LiMn2O4 cathode material doped with an actinide

    International Nuclear Information System (INIS)

    Eftekhari, Ali; Moghaddam, Abdolmajid Bayandori; Solati-Hashjin, Mehran

    2006-01-01

    Metal substation as an efficient approach for improvement of battery performance of LiMn 2 O 4 was performed by an actinide dopant. Uranium as the last natural element and most common actinide was employed for this purpose. Cyclic voltammetric studies revealed that incorporation of uranium into LiMn 2 O 4 spinel significantly improves electrochemical performance. It also strengthens the spinel stability to exhibit better cycleability. Surprisingly, the capacity increases upon cycling of LiU 0.01 Mn 1.99 O 4 cathode. This inverse behavior is attributed to uniform distribution of dopant during insertion/extraction process. In other words, this is an electrochemical refinement of the nanostructure which is not detectable in microscale morphology, as rearrangement of dopant in nanoscale occurs and this is an unexceptional nanostructural ordering. In addition, uranium doping strengthens the Li diffusion, particularly at redox potentials

  4. Mechanosynthesis of MFe2O4 (M = Co, Ni, and Zn Magnetic Nanoparticles for Pb Removal from Aqueous Solution

    Directory of Open Access Journals (Sweden)

    America R. Vazquez-Olmos

    2016-01-01

    Full Text Available Adsorption of Pb(II from aqueous solution using MFe2O4 nanoferrites (M = Co, Ni, and Zn was studied. Nanoferrite samples were prepared via the mechanochemical method and were characterized by X-ray powder diffraction (XRD, Fourier transform infrared spectroscopy (FTIR, micro-Raman, and vibrating sample magnetometry (VSM. XRD analysis confirms the formation of pure single phases of cubic ferrites with average crystallite sizes of 23.8, 19.4, and 19.2 nm for CoFe2O4, NiFe2O4, and ZnFe2O4, respectively. Only NiFe2O4 and ZnFe2O4 samples show superparamagnetic behavior at room temperature, whereas CoFe2O4 is ferromagnetic. Kinetics and isotherm adsorption studies for adsorption of Pb(II were carried out. A pseudo-second-order kinetic describes the sorption behavior. The experimental data of the isotherms were well fitted to the Langmuir isotherm model. The maximum adsorption capacity of Pb(II on the nanoferrites was found to be 20.58, 17.76, and 9.34 mg·g−1 for M = Co, Ni, and Zn, respectively.

  5. Micro-XANES measurements on experimental spinels and the oxidation state of vanadium in coexisting spinel and silicate melt

    International Nuclear Information System (INIS)

    Righter, K.; Sutton, S.R.; Newville, M.; Le, L.; Schwandt, C.S.

    2006-01-01

    We show that experimental spinels coexisting with silicate melt always have lower valence vanadium, and that spinels typically have 3+, whereas the coexisting melt has 4+ or 5+. Implications of these results for planetary basalts will be discussed. Spinel can be a significant host phase for V which has multiple oxidation states V 2+ , V 3+ , V 4+ or V 5+ at oxygen fugacities relevant to natural systems. The magnitude of D(V) spinel/melt is known to be a function of composition, temperature and fO 2 , but the uncertainty of the oxidation state under the range of natural conditions has made elusive a thorough understanding of D(V) spinel/melt. For example, V 3+ is likely to be stable in spinels, based on exchange with Al in experiments in the CaO-MgO-Al 2 O 3 -SiO 2 system. On the other hand, it has been argued that V 4+ will be stable across the range of natural oxygen fugacities in nature. In order to build on our previous work in more oxidized systems, we have carried out experiments at relatively reducing conditions from the FMQ buffer to 2 log fO 2 units below the IW buffer. These spinel-melt pairs, where V is present in the spinel at natural levels (∼300 ppm V), were analyzed using an electron microprobe at NASA-JSC and mi-cro-XANES at the Advanced Photon Source at Argonne National Laboratory. The new results will be used together with previous results to understand the valence of V in spinel-melt systems across 12 orders of magnitude of oxygen fugacity, and with application to natural systems.

  6. Physical investigations on NiMn{sub 2}O{sub 4} sprayed magnetic spinel for sensitivity applications

    Energy Technology Data Exchange (ETDEWEB)

    Larbi, T.; Amara, A.; Ouni, B. [Unité de physique des dispositifs a semi-conducteurs, Faculté des sciences de Tunis, Tunis El Manar University, 2092 Tunis (Tunisia); Inoubli, A. [Faculté des Sciences de Bizerte Laboratoire de Physique des Matériaux Département de Physique, Zarzouna, 7021 Bizerte (Tunisia); Karyaoui, M. [Laboratoire de photovoltaïque, Centre de Recherches et des Technologies de l’Énergie, Technopole de Borj-Cédria BP 95, 2050 Hammam-Lif (Tunisia); Yumak, A. [Physics Department, Faculty of Arts and Sciences, Marmara University, Göztepe, 34722 Istanbul (Turkey); Saadallah, F. [Phothermal laboratory IPEIN, Mrezka, BP 62, 8000 Nabeul (Tunisia); Boubaker, K., E-mail: mmbb11112000@yahoo.fr [Unité de physique des dispositifs a semi-conducteurs, Faculté des sciences de Tunis, Tunis El Manar University, 2092 Tunis (Tunisia); Amlouk, M. [Unité de physique des dispositifs a semi-conducteurs, Faculté des sciences de Tunis, Tunis El Manar University, 2092 Tunis (Tunisia)

    2015-08-01

    NiMn{sub 2}O{sub 4} ternary nickel manganese oxide thin films spinels have been grown on glass substrates at 350 °C through spray pyrolysis technique. X-ray diffraction and Raman spectroscopy analyses show that the synthesized film has mainly cubic spinel structure with a preferred orientation along (111) plane. Some optical constants such as the refractive index (n), extinction coefficient (k), Urbach energy (E{sub U}=342 eV) and optical energy band gap (E{sub g}=1.07 eV) have been calculated from reflection-transmission spectra. The mirage effect technique has been used to estimate the thermal conductivity (K{sub c}). Its value is K{sub c}=25 W m{sup −1} K{sup −1}. The real part of the ac the conductivity behaviour has been investigated in the frequency range 100 Hz to 1 MHz. It was found that the real conductivity follows a power law (Aω{sup s}). The dc conductivity has been studied in the temperature range from 250 °C to 375 °C and supports the variable range hopping model proposed by Mott. The activation energy value estimated from the relaxation frequency is Ea~0.32 eV. Moreover, the temperature dependency of the resistance indicates that conduction was well described by a variable range hopping model, in which electron transfer takes place between Mn{sup 3+} and Mn{sup 4+} ions. - Highlights: • The nickel manganese oxide (NiMn{sub 2}O{sub 4}) has been prepared by the low-cost spray pyrolysis technique. • The optical band gap of this ternary oxide is around 1 eV and the crystallites are oriented preferentially along (111) direction. • Presenting an accurate technique “Mirage effect” for original investigation of thermal properties. • DC and AC conductivity can be both attributed to a hopping transport, while at high frequency a metallic-like behavior is observed. • A deep analysis within correlated barrier hopping (CBH) model was carried out. • Outlining a correlation between Magnetic and electrical properties.

  7. Valence states and occupation sites in (Fe,Mn){sub 3}O{sub 4} spinel oxides investigated by soft x-ray absorption spectroscopy and magnetic circular dichroism

    Energy Technology Data Exchange (ETDEWEB)

    Lee, H J; Kim, G; Kim, D H; Kang, J-S [Department of Physics, Catholic University of Korea (CUK), Bucheon 420-743 (Korea, Republic of); Zhang, C L; Cheong, S-W [Rutgers Center for Emergent Materials and Department of Physics, Rutgers University, Piscataway, NJ 08854 (United States); Shim, J H; Lee, Soonchil [Department of Physics, KAIST, Daejeon 305-701 (Korea, Republic of); Lee, Hangil; Kim, J-Y [Pohang Accelerator Laboratory (PAL), POSTECH, Pohang 790-784 (Korea, Republic of); Kim, B H; Min, B I [Department of Physics, POSTECH, Pohang 790-784 (Korea, Republic of)], E-mail: kangjs@catholic.ac.kr

    2008-07-23

    The electronic structures of (Fe,Mn){sub 3}O{sub 4} spinel oxides have been investigated by employing soft-x-ray absorption spectroscopy (XAS) and soft x-ray magnetic circular dichroism (XMCD). We have determined the valence states as well as the occupation sites of Mn and Fe ions in Fe{sub 0.9}Mn{sub 2.1}O{sub 4} and MnFe{sub 2}O{sub 4}. Fe{sub 0.9}Mn{sub 2.1}O{sub 4} is found to be close to the inverse spinel (the inversion parameter y{approx}0.85), while MnFe{sub 2}O{sub 4} is close to the normal spinel (y{approx}0.2). In Fe{sub 0.9}Mn{sub 2.1}O{sub 4}, Fe ions are mainly trivalent and the majority of Fe{sup 3+} ions occupy the octahedral B sites, while Mn ions are mixed-valent with approximately 45% Mn{sub A}{sup 2+} at the tetrahedral A sites and 55% Mn{sub B}{sup 3+} ions at the octahedral B sites. In MnFe{sub 2}O{sub 4}, Mn ions are mainly divalent and the majority of Mn{sup 2+} ions occupy the tetrahedral A sites, while Fe ions are mainly trivalent and the majority of Fe{sup 3+} ions occupy the octahedral B sites.

  8. Mechanical characterization of magnesium aluminate MgO·nAl2O3 spinel single crystals irradiated with Cu- ions

    International Nuclear Information System (INIS)

    Ohmura, Takahito; Lee, Chi-Gyu; Kishimoto, Naoki

    2003-01-01

    Ion-irradiation response of spinel single crystals was investigated using a nanoindentation technique. Specimens of stoichiometric (n=1) and non-stoichiometric (n=2.4) single crystals of MgO n(Al 2 O 3 ) spinel were irradiated with 60 keV Cu - ion at room temperature. Dose rate ranged from 1 to 100 μA/cm 2 , and a total dose was kept constant at 3x10 16 ions/cm 2 . Both plastic hardness and elastic modulus of all the irradiated specimens were softened. Radiation-induced swelling simultaneously occurred. Rutherford back scattering spectroscopy detected disordering of spinel crystalline structure. Accordingly, the radiation-induced softening and swelling are ascribed to accumulation of point defects associated with the disordering. In comparison between the stoichiometric and the non-stoichiometric specimens, the radiation-induced softening is suppressed in the non-stoichiometric composition. (author)

  9. Cellulose-precursor synthesis of nanocrystalline Co0.5Cu0.5Fe2O4 spinel ferrites

    International Nuclear Information System (INIS)

    Ounnunkad, Kontad; Phanichphant, Sukon

    2012-01-01

    Highlights: ► Synthesis of spinel copper cobalt nanoferrite particles from a cellulose precursor for the first time. Control of nanosize and properties of nanoferrites can take place by varying the calcining temperature. The simple, low cost, easy cellulose process is a choice of nanoparticle processing technology. -- Abstract: Nanocrystalline Cu 0.5 Co 0.5 Fe 2 O 4 powders were prepared via a metal-cellulose precursor synthetic route. Cellulose was used as a fuel and a dispersing agent. The resulting precursors were calcined in the temperature range of 450–600 °C. The phase development of the samples was determined by using Fourier transform infrared (FT-IR) spectroscopy and powder X-ray diffraction (XRD). The field-dependent magnetizations of the nanopowders were measured by vibrating sample magnetometer (VSM). All XRD patterns are of a spinel ferrite with cubic symmetry. Microstructure of the ferrites showed irregular shapes and uniform particles with agglomeration. From XRD data, the crystallite sizes are in range of 16–42 nm. Saturation magnetization and coercivity increased with increasing calcining temperature due to enhancement of crystallinity and reduction of oxygen vacancies.

  10. Synthesis and sonocatalytic performance of a ternary magnetic MIL-101(Cr)/RGO/ZnFe2O4 nanocomposite for degradation of dye pollutants.

    Science.gov (United States)

    Nirumand, Ladan; Farhadi, Saeed; Zabardasti, Abedin; Khataee, Alireza

    2018-04-01

    In this study, new ternary magnetic MIL-101(Cr)/RGO/ZnFe 2 O 4 catalyst (with 30% wt of ZnFe 2 O 4 ) was synthesized via a hydrothermal route for sonodegradation of organic dyes. The structural, optical and magnetic properties of the nanocomposite were detected by means of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), UV-visible spectroscopy (UV-visible), field emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX) spectroscopy, vibrating sample magnetometer (VSM), atomic force microscopy (AFM), Raman spectroscopy and BET surface area analysis. To evaluate the sonocatalytic activity of the as-prepared MIL-101(Cr)/RGO/ZnFe 2 O 4 nanocomposite, the H 2 O 2 -assisted degradation of organic dyes such as congo red (CR), methylene blue (MB), Rhodamine B (RhB) and methyl orange (MO) in aqueous solution was studied under ultrasound irradiation. The obtained results indicated that the ternary MIL-101(Cr)/RGO/ZnFe 2 O 4 nanocomposite had better performance for sonodegradation of these dyes than MIL-101(Cr)/RGO, pure MIL-101(Cr) or ZnFe 2 O 4 . The enhanced sonocatalytic performance of the as-prepared ternary nanocomposite could be attributed to the fast generation and separation of charge carriers (electrons and holes) in ZnFe 2 O 4 and MIL-101(Cr) and their transfer to the surface of graphene sheets. Moreover, the relatively high specific surface area of the MIL-101(Cr)/rGO and magnetic property of ZnFe 2 O 4 improve the degradation efficiency of the dyes. The recovery of the ternary magnetic sonocatalyst from treated water could be easily achieved using an external magnetic field. The main influence factors on the sonocatalytic activity such as catalyst dosage and dye initial concentration were also investigated. The trapping experiments indicated that OH radicals are the prominent active species in dye degradation. In addition, the reusability test, was also carried out to ensure the stability of the employed sonocatalyst

  11. Enhancement photocatalytic activity of spinel oxide (Co, Ni3O4 by combination with carbon nanotubes

    Directory of Open Access Journals (Sweden)

    Kahdum Bashaer J.

    2017-09-01

    Full Text Available In this study, some types of composites consisting of multi-walled carbon nanotubes (MWCNTs and spinel oxide (Co, Ni3O4 were synthesized by simple evaporation method. These composites were characterized by UV–Vis diffuse reflectance spectroscopy, X-rays diffraction(XRD, Scanning electron microscopy (SEM and specific surface area(SBET. The photocatalytic activity of the prepared composites was investigated by the following removal of Bismarck brown G (BBG dye from its aqueous solutions. The obtained results showed that using MWCNTs in combination with spinel oxide to produced composites (spinel/MWCNTs which succeeded in increasing the activity of spinel oxide and exhibited higher photocatalytic activity than spinel oxide alone. Also it was found that, multiwalled carbon nanotubes were successful in increasing the adsorption and improving the activity of photocatalytic degradation of Bismarck brown G dye(BBG. The obtained results showed that spinel/MWCNTs was more active in dye removal in comparison with each of spinel oxide and MWCNTs alone under the same reaction conditions. Also band gap energies for the prepared composites showed lower values in comparison with neat spinel. This point represents a promising observation as these composites can be excited using a lower energy radiation sources.

  12. Synthesis and property of spinel porous ZnMn2O4 microspheres

    Science.gov (United States)

    Guo, N.; Wei, X. Q.; Deng, X. L.; Xu, X. J.

    2015-11-01

    Mesoporous ternary zinc manganese oxides on the Ti sheet substrate are prepared by easy and fast hydrothermal method for the first time. The obtained ZnMn2O4 materials with homogenously distributed pores have been characterized by XRD, SEM and Raman spectra, which show the good crystal phase and particles for improving supercapacitive performance. XRD and SEM images show that the as-prepared samples have good crystallinity, and ZnMn2O4 microsphere has an average diameter of 10 μm. In addition, ZnMn2O4 are also characterized in 2 M KOH solution using three-electrode system. In the work, we study that different substrates (Ti, carbon and nickel foam) have an important effect on the electrochemical performance of the samples. The research of cyclic voltammogram (CV) indicates that the obtained specific capacitance (155 F g-1) values on nickel foam substrate for the ZnMn2O4 microspheres are higher than the values reported for some inexpensive oxides. However, the specific capacitance of all ZnMn2O4 samples has almost no change at two different scan rates which shows good long-term cycling stability. The electrochemical impedance spectroscopy with a small resistance reveals that the as-synthesized samples have good frequency response characteristics. These results indicate that the unique ZnMn2O4 electrode would be a promising electrode for high-performance supercapacitor applications.

  13. ZnFe{sub 2}O{sub 4} antiferromagnetic structure redetermination

    Energy Technology Data Exchange (ETDEWEB)

    Kremenović, Aleksandar, E-mail: akremenovic@rgf.bg.ac.rs [Laboratory for Crystallography, Faculty of Mining and Geology, University of Belgrade, Đušina 7, Belgrade 11000 (Serbia); Antić, Bratislav [Condensed Matter Physics Laboratory, Institute of Nuclear Sciences “Vinča”, University of Belgrade, P.O. Box 522, Belgrade 11001 (Serbia); Vulić, Predrag [Laboratory for Crystallography, Faculty of Mining and Geology, University of Belgrade, Đušina 7, Belgrade 11000 (Serbia); Blanuša, Jovan [Condensed Matter Physics Laboratory, Institute of Nuclear Sciences “Vinča”, University of Belgrade, P.O. Box 522, Belgrade 11001 (Serbia); Tomic, Aleksandra [Condensed Matter Physics Laboratory, Institute of Nuclear Sciences “Vinča”, University of Belgrade, P.O. Box 522, Belgrade 11001 (Serbia); Department of Applied Physics and Applied Mathematics, Columbia University, New York, NY, 10027 (United States)

    2017-03-15

    Magnetic structure of ZnFe{sub 2}O{sub 4} normal spinel is re-examined. Antiferromagnetic structure non-collinear model is established within C{sub a}2 space group having four different crystallographic/magnetic sites for 32 Fe{sup 3+} spins within magnetic unit cell. - Highlights: • Magnetic structure of ZnFe{sub 2}O{sub 4} normal spinel is re-examined. • Antiferromagnetic non-collinear structure model is established within C{sub a}2 space group. • Four different crystallographic/magnetic sites contain 32 Fe{sup 3+} spins within magnetic unit cell.

  14. NiCo2O4-Based Supercapacitor Nanomaterials

    Science.gov (United States)

    Wang, Chenggang; Zhou, E; He, Weidong; Deng, Xiaolong; Huang, Jinzhao; Ding, Meng; Wei, Xianqi; Liu, Xiaojing; Xu, Xijin

    2017-01-01

    In recent years, the research on supercapacitors has ushered in an explosive growth, which mainly focuses on seeking nano-/micro-materials with high energy and power densities. Herein, this review will be arranged from three aspects. We will summarize the controllable architectures of spinel NiCo2O4 fabricated by various approaches. Then, we introduce their performances as supercapacitors due to their excellent electrochemical performance, including superior electronic conductivity and electrochemical activity, together with the low cost and environmental friendliness. Finally, the review will be concluded with the perspectives on the future development of spinel NiCo2O4 utilized as the supercapacitor electrodes. PMID:28336875

  15. NiCo2O4-Based Supercapacitor Nanomaterials

    Directory of Open Access Journals (Sweden)

    Chenggang Wang

    2017-02-01

    Full Text Available In recent years, the research on supercapacitors has ushered in an explosive growth, which mainly focuses on seeking nano-/micro-materials with high energy and power densities. Herein, this review will be arranged from three aspects. We will summarize the controllable architectures of spinel NiCo2O4 fabricated by various approaches. Then, we introduce their performances as supercapacitors due to their excellent electrochemical performance, including superior electronic conductivity and electrochemical activity, together with the low cost and environmental friendliness. Finally, the review will be concluded with the perspectives on the future development of spinel NiCo2O4 utilized as the supercapacitor electrodes.

  16. Evaluation of the magnetic properties of hybrids MnFe{sub 2}O{sub 4}/SiO{sub 2} /chitosan aiming its application as biosensors; Avaliacao das propriedades magneticas de hibridos MnFe{sub 2}O{sub 4}/SiO{sub 2}/quitosana visando sua aplicacao como biosensores

    Energy Technology Data Exchange (ETDEWEB)

    Leal, E.; Santos, P.T. A.; Costa, F.M., E-mail: elvialeal@gmail.com [Universidade Federal de Campina Grande (LabSMaC/UFCG), PB (Brazil). Laboratorio de Sintese de Materiais Ceramicos; Barbosa, D.C. [Universidade Federal de Alagoas (UFAL), Maceio, AL (Brazil). Instituto de Quimica e Biotecnologia; Cornejo, D.R. [Universidade de Sao Paulo (USP), SP (Brazil). Instituto de Fisica; Kiminami, R.H.G.A. [Universidade Federal de Sao Carlos (UFSCar), SP (Brazil). Departamento de Engenharia de Materiais

    2014-07-01

    Magnetic nanoparticles have potential application in biomedicine since their features allow a wide variety of applications, such as biosensors, drug carriers, destruction of tumor cells and magnetic separation of cells and proteins. Overlooking that, the proposal is to obtain the hybrid MnFe{sub 2}O{sub 4}/SiO{sub 2}/ chitosan, to evaluate it as its magnetic property, aiming to obtain a biocompatible hybrid for biological applications, such as, e.g., biosensors. The samples were analyzed by XRD, FTIR, SEM and magnetic measurements. The results revealed that the samples of pure MnFe{sub 2}O{sub 4}, silanized and with chitosan presented the formation of the spinel with crystallite sizes of 77, 80 and 79 nm, respectively. The FTIR spectra confirmed the presence of characteristic absorption bands of the spinel and groups present in silanol and chitosan, confirming the formation of the hybrid. The silane introduction kept the ferrimagnetic characteristic of the material and led to a slight increase in the saturation magnetization, going from 55 to 61 emu/g. (author)

  17. Magnetic properties of Co{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} spinel ferrite nanoparticles synthesized by starch-assisted sol–gel autocombustion method and its ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Yadav, Raghvendra Singh, E-mail: yadav@fch.vutbr.cz [Materials Research Centre, Brno University of Technology, Purkyňova 464/118, 61200 Brno (Czech Republic); Havlica, Jaromir [Materials Research Centre, Brno University of Technology, Purkyňova 464/118, 61200 Brno (Czech Republic); Hnatko, Miroslav; Šajgalík, Pavol [Institute of Inorganic Chemistry, Slovak Academy of Sciences, Dúbravská cesta 9, SK-845 36 Bratislava (Slovakia); Alexander, Cigáň [Institute of Measurement Science, Slovak Academy of Sciences, Dúbravská cesta 9, SK-841 04 Bratislava (Slovakia); Palou, Martin; Bartoníčková, Eva; Boháč, Martin; Frajkorová, Františka; Masilko, Jiri; Zmrzlý, Martin; Kalina, Lukas; Hajdúchová, Miroslava; Enev, Vojtěch [Materials Research Centre, Brno University of Technology, Purkyňova 464/118, 61200 Brno (Czech Republic)

    2015-03-15

    In this article, Co{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} (x=0.0 and 0.5) spinel ferrite nanoparticles were achieved at 800 °C by starch-assisted sol–gel autocombustion method. To further reduce the particle size, these synthesized ferrite nanoparticles were ball-milled for 2 h. X-ray diffraction patterns demonstrated single phase formation of Co{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} (x=0.0 and 0.5) spinel ferrite nanoparticles. FE-SEM analysis indicated the nanosized spherical particles formation with spherical morphology. The change in Raman modes and relative intensity were observed due to ball milling and consequently decrease of particle size and cationic redistribution. An X-ray Photoelectron Spectroscopy (XPS) result indicated that Co{sup 2+}, Zn{sup 2+} and Fe{sup 3+} exist in octahedral and tetrahedral sites. The cationic redistribution of Zn{sup 2+} and consequently Fe{sup 3+} occurred between octahedral and tetrahedral sites after ball-milling. The change in saturation magnetization (M{sub s}) and coercivity (H{sub c}) with decrease of nanocrystalline size and distribution of cations in spinel ferrite were observed. - Highlights: • Co{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} spinel ferrite nanoparticles. • Starch-assisted sol–gel auto-combustion method. • Effect of ball-milling on particle size and cation distribution. • Magnetic property dependent on cations and particle size.

  18. Crystallographic origin of cycle decay of the high-voltage LiNi0.5Mn1.5O4 spinel lithium-ion battery electrode.

    Science.gov (United States)

    Pang, Wei Kong; Lu, Cheng-Zhang; Liu, Chia-Erh; Peterson, Vanessa K; Lin, Hsiu-Fen; Liao, Shih-Chieh; Chen, Jin-Ming

    2016-06-29

    High-voltage spinel LiNi0.5Mn1.5O4 (LNMO) is considered a potential high-power-density positive electrode for lithium-ion batteries, however, it suffers from capacity decay after extended charge-discharge cycling, severely hindering commercial application. Capacity fade is thought to occur through the significant volume change of the LNMO electrode occurring on cycling, and in this work we use operando neutron powder diffraction to compare the structural evolution of the LNMO electrode in an as-assembled 18650-type battery containing a Li4Ti5O12 negative electrode with that in an identical battery following 1000 cycles at high-current. We reveal that the capacity reduction in the battery post cycling is directly proportional to the reduction in the maximum change of the LNMO lattice parameter during its evolution. This is correlated to a corresponding reduction in the MnO6 octahedral distortion in the spinel structure in the cycled battery. Further, we find that the rate of lattice evolution, which reflects the rate of lithium insertion and removal, is ∼9 and ∼10% slower in the cycled than in the as-assembled battery during the Ni(2+)/Ni(3+) and Ni(3+)/Ni(4+) transitions, respectively.

  19. Stress Induced Charge-Ordering Process in LiMn_2O_4

    International Nuclear Information System (INIS)

    Chen, Yan; Yu, Dunji; An, Ke

    2016-01-01

    In this letter we report the stress-induced Mn charge-ordering process in the LiMn_2O_4 spinel, evidenced by the lattice strain evolutions due to the Jahn–Teller effects. In situ neutron diffraction reveals the initial stage of this process at low stress, indicating the eg electron localization at the preferential Mn sites during the early phase transition as an underlying charge-ordering mechanism in the charge-frustrated LiMn_2O_4. The initial stage of this transition exhibits as a progressive lattice and charge evolution, without showing a first-order behavior.

  20. A facile enhancement in battery-type of capacitive performance of spinel NiCo2O4 nanostructure via directly tuning thermal decomposition temperature

    International Nuclear Information System (INIS)

    Jiang, Shu; Sun, Yujing; Dai, Haichao; Ni, Pengjuan; Lu, Wangdong; Wang, Yilin; Li, Zhen; Li, Zhuang

    2016-01-01

    A facile, low cost and time-saving method to synthesize porous NiCo 2 O 4 nanoplatelet and nanorod structures is developed via a simple two-step route. A flakes assembled precursor containing Ni-Co hydroxides is firstly prepared via a facile, low-cost chemical bath coprecipitation process only using diluted ammonia solution as a precipitant to govern over the nucleation, growth, and agglomeration processes.Then, porous NiCo 2 O 4 nanoplatelet and nanorod structures are successfully obtained through pyrolyzing the above precursor. The influence of the calcination temperature is mainly studied on the pyrolysis reaction. The calcination temperature has statistically significant effects on the morphology and structure evolution, crystallinity, electronic conductivity and the electrochemical performances of the products. The optimized, nanoplatelet predominated NiCo 2 O 4 spinel, calcinated at 300 ∘C for 6 h (denoted as NC300), has excellent crystallinity and electric conductivity. It shows a superior-specific capacitance of 1362F g −1 at a current density of 1 A g −1 .When the current density increases to 16 A g −1 , the specific capacity still retains 964 F g −1 (70.8% capacity retention). Ragone plot indicates maximum energy density of our porous NC300 electrode is 75.67 W h kg −1 at a power density of 499.82 W kg −1 . Cycle-life tests show that the specific capacitance of NC300 is nearly stable between 300 and 1500 cycles, indicating its potential use in energy-storage field.The simplicity and practicability of the modified pyrolysis process may facilitate the successful commercial applications in electrochemical capacitors for nanostructured NiCo 2 O 4 spinel.

  1. Magnetic properties of nanostructured CuFe2O4

    DEFF Research Database (Denmark)

    Jiang, Jianzhong; Goya, G.F.; Rechenberg, H.R.

    1999-01-01

    The structural evolution and magnetic properties of nanostructured copper ferrite, CuFe2O4, have been investigated by X-ray diffraction, Mossbauer spectroscopy, and magnetization measurements. Nanometre-sized CuFe2O4 particles with a partially inverted spinel structure were synthesized by high...

  2. Facile Synthesis of Carbon-Coated Spinel Li4Ti5O12/Rutile-TiO2 Composites as an Improved Anode Material in Full Lithium-Ion Batteries with LiFePO4@N-Doped Carbon Cathode.

    Science.gov (United States)

    Wang, Ping; Zhang, Geng; Cheng, Jian; You, Ya; Li, Yong-Ke; Ding, Cong; Gu, Jiang-Jiang; Zheng, Xin-Sheng; Zhang, Chao-Feng; Cao, Fei-Fei

    2017-02-22

    The spinel Li 4 Ti 5 O 12 /rutile-TiO 2 @carbon (LTO-RTO@C) composites were fabricated via a hydrothermal method combined with calcination treatment employing glucose as carbon source. The carbon coating layer and the in situ formed rutile-TiO 2 can effectively enhance the electric conductivity and provide quick Li + diffusion pathways for Li 4 Ti 5 O 12 . When used as an anode material for lithium-ion batteries, the rate capability and cycling stability of LTO-RTO@C composites were improved in comparison with those of pure Li 4 Ti 5 O 12 or Li 4 Ti 5 O 12 /rutile-TiO 2 . Moreover, the potential of approximately 1.8 V rechargeable full lithium-ion batteries has been achieved by utilizing an LTO-RTO@C anode and a LiFePO 4 @N-doped carbon cathode.

  3. Attestation in self-propagating combustion approach of spinel AFe{sub 2}O{sub 4} (A = Co, Mg and Mn) complexes bearing mixed oxidation states: Magnetostructural properties

    Energy Technology Data Exchange (ETDEWEB)

    Bennet, J., E-mail: b.eenneett@gmail.com [Department of Physics, College of Engineering, Guindy, Anna University, Sardar Patel Road, Chennai,600025 (India); Tholkappiyan, R. [Department of Physics, College of Engineering, Guindy, Anna University, Sardar Patel Road, Chennai,600025 (India); Department of Physics, College of Science, UAE University, Al Ain 15551 (United Arab Emirates); Vishista, K.; Jaya, N. Victor [Department of Physics, College of Engineering, Guindy, Anna University, Sardar Patel Road, Chennai,600025 (India); Hamed, Fathalla [Department of Physics, College of Science, UAE University, Al Ain 15551 (United Arab Emirates)

    2016-10-15

    Highlights: • Spinel type ferrite compounds AFe{sub 2}O{sub 4} (A = Co, Mg and Mn) have been successfully prepared by self-propagating combustion method using glycine as fuel. • To investigate and confirms the presence of phases in the synthesized ferrite nanoparticles by XRD and FTIR analysis. • The formation of mixed oxidation state of cobalt (Co{sup 2+} and Co{sup 3+}), iron (Fe{sup 2+} and Fe{sup 3+}) and manganese (Mn{sup 2+} and Mn{sup 3+}) ions were studied and confirmed from XPS analysis. • The magnetic properties of the synthesized ferrites were studied by VSM measurement. - Abstract: Spinel type nano-sized ferrite compounds AFe{sub 2}O{sub 4} (A = Co, Mg and Mn) have been successfully prepared by self-propagating combustion method using glycine as fuel at 400 °C under air atmosphere for 4 h. The crystal structure, chemical composition, morphology and magnetic properties of the synthesized samples were characterized by X−ray diffraction, Fourier transform infrared spectroscopy, X−ray photoelectron spectroscopy, Energy dispersive X−ray, Scanning and Transmission electron microscopy and vibrating sample magnetometer. The chemical reaction and role of fuel on the nanoparticles formation were discussed. The XRD pattern of the synthesized samples shows the formation of pure phase with average crystallite size of 97, 57 and 98 nm from Scherrer formula and 86, 54 and 87 nm from Williamson and Hall (W–H) formula respectively. FTIR absorption spectra revealed that the presence of strong absorption peaks near 400–600 cm{sup −1} corresponds to tetrahedral and octahedral complex of spinel ferrites. The relative concentrations of electronic states of elements such as cobalt (Co{sup 2+} and Co{sup 3+}), iron (Fe{sup 2+} and Fe{sup 3+}) and manganese (Mn{sup 2+} and Mn{sup 3+}) oxidation states were studied from XPS and it is found that 55% of Fe ions are in Fe{sup 2+} state and the remaining is in Fe{sup 3+} state and thus the cationic distribution

  4. Thermodynamic investigation on the formation of inclusions containing MgAl2O4 spinel during 16Cr-14Ni austenitic stainless steel manufacturing processes

    International Nuclear Information System (INIS)

    Park, J.H.

    2008-01-01

    The formation mechanism of the inclusions containing the spinel crystals has been developed based on the experimental results for the equilibrium between the Fe-16%Cr-14%Ni stainless steel melts and the inclusions as well as the compositions of the inclusions in the plant samples. In the laboratory experiments, the molar content of alumina in the inclusions linearly increases with increasing content of aluminum according to the theoretical expectation and the composition of the inclusions could be described as a function of the activity of aluminum and silicon. From the analysis of the plant samples, the content of MgO and Al 2 O 3 in the calcium silicate type inclusions continuously increases as the steel melts transfer from AOD converter to LT processes and thus, the spinel phase could be crystallized and grown in the calcium silicate matrix during cooling through tundish to cast slabs. On the other hand, the manganese silicate type inclusions were observed after tapping molten steel to the ladle, and then the MnO and Cr 2 O 3 (and SiO 2 ) in the inclusions were reduced by silicon and aluminum through LT to CC mold. The fraction of the inclusions containing spinel crystals at cast slabs was null at (Al 2 O 3 ) 2 O 3 ) > 20 mass%

  5. Structural and optical properties of NiFe2O4 synthesized via green technology

    Science.gov (United States)

    Patel, S.; Saleem, M.; Varshney, Dinesh

    2018-05-01

    The nanoparticles of NiFe2O4 were successfully synthesized via green technology using banana peel extract as the catalyst as well as the medium for reaction technique is reported. Analysis of X-ray diffraction spectrum revealed the cubic structure for the prepared spinel ferrite samples crystallized into cubic spinel structure with the space group Fd3m. The Retvield refinement was carried out which obeyed the results obtained from the XRD spectrum analysis of the sample. Raman spectrum provided confirmation for the spinel structure formation and five active Raman modes were observed. Since the optical band-gap value shows inverse response to the crystallite size, The UV-Vis spectrum study confirmed dual but reduced band-gap value.

  6. Electrochemical and Electronic Charge Transport Properties of Ni-Doped LiMn2O4 Spinel Obtained from Polyol-Mediated Synthesis

    Directory of Open Access Journals (Sweden)

    Shuo Yang

    2018-05-01

    Full Text Available LiNi0.5Mn1.5O4 (LNMO spinel has been extensively investigated as one of the most promising high-voltage cathode candidates for lithium-ion batteries. The electrochemical performance of LNMO, especially its rate performance, seems to be governed by its crystallographic structure, which is strongly influenced by the preparation methods. Conventionally, LNMO materials are prepared via solid-state reactions, which typically lead to microscaled particles with only limited control over the particle size and morphology. In this work, we prepared Ni-doped LiMn2O4 (LMO spinel via the polyol method. The cycling stability and rate capability of the synthesized material are found to be comparable to the ones reported in literature. Furthermore, its electronic charge transport properties were investigated by local electrical transport measurements on individual particles by means of a nanorobotics setup in a scanning electron microscope, as well as by performing DFT calculations. We found that the scarcity of Mn3+ in the LNMO leads to a significant decrease in electronic conductivity as compared to undoped LMO, which had no obvious effect on the rate capability of the two materials. Our results suggest that the rate capability of LNMO and LMO materials is not limited by the electronic conductivity of the fully lithiated materials.

  7. Delithiation/relithiation process of LiCoMnO4 spinel as 5 V electrode material

    Science.gov (United States)

    Dräger, Christoph; Sigel, Florian; Indris, Sylvio; Mikhailova, Daria; Pfaffmann, Lukas; Knapp, Michael; Ehrenberg, Helmut

    2017-12-01

    In this work, the LiCoMnO4 spinel has been synthesized by a two-step sol-gel based method, followed by sintering at temperatures up to 750 °C in oxygen. After structural characterization of the pristine material via synchrotron and neutron diffraction, the material was characterized via SEM and 6Li-MAS-NMR spectroscopy. 6Li-MAS-NMR spectroscopy in different states of charge revealed, that manganese and cobalt are distributed homogenously throughout the material and the delithiation primary occurs from the manganese environments. It was also shown, that it is not possible to fully delithiate the material in a practical voltage range of an electrolyte. Electrochemical cycling results reveal that about 70% of the lithium can be extracted and reinserted electrochemically in the voltage window from 4.5 to 5.4 V against lithium from/into LiCoMnO4. In situ synchrotron powder diffraction results show that lithium extraction/insertion occurs via a single-phase mechanism over the whole range of lithium contents and that the discharge capacity is mainly restricted by the voltage-window of the electrolyte. Furthermore it was shown, that the delithiation occurs up to a potential of 5.6 V.

  8. Mesoporous Spinel Li4Ti5O12 Nanoparticles for High Rate Lithium-ion Battery Anodes

    International Nuclear Information System (INIS)

    Liu, Weijian; Shao, Dan; Luo, Guoen; Gao, Qiongzhi; Yan, Guangjie; He, Jiarong; Chen, Dongyang; Yu, Xiaoyuan; Fang, Yueping

    2014-01-01

    Graphical abstract: - Highlights: • Mesoporous Li 4 Ti 5 O 12 nanoparticles were prepared by a simple hydrothermal method. • The mesoporous Li 4 Ti 5 O 12 nanoparticles exhibited a diameter of 40 ± 5 nm and a pore-size distribution of 6 - 8 nm. • Cells with the mesoporous Li 4 Ti 5 O 12 anode showed excellent high rate electrochemical properties. - Abstract: Mesoporous spinel lithium titanate (Li 4 Ti 5 O 12 ) nanoparticles with the diameter of 40 ± 5 nm and the pore-size distribution of 6 - 8 nm were prepared by a simple hydrothermal method. As an anode material for lithium-ion batteries, these spinel Li 4 Ti 5 O 12 mesoporous nanoparticles exhibited desirable lithium storage properties with an initial discharge capacity of 176 mAh g −1 at 1 C rate and a capacity of approximately 145 mAh g −1 after 200 cycles at a high rate of 20 C. These excellent electrochemical properties at high charge/discharge rates are due to the mesoporous nano-scale structures with small size particles, uniform mesopores and larger electrode/electrolyte contact area, which shortens the diffusion path for both electrons and Li + ions, and offers more active sites for Li + insertion-extraction process

  9. Synthesis of ZnMn2O4 Nanoparticles by a Microwave-Assisted Colloidal Method and their Evaluation as a Gas Sensor of Propane and Carbon Monoxide

    Directory of Open Access Journals (Sweden)

    Juan Pablo Morán-Lázaro

    2018-02-01

    Full Text Available Spinel-type ZnMn2O4 nanoparticles were synthesized via a simple and inexpensive microwave-assisted colloidal route. Structural studies by X-ray diffraction showed that a spinel crystal phase of ZnMn2O4 was obtained at a calcination temperature of 500 °C, which was confirmed by Raman and UV-vis characterizations. Spinel-type ZnMn2O4 nanoparticles with a size of 41 nm were identified by transmission electron microscopy. Pellet-type sensors were fabricated using ZnMn2O4 nanoparticles as sensing material. Sensing measurements were performed by exposing the sensor to different concentrations of propane or carbon monoxide at temperatures in the range from 100 to 300 °C. Measurements performed at an operating temperature of 300 °C revealed a good response to 500 ppm of propane and 300 ppm of carbon monoxide. Hence, ZnMn2O4 nanoparticles possess a promising potential in the gas sensors field.

  10. The characterization of Co xZn7-xSb2O12 spinel obtained by the pechini method

    Directory of Open Access Journals (Sweden)

    Deiby Santos Gouveia

    2005-06-01

    Full Text Available Oxides with spinel structures have been studied for many decades as they have been used in a variety of applications like pigments and refractories. They have also been used as a model structure to evaluate the relative stability of ions in octahedral and tetrahedral sites. Zinc- antimony spinels (Zn7Sb2O12 were synthesized by the Pechini method and the cation Zn2+ was substituted by Co2+, taking into consideration the stoichiometry of Co xZn7-xSb2O12 (x = 0 - 7. Characterization of the thermal properties of pyrolyzed powders was carried out with a TG/DTA analyzer, and mass losses were determined as a function of the cobalt content in the resin. The powders were calcined at temperatures in the range 600 to 1000 °C and characterized by XRD, BET and IR spectroscopy. Maximum cristalinity was obtained in powders calcined at 1000 °C. Materials with x = 5 - 7 revealed the presence of a secondary phase (Co, ZnSb2O6. Infrared analysis facilitated in the determination of the possible sites of Zn2+, Co2+ and Sb2+ ions in the lattice.

  11. Structural characterisation and physical properties of Li MMnO 4 ( M=Cr, Ti) spinels

    Science.gov (United States)

    Arillo, M. A.; Cuello, G.; López, M. L.; Martín, P.; Pico, C.; Veiga, M. L.

    2005-01-01

    New spinel-type phases of general formula Li MMnO 4 ( M=Cr, Ti), derived from LiMn 2O 4 by substitution of Mn 3+ by Cr 3+ or Mn 4+ by Ti 4+, have been obtained and characterised. Neutron diffraction refinements confirm that both phases crystallise in the Fd3m space group, giving the cation distributions [Li] 8 a[CrMn] 16 dO 4 and [Li 0.66Ti 0.34] 8 a[Li 0.34MnTi 0.66] 16 dO 4. Electrical conductivity has been examined by various techniques showing that these materials behave as semiconductors. The electrochemical behaviour indicates different oxidation-reduction steps in both cases concomitant with the insertion/deinsertion of lithium in non-reversible processes. X-ray diffraction patterns show that the above process is topotactic in LiCrMnO 4. Magnetic data and neutron diffraction measurements show that no long-range magnetic ordering is present, suggesting a spin-glass transition for M=Cr at low temperature, while for M=Ti the presence of non-magnetic ions in the octahedral sublattice provokes an inherent magnetic frustration.

  12. A photochemical proposal for the preparation of ZnAl{sub 2}O{sub 4} and MgAl{sub 2}O{sub 4} thin films from β-diketonate complex precursors

    Energy Technology Data Exchange (ETDEWEB)

    Cabello, G., E-mail: gerardocabelloguzman@hotmail.com [Departamento de Ciencias Básicas, Facultad de Ciencias, Universidad del Bío-Bío, Chillán (Chile); Lillo, L.; Caro, C.; Seguel, M.; Sandoval, C. [Departamento de Ciencias Básicas, Facultad de Ciencias, Universidad del Bío-Bío, Chillán (Chile); Buono-Core, G.E. [Instituto de Química, Pontificia Universidad Católica de Valparaíso, Valparaíso (Chile); Chornik, B.; Flores, M. [Deparamento de Física, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Santiago 8370415 (Chile)

    2016-05-15

    Highlights: • ZnAl{sub 2}O{sub 4} and MgAl{sub 2}O{sub 4} thin films were prepared by photo-chemical method. • The Zn(II), Mg(II) and Al(III) β-diketonate complexes were used as precursors. • The photochemical reaction was monitored by UV–vis and FT-IR spectroscopy. • The results reveal spinel oxide formation and the generation of intermediate products. - Abstract: ZnAl{sub 2}O{sub 4} and MgAl{sub 2}O{sub 4} thin films were grown on Si(100) and quartz plate substrates using a photochemical method in the solid phase with thin films of β-diketonate complexes as the precursors. The films were deposited by spin-coating and subsequently photolyzed at room temperature using 254 nm UV light. The photolysis of these films results in the deposition of metal oxide thin films and fragmentation of the ligands from the coordination sphere of the complexes. The obtained samples were post-annealed at different temperatures (350–1100 °C) for 2 h and characterized by FT-Infrared spectroscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), atomic force miscroscopy (AFM), and UV–vis spectroscopy. The results indicate the formation of spinel-type structures and other phases. These characteristics determined the quality of the films, which were obtained from the photodeposition of ternary metal oxides.

  13. Synthesis and structural characteristics of the spinel-type solid solutions in the Mn-V-Fe-O system

    International Nuclear Information System (INIS)

    Ponomaryov, V.I.; Dubrovina, I.N.; Zakharov, R.G.

    1976-01-01

    The part of the spinel region bounded by the compounds Mn 3 O 4 , Mn 2 VO 4 , Fe 2 VO 4 , and Fe 3 O 4 in the four-component system Mn-V-Fe-O was studied. The compounds were synthesized by ceramic technology. Samples were heated in a CO 2 atmosphere free of oxygen at 1100 0 C for 25-50 hr. It was found that the average composition of the spinel compound in the system had the formula Mnsub(1.00)Fesub(1.33)Vsub(0.67)O 4 . X-ray and neutron radiogrphic analyses were made. Crystallo-chemical formulas of the solid solutions considered are tabulated. The magnetic moments of saturation, calculated by the Neel model, are shown, and their experimental values are presented. The crystallo-chemical formulas of the spinel solid solutions in the Mn-V-Fe-O system are of interest in interpreting the concentration dependence of the physico-chemical properties of solid solutions of oxides based on metals with varying valence

  14. MnFe 2 O 4 /bentonite nano composite as a novel magnetic material ...

    African Journals Online (AJOL)

    It is also found that the presence of bentonite in the magnetic composite has not made any changes in the spinel structure of MnFe2O4. SEM images of the sorbent shows nanocomposite with a uniform structure and nanochannels from 0.3 to 0.8 mμ in diameter having a surface area of 130 m2 g-1. The results also revealed ...

  15. Effect of different MnO{sub 2} precursors on the electrochemical properties of spinel LiNi{sub 0.5}Mn{sub 1.5}O{sub 4} cathode active materials for high-voltage lithium ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Ye, E-mail: mayetju@tju.edu.cn [Department of Applied Chemistry, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China); Collaborative Innovation Center of Chemical Science and Engineering, Tianjin (China); Tang, Haoqing [Department of Applied Chemistry, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China); Tang, Zhiyuan, E-mail: zytang46@163.com [Department of Applied Chemistry, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China); Collaborative Innovation Center of Chemical Science and Engineering, Tianjin (China); Mao, Wenfeng [Department of Applied Chemistry, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China); Zhang, Xinhe [McNair Technology Company Limited, Dongguan, Guangdong 523700 (China)

    2016-11-15

    Highlights: • Synthesis of spinel LNMO via a facile template method. • The specific morphology of LNMO is closely related to that of MnO{sub 2} precursor. • LNMO using NH{sub 4}HCO{sub 3} as precipitant exhibits superior electrochemical performance. - Abstract: LiNi{sub 0.5}Mn{sub 1.5}O{sub 4} (LNMO) cathode materials with different morphologies are prepared via a facile template method using various MnO{sub 2} precursors. The structures, morphologies and electrochemical properties of the as-prepared LiNi{sub 0.5}Mn{sub 1.5}O{sub 4} samples are tested by various physical and electrochemical methods. The results of characterization show that the spinel LNMO cathode materials have good crystal structure and the MnO{sub 2} precursors have no effect on the final products. Moreover, the specific morphology of LNMO is closely related to that of MnO{sub 2} precursor, and further influence the electrochemical performance. In addition, the LNMO sample using NH{sub 4}HCO{sub 3} as precipitant exhibits excellent rate capability and cyclic stability in all as-prepared samples. Cycled at 0.5 and 1 C, the discharge capacities of LNMO cathode active particles using NH{sub 4}HCO{sub 3} as precipitant are 110.6 and 102.2 after 200 charge–discharge cycles, respectively, which are the largest compared with the LNMO using (NH{sub 4}){sub 2}S{sub 2}O{sub 8} and KMnO{sub 4} as oxidants.

  16. Investigation of spinel-related and orthorhombic LiMNO2 cathodes for rechargeable lithium batteries

    CSIR Research Space (South Africa)

    Gummow, RJ

    1994-05-01

    Full Text Available ~ and with carbon at 600~ have been evaluated in rechargeable lithium cells. The cathodes which initially have a composition close to LiMnO2 contain structures related to the lithiated-spinel phase Li2\\[Mn2104 and/or orthorhombic Li... the cathode structure to yield an "over-discharged" state which is possible, for example, with a Lix\\[Mn2104 spinel cathode. 7 Lix\\[Mn2\\]O4 operates at approximately 4 V vs. lithium over the range 0 < x -< 1 and has a...

  17. Solution-combustion synthesized nickel-substituted spinel cathode materials (LiNixMn2-xO4; 0≤x≤0.2) for lithium ion battery: enhancing energy storage, capacity retention, and lithium ion transport

    CSIR Research Space (South Africa)

    Kebede, MA

    2014-01-01

    Full Text Available Spherically shaped Ni-substituted LiNi(subx)Mn(sub2-x)O(sub4) (x=0, 0.1, 0.2) spinel cathode materials for lithium ion battery with high first cycle discharge capacity and remarkable cycling performance were synthesized using the solution...

  18. The effect of Cr substitution on the structural, electronic and magnetic properties of pulsed laser deposited NiFe_2O_4 thin films

    International Nuclear Information System (INIS)

    Panwar, Kalpana; Tiwari, Shailja; Bapna, Komal; Heda, N.L.; Choudhary, R.J.; Phase, D.M.; Ahuja, B.L.

    2017-01-01

    We have studied the structural, electronic and magnetic properties of pulsed laser deposited thin films of Ni_1_−_xCr_xFe_2O_4 (x=0.02 and 0.05) on Si (111) and Si (100) substrates. The films reveal single phase, polycrystalline structure with larger grain size on Si (111) substrate than that on Si (100) substrate. Contrary to the expected inverse spinel structure, x-ray photoemission (XPS) studies reveal the mixed spinel structure. XPS results suggest that Ni and Fe ions exist in 2+ and 3+ states, respectively, and they exist in tetrahedral as well as octahedral sites. The deviation from the inverse spinel leads to modified magnetic properties. It is observed that saturation magnetization drastically drops compared to the expected saturation value for inverse spinel structure. Strain in the films and lattice distortion produced by the Cr doping also appear to influence the magnetic properties. - Highlights: • Thin films of Ni_1_−_xCr_xFe_2O_4 are grown on Si(111) and Si(100) substrates. • Films on Si(111) substrate are better crystalline than those on Si(100). • XRD and FTIR results confirm the single phase growth of the films. • Cationic distribution deviates from inverse spinel structure, as revealed by XPS. • Saturation magnetization is larger on Si(100) but lower than the bulk value.

  19. Magnetic behavior of the oxide spinels:

    Indian Academy of Sciences (India)

    Magnetic behavior of the oxide spinels: Li0.5Fe2.5−2xAlxCrxO4. U N TRIVEDI, K B MODI and H H JOSHI. Department of Physics, Saurashtra University, Rajkot 360 005, India. Abstract. In order to study the effect of substitution of Fe3+ by Al3+ and Cr3+ in Li0.5Fe2.5O4 on its structural and magnetic properties, the spinel ...

  20. Conduction mechanism in operating a LiMn{sub 2}O{sub 4} cathode

    Energy Technology Data Exchange (ETDEWEB)

    Marzec, J.; Swierczek, K.; Molenda, J. [Faculty of Materials Science and Ceramics, Stanislaw Staszic University of Mining and Metallurgy, Al. Mickiewicza 30, 30-059 Cracow (Poland); Przewoznik, J. [Faculty of Physics and Nuclear Techniques, Stanislaw Staszic University of Mining and Metallurgy, Al. Mickiewicza 30, 30-059 Cracow (Poland); Simon, D.R.; Kelder, E.M.; Schoonman, J. [Delft Interfaculty Research Center: Sustainable Energy, Delft University of Technology, Julianalaan 136, 2628 DL Delft (Netherlands)

    2002-02-02

    Two series of the Li{sub x}Mn{sub 2}O{sub 4} spinel samples were studied at low temperatures (200-300 K) on electrical, thermal (DSC) and structural (X-ray diffraction (XRD)) properties for different lithium contents. Results obtained for deintercalated spinel samples with x=1 revealed the existence of a broad (100 K) phase transition that can be attributed to the molecular polaron condensation, leading to the orthorhombic distortion of the initial cubic form. The differential scanning calorimetry (DSC) measurement results enable us to regard the phase transition as a form of order-disorder one. Corresponding thermoelectric power (TEP) and electrical conductivity measurements fall within such description, moreover, indicating clear inconsistency between the measured regular DC conductivity of the spinel sample and that observed for the cathode in the working lithium cell. This discrepancy points to an alternative charge transport mechanism existing in the manganese spinel cathode, and it seems to be essential for the lithium cell performance.

  1. Oleic-acid-coated CoFe2O4 nanoparticles synthesized by co-precipitation and hydrothermal synthesis

    International Nuclear Information System (INIS)

    Gyergyek, Sašo; Drofenik, Miha; Makovec, Darko

    2012-01-01

    Highlights: ► Synthesis of oleic-acid-coated CoFe 2 O 4 nanoparticles from an aqueous solution. ► During the co-precipitation of Co 2+ /Fe 3+ single-phase spinel forms. ► During the co-precipitation of Co 2+ /Fe 2+ , feroxyhyte forms in addition to spinel. ► Oleic acid increases the spinel formation temperature and limits particle growth. ► Colloidal suspensions of ferrimagnetic CoFe 2 O 4 were prepared. - Abstract: Oleic-acid-coated CoFe 2 O 4 nanoparticles were synthesized by co-precipitation and hydrothermal synthesis. The coprecipitation of the nanoparticles was achieved by the rapid addition of a strong base to an aqueous solution of cations in the presence of the oleic acid surfactant, or without this additive. The nanoparticles were also synthesized by a hydrothermal treatment of suspensions of the precipitates, coprecipitated at room temperature in the presence of the oleic acid, or without it. The influence of the synthesis conditions, such as the valence state of the iron cation in the starting aqueous solution, the temperature of the treatment and the presence of oleic acid, on the particles size was systematically studied. X-ray powder diffractometry (XRD) and transmission electron microscopy (TEM) coupled with energy-dispersive X-ray spectroscopy (EDS) revealed that, although spinel forms at room temperature, a substantial amount of Co was incorporated within the secondary, feroxyhyte-like phase when the iron cation was in the 2+ state. In contrast, when iron was in the 3+ state, the spinel forms at elevated temperatures of approximately 60 °C. The presence of the oleic acid further increased the formation temperature for the stoichiometric spinel. Moreover, the oleic acid impeded the particles’ growth and enabled the preparation of colloidal suspensions of the nanoparticles in non-polar organic solvents. The nanoparticles’ size was successfully controlled by the temperature of the synthesis in the region where superparamagnetism

  2. Mössbauer and magnetic studies of Mg{sub 1+2x}Sb{sub x}Fe{sub 2−3x}O{sub 4} spinel ferrites

    Energy Technology Data Exchange (ETDEWEB)

    Widatallah, H.M., E-mail: hishammw@squ.edu.om [Department of Physics, College of Science, Sultan Qaboos University, 123 Muscat (Oman); Al-Mamari, F.A.S.; Al-Saqri, N.A.M.; Gismelseed, A.M.; Al-Omari, I.A.; Al-Shahumi, T.M.H. [Department of Physics, College of Science, Sultan Qaboos University, 123 Muscat (Oman); Alhaj, A.F. [Department of Physics, Qasim University, Al-Qasim (Saudi Arabia); Abo El Ata, A.M. [Department of Physics, Faculty of Science, Tanta University, Tanta (Egypt); Elzain, M.E. [Department of Physics, College of Science, Sultan Qaboos University, 123 Muscat (Oman)

    2013-06-15

    Spinel-related Mg{sub 1+2x}Sb{sub x}Fe{sub 2−3x}O{sub 4} samples (x = 0.0, 0.05, 0.10, 0.15, 0.20, and 0.30) prepared using the conventional double sintering technique were investigated using {sup 57}Fe Mössbauer spectroscopy and magnetic measurements. Mössbauer spectra favor a cationic distribution of the form (Mg{sub δ}Fe{sub 1−δ}){sup A}[Mg{sub 1+2x−δ}Sb{sub x}Fe{sub 1+δ−3x}]{sup B}O{sub 4} among the tetrahedral-A and octahedral-B sites of the spinel structure. The cation distribution parameter (δ) was found to vary with the Sb{sup 5+} concentration (x). The Mössbauer hyperfine magnetic fields at both sites and the Curie temperatures of the ferrites decrease as x increases. This was attributed to gradual weakening in the magnetic exchange interaction as more Fe{sup 3+} ions are substituted by diamagnetic Sb{sup 5+} and Mg{sup 2+} ones. The sample with x = 0.30 exhibits short range magnetic order due to cationic clustering and/or superparamagnetism. The magnetization of all samples was found to be temperature-dependent implying that δ depends on temperature in addition to x. At low temperatures the substituted ferrites (x ≠ 0.0) unexpectedly exhibit higher magnetization values relative to that of the pure ferrite MgFe{sub 2}O{sub 4}. This behavior, while at variance with the Néel's model for ferrimagnetism, is explicable in terms of the spin canting mechanism proposed in the Yafet–Kittel model. - Highlights: ► A Mössbauer and magnetic study of Sb{sup 5+} and Mg{sup 2+} co-substituted ferrites of the composition Mg{sub 1+2x}Sb{sub x}Fe{sub 2−3x}O{sub 4} is reported. ► The cation distribution in Mg{sub 1+2x}Sb{sub x}Fe{sub 2−3x}O{sub 4} is shown to depend on both the Sb{sup 5+} ionic concentration and the temperature. ► The A–B magnetic exchange interaction and Mössbauer hyperfine fields weaken with increasing Sb{sup 5+} and Mg{sup 2+} concentrations. ► The magnetization of the substituted samples with x ≠ 0.00 increases

  3. Bulletin of Materials Science | Indian Academy of Sciences

    Indian Academy of Sciences (India)

    This paper deals with the development and characterization of nickel–zinc spinel ferrite (Ni(1–) ZnFe2O4) for microwave absorption at 2.4 GHz (ISM band). The ferrite powder was prepared by dry attrition and sintering process. Complex permittivity and permeability of the prepared sample have been determined by ...

  4. An electrochemical study of the systems Li1+-xV2O4 and Li1-xVO2 (0≤x≤1)

    International Nuclear Information System (INIS)

    De Picciotto, L.A.; Thackeray, M.M.; Pistoia, G.

    1988-01-01

    Electrochemical properties of the systems Li 1±x V 2 O 4 (0≤x≤1), Li 1-x VO 2 (0≤x 2 O 4 is reversible, which confirms that lithium may be cycled, topotactically, in and out of the Li 1+x V 2 O 4 spinel structure. Delithiation of the LiV 2 O 4 spinel is irreversible; during this process the vanadium ions migrate through the oxide layers. This results in a defect rocksalt phase, which can, in turn, be relithiated by a different mechanism. Lithium extraction for the layered compound LiVO 2 yields a structure similar to the delithiated LiV 2 O 4 product. The spinel-derived compounds Li 1 +-x/V 2 O 4 (0 -3 Ω -1 cm -1 at x=0 and 10 -6 Ω -1 cm -1 at x=1. Lithium diffusion rates in Li 1±x V 2 O 4 samples increase with lithiation from D=4x10 -10 cm 2 /s in LiV 2 O 4 to D=6x10 -8 cm 2 /s in Li 2 V 2 O 4 . Intermediate values of D are obtained in the delithiated compound Li 0.28 V 2 O 4 and in the layered oxide LiVO 2 ; significantly lower values of D, viz. 1x10 -11 cm 2 /s and 4x10 -11 cm 2 /s , are found in the spinels LiMn 2 O 4 and Fe 3 O 4 respectively. 28 refs.; 5 figs.; 1 table

  5. Size dependent magnetic and magneto-optical properties of Ni{sub 0.2}Zn{sub 0.8}Fe{sub 2}O{sub 4} nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Li, Oksana A., E-mail: log85@mail.ru [Department of Applied Physics, National Pingtung University, Pingtung 90003, Taiwan (China); Siberian Federal University, Krasnoyarsk 660041 (Russian Federation); Lin, Chun-Rong, E-mail: crlin@mail.nptu.edu.tw [Department of Applied Physics, National Pingtung University, Pingtung 90003, Taiwan (China); Chen, Hung-Yi; Hsu, Hua-Shu [Department of Applied Physics, National Pingtung University, Pingtung 90003, Taiwan (China); Shih, Kun-Yauh [Department of Applied Chemistry, National Pingtung University, Pingtung 90003, Taiwan (China); Edelman, Irina S. [L.V. Kirensky Institute of Physics, SB RAS, Krasnoyarsk 660036 (Russian Federation); Wu, Kai-Wun; Tseng, Yaw-Teng [Department of Applied Physics, National Pingtung University, Pingtung 90003, Taiwan (China); Ovchinnikov, Sergey G. [Siberian Federal University, Krasnoyarsk 660041 (Russian Federation); L.V. Kirensky Institute of Physics, SB RAS, Krasnoyarsk 660036 (Russian Federation); Lee, Jiann-Shing [Department of Applied Physics, National Pingtung University, Pingtung 90003, Taiwan (China)

    2016-06-15

    Ni{sub 0.2}Zn{sub 0.8}Fe{sub 2}O{sub 4} spinel nanoparticles have been synthesized by combustion method. Average particles size varies from 15.5 to 50.0 nm depending on annealing temperature. Correlations between particles size and magnetic and magneto-optical properties are investigated. Magnetization dependences on temperature and external magnetic field correspond to the sum of paramagnetic and superparamagnetic response. Critical size of single-domain transition is found to be 15.9 nm. Magnetic circular dichroism (MCD) studies of nickel zinc spinel are presented here for the first time. The features in magnetic circular dichroism spectrum are assigned to the one-ion d–d transitions in Fe{sup 3+} and Ni{sup 2+} ions, as well to the intersublattice and intervalence charge transfer transitions. The MCD spectrum rearrangement was revealed with the change of the nanoparticles size. - Highlights: • Ni{sub 0.2}Zn{sub 0.8}Fe{sub 2}O{sub 4} nanoparticles were synthesized by combustion method. • Structure and magnetic properties are studied. • Magnetic circular dichroism (MCD) of nickel zinc spinel was measured for the first time. • The MCD spectrum rearrangement was revealed with the change of the nanoparticles size.

  6. Nanocrystalline LiMn2O4 thin film cathode material prepared by polymer spray pyrolysis method for Li-ion battery

    International Nuclear Information System (INIS)

    Karthick, S.N.; Richard Prabhu Gnanakan, S.; Subramania, A.; Kim, Hee-Je

    2010-01-01

    Nanocrystalline cubic spinel lithium manganese oxide thin film was prepared by a polymer spray pyrolysis method using lithium acetate and manganese acetate precursor solution and polyethylene glycol-4000 as a polymeric binder. The substrate temperature was selected from the thermogravimetric analysis by finding the complete crystallization temperature of LiMn 2 O 4 precursor sample. The deposited LiMn 2 O 4 thin films were annealed at 450, 500 and 600 o C for 30 min. The thin film annealed at 600 o C was found to be the sufficient temperature to form high phase pure nanocrystalline LiMn 2 O 4 thin film. The formation of cubic spinel thin film was confirmed by X-ray diffraction study. Scanning electron microscopy and atomic force microscopy analysis revealed that the thin film annealed at 600 o C was found to be nanocrystalline in nature and the surface of the films were uniform without any crack. The electrochemical charge/discharge studies of the prepared LiMn 2 O 4 film was found to be better compared to the conventional spray pyrolysed thin film material.

  7. Novel synthesis of Ni-ferrite (NiFe2O4) electrode material for supercapacitor applications

    International Nuclear Information System (INIS)

    Venkatachalam, V.; Jayavel, R.

    2015-01-01

    Novel nanocrystalline NiFe 2 O 4 has been synthesized through combustion route using citric acid as a fuel. Phase of the synthesized material was analyzed using powder X-ray diffraction. The XRD study revealed the formation of spinel phase cubic NiFe 2 O 4 with high crystallinity. The average crystallite size of NiFe 2 O 4 nanomaterial was calculated from scherrer equation. The electrochemical properties were realized by cyclic voltammetry, chronopotentiometry and electrochemical impedance spectroscopy. The electrode material shows a maximum specific capacitance of 454 F/g with pseudocapacitive behavior. High capacitance retention of electrode material over 1000 continuous charging-discharging cycles suggests its excellent electrochemical stability. The results revealed that the nickel ferrite electrode is a potential candidate for energy storage applications in supercapacitor

  8. Magnetic properties of NiFe{sub 2}O{sub 4}/carbon nanofibers from Venezuelan petcoke

    Energy Technology Data Exchange (ETDEWEB)

    Briceño, Sarah, E-mail: sbriceno@ivic.gob.ve [Laboratorio de Física de la Materia Condensada, Centro de Física, Instituto Venezolano de Investigaciones Científicas IVIC, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); Silva, Pedro; Molina, Wilmer; Brämer-Escamilla, Werner; Alcalá, Olgi [Laboratorio de Física de la Materia Condensada, Centro de Física, Instituto Venezolano de Investigaciones Científicas IVIC, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); Cañizales, Edgard [Área de Análisis Químico Inorgánico, PDVSA, INTEVEP, Los Teques 1070-A (Venezuela, Bolivarian Republic of)

    2015-05-01

    NiFe{sub 2}O{sub 4}/carbon nanofibers (NiFe{sub 2}O{sub 4}/CNFs) have been successfully synthesized by hydrotermal method using Venezuelan petroleum coke (petcoke) as carbon source and NiFe{sub 2}O{sub 4} as catalyst. The morphology, structural and magnetic properties of nanocomposite products were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HR-TEM), vibrating sample magnetometry (VSM) and electron paramagnetic resonance (EPR). XRD analysis revealed a cubic spinel structure and ferrite phase with high crystallinity. HR-TEM reveals the presence of CNFs with diameters of 4±2 nm. At room temperature, NiFe{sub 2}O{sub 4}/CNFs show superparamagnetic behavior with a maximum magnetization of 15.35 emu/g. Our findings indicate that Venezuelan petroleum coke is suitable industrial carbon source for the growth of magnetic CNFs. - Highlights: • NiFe{sub 2}O{sub 4}/CNFs have been synthesized by hydrothermal method using petroleum coke. • Nickel ferrite nanoparticles were used as the catalyst. • HR-TEM reveals the presence of CNFs with diameters of 4±2 nm. • The size of the nanoparticles defines the diameter of the CNFs.

  9. Morphology, Structure and Nonstoichiometry of ZnCr2O4 Nanophased Powder

    Directory of Open Access Journals (Sweden)

    O. Milosevic

    2003-10-01

    Full Text Available It is well established that gas/humidity-sensing properties of spinels are markedly influenced by their stoichiometry and microstructure. In this work nucleation and spinel phase development in the Zn-Cr-O system were investigated from the viewpoint of structural and morphological phenomena occurred during nanophased particle synthesis through aerosol reaction. The aerosol was generated from nitrates precursor solution using ultrasonic atomizer operated at 1.7 MHz. The influence of different decomposition schedules on the particle chemical content and morphology was determined by adjusting the processing parameters (aerosol droplet density 3.9x106 droplets/cm3, droplet velocity 0.035m/s, max. temperature 900oC and residence times 3, 6 and 9s. A composite particle structure comprised of primary crystallites sized from 22 to 44nm is revealed by SEM and TEM analysis. XRD structural analysis (crystallite size, microstrains, unit cell and ionic occupancies is performed in accordance with procedure based on Koalariet-Xfit program. A certain degree of non-stochiometry is characteristic for all powders. Homogenous distribution of the constituting elements and Zn/Cr ratio of about 0.68 are proved by EDAX mapping analysis in 470nm sized as-prepared particles. After additional treatment at 1000oC octahedral crystals form with the (111 surface dominat. Evaluated spinel non-stochiometry (Zn/Cr=0.58 is a result of the ZnO dissolving (1.9%wt in the stoichiometric ZnCr2O4. Determination of the way by which the ZnO is incorporated into the spinel lattice is performed according to the procedure based on calculation of both formation and attachment energies.

  10. Electrospinning direct synthesis of magnetic ZnFe{sub 2}O{sub 4}/ZnO multi-porous nanotubes with enhanced photocatalytic activity

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Chunlei [College of Chemistry and Environmental Engineering, Wuhan Polytechnic University, Wuhan 430023 (China); Tan, Xing [College of Biology and Pharmaceutical Engineering, Wuhan Polytechnic University, Wuhan 430023 (China); Yan, Juntao, E-mail: yanjuntaonihao@163.com [College of Chemistry and Environmental Engineering, Wuhan Polytechnic University, Wuhan 430023 (China); Chai, Bo [College of Chemistry and Environmental Engineering, Wuhan Polytechnic University, Wuhan 430023 (China); Li, Jianfen, E-mail: lijfen@163.com [College of Chemistry and Environmental Engineering, Wuhan Polytechnic University, Wuhan 430023 (China); Chen, Shizhong [College of Food Science and Engineering, Wuhan Polytechnic University, Wuhan 430023 (China)

    2017-02-28

    Highlights: • ZnFe2O4/ZnO heterojunctions are firstly fabricated by electrospinning method. • ZnFe{sub 2}O{sub 4}/ZnO heterojunctions possess multi-porous nanotube structure. • ZnFe{sub 2}O{sub 4}/ZnO heterojunctions can significantly enhance photocatalytic activity. - Abstract: Magnetic ZnFe{sub 2}O{sub 4}/ZnO (ZFO/ZnO) multi-porous nanotubes have been first fabricated via a facile electrospinning and subsequent calcination process. A series of ZFO/ZnO photocatalysts with different ZFO molar content and morphologies are also obtained by varying the molar ratio of Zn/Fe metal salt and its dosage. The morphology, composition, crystal structure and specific surface area of achieved photocatalysts are systematically examined. TEM images demonstrate ZFO/ZnO-3 multi-porous nanotubes possess perfect 1D nanotube profile with hierarchical pores. HRTEM images confirm the formation of ZFO/ZnO heterojunctions. DRS spectra show that ZFO/ZnO-3 multi-porous nanotubes exhibit an enhanced absorption both in UV and visible-light region. PL spectra and photocurrent responses of ZFO/ZnO-3 multi-porous nanotube demonstrated that the photogenerated electrons and holes are effectively separated. Above all, ZFO/ZnO-3 multi-porous nanotubes photocatalysts with a larger specific surface area of 57.79 m{sup 2} g{sup −1} exhibit the best photocatalytic efficiency of 99% after 150 min under the solar irradiation for the decolorization of RhB. Moreover, ZFO/ZnO photocatalysts not only possess magnetic separation property, but also keep a relatively high photocatalytic efficiency even after four cycles, which is beneficial for practical application. In addition, both the formation and potential photocatalytic mechanisms of ZFO/ZnO-3 multi-porous nanotubes are proposed in detail.

  11. Rapid synthesis of monodispersed highly porous spinel nickel cobaltite (NiCo{sub 2}O{sub 4}) electrode material for supercapacitors

    Energy Technology Data Exchange (ETDEWEB)

    Naveen, A. Nirmalesh, E-mail: nirmalesh.naveen@gmail.com; Selladurai, S. [Ionics Laboratory, Department of Physics, Anna University, Chennai-600025 (India)

    2015-06-24

    Monodispersed highly porous spinel nickel cobaltite electrode material was successfully synthesized in a short time using combustion technique. Single phase cubic nature of the spinel nickel cobaltite with average crystallite size of 24 nm was determined from X-ray diffraction study. Functional groups present in the compound were determined from FTIR study and it further confirms the spinel formation. FESEM images reveal the porous nature of the prepared material and uniform size distribution of the particles. Electrochemical evaluation was performed using Cyclic Voltammetry (CV) technique, Chronopotentiometry (CP) and Electrochemical Impedance Spectroscopy (EIS). Results reveal the typical pseudocapacitive behaviour of the material. Maximum capacitance of 754 F/g was calculated at the scan rate of 5 mV/s, high capacitance was due to the unique porous morphology of the electrode. Nyquist plot depicts the low resistance and good electrical conductivity of nickel cobaltite. It has been found that nickel cobaltite prepared by this typical method will be a potential electrode material for supercapcitor application.

  12. Ferri-magnetic order in Mn induced spinel Co3-xMnxO4 (0.1≤x≤1.0) ceramic compositions

    Science.gov (United States)

    Meena, P. L.; Sreenivas, K.; Singh, M. R.; Kumar, Ashok; Singh, S. P.; Kumar, Ravi

    2016-04-01

    We report structural and magnetic properties of spinel Co3-xMnxO4 (x=0.1-1.0) synthesized by solid state reaction technique. Rietveld refinement analysis of X-ray diffraction (XRD) data, revealed the formation of polycrystalline single phase Co3-xMnxO4 without any significant structural change in cubic crystal symmetry with Mn substitution, except change in lattice parameter. Temperature dependent magnetization data show changes in magnetic ordering temperature, indicating formation of antiferromagnetic (AFM) and ferrimagnetic (FM) phase at low Mn concentration (x≤0.3) and well-defined FM phase at high Mn concentration (x≥0.5). The isothermal magnetization records established an AFM/FM mixed phase for composition ranging 0.10.5.

  13. Ceramic compositions based on nano forsterite/nano magnesium aluminate spinel powders

    International Nuclear Information System (INIS)

    Khattab, R.M.; Wahsh, M.M.S.; Khalil, N.M.

    2015-01-01

    According to the wide applications in the field of chemical and engineering industries, forsterite (Mg_2SiO_4)/spinel (MgAl_2O_4) ceramic compositions were the matter of interest of several research works during the last three decades. This work aims at preparation and characterization of improved ceramic bodies based on forsterite and spinel nano powders through controlling the forsterite and spinel contents in the prepared mixes. These prepared ceramic compositions have been investigated through measuring the densification parameters, cold crushing strength as well as volume resistively. Nano spinel was added from 0 to 30 mass% on expense of nano forsterite matrix and fired at 1550 °C for 2 h. The phase composition of the fired samples was examined using x-ray diffraction (XRD) technique. The microstructure of some selected samples was shown using scanning electron microscope (SEM). A pronounced improvement in the sintering, mechanical properties and volume resistively were achieved with increasing of nano spinel addition up to 15 mass%. This is due to the improvement in the matrix of the prepared forsterite/spinel bodies as a result of well distribution of spinel in the forsterite matrix as depicted by SEM analysis. - Highlights: • Ceramic compositions based on nano forsterite/nano-MgAl_2O_4 spinel were synthesized. • CCS was improved (333.78 MPa) through 15 mass% of nano-MgAl_2O_4 spinel addition. • Volume resistivity was enhanced to 203*10"1"3 Ohm cm with 15 mass% of spinel addition. • Beyond 15 mass% spinel, CCS and volume resistivity were decreased.

  14. Neutron diffraction study of the inverse spinels Co2TiO4 and Co2SnO4

    Science.gov (United States)

    Thota, S.; Reehuis, M.; Maljuk, A.; Hoser, A.; Hoffmann, J.-U.; Weise, B.; Waske, A.; Krautz, M.; Joshi, D. C.; Nayak, S.; Ghosh, S.; Suresh, P.; Dasari, K.; Wurmehl, S.; Prokhnenko, O.; Büchner, B.

    2017-10-01

    We report a detailed single-crystal and powder neutron diffraction study of Co2TiO4 and Co2SnO4 between the temperature 1.6 and 80 K to probe the spin structure in the ground state. For both compounds the strongest magnetic intensity was observed for the (111)M reflection due to ferrimagnetic ordering, which sets in below TN=48.6 and 41 K for Co2TiO4 and Co2SnO4 , respectively. An additional low intensity magnetic reflection (200)M was noticed in Co2TiO4 due to the presence of an additional weak antiferromagnetic component. Interestingly, from both the powder and single-crystal neutron data of Co2TiO4 , we noticed a significant broadening of the magnetic (111)M reflection, which possibly results from the disordered character of the Ti and Co atoms on the B site. Practically, the same peak broadening was found for the neutron powder data of Co2SnO4 . On the other hand, from our single-crystal neutron diffraction data of Co2TiO4 , we found a spontaneous increase of particular nuclear Bragg reflections below the magnetic ordering temperature. Our data analysis showed that this unusual effect can be ascribed to the presence of anisotropic extinction, which is associated to a change of the mosaicity of the crystal. In this case, it can be expected that competing Jahn-Teller effects acting along different crystallographic axes can induce anisotropic local strain. In fact, for both ions Ti3 + and Co3 +, the 2 tg levels split into a lower dx y level yielding a higher twofold degenerate dx z/dy z level. As a consequence, one can expect a tetragonal distortion in Co2TiO4 with c /a <1 , which we could not significantly detect in the present work.

  15. Liquid flow deposited spinel (Ni,Mn){sub 3}O{sub 4} thin films for microbolometer applications

    Energy Technology Data Exchange (ETDEWEB)

    Le, Duc Thang, E-mail: ducthang36@skku.edu [Intelligent Electronic Component Team, Electronic Materials Convergence Division, Korea Institute of Ceramic Engineering and Technology, Seoul 153-801 (Korea, Republic of); School of Advanced Materials Science & Engineering, Sungkyunkwan University, Suwon 440-746 (Korea, Republic of); Jeon, Chang Jun; Lee, Kui Woong; Jeong, Young Hun; Yun, Ji Sun [Intelligent Electronic Component Team, Electronic Materials Convergence Division, Korea Institute of Ceramic Engineering and Technology, Seoul 153-801 (Korea, Republic of); Yoon, Dae Ho, E-mail: dhyoon@skku.edu [School of Advanced Materials Science & Engineering, Sungkyunkwan University, Suwon 440-746 (Korea, Republic of); Cho, Jeong Ho, E-mail: goedc@kicet.re.kr [Intelligent Electronic Component Team, Electronic Materials Convergence Division, Korea Institute of Ceramic Engineering and Technology, Seoul 153-801 (Korea, Republic of)

    2015-03-01

    Highlights: • Highly quality (Ni,Mn){sub 3}O{sub 4} thin films were grown using liquid flow deposited (LFD) technique. • It is possible to deposit multi–component manganite–oxide thin films by LFD at low temperatures. • Nickel–manganite films showed a good negative temperature coefficient (NTC) characteristic. • Liquid flow deposited (Ni,Mn){sub 3}O{sub 4} thin films are very potential for microbolometer applications. - Abstract: A liquid flow deposition (LFD) technique was initially used for the fabrication of single-component Mn{sub 3}O{sub 4} thin films onto Si wafer substrates at a range of substrate temperatures of 30–80 °C, with the introduction of an oxidizing reagent (H{sub 2}O{sub 2}). As a result, solid thin films were well formed from an aqueous solution. An X-ray diffraction (XRD) analysis showed typical characteristics of hausmannite Mn{sub 3}O{sub 4} with a spinel tetragonal phase. Field-emission scanning electron microscopy (FE-SEM) observations revealed nano-sized grains arranged uniformly on a dense and smooth surface for all of the as-deposited films. On the other hand, the LFD method was then extended to prepare two-component nickel–manganite films according to the binary chemical composition of Ni{sub x}Mn{sub 3−x}O{sub 4} with x = 0.02–0.2. The as-grown nickel–manganite films showed a surface with a good quality with a spherical bead-like architecture when x ≤ 0.10, while a conversion from spherical grains into highly porous nanowalls in the microstructure was noted in films when x ≥ 0.12. These results signify that it is possible to fabricate various multi-component manganite-oxide thin films at a low temperature. In addition, the dependences of the room-temperature electrical resistivity (ρ) and the temperature coefficient of resistance (TCR) on the Ni substitution level (x) were investigated on films annealed at 400 °C.

  16. Gas response properties of citrate gel synthesized nanocrystalline MgFe2O4: Effect of sintering temperature

    International Nuclear Information System (INIS)

    Patil, J.Y.; Mulla, I.S.; Suryavanshi, S.S.

    2013-01-01

    Graphical abstract: Display Omitted Highlights: ► Synthesis of nanocrystalline MgFe 2 O 4 by economical citrate gel combustion method. ► Structural, morphological, and gas response properties of MgFe 2 O 4 . ► Enhancement in selectivity of MgFe 2 O 4 towards LPG with sintering temperature. ► Use of MgFe 2 O 4 to detect different gases at different operating temperatures. -- Abstract: Spinel type MgFe 2 O 4 material was synthesized by citrate gel combustion method. The effect of sintering temperature on structural, morphological, and gas response properties was studied. The powder X-ray diffraction pattern and transmission electron microscope study confirms nanocrystalline spinel structure of the synthesized powder. The material was tested for response properties to various reducing gases like liquid petroleum gas (LPG), acetone, ethanol, and ammonia. The results demonstrated n-type semiconducting behavior of MgFe 2 O 4 material. It was revealed that MgFe 2 O 4 sintered at 973 K was most sensitive to LPG at 648 K and to acetone at 498 K. However MgFe 2 O 4 sintered at 1173 K exhibited higher response and selectivity to LPG with marginal increase in the operating temperature. Furthermore, the sensor exhibited a fast response and a good recovery. It was observed that the particles size, porosity, and surface activity of the sensor material is affected by the sintering temperature.

  17. Humidity sensitive electrical responce of K2CrO4 doped ZnCr2O4 ceramic sensors

    International Nuclear Information System (INIS)

    Kavasoglu, N.

    2005-01-01

    The effects of the addition of various percentages of potassium chromate as a sintering aid on the response to air moisture of ZnCr 2 O 4 ceramic body along with its crystalline structure and surface morphology were studied. The fired ceramic body, which proved to be mainly constructed from about 1μm sized ZnCr 2 O 4 spinel grains, was porous. The humidity sensing behaviour of the sensors reveals that the electrical conduction is due mainly to protonic and is controlled through the thin layers of water, adsorbed on the surface of the grains, with charge transfer to the electrodes. Only the material containing 20% K 2 CrO 4 in ZnCr 2 O 4 exhibited an exponential behaviour to humidity, which shows about three orders change in the d.c. resistance over the relative humidity in the range between 25 and 90%. The addition of CuO resulted in an increase in the conductivity but had a deleterious effect on the humidity. Based on a.c. impedance measurements, an equivalent circuit associated with a net work of RC parallel circuit in series with constant phase elements (CPEs) has been suggested. It can be therefore assumed that such equivalent circuit model of the sensor under moderate moist condition indicates the charge transport processes mediated by proton hopping and diffusion. A homemade prototype of such a humidity sensor has also been successfully demonstrated in door

  18. Phase diagram study for the PbO-ZnO-CaO-SiO_2 -“Fe_2O_3 ” system in air with CaO/SiO_2 in 1.1 and PbO/(CaO+SiO_2) in 2.4 weight ratios

    International Nuclear Information System (INIS)

    Lopez-Rodriguez, Josue; Romero-Serrano, Antonio; Hernandez-Ramirez, Aurelio; Cruz-Ramirez, Alejandro; Almaguer-Guzman, Isaias; Benavides-Perez, Ricardo; Flores-Favela, Manuel

    2017-01-01

    An experimental study on the phase equilibrium and the liquidus isotherms for the PbO-ZnO-CaO-SiO_2 -“Fe_2O_3 ” system with CaO/SiO_2 in 1.1 and PbO/(CaO+SiO_2) in 2.4 weight ratios, respectively, was carried out in the temperature range 1100-1300 deg C (1373-1573 K). High temperature phases were determined by the equilibrium-quenching method. Results are presented in the form of pseudo-ternary sections “Fe_2O_3 ”-ZnO-(PbO+CaO+SiO_2). X-Ray diffraction (XRD) and SEM-EDS results showed that the phase equilibria in this system are dominated by the high melting temperature spinel and zincite phases. It was observed that if the system is at a temperature below 1300 deg C and the total (Fe_2O_3 + ZnO) is greater than 20 wt%, spinel and/or zincite will be present in the slag system. As an application of the phase diagram, the liquid phase compositions below the liquidus surface were estimated, then their viscosities were calculated using FACTSage software. (author)

  19. Profound Interfacial Effects in CoFe2O4/Fe3O4 and Fe3O4/CoFe2O4 Core/Shell Nanoparticles

    Science.gov (United States)

    Polishchuk, Dmytro; Nedelko, Natalia; Solopan, Sergii; Ślawska-Waniewska, Anna; Zamorskyi, Vladyslav; Tovstolytkin, Alexandr; Belous, Anatolii

    2018-03-01

    Two sets of core/shell magnetic nanoparticles, CoFe2O4/Fe3O4 and Fe3O4/CoFe2O4, with a fixed diameter of the core ( 4.1 and 6.3 nm for the former and latter sets, respectively) and thickness of shells up to 2.5 nm were synthesized from metal chlorides in a diethylene glycol solution. The nanoparticles were characterized by X-ray diffraction, transmission electron microscopy, and magnetic measurements. The analysis of the results of magnetic measurements shows that coating of magnetic nanoparticles with the shells results in two simultaneous effects: first, it modifies the parameters of the core-shell interface, and second, it makes the particles acquire combined features of the core and the shell. The first effect becomes especially prominent when the parameters of core and shell strongly differ from each other. The results obtained are useful for optimizing and tailoring the parameters of core/shell spinel ferrite magnetic nanoparticles for their use in various technological and biomedical applications.

  20. Ferromagnetic-phase transition in the spinel-type CuCr2Te4

    International Nuclear Information System (INIS)

    Suzuyama, Takeshi; Awaka, Junji; Yamamoto, Hiroki; Ebisu, Shuji; Ito, Masakazu; Suzuki, Takashi; Nakama, Takao; Yagasaki, Katsuma; Nagata, Shoichi

    2006-01-01

    Ferromagnetic-phase transition in spinel-type CuCr 2 Te 4 has been clearly observed. CuCr 2 Te 4 is a telluride-spinel with the lattice constant a=11.134A, which has been synthesized successfully. The heat capacity exhibits a sharp peak due to the ferromagnetic-phase transition with the Curie temperature T C =326K. This value of T C corresponds exactly to that of the negative peak of dM/dT in low field of 1.0Oe. The magnetic susceptibility shows the Curie-Weiss behavior between 380 and 650K with the effective magnetic moment μ eff =4.14μ B /Cr-ion and the Weiss constant θ=+357K. The low temperature magnetization indicates the spin-wave excitations, where the existence of first term of Bloch T 3/2 law and the next T 5/2 term are verified experimentally. This spin-wave excitation is detected up to approximately 250K which is a fairly high temperature

  1. Order-disorder transition in the complex lithium spinel Li2CoTi3O8

    International Nuclear Information System (INIS)

    Reeves, Nik; Pasero, Denis; West, Anthony R.

    2007-01-01

    Li 2 CoTi 3 O 8 has an ordered Li 2 BB' 3 O 8 spinel structure, space group P4 3 32, at room temperature with 3:1 ordering of Ti and Li on the octahedral sites, and Li, Co disordered over the tetrahedral site. Rietveld refinement of variable temperature neutron powder diffraction data has shown an order-disorder phase transition in Li 2 CoTi 3 O 8 which commences at ∼500 deg. C with Li and Co mixing on the tetrahedral and 4-fold octahedral sites and is complete at a first order structural discontinuity at ∼915 deg. C. The fraction of Ti on the 12-fold octahedral site exhibits a small decrease with increasing temperature, which may suggest that the disordering involves all three cations. Above 930 deg. C, the structure, space group Fd3-barm, has Li, Co and Ti sharing a single-octahedral site and Li, Co sharing a tetrahedral site, although Co still exhibits a preference for tetrahedral coordination. A labelling scheme for ordered and partially ordered 3:1 spinels is devised which focuses on the occupancy of the Li,B cations. - Graphical abstract: Rietveld refinement of variable temperature neutron powder diffraction data shows an order-disorder phase transition in Li 2 CoTi 3 O 8 commencing at ∼500 deg. C with Li,Co mixing on tetrahedral and octahedral sites. This becomes complete at a first-order structural discontinuity at ∼915 deg. C. Above 930 deg. C, the structure, space group Fd3-barm, has Li, Co and Ti sharing a single-octahedral site and Li, Co sharing a tetrahedral site

  2. Electrochemically synthesized nanocrystalline spinel thin film for high performance supercapacitor

    Energy Technology Data Exchange (ETDEWEB)

    Gupta, Vinay [Carbon Technology Unit, Engineering Materials Division, National Physical Laboratory, New-Delhi, 110012 (India); Art, Science and Technology Center for Cooperative Research, Kyushu University, Kasuga-shi, Fukuoka, 816-8580 (Japan); Japan Science and Technology Agency, Kawaguchi-shi, Saitama, 332-0012 (Japan); Gupta, Shubhra; Miura, Norio [Art, Science and Technology Center for Cooperative Research, Kyushu University, Kasuga-shi, Fukuoka, 816-8580 (Japan)

    2010-06-01

    Spinels are not known for their supercapacitive nature. Here, we have explored electrochemically synthesized nanostructured NiCo{sub 2}O{sub 4} spinel thin-film electrode for electrochemical supercapacitors. The nanostructured NiCo{sub 2}O{sub 4} spinel thin film exhibited a high specific capacitance value of 580 F g{sup -1} and an energy density of 32 Wh kg{sup -1} at the power density of 4 kW kg{sup -1}, accompanying with good cyclic stability. (author)

  3. Preparation of the electrochemically formed spinel-lithium manganese oxides

    Energy Technology Data Exchange (ETDEWEB)

    Katakura, Katsumi; Wada, Kohei; Kajiki, Yoshiyuki; Yamamoto, Akiko [Department of Chemical Engineering, Nara National College of Technology, 22 Yata-cho Yamotokoriyama, Nara 639-1080 (Japan); Ogumi, Zempachi [Graduate School of Engineering, Kyoto University, Nishikyo-ku, Kyoto 615-8510 (Japan)

    2009-04-01

    Electrochemically formed spinel-lithium manganese oxides were synthesized from manganese hydroxides prepared by a cathodic electrochemical precipitation from various concentrations of manganese nitrate solutions. Two types of manganese hydroxides were formed from diluted and concentrated Mn(NO{sub 3}){sub 2} aqueous solutions. Uniform and equi-sized disk shaped Mn(OH){sub 2} crystals of 0.2-5 {mu}m in diameter were obtained on a Pt substrate after the electrochemical precipitation from lower concentration of ranging from 2 mmol dm{sup -3} to 2 mol dm{sup -3} Mn(NO{sub 3}){sub 2} aq., while the grass blade-like precipitate which is ascribed to manganese hydroxide with 20-80 {mu}m long and 1-5 {mu}m wide were formed from concentrated Mn(NO{sub 3}){sub 2} aq. Both manganese hydroxides gave the electrochemically formed spinel-LiMn{sub 2}O{sub 4} onto a Pt sheet, which is ready for electrochemical measurement, after calcination of the Li incorporated precipitate at 750 C without any additives. While the shape and size of the secondary particle frameworks (aggregates) of the electrochemically formed spinel-LiMn{sub 2}O{sub 4} can be controlled by the electrolysis conditions, the nanostructured primary crystals of 200 nm in diameter were obtained in all cases except that the fiber-like nanostructured spinel-LiMn{sub 2}O{sub 4} crystals with 200 nm in diameter were obtained from concentrated Mn(NO{sub 3}){sub 2} aq. Though these two types of electrochemically formed spinel-LiMn{sub 2}O{sub 4} showed well-shaped CVs even in higher scan rates, it would be suitable for high power density battery applications. These behaviors are assumed to be ascribed to the crystal size and shape of the processed spinel-LiMn{sub 2}O{sub 4}. (author)

  4. Photoelectrochemical and theoretical investigations of spinel type ferrites (MxFe3-xO4) for water splitting: a mini-review

    Science.gov (United States)

    Taffa, Dereje H.; Dillert, Ralf; Ulpe, Anna C.; Bauerfeind, Katharina C. L.; Bredow, Thomas; Bahnemann, Detlef W.; Wark, Michael

    2017-01-01

    Solar-assisted water splitting using photoelectrochemical cells (PECs) is one of the promising pathways for the production of hydrogen for renewable energy storage. The nature of the semiconductor material is the primary factor that controls the overall energy conversion efficiency. Finding semiconductor materials with appropriate semiconducting properties (stability, efficient charge separation and transport, abundant, visible light absorption) is still a challenge for developing materials for solar water splitting. Owing to the suitable bandgap for visible light harvesting and the abundance of iron-based oxide semiconductors, they are promising candidates for PECs and have received much research attention. Spinel ferrites are subclasses of iron oxides derived from the classical magnetite (FeIIFe2IIIO4) in which the FeII is replaced by one (some cases two) additional divalent metals. They are generally denoted as MxFe3-xO4 (M=Ca, Mg, Zn, Co, Ni, Mn, and so on) and mostly crystallize in spinel or inverse spinel structures. In this mini review, we present the current state of research in spinel ferrites as photoelectrode materials for PECs application. Strategies to improve energy conversion efficiency (nanostructuring, surface modification, and heterostructuring) will be presented. Furthermore, theoretical findings related to the electronic structure, bandgap, and magnetic properties will be presented and compared with experimental results.

  5. Cation distribution and crystallographic characterization of the spinel oxides MgCr{sub x}Fe{sub 2−x}O{sub 4} by neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Zakaria, A.K.M., E-mail: zakaria6403@yahoo.com [Institute of Nuclear Science & Technology, Bangladesh Atomic Energy Commission, Dhaka (Bangladesh); Nesa, Faizun [Department of Natural Science, Daffodil International University, Dhaka (Bangladesh); Department of Physics, Jahangirnagar University, Savar, Dhaka (Bangladesh); Saeed Khan, M.A. [Department of Physics, Jahangirnagar University, Savar, Dhaka (Bangladesh); Datta, T.K.; Aktar, Sanjida; Liba, Samia Islam; Hossain, Shahzad; Das, A.K.; Kamal, I.; Yunus, S.M. [Institute of Nuclear Science & Technology, Bangladesh Atomic Energy Commission, Dhaka (Bangladesh); Eriksson, S.-G. [Department of Chemical and Biological Engineering, Chalmers University of Technology, Gothenburg (Sweden)

    2015-06-05

    Highlights: • MgCr{sub x}Fe{sub 2−x}O{sub 4} ferrites crystallize at 1300 °C and possess cubic symmetry. • Cation distribution and crystallographic parameters have been determined precisely. • Cell parameter decreases with increasing Cr content in the system. • Ferrimagnetic ordering was found at room temperature for all the samples. - Abstract: The spinel system MgCr{sub x}Fe{sub 2−x}O{sub 4} (x = 0.0, 0.2, 0.4, 0.6, 0.8 and 1.0) has been prepared by solid state sintering method in air at 1573 K. X-ray and neutron powder diffraction experiments have been performed on the samples at room temperature for structural characterization. Rietveld refinement of the neutron diffraction data reveals that all the samples of the series possess cubic symmetry corresponding to the space group F d-3m. The distribution of the three cations Mg, Fe and Cr over the two sublattices and other crystallographic parameters has been determined precisely. The results reveal that Cr has been substituted for Fe selectively. Cr ions invariably occupy the octahedral (B) site for all values of x. Mg and Fe ions are distributed over both A and B sites for all x values. With increasing x the occupation of Mg increases in the A site and decreases in the B site for all the samples, while the Fe ions gradually decreases in both the sites for all values of x. The lattice constant decreases with increasing Cr content in the system. The magnetic structure at room temperature was ferrimagnetic for all the samples.

  6. Forecasting of chalcogenide spinels of the general formula AB2X4 using the method of training of an electronic computer

    International Nuclear Information System (INIS)

    Kiseleva, N.N.; Savitskij, E.M.

    1979-01-01

    Experimental evidence on the existence of AB 2 X 4 compounds in A-B-X systems (A and B are any elements of the periodic system, in particular, rare earth elements, X is S or Se) and the data on the properties of elements and simple sulphides (selenides) were used for an attempt to find the probability of formation of AB 2 X 4 compounds as a function of the component properties. The experimental evidence was analyzed by a computer employing algorithms of concept formation training. The results were used to predict new AB 2 X 4 compounds. The computer training method proved an efficient means of revealing the connection between probability of spinel type compounds existence with the component properties. Certain compounds of general formula AB 2 X 4 were predicted and the probability that they possess spinel structure was evaluated

  7. Cation Distribution and Magnetism in Quenched ZnFe2O4

    Science.gov (United States)

    Yuan, Qiao; Pan, Linlin; Liu, Run; Wang, Jingming; Liao, Zuzhen; Qin, Lili; Bi, Jian; Gao, Daojiang; Wu, Jiangtao

    2018-03-01

    Spinel ferrites constitute one of the most important families of magnets; their properties are believed to be highly dependent on cation occupancy. Zinc ferrite materials synthesized by various methods are usually reported to exhibit enhanced magnetism, but the mechanism underlying such enhancement remains poorly understood, with at least three effects being considered, namely cation distribution, oxygen vacancies, and surface spin disorder. We report herein the individual influence of cation distribution on the magnetic properties of zinc ferrite microparticles, synthesized by solid-state reaction with a fast (200 K/s) quench process. Based on structure analyses including x-ray powder diffraction, scanning electron microscopy, x-ray photoelectron spectroscopy, Mössbauer spectroscopy, and magnetic measurements, it is concluded that the as-prepared samples exhibited different cation distribution with inversion degree increasing from approximately 0.18 to 0.28 with increasing calcination temperature from 800°C to 1200°C. The magnetism measured at 2 K was found to be enhanced with increase of the inversion degree, while that measured at 300 K was found to be independent of inversion degree. The mechanism of the enhanced magnetization is that the indirect interaction between A and B site at low temperature is stronger than that between two nearest B sites.

  8. Experimental heat capacities, excess entropies, and magnetic properties of bulk and nano Fe3O4-Co3O4 and Fe3O4-Mn3O4 spinel solid solutions

    Science.gov (United States)

    Schliesser, Jacob M.; Huang, Baiyu; Sahu, Sulata K.; Asplund, Megan; Navrotsky, Alexandra; Woodfield, Brian F.

    2018-03-01

    We have measured the heat capacities of several well-characterized bulk and nanophase Fe3O4-Co3O4 and Fe3O4-Mn3O4 spinel solid solution samples from which magnetic properties of transitions and third-law entropies have been determined. The magnetic transitions show several features common to effects of particle and magnetic domain sizes. From the standard molar entropies, excess entropies of mixing have been generated for these solid solutions and compared with configurational entropies determined previously by assuming appropriate cation and valence distributions. The vibrational and magnetic excess entropies for bulk materials are comparable in magnitude to the respective configurational entropies indicating that excess entropies of mixing must be included when analyzing entropies of mixing. The excess entropies for nanophase materials are even larger than the configurational entropies. Changes in valence, cation distribution, bonding and microstructure between the mixing ions are the likely sources of the positive excess entropies of mixing.

  9. Synthesis of LiMn2O4 and LiCr0.2Mn1.8O4 powders by modified Pechini process

    Directory of Open Access Journals (Sweden)

    Alexandre Urbano

    2009-03-01

    Full Text Available LiMn2O4 and LiCr0.2Mn1.8O4 powders were synthesized by Pechini process, modified in order to reduce the number of steps and to work at temperatures below or equal to 400oC. Both phases crystallize in the same spinel structure with lattice constants of 8.21 and 8.22 Å respectively. Although the annealing temperature was low, the cristallinity is good and no residual amounts of organic material were detected.

  10. Facile synthesis of electrospun MFe2O4 (M = Co, Ni, Cu, Mn) spinel nanofibers with excellent electrocatalytic properties for oxygen evolution and hydrogen peroxide reduction

    Science.gov (United States)

    Li, Mian; Xiong, Yueping; Liu, Xiaotian; Bo, Xiangjie; Zhang, Yufan; Han, Ce; Guo, Liping

    2015-05-01

    Designing and preparing porous transition metal ferrites without using any template, shape-directing agent, and surfactant is a challenge. Herein, heterojunction MFe2O4 (M = Co, Ni, Cu, Mn) nanofiber (NF) based films with three-dimensional configurations were synthesized by electrospinning and the subsequent thermal treatment processes. Characterization results indeed show the 3D net-like textural structures of the electrospun spinel-type MFe2O4 NFs. In particular, the resulting MFe2O4 NFs have lengths up to several dozens of micrometers with an average diameter size of about 150 nm and possess abundant micro/meso/macropores on both the surface and within the films. The hierarchically porous structures and high surface areas of these MFe2O4 NFs (for example, the CoFe2O4 NFs possess a larger BET specific surface area (61.48 m2 g-1) than those of the CoFe2O4 NPs (5.93 m2 g-1)) can afford accessible transport channels for effectively decreasing the mass transport resistances, enhancing the electrical conductivity, and increasing the density and reactivity of the exposed catalytic active sites. All these advantages will be responsible for the better electrocatalytic performances of these MFe2O4 NFs compared with their structural isomers (i.e. the MFe2O4 NPs) for the oxygen evolution reaction (OER) and H2O2 reduction in alkaline solution. Meanwhile, both the OER and H2O2 reduction catalytic activities for these MFe2O4 NFs obey the order of CoFe2O4 NFs > CuFe2O4 NFs > NiFe2O4 NFs > MnFe2O4 NFs > Fe2O3 NFs. The CoFe2O4 NFs represent a new class of highly efficient non-noble-metal catalysts for both OER and H2O2 reduction/detection in alkaline media.Designing and preparing porous transition metal ferrites without using any template, shape-directing agent, and surfactant is a challenge. Herein, heterojunction MFe2O4 (M = Co, Ni, Cu, Mn) nanofiber (NF) based films with three-dimensional configurations were synthesized by electrospinning and the subsequent thermal treatment

  11. Structural study of the controlled hydrothermal synthesis of LiMn2O4 and LixMnyO2

    DEFF Research Database (Denmark)

    Christiansen, Troels Lindahl; Jensen, Kirsten Marie Ørnsbjerg; Shen, Yanbin

    , a layered structure, which can also be described as a defective spinel structure. Here, we show that both LiMn2O4 and LixMnyO2 nanoparticles can be synthesized from a simple, low-temperature hydrothermal synthesis. By tuning a single synthesis parameter (Li-concentration) each of the 2 structures...

  12. The effect of Cr substitution on the structural, electronic and magnetic properties of pulsed laser deposited NiFe{sub 2}O{sub 4} thin films

    Energy Technology Data Exchange (ETDEWEB)

    Panwar, Kalpana [Department of Physics, Govt. Women Engineering College, Ajmer, 305002 India (India); Department of Pure and Applied Physics, University of Kota, Kota, 324010 India (India); Tiwari, Shailja, E-mail: tiwari_shailja@rediffmail.com [Department of Physics, Govt. Women Engineering College, Ajmer, 305002 India (India); Bapna, Komal [Department of Physics, M. L. Sukhadia University, Udaipur, 313001 India (India); Heda, N.L. [Department of Pure and Applied Physics, University of Kota, Kota, 324010 India (India); Choudhary, R.J.; Phase, D.M. [UGC-DAE Consortium for Scientific Research, University Campus, Indore, 452001 India (India); Ahuja, B.L. [Department of Physics, M. L. Sukhadia University, Udaipur, 313001 India (India)

    2017-01-01

    We have studied the structural, electronic and magnetic properties of pulsed laser deposited thin films of Ni{sub 1−x}Cr{sub x}Fe{sub 2}O{sub 4} (x=0.02 and 0.05) on Si (111) and Si (100) substrates. The films reveal single phase, polycrystalline structure with larger grain size on Si (111) substrate than that on Si (100) substrate. Contrary to the expected inverse spinel structure, x-ray photoemission (XPS) studies reveal the mixed spinel structure. XPS results suggest that Ni and Fe ions exist in 2+ and 3+ states, respectively, and they exist in tetrahedral as well as octahedral sites. The deviation from the inverse spinel leads to modified magnetic properties. It is observed that saturation magnetization drastically drops compared to the expected saturation value for inverse spinel structure. Strain in the films and lattice distortion produced by the Cr doping also appear to influence the magnetic properties. - Highlights: • Thin films of Ni{sub 1−x}Cr{sub x}Fe{sub 2}O{sub 4} are grown on Si(111) and Si(100) substrates. • Films on Si(111) substrate are better crystalline than those on Si(100). • XRD and FTIR results confirm the single phase growth of the films. • Cationic distribution deviates from inverse spinel structure, as revealed by XPS. • Saturation magnetization is larger on Si(100) but lower than the bulk value.

  13. The Formation of Lithiated Ti-Doped α-Fe2O3 Nanocrystalline Particles by Mechanical Milling of Ti-Doped Lithium Spinel Ferrite

    International Nuclear Information System (INIS)

    Widatallah, H. M.; Gismelseed, A. M.; Bouziane, K.; Berry, F. J.; Al Rawas, A. D.; Al-Omari, I. A.; Yousif, A. A.; Elzain, M. E.

    2004-01-01

    The milling of spinel-related Ti-doped Li 0.5 Fe 2.5 O 4 for different times is studied with XRD, Moessbauer spectroscopy and magnetic measurements. Milling converts the material to Li-Ti-doped α-Fe 2 O 3 nanocrystalline particles via an intermediate γ-LiFeO 2 -related phase. The role played by the dopant Ti-ion in the process is emphasized.

  14. Ab-initio study of electronic, magnetic and thermoelectric behaviors of LiV2O4 and LiCr2O4 using modified Becke-Johson (mBJ) potential

    Science.gov (United States)

    Ali, Saima; Rashid, Muhammad; Hassan, M.; Noor, N. A.; Mahmood, Q.; Laref, A.; Haq, Bakhtiar Ul

    2018-05-01

    Owing to the large energy storage capacity and higher working voltage, the spinel oxides LiV2O4 and LiCr2O4, have remained under intense research attention for utilization as electrode materials in lithium-ion batteries. In this study, we explore the half-metallic nature and thermoelectric response in both LiV2O4 and LiCr2O4 spinel oxides using ab-initio density functional theory (DFT) based computations. The ground-state energies of these compounds have been studied at the optimized structural parameters in the ferromagnetic phase. In order to obtain a correct picture of the electronic structure and magnetic properties, the modified Becke-Johnson (mBJ) potential is applied to compute the electronic structures. The half-metallic behavior is confirmed by the spin-polarized electronic band structures and density of state plots. The magnetic nature is elucidated by computing the John-Teller energy, direct and indirect exchange and crystal field splitting energies. Our computations indicate strong hybridization decreasing the V/Cr site magnetic moments and increasing magnetic momenta at the nonmagnetic atomic sites. We also present the computed parameters significant for expressing the thermoelectric response, which are electrical conductivity, thermal conductivity, See-beck coefficient and power factor. The computed properties are of immense interest owing to the potential spintronics and Li-ion battery applications of the studied spinel materials.

  15. Obtainment the reverse phase spinel [Zn2+0,5Fe3+0,5](Ni2+0,5Fe3+ 1,5)O4 by the method combustion reaction: the form of assessment heating

    International Nuclear Information System (INIS)

    Silva, M.C.; Costa, A.C.F.; Coutinho, J.P.; Silva, A.T.C.; Freitas, N.L.

    2011-01-01

    This paper aims to synthesize the inverse spinel phase of by combustion reaction method and to evaluate how [Zn 2+ 0,5Fe 3+ 0,5](Ni 2+ 0,5Fe 3+ 1,5)O 4 the heat source influences the structural and morphological this phase. The forms of heating were muffle oven and ceramic plate with built-in resistance and aniline as reducing agent. Comparisons were made between temperature, reaction time and physical changes undergone by the material during the combustion carried out in two warm-up. The material was characterized by XRD, SEM, and textural analysis. Based on the results showed that the spinel phase was successfully obtained, were found traces of the phases ZnO and Fe2O3. The Most crystallite size and higher reaction temperature were presented by the material produced in the plate. As for surface area and pore volume, the highest values were achieved by the material synthesized in the oven. The agglomerates were presented in the form of skeins made of pre-sintered particles. (author)

  16. Studies on structural and magnetic properties of ternary cobalt magnesium zinc (CMZ) Co{sub 0.6-x}Mg{sub x}Zn{sub 0.4} Fe{sub 2}O{sub 4} (x = 0.0, 0.2, 0.4, 0.6) ferrite nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Kaur, Manpreet, E-mail: manpreetchem@pau.edu; Jain, Palak; Singh, Mandeep

    2015-07-15

    In this paper we report the variation in structural and magnetic properties of ternary ferrite nanoparticles (NPs) having stoichiometery Co{sub 0.6-x}Mg{sub x}Zn{sub 0.4} Fe{sub 2}O{sub 4} (x = 0.0, 0.2, 0.4, 0.6) and pure spinel ferrites MFe{sub 2}O{sub 4} (M = Mg, Co). NPs with average particle diameter of 25–45 nm were synthesized employing self-propagating oxalyl dihydrazide - metal nitrate combustion method. The products were characterized using X-ray diffraction (XRD), Vibrating sample magnetometer (VSM), Transmission electron microscopy (TEM) and FT-IR spectroscopy. FT-IR spectral analysis revealed two bands centered at 560 and 440 cm{sup −1} for tetrahedral and octahedral metal–oxygen bond stretching. Zinc doping caused red shift in the frequency band of tetrahedral M−O stretching. XRD powder diffraction patterns confirmed the formation of spinel ferrite nanoparticles, expansion of the lattice on zinc doping and enhancement of spinel phase purity in the doped ferrites. Cobalt ferrite displayed lowering of the magnetic parameters on zinc doping which further decreased in ternary ferrites Co{sub 0.6-x}Mg{sub x}Zn{sub 0.4}Fe{sub 2}O{sub 4} on replacing cobalt ions with non-magnetic magnesium ions up to x = 0.4. At x = 0.6 reverse trend was observed and Ms was enhanced. Magnesium zinc ferrite Mg{sub 0.6}Zn{sub 0.4} Fe{sub 2}O{sub 4} with high value of Ms was obtained. Combustion process employed in the present studies serves as a low temperature facile route for the synthesis and structural analysis of ternary doped ferrite nanoparticles. - Highlights: • Ternary doped cobalt magnesium zinc ferrite nanoparticles are synthesized. • FT-IR displayed red shift in tetrahedral stretching band on Zinc doping. • Expansion of lattice and enhancement of spinel phase purity on zinc doping. • The variation in saturation magnetization (Ms) on doping is explained.

  17. Spinel Li{sub 2}CoTi{sub 3}O{sub 8} nanometer obtained for application as pigment; Espinela Li{sub 2}CoTi{sub 3}O{sub 8} nanometrica obtenida para aplicacion como pigmento

    Energy Technology Data Exchange (ETDEWEB)

    Costa de Camara, M. S.; Alves Pimentel, L.; Longo, E.; Nobrega Azevedo, L. da; Araujo Melo, D. M. de

    2016-05-01

    Pigments are used in ceramics, cosmetics, inks, and other applications widely materials. To this must be single and easily reproducible. Moreover, the pigments obtained in the nanoscale are more stable, reproducible and highlight color in small amounts compared with those obtained in micrometer scale. The mixed oxides with spinel structures AB{sub 2}O{sub 4} have important applications, including: pigments, refractories, catalytic and electronic ceramics. In this context, the aim of this work was the preparation of powder Li{sub 2}CoTi{sub 3}O{sub 8} spinel phase with nanometer particle size of the polymeric precursor method (Pechini) and characterization by means of thermal analysis (TG/DTA) X-ray diffraction (XRD), refined by the Rietveld method, BET, transmission electron microscopy (TEM), Raman and colorimetric coordinates. The pigment was obtained by heat treatment of 400 degree centigrade to 1000 degree centigrade after pyrolysis at 300 degree centigrade/1 h for removing the organic material. Li{sub 2}CoTi{sub 3}O{sub 8} desired spinel phase was obtained from 500 degree centigrade, and presenting stability nanometer to about 1.300 degree centigrade. Spinel green phase introduced at temperatures in the range of 400 degree centigrade and 500 degree centigrade, and 600 degree centigrade at temperatures between blue and 1000 degree centigrade. (Author)

  18. Study of surface reaction of spinel Li4Ti5O12 during the first lithium insertion and extraction processes using atomic force microscopy and analytical transmission electron microscopy.

    Science.gov (United States)

    Kitta, Mitsunori; Akita, Tomoki; Maeda, Yasushi; Kohyama, Masanori

    2012-08-21

    Spinel lithium titanate (Li(4)Ti(5)O(12), LTO) is a promising anode material for a lithium ion battery because of its excellent properties such as high rate charge-discharge capability and life cycle stability, which were understood from the viewpoint of bulk properties such as small lattice volume changes by lithium insertion. However, the detailed surface reaction of lithium insertion and extraction has not yet been studied despite its importance to understand the mechanism of an electrochemical reaction. In this paper, we apply both atomic force microscopy (AFM) and transmission electron microscopy (TEM) to investigate the changes in the atomic and electronic structures of the Li(4)Ti(5)O(12) surface during the charge-discharged (lithium insertion and extraction) processes. The AFM observation revealed that irreversible structural changes of an atomically flat Li(4)Ti(5)O(12) surface occurs at the early stage of the first lithium insertion process, which induces the reduction of charge transfer resistance at the electrolyte/Li(4)Ti(5)O(12) interface. The TEM observation clarified that cubic rock-salt crystal layers with a half lattice size of the original spinel structure are epitaxially formed after the first charge-discharge cycle. Electron energy loss spectroscopy (EELS) observation revealed that the formed surface layer should be α-Li(2)TiO(3). Although the transformation of Li(4)Ti(5)O(12) to Li(7)Ti(5)O(12) is well-known as the lithium insertion reaction of the bulk phase, the generation of surface product layers should be inevitable in real charge-discharge processes and may play an effective role in the stable electrode performance as a solid-electrolyte interphase (SEI).

  19. Black and green pigments based on chromium-cobalt spinels

    Energy Technology Data Exchange (ETDEWEB)

    Eliziario, Sayonara A., E-mail: sayonaraea@iq.unesp.br [Departamento de Fisico-Quimica, Instituto de Quimica, UNESP - Univ Estadual Paulista, Araraquara, SP (Brazil); Departamento de Quimica, CCEN, Universidade Federal da Paraiba, Campus I, Joao Pessoa, PB (Brazil); Andrade, Jeferson M. de [Departamento de Quimica, CCEN, Universidade Federal da Paraiba, Campus I, Joao Pessoa, PB (Brazil); Lima, Severino J.G. [Departamento de Engenharia Mecanica, CT, Universidade Federal da Paraiba, Campus I, Joao Pessoa, PB (Brazil); Paskocimas, Carlos A. [Universidade Federal do Rio Grande do Norte, CT, Natal, RN (Brazil); Soledade, Luiz E.B. [Departamento de Quimica, CCEN, Universidade Federal da Paraiba, Campus I, Joao Pessoa, PB (Brazil); Hammer, P.; Longo, E. [Departamento de Fisico-Quimica, Instituto de Quimica, UNESP - Univ Estadual Paulista, Araraquara, SP (Brazil); Souza, Antonio G.; Santos, Ieda M.G. [Departamento de Quimica, CCEN, Universidade Federal da Paraiba, Campus I, Joao Pessoa, PB (Brazil)

    2011-09-15

    Highlights: {yields} Co(Co{sub 2-x}Cr{sub x})O{sub 4} powders with different chromium concentrations (x = 0, 0.25 and 1) were prepared by the polymeric precursor method. {yields} Co(CoCr)O{sub 4} and Co(Co{sub 1.75}Cr{sub 0.25})O{sub 4} displayed a dark color and CoCr{sub 2}O{sub 4} was green. {yields} The colors were related to the different oxidation states of Cr and Co. {yields} Cobalt enrichment result in an increasing presence of Co(III) and a decrease amount of Cr(VI). - Abstract: Chromium and cobalt oxides are widely used in the manufacture of industrial pigments. In this work, the Co(Co{sub 2-x}Cr{sub x})O{sub 4} powders with different chromium concentrations (x = 0, 0.25 and 1) were synthesized by the polymeric precursor method, heat treatment between 600 and 1000 deg. C. These powders were characterized by X-ray diffraction, infrared spectroscopy, colorimetry, UV-vis absorption and X-ray photoelectron spectroscopies. Even with the addition of chromium, the XRD patterns revealed that all powders crystallize in a single spinel cubic structure. The spinels with higher cobalt amount, Co(CoCr)O{sub 4} and Co(Co{sub 1.75}Cr{sub 0.25})O{sub 4}, displayed a dark color, without the Co{sup 3+} reduction observed in Co{sub 3}O{sub 4} between 900 and 950 deg. C. The spinel with higher chromium amount, CoCr{sub 2}O{sub 4}, was green. The colors were directly related to the occupation of tetrahedral and octahedral sites by the chromophores, as well as to the different oxidation states of chromium and cobalt. The different optical band gap values estimated from UV-vis spectra suggested the existence of intermediary energy levels within the band gap. X-ray photoelectron spectroscopy confirmed an increasing presence of Co(III) and a decreasing amount of Cr(VI) with cobalt enrichment.

  20. Characterization of magnetic nano particles of CoFe{sub 2}O{sub 4} and CoZnFe{sub 2}O{sub 4} prepared by the chemical co-precipitation method; Caracterizacion de nanoparticulas magneticas de CoFe{sub 2}O{sub 4} y CoZnFe{sub 2}O{sub 4} preparadas por el metodo de coprecipitacion quimica

    Energy Technology Data Exchange (ETDEWEB)

    Lopez, J.; Zambrano, G.; Gomez, M. E. [Universidad del Valle, Departamento de Fisica, Laboratorio de Peliculas Delgadas, Ciudad Universitaria Melendez, 25360 Cali (Colombia); Prieto, P. [Universidad del Valle, Centro de Excelencia en Nuevos Materiales, Ciudad Universitaria Melendez, 25360 Cali (Colombia); Espinoza B, F. J., E-mail: javierlo21@gmail.com [IPN, Centro de Investigacion y de Estudios Avanzados, Unidad Queretaro, Libramiento Norponiente No. 2000, Fracc. Real de Juriquilla, 76230 Queretaro (Mexico)

    2012-07-01

    Magnetic cobalt ferrite nanoparticles of CoFe{sub 2}O{sub 4} and CoZnFe{sub 2}O{sub 4} were prepared by co-precipitation technique from aqueous salt solutions of Co (II), ZnSO{sub 4} and Fe (III), in an alkaline medium. CoFe{sub 2}O{sub 4} powder samples were structurally characterized by X-ray diffraction, showing the presence of the most intense peat at 2{theta} = 413928{sup o} (Co K{alpha}1) corresponding to the (311) crystallographic orientation of the CoFe{sub 2}O{sub 4} spinel phase. The mean size of the crystalline of CoFe{sub 2}O{sub 4} and CoZnFe{sub 2}O{sub 4} nanoparticles determined from the full width at half maximum of the strongest reflection of the (311) peak by using the Scherrer approximation was calculated to be 11.4 and 7.0 ({+-} o.2) nm, respectively. Transmission electron microscopy studies permitted determining nanoparticle size of CoZnFe{sub 2}O{sub 4}. Fourier transform infrared spectroscopy was used to confirm the formation of Fe-O bonds, allowing identifying the presence of ferrite spinel structure. Magnetic properties were investigated with the aid of a vibrating sample magnetometer at room temperature Herein, the sample showed superparamagnetic behavior, determined by the hysteresis loop finally, due to the hysteresis loop of the CoZnFe{sub 2}O{sub 4} is very small, our magnetic nanoparticles can be considered as a soft magnetic material. These magnetic nanoparticles have interesting technological applications in biomedicine given their biocompatibility, in nano technology, and in ferro fluid preparation. (Author)

  1. Production of sulfate radical from peroxymonosulfate induced by a magnetically separable CuFe2O4 spinel in water: Efficiency, stability, and mechanism

    KAUST Repository

    Zhang, Tao

    2013-03-19

    A simple, nonhazardous, efficient and low energy-consuming process is desirable to generate powerful radicals from peroxymonosulfate (PMS) for recalcitrant pollutant removal. In this work, the production of radical species from PMS induced by a magnetic CuFe2O4 spinel was studied. Iopromide, a recalcitrant model pollutant, was used to investigate the efficiency of this process. CuFe2O4 showed higher activity and 30 times lower Cu2+ leaching (1.5 μg L-1 per 100 mg L-1) than a well-crystallized CuO at the same dosage. CuFe 2O4 maintained its activity and crystallinity during repeated batch experiments. In comparison, the activity of CuO declined significantly, which was ascribed to the deterioration in its degree of crystallinity. The efficiency of the PMS/CuFe2O4 was highest at neutral pH and decreased at acidic and alkaline pHs. Sulfate radical was the primary radical species responsible for the iopromide degradation. On the basis of the stoichiometry of oxalate degradation in the PMS/CuFe 2O4, the radical production yield from PMS was determined to be near 1 mol/mol. The PMS decomposition involved an inner-sphere complexation with the oxide\\'s surface Cu(II) sites. In situ characterization of the oxide surface with ATR-FTIR and Raman during the PMS decomposition suggested that surface Cu(II)-Cu(III)-Cu(II) redox cycle was responsible for the efficient sulfate radical generation from PMS. © 2013 American Chemical Society.

  2. Preparation, characteristics and electrochemical properties of surface-modified LiMn2O4 by doped LiNi0.05Mn1.95O4

    International Nuclear Information System (INIS)

    Yuan, Y.F.; Wu, H.M.; Guo, S.Y.; Wu, J.B.; Yang, J.L.; Wang, X.L.; Tu, J.P.

    2008-01-01

    The surface-modified spinel LiMn 2 O 4 by doped LiNi 0.05 Mn 1.95 O 4 was prepared by a tartaric acid gel method. Transmission electron microscope (TEM) images indicated that some small particles with 100-200 nm in diameter modified the surface of large particle LiMn 2 O 4 . Energy dispersive spectrometry (EDS) showed that the particles were LiNi 0.05 Mn 1.95 O 4 . Electrochemical properties of LiNi 0.05 Mn 1.95 O 4 -modified spinel LiMn 2 O 4 were intensively investigated by the galvanostatic charge-discharge tests, cyclic voltammetry (CV) and AC impedance measurements. The doped LiNi 0.05 Mn 1.95 O 4 -modified LiMn 2 O 4 cathode delivered the same initial discharge capacity as the unmodified LiMn 2 O 4 , but its cyclic stability was evidently improved, the capacity retention ratio reached 96% after 20 cycles, being higher than 89% of the unmodified LiMn 2 O 4 . Cyclic voltammograms of the LiNi 0.05 Mn 1.95 O 4 -modified LiMn 2 O 4 did not markedly change while the semicircle diameter of AC impedance spectra evidently decreased after 20 cycles, which showed that the surface modification with LiNi 0.05 Mn 1.95 O 4 improved the electrochemical activity and cycling stability of LiMn 2 O 4 .

  3. Enhanced high-potential and elevated-temperature cycling stability of LiMn2O4 cathode by TiO2 modification for Li-ion battery

    International Nuclear Information System (INIS)

    Yu Lihong; Qiu Xinping; Xi Jingyu; Zhu Wentao; Chen Liquan

    2006-01-01

    The surface of spinel LiMn 2 O 4 was modified with TiO 2 by a simple sol-gel method to improve its electrochemical performance at elevated temperatures and higher working potentials. Compared with pristine LiMn 2 O 4 , surface-modification improved the cycling stability of the material. The capacity retention of TiO 2 -modified LiMn 2 O 4 was more than 85% after 60 cycles at high potential cycles between 3.0 and 4.8 V at room temperature and near to 90% after 30 cycles at elevated temperature of 55 deg. C at 1C charge-discharge rate. SEM studies shows that the surface morphology of TiO 2 -modified LiMn 2 O 4 was different from that of pristine LiMn 2 O 4 . Powder X-ray diffraction indicated that spinel was the only detected phase in TiO 2 -modified LiMn 2 O 4 . Introduction of Ti into LiMn 2 O 4 changed the electronic structures of the particle surface. Therefore a surface solid compound of LiTi x Mn 2-x O 4 may be formed on LiMn 2 O 4 . The improved electrochemical performance of surface-modified LiMn 2 O 4 was attributed to the improved stability of crystalline structure and the higher Li + conductivity

  4. The effect of solution pH on the electrochemical performance of nanocrystalline metal ferrites MFe2O4 (M=Cu, Zn, and Ni) thin films

    Science.gov (United States)

    Elsayed, E. M.; Rashad, M. M.; Khalil, H. F. Y.; Ibrahim, I. A.; Hussein, M. R.; El-Sabbah, M. M. B.

    2016-04-01

    Nanocrystalline metal ferrite MFe2O4 (M=Cu, Zn, and Ni) thin films have been synthesized via electrodeposition-anodization process. Electrodeposited (M)Fe2 alloys were obtained from aqueous sulfate bath. The formed alloys were electrochemically oxidized (anodized) in aqueous (1 M KOH) solution, at room temperature, to the corresponding hydroxides. The parameters controlling the current efficiency of the electrodeposition of (M)Fe2 alloys such as the bath composition and the current density were studied and optimized. The anodized (M)Fe2 alloy films were annealed in air at 400 °C for 2 h. The results revealed the formation of three ferrite thin films were formed. The crystallite sizes of the produced films were in the range between 45 and 60 nm. The microstructure of the formed film was ferrite type dependent. The corrosion behavior of ferrite thin films in different pH solutions was investigated using open circuit potential (OCP) and potentiodynamic polarization measurements. The open circuit potential indicates that the initial potential E im of ZnFe2O4 thin films remained constant for a short time, then sharply increased in the less negative direction in acidic and alkaline medium compared with Ni and Cu ferrite films. The values of the corrosion current density I corr were higher for the ZnFe2O4 films at pH values of 1 and 12 compared with that of NiFe2O4 and CuFe2O4 which were higher only at pH value 1. The corrosion rate was very low for the three ferrite films when immersion in the neutral medium. The surface morphology recommended that Ni and Cu ferrite films were safely used in neutral and alkaline medium, whereas Zn ferrite film was only used in neutral atmospheres.

  5. Dielectric and impedance study of praseodymium substituted Mg-based spinel ferrites

    Energy Technology Data Exchange (ETDEWEB)

    Farid, Hafiz Muhammad Tahir, E-mail: tahirfaridbzu@gmail.com [Department of Physics, Bahauddin Zakariya, University Multan, 60800 (Pakistan); Ahmad, Ishtiaq; Ali, Irshad [Department of Physics, Bahauddin Zakariya, University Multan, 60800 (Pakistan); Ramay, Shahid M. [College of Science, Physics and Astronomy Department, King Saud University, P.O. Box 2455, 11451 Riyadh (Saudi Arabia); Mahmood, Asif [Chemical Engineering Department, College of Engineering, King Saud University, Riyadh (Saudi Arabia); Murtaza, G. [Centre for Advanced Studies in Physics, GC University, Lahore 5400 (Pakistan)

    2017-07-15

    Highlights: • Magnesium based spinel ferrites were successfully synthesized by sol-gel method. • Dielectric constant shows the normal spinel ferrites behavior. • The dc conductivity are found to decrease with increasing temperature. • The samples with low conductivity have high values of activation energy. • The Impedance decreases with increasing frequency of applied field. - Abstract: Spinel ferrites with nominal composition MgPr{sub y}Fe{sub 2−y}O{sub 4} (y = 0.00, 0.025, 0.05, 0.075, 0.10) were prepared by sol-gel method. Temperature dependent DC electrical conductivity and drift mobility were found in good agreement with each other, reflecting semiconducting behavior. The dielectric properties of all the samples as a function of frequency (1 MHz–3 GHz) were measured at room temperature. The dielectric constant and complex dielectric constant of these samples decreased with the increase of praseodymium concentration. In the present spinel ferrite, Cole–Cole plots were used to separate the grain and grain boundary’s effects. The substitution of praseodymium ions in Mg-based spinel ferrites leads to a remarkable rise of grain boundary’s resistance as compared to the grain’s resistance. As both AC conductivity and Cole–Cole plots are the functions of concentration, they reveal the dominant contribution of grain boundaries in the conduction mechanism. AC activation energy was lower than dc activation energy. Temperature dependence normalized AC susceptibility of spinel ferrites reveals that MgFe{sub 2}O{sub 4} exhibits multi domain (MD) structure with high Curie temperature while on substitution of praseodymium, MD to SD transitions occurs. The low values of conductivity and low dielectric loss make these materials best candidate for high frequency application.

  6. Spin-Coating and Characterization of Multiferroic MFe2O4 (M=Co, Ni) / BaTiO3 Bilayers

    Science.gov (United States)

    Quandt, Norman; Roth, Robert; Syrowatka, Frank; Steimecke, Matthias; Ebbinghaus, Stefan G.

    2016-01-01

    Bilayer films of MFe2O4 (M=Co, Ni) and BaTiO3 were prepared by spin coating of N,N-dimethylformamide/acetic acid solutions on platinum coated silicon wafers. Five coating steps were applied to get the desired thickness of 150 nm for both the ferrite and perovskite layer. XRD, IR and Raman spectroscopy revealed the formation of phase-pure ferrite spinels and BaTiO3. Smooth surfaces with roughnesses in the order of 3 to 5 nm were found in AFM investigations. Saturation magnetization of 347 emu cm-3 for the CoFe2O4/BaTiO3 and 188 emu cm-3 for the NiFe2O4/BaTiO3 bilayer, respectively were found. For the CoFe2O4/BaTiO3 bilayer a strong magnetic anisotropy was observed with coercivity fields of 5.1 kOe and 3.3 kOe (applied magnetic field perpendicular and parallel to film surface), while for the NiFe2O4/BaTiO3 bilayer this effect is less pronounced. Saturated polarization hysteresis loops prove the presence of ferroelectricity in both systems.

  7. Thin (111) oriented CoFe{sub 2}O{sub 4} and Co{sub 3}O{sub 4} films prepared by decomposition of layered cobaltates

    Energy Technology Data Exchange (ETDEWEB)

    Buršík, Josef, E-mail: bursik@iic.cas.cz [Institute of Inorganic Chemistry of the Academy of Sciences of the Czech Republic, v.v.i., 250 68 Husinec-Řež 1001 (Czech Republic); Soroka, Miroslav, E-mail: soroka@iic.cas.cz [Institute of Inorganic Chemistry of the Academy of Sciences of the Czech Republic, v.v.i., 250 68 Husinec-Řež 1001 (Czech Republic); Uhrecký, Róbert, E-mail: uhrecky@iic.cas.cz [Institute of Inorganic Chemistry of the Academy of Sciences of the Czech Republic, v.v.i., 250 68 Husinec-Řež 1001 (Czech Republic); Kužel, Radomír, E-mail: kuzel@karlov.mff.cuni.cz [Charles University in Prague, Faculty of Mathematics and Physics, Ke Karlovu 5, 121 16 Praha 2 (Czech Republic); Mika, Filip, E-mail: filip.mika@isibrno.cz [Institute of Scientific Instruments, Academy of Sciences of the Czech Republic, v.v.i., Královopolská 147, 612 64 Brno (Czech Republic); Huber, Štěpán, E-mail: stepan.huber@vscht.cz [University of Chemistry and Technology, Faculty of Chemical Technology, Technická 5, 166 28 Prague 6 (Czech Republic)

    2016-07-15

    Graphical abstract: Pole figures of NaCoO{sub 2} (left) and of CoFe{sub 2}O{sub 4} (right) films formed through the transformation of O3-type NaCoO{sub 2} phase in consequence of sodium deintercalation occurring at 800 °C. Films were prepared by chemical solution deposition on MgO(111) substrate. - Highlights: • Epitaxial Na(CoFe)O{sub 2} thin films by means of chemical solution deposition were prepared. • Oriented spinel films through transformation of Na(CoFe)O{sub 2} were obtained. • Orientation relation to MgO, SrTiO{sub 3} and Zr(Y)O{sub 2} substrates were determined. • Structural aspects of Na(CoFe)O{sub 2} → CoFe{sub 2}O{sub 4} transformation pathway were elucidated. - Abstract: The formation and structural characterization of highly (111)-oriented Co{sub 3}O{sub 4} and CoFe{sub 2}O{sub 4} films prepared by a novel procedure from 00l-oriented NaCoO{sub 2} and Na(CoFe)O{sub 2} is reported. The Na(CoFe)O{sub 2} films were deposited on MgO, SrTiO{sub 3}, LaAlO{sub 3}, and Zr(Y)O{sub 2} single crystals with (100) and (111) orientations by chemical solution deposition method and crystallized at 700 °C. Subsequently they were transformed into (111)-oriented spinel phase during post-growth annealing at 800–1000 °C. Morphology and structure of the films was investigated by means of scanning electron microscopy and X-ray diffraction. While all spinel films exhibit pronounced out-of-plane orientation irrespective of substrate, the rate of in-plane orientation strongly depend on lattice misfit values. Different epitaxial phenomena ranging from true one-to-one epitaxy to the existence of many-to-one epitaxy involving two or more orientations were determined by full 3D texture analysis.

  8. AC conductivity and dielectric properties of Ti-doped CoCr{sub 1.2}Fe{sub 0.8}O{sub 4} spinel ferrite

    Energy Technology Data Exchange (ETDEWEB)

    Elkestawy, M.A., E-mail: mkestawy@hotmail.co [Physics Department, Faculty of Science, Suez Canal University, Suez (Egypt); Abdel kader, S.; Amer, M.A. [Physics Department, Faculty of Science, Tanta University, Tanta (Egypt)

    2010-01-15

    Dielectric properties of spinel ferrite samples Co{sub 1+x}Ti{sub x}Cr{sub 1.2-2x}Fe{sub 0.8}O{sub 4} (0<=x<=0.5) were investigated as a function of frequency at different temperatures using a complex impedance technique. Also Cole-Cole diagrams of both permittivity and electric modulus were investigated at different temperatures to have an insight into the electric nature of the studied solids. It has been found that the electric modulus M* is the dominating property clarifying the intrinsic picture of these polycrystalline ferrites. The low conductivity and loss factor values indicate that the studied compositions may be good candidates for practical applications.

  9. Studies of the magnetic behavior of the spinel system GaxCoCrFe1-xO4 by neutron diffraction

    International Nuclear Information System (INIS)

    Yunus, S.M.; Azad, A.K.; Eriksson, S.-G.; Eriksen, J.; Rundloef, H.; Mathieu, R.

    2003-01-01

    Temperature dependent neutron diffraction studies have been done on the spinel series Ga x CoCrFe 1-x O 4 with x=0.0, 0.2, 0.4, 0.6, 0.8 and 1.0. Magnetic properties of the system have been determined from the analysis of neutron data recorded at a number of temperatures. The sublattice and net magnetizations and the paramagnetic transition temperatures of all the members of the series have been found out. A decreasing ferrimagnetic order with increasing x is apparent from the progressive loss of magnetization and transition temperature. Evidence of magnetic spin clusters has been revealed from the reduced sublattice moments and diffuse signal appearing below the (1 1 1) Bragg peak at low temperature neutron patterns. A weak magnetic ordering has also been revealed from the magnetization measurements on the sample x=1.0. The system has been found to exhibit a complex magnetic phenomenon in which short-range magnetic spin clusters are superimposed on the ferrimagnetic long-range order together with a little extension of the short-range ordering of spin clusters at very low temperatures giving rise to a weak (2 0 0) superlattice reflection

  10. TL and OSL properties of Mn2+-doped MgGa2O4 phosphor

    Science.gov (United States)

    Luchechko, A.; Zhydachevskyy, Ya; Maraba, D.; Bulur, E.; Ubizskii, S.; Kravets, O.

    2018-04-01

    The oxide MgGa2O4 spinel ceramics doped with Mn2+ ions was synthesized by a solid-state reaction at 1200 °C in air. The activator concentration was equal 0.05 mol% of MnO. Phase purity of the synthesized samples was analyzed by X-ray diffraction technique. This spinel ceramics show efficient green emission in the range from 470 to 550 nm with a maximum at about 505 nm under UV or X-ray excitations, which is due to Mn2+ ions. MgGa2O4: Mn2+ exhibits intense thermoluminescence (TL) and optically stimulated luminescence (OSL) after influence of ionizing radiation. Are complex nature of the TL glow curves is associated with a significant number of structural defects that are responsible for the formation of shallow and deep electron traps. In this work, time-resolved OSL characteristics of the samples exposed to beta particles are reported for the first time. A light from green LED was used for optical stimulation. Obtained TL and OSL results suggest MgGa2O4:Mn2+ as perspective material for further research and possible application in radiation dosimetry.

  11. Structural and optical high-pressure study of spinel-type MnIn2S4

    International Nuclear Information System (INIS)

    Manjon, F.J.; Segura, A.; Pellicer-Porres, J.; Sanchez-Royo, J.F.; Amboage, M.; Itie, J.P.; Flank, A.M.; Lagarde, P.; Polian, A.; Ursaki, V.V.; Tiginyanu, I.M.

    2007-01-01

    We report a combined study of the structural and electronic properties of the spinel-type semiconductor MnIn 2 S 4 under high pressures by means of X-ray diffraction (ADXRD), X-ray absorption (XAS), and optical absorption measurements. The three techniques evidence a reversible structural phase transition near 7 GPa, that according to ADXRD measurements is to a double-NaCl structure. XAS measurements evidence predominant tetrahedral coordination for Mn in the spinel phase that does not noticeably change with increasing pressure up to the phase transition. XAS measurements indicate that the static disorder increases considerably when the sample reverts from the double-NaCl phase to the spinel phase. Optical absorption measurements show that the direct gap of MnIn 2 S 4 exhibits a nonlinear behaviour with a positive pressure coefficient at pressures below 2.5 GPa and a negative pressure coefficient between 2.5 and 7 GPa. The pressure behavior of the bandgap seems to be affected by the defect concentration. The double-NaCl phase also exhibits a bandgap with a negative pressure coefficient. (copyright 2007 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  12. Structural and magnetic properties of Zn.sub.x./sub.Mn.sub.3-x./sub.O.sub.4./sub. spinels

    Czech Academy of Sciences Publication Activity Database

    Nádherný, L.; Maryško, Miroslav; Sedmidubský, D.; Martin, C.

    2016-01-01

    Roč. 413, Sep (2016), s. 89-96 ISSN 0304-8853 Institutional support: RVO:68378271 Keywords : Zn-Mn-O spinels * solid-state reaction * ferrimagnetic clusters * ZnO Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.630, year: 2016

  13. Spinel ferrite nanocrystals embedded inside ZnO: magnetic, electronic andmagneto-transport properties

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Shengqiang; Potzger, K.; Xu, Qingyu; Kuepper, K.; Talut, G.; Marko, D.; Mucklich, A.; Helm, M.; Fassbender, J.; Arenholz, E.; Schmidt, H.

    2009-08-21

    In this paper we show that spinel ferrite nanocrystals (NiFe{sub 2}O{sub 4}, and CoFe{sub 2}O{sub 4}) can be texturally embedded inside a ZnO matrix by ion implantation and post-annealing. The two kinds of ferrites show different magnetic properties, e.g. coercivity and magnetization. Anomalous Hall effect and positive magnetoresistance have been observed. Our study suggests a ferrimagnet/semiconductor hybrid system for potential applications in magneto-electronics. This hybrid system can be tuned by selecting different transition metal ions (from Mn to Zn) to obtain various magnetic and electronic properties.

  14. Stable nickel-substituted spinel cathode material (LiMn1.9Ni0.1O4) for lithium-ion batteries obtained by using a low temperature aqueous reduction technique

    CSIR Research Space (South Africa)

    Kunjuzwa, Niki

    2016-11-01

    Full Text Available A nickel substituted spinel cathode material (LiMn1.9Ni0.1O4) with enhanced electrochemical performance was successfully synthesized by using a locally-sourced, low-cost manganese precursor, electrolytic manganese dioxide (EMD), and NiSO4·6H2O as a...

  15. The use of emanation thermal analysis for the evaluation of Fe2O3 reactivity

    International Nuclear Information System (INIS)

    Balek, V.

    1977-01-01

    The ETA method using 220 Rn was applied in studying the ZnO - Fe 2 O 3 reaction. The higher is the temperature at which the maximum is reached on the emanation vs. temperature curve of the mixture, the lower the indicated reactivity of Fe 2 O 3 used (temperature range 790 to 980 degC). The degree of order in the lattice of the ZnFe 2 O 4 formed may be judged from the emanation power at 850 to 1000 degC. Fe 2 O 3 pre-annealed to 1100 degC shows the lowest reactivity with ZnO. Associated with it is a lower capacity of forming the perfect ZnFe 2 O 4 structure. The ETA results are compared with those obtained by DTA and by dilatometry. (M.K.)

  16. Improvement of catalytic activity in selective oxidation of styrene with H{sub 2}O{sub 2} over spinel Mg–Cu ferrite hollow spheres in water

    Energy Technology Data Exchange (ETDEWEB)

    Tong, Jinhui, E-mail: jinhuitong@126.com [Key Laboratory of Eco-Environment-Related Polymer Materials, Ministry of Education, Lanzhou 730070 (China); Key Laboratory of Gansu Polymer Materials, College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070 (China); Cai, Xiaodong; Wang, Haiyan; Zhang, Qianping [Key Laboratory of Eco-Environment-Related Polymer Materials, Ministry of Education, Lanzhou 730070 (China); Key Laboratory of Gansu Polymer Materials, College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070 (China)

    2014-07-01

    Graphical abstract: Uniform spinel Mg–Cu ferrite hollow spheres were prepared using carbon spheres as templates. Solid spinel Mg{sub 0.5}Cu{sub 0.5}Fe{sub 2}O{sub 4} ferrite nanocrystals were also prepared by sol–gel auto-combustion, hydrothermal and coprecipitation methods for comparison. The samples were found to be efficient catalysts for oxidation of styrene using hydrogen peroxide as oxidant. Especially, in the case of Mg{sub 0.5}Cu{sub 0.5}Fe{sub 2}O{sub 4} hollow spheres, obvious improvement on catalytic activity was observed and 21.2% of styrene conversion and 75.2% of selectivity for benzaldehyde were obtained at 80 °C for 6 h reaction in water. The catalyst can be magnetically separated easily for reuse and no obvious loss of activity was observed when reused in six consecutive runs. - Highlights: • Uniform spinel ferrite hollow spheres were prepared by a simple method. • The catalyst has been proved much more efficient for styrene oxidation than the reported analogues. • The catalyst can be easily separated by external magnetic field and has exhibited excellent reusability. • The catalytic system is environmentally friendly. - Abstract: Uniform spinel Mg–Cu ferrite hollow spheres were prepared using carbon spheres as templates. For comparison, solid Mg–Cu ferrite nanocrystals were also prepared by sol–gel auto-combustion, hydrothermal and coprecipitation methods. All the samples were characterized by Fourier transform infrared spectrophotometry (FT-IR), X-ray diffractometry (XRD), transmission electron microscopy (TEM) and N{sub 2} physisorption. The samples were found to be efficient catalysts for oxidation of styrene using hydrogen peroxide as oxidant. Especially, in the case of Mg{sub 0.5}Cu{sub 0.5}Fe{sub 2}O{sub 4} hollow spheres, obvious improvement on catalytic activity was observed, and 21.2% of styrene conversion and 75.2% of selectivity for benzaldehyde were obtained at 80 °C for 6 h reaction in water. The catalyst can be

  17. Chemical synthesis of spinel cobalt ferrite (CoFe2O4) nano-flakes for supercapacitor application

    International Nuclear Information System (INIS)

    Kumbhar, V.S.; Jagadale, A.D.; Shinde, N.M.; Lokhande, C.D.

    2012-01-01

    Highlights: ► The first time preparation of cobalt ferrite material in thin film form, using chemical method at low temperature. ► A nano-flake like morphology of the cobalt ferrite thin film. ► An application of the film as an electrode in supercapacitor cell. - Abstract: The present paper reveals the formation of cobalt ferrite (CoFe 2 O 4 ) thin film on stainless steel substrate by simple chemical route from an alkaline bath containing Co 2+ and Fe 2+ ions. The films are characterised for structural, surface morphological and FT-IR properties. The XRD and FT-IR studies revealed formation of single phase of CoFe 2 O 4 . The formation of nano-flakes-like morphology is observed from scanning electron microscope. The electrochemical behaviour of CoFe 2 O 4 film has been studied using cyclic voltammetry in 1 M NaOH electrolyte. The maximum specific capacitance of 366 F g −1 is obtained at the scan rate of 5 mV s −1 . Using AC impedance technique equivalent series resistance (ESR) value is found to be 1.1 Ω.

  18. Melting relations of model lherzolite in the system CaO-MgO-Al2O3-SiO2 at 2.4-3.4 GPa and the generation of komatiites

    Science.gov (United States)

    Gudfinnsson, Gudmundur H.; Presnall, Dean C.

    1996-12-01

    Isobarically invariant phase relations in the CaO-MgO-Al2O3-SiO2 system (CMAS) involving the lherzolite phase assemblage in equilibrium with liquid have been determined at 2.4-3.4 GPa. These phase relations form the solidus of model lherzolite in the CMAS system. Our data, which include determinations of all phase compositions, are in excellent agreement with the 3.0 and 4.0 GPa points of Milholland and Presnall [1991] and Davis and Schairer [1965], respectively. The invariant transition on the P-T solidus curve from spinel- to garnet-lherzolite at 3.0 GPa, 1575°C [Milholland and Presnall, 1991], is confirmed, but we observe that the theoretically required temperature depression on the solidus curve at this point is not experimentally detectable. Composition trends along the solidus take a sharp turn at the transition. In the spinel-lherzolite stability field, melt compositions become increasingly Fo-normative and less En-normative with increasing pressure, but become less Fo-normative and more pyroxenitic as pressure increases in the garnet-lherzolite stability field. Calculated melting reactions indicate that forsterite is in reaction relationship with the melt up to 3.0 GPa. Orthopyroxene is also in reaction relationship at pressures higher than just over 2.8 GPa and is the only phase in reaction relationship with the melt in the garnet-lherzolite stability field. Comparison of the normative compositions and the CaO/Al2O3 values of the komatiites of Gorgona Island and of the Reliance Formation in Zimbabwe with the compositions of liquids along the solidus of model lherzolite in the CMAS system indicates that the former komatiites were generated at pressures close to 3.7 GPa and the latter at close to 4.5 GPa, assuming that the melt generation occurred in the presence of the complete garnet-lherzolite assemblage.

  19. Developments in the Material Fabrication and Performance of LiMn2O4 dCld Cathode Material

    Science.gov (United States)

    2016-06-13

    manganese oxide spinel materials exhibit promising electrochemical performance and good thermodynamic and kinetic stability when used as a cathode in... oxide spinel (LiMn2O4) is a potential viable active cathode material for use in these versatile applications due to its low toxicity, good capacity...Developments in the Material Fabrication and Performance of LiMn2O4-dCld Cathode Material Paula C Latorre, Ashley L Ruth, and Terrill B Atwater

  20. Lattice dynamics of ZnAl{sub 2}O{sub 4} and ZnGa{sub 2}O{sub 4} under high pressure

    Energy Technology Data Exchange (ETDEWEB)

    Lopez-Moreno, S.; Rodriguez-Hernandez, P.; Munoz, A. [Departamento de Fisica Fundamental II, MALTA Consolider Team, Instituto de Materiales y Nanotecnologia Universidad de La Laguna, La Laguna 38205, Tenerife (Spain); Romero, A.H. [CINVESTAV-Queretaro Libramiento Norponiente No 2000 Real de Juriquilla 76230 Queretaro, Qro (Mexico); Manjon, F.J. [Instituto de Diseno para la Fabricacion y Produccion Automatizada, MALTA Consolider Team, Universitat Politecnica de Valencia, 46022 Valencia (Spain); Errandonea, D. [Fundacion General de la Universidad de Valencia ICMUV, MALTA Consolider Team, Edificio de Investigacion, C/Dr. Moliner 50, Burjassot, 46100 Valencia (Spain); Rusu, E.; Ursaki, V.V. [Institute of Applied Physics, Academy of Sciences of Moldova, 2028 Chisinau (Moldova)

    2011-01-15

    In this work we present a first-principles density functional study of the vibrational properties of ZnAl{sub 2}O{sub 4} and ZnGa{sub 2}O{sub 4} as function of hydrostatic pressure. Based on our previous structural characterization of these two compounds under pressure, herewith, we report the pressure dependence on both systems of the vibrational modes for the cubic spinel structure, for the CaFe{sub 2}O{sub 4}-type structure (Pnma) in ZnAl{sub 2}O{sub 4} and for marokite (Pbcm) ZnGa{sub 2}O{sub 4}. Additionally we report a second order phase transition in ZnGa{sub 2}O{sub 4} from the marokite towards the CaTi{sub 2}O{sub 4}-type structure (Cmcm), for which we also calculate the pressure dependence of the vibrational modes at the {gamma} point. Our calculations are complemented with Raman scattering measurements up to 12 GPa that show a good overall agreement between our calculated and measured mode frequencies. (Copyright copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  1. Microwave-assisted synthesis of high-voltage nanostructured LiMn1.5Ni0.5O4 spinel: tuning the Mn3+ content and electrochemical performance

    CSIR Research Space (South Africa)

    Jafta, CJ

    2013-08-01

    Full Text Available on the Mn3+ concentration and electrochemistry of the LiMn1.5Ni0.5O4 spinel. It is shown that microwave is capable of tuning the Mn3+ content of the spinel for enhanced electrochemical performance (high capacity, high capacity retention, excellent rate...

  2. Epitaxial Fe{sub 3-x}Ti{sub x}O{sub 4} films from magnetite to ulvöspinel by pulsed laser deposition

    Energy Technology Data Exchange (ETDEWEB)

    Droubay, T.C.; Pearce, C.I.; Ilton, E.S.; Engelhard, M.H.; Engelhard, M.H.; Heald, S.M.; Arenholz, E.; Rosso, K.M.

    2011-07-21

    Epitaxial films along the Fe{sub 3-x}Ti{sub x}O{sub 4} (titanomagnetite) compositional series from pure end-members magnetite (Fe{sub 3}O{sub 4}) to ulvöspinel (Fe{sub 2}TiO{sub 4}) were successfully grown by pulsed laser deposition on MgO(100) substrates. Spectroscopic characterization including high resolution x-ray diffraction, x-ray photoelectron spectroscopy, and synchrotron-based x-ray absorption and magnetic circular dichroism consistently shows that Ti(IV) substitutes for Fe(III) in the inverse spinel lattice with a proportional increase in lattice Fe(II) concentration. No evidence of Ti interstitials, spinodal decomposition, or secondary phases was found in the bulk of the grown films. At the uppermost few nanometers of the Ti-bearing film surfaces, evidence suggests that Fe(II) is susceptible to facile oxidation, and that an associated lower Fe/Ti ratio in this region is consistent with surface compositional incompleteness or alteration to a titanomaghemite-like composition and structure. The surface of these films nonetheless appear to remain highly ordered and commensurate with the underlying structure despite facile oxidation, a surface condition that is found to be reversible to some extent by heating in low oxygen environments.

  3. Influence of surface morphology and UFG on damping and mechanical properties of composite reinforced with spinel MgAl{sub 2}O{sub 4}-SiC core-shell microcomposites

    Energy Technology Data Exchange (ETDEWEB)

    Singh, Subhash; Pal, Kaushik, E-mail: pl_kshk@yahoo.co.in

    2017-01-15

    Interface between ceramic particulate and matrix is known to control the response of the materials and functionality of the composite. Among numerous physical properties, grain structure of the materials has also played a significant role in defining the behaviour of metal matrix composites. Usually, silicon carbide (SiC) particles show poor interfacial wettability in aluminium melt. Herein, we were successfully synthesized magnesium oxide (MgO) and nanocrystalline magnesium aluminate (MgAl{sub 2}O{sub 4}) spinel coated silicon carbide (SiC) core-shell micro-composites through sol-gel technique to improve the wettability of dispersoids. Core-shell structures of submicron size were thoroughly investigated by various characterization techniques. Further, aluminium matrix composites incorporated with pristine SiC, MgO grafted SiC and MgAl{sub 2}O{sub 4} grafted SiC particles were fabricated by stir casting technique, respectively. Additionally, as-cast composites were processed via friction stir processing (FSP) technique to observe the influence of grain refinement on mechanical and damping properties. Electron back scattered diffraction (EBSD), Field emission scanning electron microscopy (FE-SEM) and X-ray energy dispersion spectroscopy (EDX) analysis were conducted for investigating grain size refinement, adequate dispersion, stability and de-agglomeration of encapsulated SiC particles in aluminium matrix. The mechanical as well as thermal cyclic (from − 100 to 400 °C) damping performance of the as-cast and friction stir processed composites were studied, respectively. Finally, the enhanced properties were attributable to reduced agglomeration, stabilization and proper dispersion of the tailored SiC particles Al matrix. - Highlights: •Synthesizing a novel coating layer of MgO and MgAl{sub 2}O{sub 4} spinel onto SiC particles •Significant improvement in UTS and hardness by reinforcing tailored SiC in Al •Significant grain refinements were obtained through

  4. MnCo{sub 2}O{sub 4} spinel chromium barrier coatings for SOFC interconnect by HVOF

    Energy Technology Data Exchange (ETDEWEB)

    Lagerbom, J.; Varis, T.; Pihlatie, M.; Himanen, O.; Saarinen, V.; Kiviaho, J.; Turunen, E. [VTT Technical Research Centre of Finland, Espoo (Finland); Puranen, J. [Tampere Univ. of Technology (Finland). Inst. of Materials Science

    2010-07-01

    Chromia released from steel parts used for interconnect plates by evaporation and condensation can quickly degrade the cell (cathode) performance in solid oxide fuel cell SOFC. Coatings on top of the IC plate can work as a chromium evaporation barrier. The coating material should have good electrical conductivity, high temperature stability and nearly the same coefficient of thermal expansion as the cell materials. One candidate for the coating material is MnCo{sub 2}O{sub 4} spinel because of its suitable properties. High velocity oxy fuel (HVOF) spraying was used for the coating application on Crofer 22 APU steel samples. Using commercial and self made spray dried powders together with an HV2000 spray gun it was possible to successfully manufacture, well adhering, dense and reasonably uniform coatings. The samples were tested in oxidation exposure tests in air followed by post analysis in SEM. Powders and coatings microstructures are presented here, both before and after exposure. It was found out that together with spraying parameters the powder characteristics used influence clearly to the coating quality. Especially as very thin coatings was aimed with dense structure fine powders was found to be essential. (orig.)

  5. Influence of pH and fuels on the combustion synthesis, structural, morphological, electrical and magnetic properties of CoFe{sub 2}O{sub 4} nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Shanmugavani, A. [Solid State Ionics and Energy Devices Laboratory, Department of Physics, Bharathiar University, Coimbatore 641 046 (India); Selvan, R.Kalai, E-mail: selvankram@buc.edu.in [Solid State Ionics and Energy Devices Laboratory, Department of Physics, Bharathiar University, Coimbatore 641 046 (India); Layek, Samar [Department of Physics, Indian Institute of Technology, Kanpur 208016 (India); Vasylechko, Leonid [Semiconductor Electronics Department, Lviv Polytechnic National University, 12 Bandera Street, Lviv 79013 (Ukraine); Sanjeeviraja, C. [Department of Physics, Alagappa Chettiar College of Engineering and Technology, Karaikudi 630 004 (India)

    2015-11-15

    Nanocrystalline spinel cobalt ferrite particles are synthesized by simple combustion method using aspartic acid and glycine as fuels. The single phase cubic structure of CoFe{sub 2}O{sub 4} is revealed through X-ray diffraction analysis (XRD). Further the Rietveld refinement confirms the formation of inverse spinel structure of CoFe{sub 2}O{sub 4}. The characteristic functional groups of Co–O and Fe–O are identified from Fourier Transform Infrared (FT-IR) analysis. Uniform distribution of of nearly spherical particles with the size range of 40–80 nm is identified through field emission scanning electron microscope (FESEM) images. The calculated DC conductivity is 1.469 × 10{sup −7} and 2.214 × 10{sup −8} S cm{sup −1}, for CoFe{sub 2}O{sub 4} synthesized using aspartic acid and glycine, respectively. The dielectric behavior obeys the Maxwell–Wagner interfacial polarization. The ferromagnetic behavior of CoFe{sub 2}O{sub 4} is identified using VSM analysis and the calculated coercivity is 27 Oe and saturation magnetization is 68 emu/g.

  6. Gas response properties of citrate gel synthesized nanocrystalline MgFe{sub 2}O{sub 4}: Effect of sintering temperature

    Energy Technology Data Exchange (ETDEWEB)

    Patil, J.Y. [School of Physical Sciences, Solapur University Solapur-413255 (India); Mulla, I.S. [Emeritus Scientist (CSIR), Centre for Materials for Electronic Technology(C-MET) Pune-411 008 (India); Suryavanshi, S.S., E-mail: sssuryavanshi@rediffmail.com [School of Physical Sciences, Solapur University Solapur-413255 (India)

    2013-02-15

    Graphical abstract: Display Omitted Highlights: ► Synthesis of nanocrystalline MgFe{sub 2}O{sub 4} by economical citrate gel combustion method. ► Structural, morphological, and gas response properties of MgFe{sub 2}O{sub 4}. ► Enhancement in selectivity of MgFe{sub 2}O{sub 4} towards LPG with sintering temperature. ► Use of MgFe{sub 2}O{sub 4} to detect different gases at different operating temperatures. -- Abstract: Spinel type MgFe{sub 2}O{sub 4} material was synthesized by citrate gel combustion method. The effect of sintering temperature on structural, morphological, and gas response properties was studied. The powder X-ray diffraction pattern and transmission electron microscope study confirms nanocrystalline spinel structure of the synthesized powder. The material was tested for response properties to various reducing gases like liquid petroleum gas (LPG), acetone, ethanol, and ammonia. The results demonstrated n-type semiconducting behavior of MgFe{sub 2}O{sub 4} material. It was revealed that MgFe{sub 2}O{sub 4} sintered at 973 K was most sensitive to LPG at 648 K and to acetone at 498 K. However MgFe{sub 2}O{sub 4} sintered at 1173 K exhibited higher response and selectivity to LPG with marginal increase in the operating temperature. Furthermore, the sensor exhibited a fast response and a good recovery. It was observed that the particles size, porosity, and surface activity of the sensor material is affected by the sintering temperature.

  7. The effect of defects and disorder on the electronic properties of ZnIr2O4

    International Nuclear Information System (INIS)

    Ramo, David Muñoz; Bristowe, Paul D.

    2014-01-01

    We analyze by means of ab initio calculations the role of imperfections on the electronic structure of ZnIr 2 O 4 , ranging from point defects in the spinel phase to the fully amorphous phase. We find that interstitial defects and anion vacancies in the spinel have large formation energies, in agreement with the trends observed in other spinels. In contrast, cation vacancies and antisites have lower formation energies. Among them, the zinc antisite and the zinc vacancy are the defects with the lowest formation energy. They are found to act as acceptors, and may be responsible for the spontaneous hole doping in the material. They may also induce optical transitions that would reduce the transparency of the material. Amorphization of ZnIr 2 O 4 leads a large decrease of the band gap and appearance of localized states at the edges of the band gap region, which may act as charge traps and prevent amorphous ZnIr 2 O 4 from being a good hole conductor

  8. Phase diagram study for the PbO-ZnO-CaO-SiO{sub 2} -“Fe{sub 2}O{sub 3} ” system in air with CaO/SiO{sub 2} in 1.1 and PbO/(CaO+SiO{sub 2}) in 2.4 weight ratios

    Energy Technology Data Exchange (ETDEWEB)

    Lopez-Rodriguez, Josue; Romero-Serrano, Antonio; Hernandez-Ramirez, Aurelio; Cruz-Ramirez, Alejandro, E-mail: romeroipn@hotmail.com [Instituto Politecnico Nacional-ESIQIE, Zacatenco, Mexico City (Mexico); Almaguer-Guzman, Isaias; Benavides-Perez, Ricardo; Flores-Favela, Manuel [Servicios Administrativos Penoles S.A de C.V., Torreon, Coahuila (Mexico)

    2017-07-15

    An experimental study on the phase equilibrium and the liquidus isotherms for the PbO-ZnO-CaO-SiO{sub 2} -“Fe{sub 2}O{sub 3} ” system with CaO/SiO{sub 2} in 1.1 and PbO/(CaO+SiO{sub 2}) in 2.4 weight ratios, respectively, was carried out in the temperature range 1100-1300 deg C (1373-1573 K). High temperature phases were determined by the equilibrium-quenching method. Results are presented in the form of pseudo-ternary sections “Fe{sub 2}O{sub 3} ”-ZnO-(PbO+CaO+SiO{sub 2}). X-Ray diffraction (XRD) and SEM-EDS results showed that the phase equilibria in this system are dominated by the high melting temperature spinel and zincite phases. It was observed that if the system is at a temperature below 1300 deg C and the total (Fe{sub 2}O{sub 3} + ZnO) is greater than 20 wt%, spinel and/or zincite will be present in the slag system. As an application of the phase diagram, the liquid phase compositions below the liquidus surface were estimated, then their viscosities were calculated using FACTSage software. (author)

  9. Facile synthesis and characterization of ZnFe{sub 2}O{sub 4}/{alpha}-Fe{sub 2}O{sub 3} composite hollow nanospheres

    Energy Technology Data Exchange (ETDEWEB)

    Shen, Yu [Key Laboratory of Industrial Ecology and Environmental Engineering and State Key Laboratory of Fine Chemical, School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024 (China); School of Environmental and Chemical Engineering, Dalian Jiaotong University, Dalian 116028 (China); Li, Xinyong, E-mail: xyli@dlut.edu.cn [Key Laboratory of Industrial Ecology and Environmental Engineering and State Key Laboratory of Fine Chemical, School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024 (China); Department of Chemical Engineering, Curtin University, Perth, WA 6845 (Australia); Zhao, Qidong; Hou, Yang [Key Laboratory of Industrial Ecology and Environmental Engineering and State Key Laboratory of Fine Chemical, School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024 (China); Tade, Moses [Department of Chemical Engineering, Curtin University, Perth, WA 6845 (Australia); Liu, Shaomin, E-mail: Shaomin.Liu@curtin.edu.au [Department of Chemical Engineering, Curtin University, Perth, WA 6845 (Australia)

    2011-12-15

    Highlights: Black-Right-Pointing-Pointer ZnFe{sub 2}O{sub 4}/{alpha}-Fe{sub 2}O{sub 3} composite hollow nanospheres were successfully synthesized via a facile method. Black-Right-Pointing-Pointer Detailed structural, morphology and the phase composition were studied. Black-Right-Pointing-Pointer The incorporation of ZnFe{sub 2}O{sub 4} and {alpha}-Fe{sub 2}O{sub 3} gives an appropriate band gap value to utilize solar energy. -- Abstract: ZnFe{sub 2}O{sub 4}/{alpha}-Fe{sub 2}O{sub 3} composite hollow nanospheres were successfully fabricated via a facile one-pot solvothermal method, utilizing polyethylene glycol as soft template. X-ray diffraction and scanning electron microscopy analysis revealed that the prepared nanospheres with cubic spinel and rhombohedra composite structure had a uniform diameter of about 370 nm, and the hollow structure could be further confirmed by transmission electron microscopy. Energy dispersive X-ray, X-ray photoelectron spectroscopy and Fourier transform infrared techniques were also applied to characterize the elemental composition and chemical bonds in the hollow nanospheres. The ZnFe{sub 2}O{sub 4}/{alpha}-Fe{sub 2}O{sub 3} composite hollow nanospheres show attractive light absorption property for potential applications in electronics, optics, and catalysis.

  10. Mossbauer, Raman and X-ray diffraction studies of superparamagnetic NiFe2O4 nanoparticles prepared by sol-gel auto-combustion method

    International Nuclear Information System (INIS)

    Ahlawat, Anju; Sathe, V.G.; Reddy, V.R.; Gupta, Ajay

    2011-01-01

    Superparamagnetic nickel ferrite single phase nanoparticles with the average crystallite size of ∼9 nm have been synthesized at a low temperature (220 o C) by the sol-gel auto-combustion method. In the present study the as prepared powder was further calcined at different temperatures for 4 h, resulting in nanoparticles of larger size. The nanoparticles exhibited superparamagnetic behavior and changes in cation distribution as revealed by the Mossbauer, Raman and X-ray diffraction studies. The Mossbauer spectra collected at 5 K and under 5 T applied magnetic field showed mixed spinel structure and canted spin order for the nanoparticles, whereas there is collinear spin order with inverse spinel structure for larger particles. The vibrational spectra of the nanoparticles showed a redshift and broadening in the Raman line shape due to confinement effects. - Highlights: → Mossbauer spectra show a canting angle of 48 o for the nanoparticle samples measured at 5 K and 5 T applied magnetic field, the highest canting angle obtained so far in NiFe 2 O 4 nanoparticles. Site inversion in nanoparticles, thus converting it from inverse spinel to mixed spinel structure. → X-ray diffraction results showed a change in sign for the strain of the nanoparticle sample that showed mixed spinel structure. → Our Raman measurements showed a redshift and broadening for nanoparticle samples that is generally interpreted as a signature of quantum confinement.

  11. Coupling between magnetic, dielectric properties and crystal structure in MnT2O4 (T = V, Cr, Mn)

    International Nuclear Information System (INIS)

    Suzuki, T; Adachi, K; Katsufuji, T

    2006-01-01

    We measured the temperature dependence of dielectric constant and striction for spinel MnT 2 O 4 (T = V, Cr, Mn) under magnetic field. We found critical changes of the dielectric constant and striction with ferrimagnetic ordering as well as applied magnetic field in MnV 2 O 4 and Mn 3 O 4 , which have orbital degree of freedom in the T 3+ ion. This result indicates the importance of the orbital degree of freedom for the coupling between dielectric, magnetic properties and crystal structure in these spinel compounds

  12. The Formation of Lithiated Ti-Doped {alpha}-Fe{sub 2}O{sub 3} Nanocrystalline Particles by Mechanical Milling of Ti-Doped Lithium Spinel Ferrite

    Energy Technology Data Exchange (ETDEWEB)

    Widatallah, H. M., E-mail: hisham@ictp.trieste.it [Khartoum University, Department of Physics (Sudan); Gismelseed, A. M.; Bouziane, K. [Sultan Qaboos University, Department of Physics (Oman); Berry, F. J. [Open University, Department of Chemistry (United Kingdom); Al Rawas, A. D.; Al-Omari, I. A.; Yousif, A. A.; Elzain, M. E. [Sultan Qaboos University, Department of Physics (Oman)

    2004-12-15

    The milling of spinel-related Ti-doped Li{sub 0.5}Fe{sub 2.5}O{sub 4} for different times is studied with XRD, Moessbauer spectroscopy and magnetic measurements. Milling converts the material to Li-Ti-doped {alpha}-Fe{sub 2}O{sub 3} nanocrystalline particles via an intermediate {gamma}-LiFeO{sub 2}-related phase. The role played by the dopant Ti-ion in the process is emphasized.

  13. Photocatalytic degradation of methylene blue on magnetically separable MgFe2O4 under visible light irradiation

    KAUST Repository

    Shahid, Muhammad; Jingling, Liu; Ali, Zahid; Shakir, Imran; Warsi, Muhammad Farooq; Parveen, Riffat; Nadeem, Muhammad Tahir

    2013-01-01

    A magnetically separable single-phase MgFe2O4 photocatalyst with a spinel crystal structure was synthesized by using the solid-state reaction method. The formation of spinel structure is confirmed by X-ray diffraction and Fourier transform infrared

  14. Characteristics of Nanosize Spinel NixFe3-xO4 Prepared by Sol-Gel Method Using Egg White as Emulsifying Agent

    Directory of Open Access Journals (Sweden)

    Rudy Situmeang

    2015-07-01

    Full Text Available In this study, sol-gel method using egg white as emulsifying agent was applied to prepare nano size spinel NixFe3-xO4 (with x = 0.2–1. Sample preparation was carried out by mixing the solution of Fe(NO33.9 H2O and Ni(NO33.6 H2O with egg white, and then the sample was stirred thoroughly using magnetic stirrer. After freeze–drying process, the sample was subjected to calcination treatment and subsequently characterized. The phase composition was evaluated using the X-ray diffraction (XRD technique, followed by quantitative analysis using Rietveld and Debye-Scherrer Methods. The functionality of the sample was identified using Fourier Transform Infrared (FTIR spectroscopy, and surface morphology and elemental composition were analyzed using scanning electron microscopycoupled with electron dispersive spectroscopy (SEM/EDS. The results of XRD characterization indicated that materials consist of various crystalline phases, with NiFe2O4 as a major phase. FTIR Analysis revealed the existence of both Lewis and Brønsted–Lowry acid sites, with Lewis acid as the prominent site. The sample was found to display relatively homogeneous surface morphology, having the crystallite size in the range of 33 to 61 nm according to the Debye-Scherrer equation. The EDS data indicated that the ratio of Fe/Ni is in agreement with the composition of the raw materials used.

  15. Coexisting exchange bias effect and ferroelectricity in geometrically frustrated ZnCr2O4

    Science.gov (United States)

    Dey, J. K.; Majumdar, S.; Giri, S.

    2018-06-01

    Concomitant occurrence of exchange bias effect and ferroelectric order is revealed in antiferromagnetic spinel ZnCr2O4. The exchange bias effect is observed below antiferromagnetic Neél temperature (T N) with a reasonable value of exchange bias field ( Oe at 2 K). Intriguingly, the ratio is found unusually high as  ∼2.2, where H C is the coercivity. This indicates that large H C is not always primary for obtaining large exchange bias effect. Ferroelectric order is observed at T N, where non-centrosymmetric magnetic structure with space group associated with the magnetoelectric coupling correlates the ferroelectric order, proposing that, ZnCr2O4 is an improper multiferroic material. Rare occurrence of exchange bias effect and ferroelectric order in ZnCr2O4 attracts the community for fundamental interest and draws special attention in designing new materials for possible electric field control of exchange bias effect.

  16. The gas-sensing properties of thick film sensors based on nano-ZnFe2O4 prepared by hydrothermal method

    International Nuclear Information System (INIS)

    Chu Xiangfeng; Jiang Dongli; Zheng Chenmou

    2006-01-01

    ZnFe 2 O 4 sensors were fabricated from nano-ZnFe 2 O 4 powders prepared by hydrothermal method and their gas-sensing properties were investigated. It was found that the phase composition of the product and the gas-sensing properties greatly depend on the reaction pH value and the reaction temperature. Nano-ZnFe 2 O 4 powders could be obtained at a pH of 8-10 and the sensor based on the nano-ZnFe 2 O 4 powder prepared at 220 deg. C exhibited the best performance, characterized by high sensitivity to low concentrations of C 2 H 5 OH at 180 deg. C, especially, the sensitivity to 100 ppm C 2 H 5 OH was as high as 76

  17. Detoxification and immobilization of chromite ore processing residue in spinel-based glass-ceramic

    Energy Technology Data Exchange (ETDEWEB)

    Liao, Chang-Zhong [Guangdong Key Laboratory of Agricultural Environment Pollution Integrated Control, Guangdong Institute of Eco-Environmental and Soil Sciences, Guangzhou 510650 (China); Department of Civil Engineering, The University of Hong Kong, Pokfulam Road, Hong Kong Special Administrative Region (China); Tang, Yuanyuan [School of Environmental Science and Engineering, South University of Science and Technology of China, Shenzhen 518055 (China); Lee, Po-Heng [Department of Civil & Environmental Engineering, The Hong Kong Polytechnic University, Hong Kong Special Administrative Region (China); Liu, Chengshuai, E-mail: csliu@soil.gd.cn [Guangdong Key Laboratory of Agricultural Environment Pollution Integrated Control, Guangdong Institute of Eco-Environmental and Soil Sciences, Guangzhou 510650 (China); State Key Laboratory of Environmental Geochemistry, Institute of Geochemistry, Chinese Academy of Sciences, Guiyang 550009 (China); Shih, Kaimin, E-mail: kshih@hku.hk [Department of Civil Engineering, The University of Hong Kong, Pokfulam Road, Hong Kong Special Administrative Region (China); Li, Fangbai [Guangdong Key Laboratory of Agricultural Environment Pollution Integrated Control, Guangdong Institute of Eco-Environmental and Soil Sciences, Guangzhou 510650 (China)

    2017-01-05

    Graphical abstract: Schematic illustration of detoxification and immobilization of chromite ore processing residue in spinel-based glass-ceramic matrix. All Cr(VI) species is reduced to Cr(III) and most chromium contents are incorporated into spinel structure where the residual chromium are resided in the glass networks. - Highlights: • COPR was detoxified and immobilized in a spinel-based glass-ceramic matrix. • Cr-rich crystalline phase was determined to be MgCr{sub 1.32}Fe{sub 0.19}Al{sub 0.49}O{sub 4} spinel. • The partitioning ratio of Cr into spinel in the glass-ceramic can be up to 77%. • No Cr(VI) was observed after conversion of COPR into a glass-ceramic. • TCLP results demonstrate the superiority of the final product in immobilizing Cr. - Abstract: A promising strategy for the detoxification and immobilization of chromite ore processing residue (COPR) in a spinel-based glass-ceramic matrix is reported in this study. In the search for a more chemically durable matrix for COPR, the most critical crystalline phase for Cr immobilization was found to be a spinel solid solution with a chemical composition of MgCr{sub 1.32}Fe{sub 0.19}Al{sub 0.49}O{sub 4}. Using Rietveld quantitative X-ray diffraction analysis, we identified this final product is with the phases of spinel (3.5 wt.%), diopside (5.2 wt.%), and some amorphous contents (91.2 wt.%). The partitioning ratio of Cr reveals that about 77% of the Cr was incorporated into the more chemically durable spinel phase. The results of Cr K-edge X-ray absorption near-edge spectroscopy show that no Cr(VI) was observed after conversion of COPR into a glass-ceramic, which indicates successful detoxification of Cr(VI) into Cr(III) in the COPR-incorporated glass-ceramic. The leaching performances of Cr{sub 2}O{sub 3} and COPR-incorporated glass-ceramic were compared with a prolonged acid-leaching test, and the results demonstrate the superiority of the COPR-incorporated glass-ceramic matrix in the

  18. Detoxification and immobilization of chromite ore processing residue in spinel-based glass-ceramic

    International Nuclear Information System (INIS)

    Liao, Chang-Zhong; Tang, Yuanyuan; Lee, Po-Heng; Liu, Chengshuai; Shih, Kaimin; Li, Fangbai

    2017-01-01

    Graphical abstract: Schematic illustration of detoxification and immobilization of chromite ore processing residue in spinel-based glass-ceramic matrix. All Cr(VI) species is reduced to Cr(III) and most chromium contents are incorporated into spinel structure where the residual chromium are resided in the glass networks. - Highlights: • COPR was detoxified and immobilized in a spinel-based glass-ceramic matrix. • Cr-rich crystalline phase was determined to be MgCr 1.32 Fe 0.19 Al 0.49 O 4 spinel. • The partitioning ratio of Cr into spinel in the glass-ceramic can be up to 77%. • No Cr(VI) was observed after conversion of COPR into a glass-ceramic. • TCLP results demonstrate the superiority of the final product in immobilizing Cr. - Abstract: A promising strategy for the detoxification and immobilization of chromite ore processing residue (COPR) in a spinel-based glass-ceramic matrix is reported in this study. In the search for a more chemically durable matrix for COPR, the most critical crystalline phase for Cr immobilization was found to be a spinel solid solution with a chemical composition of MgCr 1.32 Fe 0.19 Al 0.49 O 4 . Using Rietveld quantitative X-ray diffraction analysis, we identified this final product is with the phases of spinel (3.5 wt.%), diopside (5.2 wt.%), and some amorphous contents (91.2 wt.%). The partitioning ratio of Cr reveals that about 77% of the Cr was incorporated into the more chemically durable spinel phase. The results of Cr K-edge X-ray absorption near-edge spectroscopy show that no Cr(VI) was observed after conversion of COPR into a glass-ceramic, which indicates successful detoxification of Cr(VI) into Cr(III) in the COPR-incorporated glass-ceramic. The leaching performances of Cr 2 O 3 and COPR-incorporated glass-ceramic were compared with a prolonged acid-leaching test, and the results demonstrate the superiority of the COPR-incorporated glass-ceramic matrix in the immobilization of Cr. The overall results suggest that

  19. Performance assessment of the catalyst ZnAl2O4 and Cu/ZnAl2O4 esterification reaction fatty acid in biodiesel

    International Nuclear Information System (INIS)

    Feitosa, A.C.; Dantas, J.; Costa, A.C.M.F.; Barbosa, D.C.; Meneghetti, S.M.P.

    2012-01-01

    This study aims to evaluate the performance of the Cu/ZnAl 2 O 4 and ZnAl 2 O 4 methyl esterification of fatty acids of soybean oil into biodiesel. The ZnAl 2 O 4 was synthesized by combustion reaction and then the sample was wet impregnated with a copper source. The samples were characterized by XRD, SEM, textural analysis and catalytic tests bench. The characterization results showed that the samples showed characteristic diffraction peaks spinel, with the characteristic of mesoporous material (10-250 Å), particles in the form of blocks and slabs of hard point. The results showed that the conversion impregnation of copper has increased by 17% conversion to biodiesel. (author)

  20. Phase control of Mn-based spinel films via pulsed laser deposition

    International Nuclear Information System (INIS)

    Feng, Zhenxing; Chen, Xiao; Fister, Timothy T.; Bedzyk, Michael J.; Fenter, Paul

    2016-01-01

    Phase transformations in battery cathode materials during electrochemical-insertion reactions lead to capacity fading and low cycle life. One solution is to keep the same phase of cathode materials during cation insertion-extraction processes. Here, we demonstrate a novel strategy to control the phase and composition of Mn-based spinel oxides for magnesium-ion battery applications through the growth of thin films on lattice-matched substrates using pulsed laser deposition. Materials at two extreme conditions are considered: fully discharged cathode MgMn_2O_4 and fully charged cathode Mn_2O_4. The tetragonal MgMn_2O_4 (MMO) phase is obtained on MgAl_2O_4 substrates, while the cubic MMO phase is obtained on MgO substrates. Similarly, growth of the empty Mn_2O_4 spinel in the cubic phase is obtained on an MgO substrate. These results demonstrate the ability to control separately the phase of spinel thin films (e.g., tetragonal vs. cubic MMO) at nominally fixed composition, and to maintain a fixed (cubic) phase while varying its composition (MgxMn_2O_4, for x = 0, 1). As a result, this capability provides a novel route to gain insights into the operation of battery electrodes for energy storage applications.

  1. Effect of the cations distribution on the magnetic properties of SnFe{sub 2}O{sub 4}: First-principles study

    Energy Technology Data Exchange (ETDEWEB)

    Lamouri, R.; Tadout, M. [Materials and Nanomaterials Center, MAScIR Foundation, Rabat Design Center, Rue Mohamed Al Jazouli – Madinat Al Irfane, Rabat 10 100 (Morocco); LaMCScI (ex LMPHE), B.P. 1014, Faculty of Science-Mohammed V University, Rabat (Morocco); Hamedoun, M. [Materials and Nanomaterials Center, MAScIR Foundation, Rabat Design Center, Rue Mohamed Al Jazouli – Madinat Al Irfane, Rabat 10 100 (Morocco); Benyoussef, A. [Materials and Nanomaterials Center, MAScIR Foundation, Rabat Design Center, Rue Mohamed Al Jazouli – Madinat Al Irfane, Rabat 10 100 (Morocco); LaMCScI (ex LMPHE), B.P. 1014, Faculty of Science-Mohammed V University, Rabat (Morocco); Hassan II Academy of Science and Technology, Rabat (Morocco); Ez-zahraouy, H.; Benaissa, M. [LaMCScI (ex LMPHE), B.P. 1014, Faculty of Science-Mohammed V University, Rabat (Morocco); Mounkachi, O., E-mail: o.mounkachi@mascir.com [Materials and Nanomaterials Center, MAScIR Foundation, Rabat Design Center, Rue Mohamed Al Jazouli – Madinat Al Irfane, Rabat 10 100 (Morocco)

    2017-08-15

    Highlights: • SnFe{sub 2}O{sub 4} a new half-metal spinel oxides for spintronic application. • The most stable normal spinel structures are identified for SnFe{sub 2}O{sub 4}. • Spin-polarized calculations give a half-metallic character for SnFe{sub 2}O{sub 4}. - Abstract: In this work, a study of the electronic and magnetic properties of SnFe{sub 2}O{sub 4} spinel ferrite for different case of octahedral and tetrahedral distribution was carried out by using the Full Potential Linearized Plane Wave (FP-LAPW) method in density functional theory (DFT) implemented in the WIEN2K package, with the generalized gradient (GGA) and Tran-Blaha modified Becke-Johnson approximations for the exchange and correlation functional. Our spin-polarized calculations based on mBJ correction show a half metallic behavior for SnFe{sub 2}O{sub 4} which confirm the usefulness of SnFe{sub 2}O{sub 4} in spintronic application. From the magnetic properties calculations, it is found that the magnetic moment per formula unit is 8.0327 µ{sub β}, 0.000015 µ{sub β} and 3.99µ{sub β} in SnFe{sub 2}O{sub 4} 100% normal, 100% inverse and 50% inverse, respectively.

  2. Electrochemically active nanocomposites of Li4Ti5O12 2D nanosheets and SnO2 0D nanocrystals with improved electrode performance

    International Nuclear Information System (INIS)

    Han, Song Yi; Kim, In Young; Lee, Sang-Hyup; Hwang, Seong-Ju

    2012-01-01

    Electrochemically active nanocomposites consisting of Li 4 Ti 5 O 12 2D nanosheets and SnO 2 0D nanocrystals are synthesized by the crystal growth of tin dioxide on the surface of 2D nanostructured lithium titanate. According to powder X-ray diffraction and electron microscopic analyses, the rutile-structured SnO 2 nanocrystals are stabilized on the surface of spinel-structured Li 4 Ti 5 O 12 2D nanosheets. The homogeneous hybridization of tin dioxide with lithium titanate is confirmed by elemental mapping analysis. Ti K-edge X-ray absorption near-edge structure and Sn 3d X-ray photoelectron spectroscopy indicate the stabilization of tetravalent titanium ions in the spinel lattice of Li 4 Ti 5 O 12 and the formation of SnO 2 phase with tetravalent Sn oxidation state. The electrochemical measurements clearly demonstrate the promising functionality of the present nanocomposites as anode for lithium secondary batteries. The Li 4 Ti 5 O 12 –SnO 2 nanocomposites show larger discharge capacity and better cyclability than do the uncomposited Li 4 Ti 5 O 12 and SnO 2 phases, indicating the synergistic effect of nanocomposite formation on the electrode performance of Li 4 Ti 5 O 12 and SnO 2 . The present experimental findings underscore the validity of 2D nanostructured lithium titanate as a useful platform for the stabilization of nanocrystalline electrode materials and also for the improvement of their functionality.

  3. High energy density layered-spinel hybrid cathodes for lithium ion rechargeable batteries

    Energy Technology Data Exchange (ETDEWEB)

    Basu, S., E-mail: sbasumajumder@yahoo.com [Department of Physics, Indian Institute of Technology Kharagpur, Kharagpur 721 302 (India); Dahiya, P.P.; Akhtar, Mainul [Materials Science Center, Indian Institute of Technology Kharagpur, Kharagpur 721 302 (India); Ray, S.K. [Department of Physics, Indian Institute of Technology Kharagpur, Kharagpur 721 302 (India); Chang, J.K. [Institute of Materials Science and Engineering, National Central University, Taiwan (China); Majumder, S.B. [Materials Science Center, Indian Institute of Technology Kharagpur, Kharagpur 721 302 (India)

    2016-11-15

    Highlights: • Structural integration of layered domains in spinel matrix of the composite particles. • Highest discharge capacity (275 mAh g{sup −1}) in composite with 30.0 mole% Li{sub 2}MnO{sub 3}. • Reasonably good rate capability of layered-spinel composite cathode. • Capacity fading with cycling is related to cubic to tetragonal structural phase transition. - Abstract: High energy density Li{sub 2}MnO{sub 3} (layered)–LiMn{sub 1.5}Ni{sub 0.5}O{sub 4} (spinel) composite cathodes have been synthesized using auto-combustion route. Rietveld refinements together with the analyses of high resolution transmission electron micrographs confirm the structural integration of Li{sub 2}MnO{sub 3} nano-domains into the LiMn{sub 1.5}Ni{sub 0.5}O{sub 4} matrix of the composite cathodes. The discharge capacity of the composite cathodes are due to the intercalation of Li{sup +} ion in the tetrahedral (8a) and octahedral (16c) sites of the spinel component and also the insertion of Li{sup +} in the freshly prepared MnO{sub 2} lattice, formed after Li{sub 2}O extraction from the Li{sub 2}MnO{sub 3} domains. The capacity fading of the composite cathodes are explained to be due to the layered to spinel transition of the Li{sub 2}MnO{sub 3} component and Li{sup +} insertion into the octahedral site of the spinel lattices which trigger cubic to tetragonal phase transition resulting volume expansion which eventually retard the Li{sup +} intercalation with cycling.

  4. Nanocrystalline spinel ferrites by solid state reaction route

    Indian Academy of Sciences (India)

    Wintec

    Nanocrystalline spinel ferrites by solid state reaction route. T K KUNDU* and S MISHRA. Department of Physics, Visva-Bharati, Santiniketan 731 235, India. Abstract. Nanostructured NiFe2O4, MnFe2O4 and (NiZn)Fe2O4 were synthesized by aliovalent ion doping using conventional solid-state reaction route. With the ...

  5. Structural, magnetic, and dielectric properties of multiferroic Co1−xMgxCr2O4 nanoparticles

    International Nuclear Information System (INIS)

    Kamran, M.; Ullah, A.; Rahman, S.; Tahir, A.; Nadeem, K.; Anis ur Rehman, M.; Hussain, S.

    2017-01-01

    Highlights: • Properties of multiferroic Co 1−x Mg x Cr 2 O 4 nanoparticles have been studied. • XRD showed that CoCr 2 O 4 and MgCr 2 O 4 are cubic normal spinel structure. • Rietveld refinement of XRD showed no impurity phases. • T c and T s showed decreasing trend with increasing Mg concentration. • Dielectric properties were improved for x = 0.6 Mg concentration. - Abstract: We examined the structural, magnetic, and dielectric properties of Co 1−x Mg x Cr 2 O 4 nanoparticles with composition x = 0, 0.2, 0.4, 0.5, 0.6, 0.8 and 1 in detail. X-ray diffraction (XRD) revealed normal spinel structure for all the samples. Rietveld refinement fitting results of the XRD showed no impurity phases which signifies the formation of single phase Co 1−x Mg x Cr 2 O 4 nanoparticles. The average crystallite size showed a peak behaviour with maxima at x = 0.6. Raman and Fourier transform infrared (FTIR) spectroscopy also confirmed the formation of single phase normal spinel for all the samples and exhibited dominant vibrational changes for x ≥ 0.6. For x = 0 (CoCr 2 O 4 ), zero field cooled/field cooled (ZFC/FC) magnetization curves showed paramagnetic (PM) to ferrimagnetic (FiM) transition at T c = 97 K and a conical spiral magnetic order at T s = 30 K. The end members CoCr 2 O 4 (x = 0) and MgCr 2 O 4 (x = 1) are FiM and antiferromagnetic (AFM), respectively. T c and T s showed decreasing trend with increasing x, followed by an additional AFM transition at T N = 15 K for x = 0.6. The system finally stabilized and changed to highly frustrated AFM structure at x = 1 due to formation of pure MgCr 2 O 4 . High field FC curves (5T) depicted nearly no effect on spiral magnetic state, which is attributed to strong exchange B-B magnetic interactions at low temperatures. Dielectric parameters showed a non-monotonous behaviour with Mg concentration and were explained with the help of Maxwell-Wagner model and Koop’s theory. Dielectric properties were improved for

  6. Chemical synthesis of nanocrystalline magnesium aluminate spinel via nitrate-citrate combustion route

    International Nuclear Information System (INIS)

    Saberi, Ali; Golestani-Fard, Farhad; Sarpoolaky, Hosein; Willert-Porada, Monika; Gerdes, Thorsten; Simon, Reinhard

    2008-01-01

    Nanocrystalline magnesium aluminate spinel (MgAl 2 O 4 ) was synthesized using metal nitrates, citric acid and ammonium solutions. The precursor and the calcined powders at different temperatures were characterized by X-ray diffraction (XRD), simultaneous thermal analysis (STA), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The combustion mechanism was also studied by a quadrupole mass spectrometer (QMS) which coupled to STA. The generated heat through the combustion of the mixture of ammonium nitrate and citrate based complexes decreased the synthesis temperature of MgAl 2 O 4 spinel. The synthesized MgAl 2 O 4 spinel at 900 deg. C has faced shape with crystallite size in the range of 18-24 nm

  7. CoFe2O4-TiO2 Hybrid Nanomaterials: Synthesis Approaches Based on the Oil-in-Water Microemulsion Reaction Method

    Directory of Open Access Journals (Sweden)

    Arturo Adrián Rodríguez-Rodríguez

    2017-01-01

    Full Text Available CoFe2O4 nanoparticles decorated and wrapped with TiO2 nanoparticles have been prepared by mixing well-dispersed CoFe2O4 with amorphous TiO2 (impregnation approach and growing amorphous TiO2 over the magnetic core (seed approach, respectively, followed by thermal treatment to achieve TiO2 crystallinity. Synthesis strategies were based on the oil-in-water microemulsion reaction method. Thermally treated nanomaterials were characterized in terms of structure, morphology, and composition, to confirm hybrid nanoparticles formation and relate with the synthesis approaches; textural, optical, and magnetic properties were evaluated. X-ray diffraction revealed coexistence of cubic spinel-type CoFe2O4 and tetragonal anatase TiO2. Electron microscopy images depicted crystalline nanoparticles (sizes below 25 nm, with homogeneous Ti distribution for the hybrid nanoparticles synthesized by seed approach. EDX microanalysis and ICP-AES corroborated established chemical composition. XPS evidenced chemical states, as well as TiO2 predominance over CoFe2O4 surface. According to BET measurements, the hybrid nanoparticles were mesoporous. UV-Vis spectroscopy showed optical response along the UV-visible light region. Magnetic properties suggested the breaking order of magnetic domains due to modification with TiO2, especially for mediated seed approach sample. The properties of the obtained hybrid nanoparticles were different in comparison with its individual components. The results highlight the usefulness of designed microemulsion approaches for the straightforward synthesis of CoFe2O4-TiO2 nanostructured hybrids.

  8. Effect of d-block element Co{sup 2+} substitution on structural, Mössbauer and dielectric properties of spinel copper ferrites

    Energy Technology Data Exchange (ETDEWEB)

    Dar, M.A.; Varshney, Dinesh, E-mail: vdinesh33@rediffmail.com

    2017-08-15

    Highlights: • Tetragonal (I41/amd) to cubic (Fd3m) phase change is observed in Cu{sub 1−x}Co{sub x}Fe{sub 2}O{sub 4}. • Raman studies reveal 2 (5) optical active modes in CuFe{sub 2}O{sub 4} and 5 (5) at room temperature. • Transmission Mössbauer spectroscopy discerns two sets of six-line hyperfine patterns. • The dielectric constant increases is maximum for Co{sup 2+}x = 0.1 composition. • ac conductivity is constant (low frequency) and increases abruptly (high frequency). - Abstract: The present work focuses on the influence of replacement of d-block element Cu{sup 2+} ion by Co{sup 2+} in Cu-spinel ferrites [Cu{sub 1−x}Co{sub x}Fe{sub 2}O{sub 4} (x = 0.0, 0.1, 0.2, 0.4, 0.6, and 1.0)] on the structural, vibrational and dielectric properties as synthesized by Solid-state reaction route. A structural transition from tetragonal (space group I41/amd)) to cubic (space group Fd3m) phase is observed due to introduction of cobalt. Cubic spinel- type structure at room temperature of Cu{sub 1−x}Co{sub x}Fe{sub 2}O{sub 4} (0.4 ≤ x ≤ 1.0) is confirmed by Rietveld – refined X-ray powder diffraction patterns. Raman spectroscopic studies reveal 2 (5) optical active modes in CuFe{sub 2}O{sub 4} (CoFe{sub 2}O{sub 4}) at room temperature. Transmission Mössbauer spectroscopy of Cu{sub 1−x}Co{sub x}Fe{sub 2}O{sub 4} (x = 0.0, 0.2 and 0.6) shows two sets of six-line hyperfine patterns for all the three samples, indicating the presence of Fe in both A and B sites. Identification of sites is accomplished by evidence from hyperfine distribution and isomer-shift data. Dielectric constant and dielectric loss tangent measured in the frequency range from 1 KHz to 1 MHz at room temperature are found to be decreasing with the increase in frequency.

  9. A simple aloe vera plant-extracted microwave and conventional combustion synthesis: Morphological, optical, magnetic and catalytic properties of CoFe2O4 nanostructures

    Science.gov (United States)

    Manikandan, A.; Sridhar, R.; Arul Antony, S.; Ramakrishna, Seeram

    2014-11-01

    Nanocrystalline magnetic spinel CoFe2O4 was synthesized by a simple microwave combustion method (MCM) using ferric nitrate, cobalt nitrate and Aloe vera plant extracted solution. For the comparative study, it was also prepared by a conventional combustion method (CCM). Powder X-ray diffraction, energy dispersive X-ray and selected-area electron diffraction results indicate that the as-synthesized samples have only single-phase spinel structure with high crystallinity and without the presence of other phase impurities. The crystal structure and morphology of the powders were revealed by high resolution scanning electron microscopy and transmission electron microscopy, show that the MCM products of CoFe2O4 samples contain sphere-like nanoparticles (SNPs), whereas the CCM method of samples consist of flake-like nanoplatelets (FNPs). The band gap of the samples was determined by UV-Visible diffuse reflectance and photoluminescence spectroscopy. The magnetization (Ms) results showed a ferromagnetic behavior of the CoFe2O4 nanostructures. The Ms value of CoFe2O4-SNPs is higher i.e. 77.62 emu/g than CoFe2O4-FNPs (25.46 emu/g). The higher Ms value of the sample suggest that the MCM technique is suitable for preparing high quality nanostructures for magnetic applications. Both the samples were successfully tested as catalysts for the conversion of benzyl alcohol. The resulting spinel ferrites were highly selective for the oxidation of benzyl alcohol and exhibit important difference among their activities. It was found that CoFe2O4-SNPs catalyst show the best performance, whereby 99.5% selectivity of benzaldehyde was achieved at close to 93.2% conversion.

  10. Anisotropic dislocation loop nucleation in ion-irradiated MgAl2O4

    International Nuclear Information System (INIS)

    Zinkle, S.J.

    1991-01-01

    Polycrystalline disks of stoichiometric magnesium aluminate spinel (MgAl 2 O 4 ) were irradiated with 2 MeV Al + ions at 650 degrees C and subsequently analyzed in cross-section using transmission electron microscopy (TEM). Interstitial dislocation loops were observed on 110 and 11 habit planes. The population of loops on both sets of habit planes was strongly dependent on their orientation with respect to the ion beam direction. The density of loops with habit plane normals nearly perpendicular to the ion beam direction much higher than loops with habit plane normals nearly parallel to the ion beam direction. On the other hand, the loop size was nearly independent of habit plane orientation. This anisotropic loop nucleation does not occur in ion-irradiated metals such as copper. An additional anomaly associated with ion-irradiated spinel is that the loops on 111 planes were partially unfaulted with a Burgers vector of b = a/4 . Previous neutron irradiation studies have never reported unfaulted loops in stoichiometric spinel. Possible cause of the unusual response of spinel to ion irradiation are discussed. 12 refs., 14 figs

  11. Full-potential calculations of structural, elastic and electronic properties of MgAl2O4 and ZnAl2O4 compounds

    International Nuclear Information System (INIS)

    Khenata, R.; Sahnoun, M.; Baltache, H.; Rerat, M.; Reshak, Ali H.; Al-Douri, Y.; Bouhafs, B.

    2005-01-01

    Theoretical studies of structural, elastic and electronic properties of spinel MgAl 2 O 4 and ZnAl 2 O 4 oxides are presented, using the full-potential linear augmented plane wave (FP-LAPW) method as implemented in the WIEN97 code. In this approach the local density approximation (LDA) is used for the exchange-correlation (XC) potential. Results are given for lattice constant, bulk modulus, and its pressure derivative. The band structure, density of states, pressure coefficients of energy gaps and elastic constants are also given. We present a detailed comparison with available experimental data and previous calculations. Good agreement is found

  12. Ferri-magnetic order in Mn induced spinel Co_3_−_xMn_xO_4 (0.1≤x≤1.0) ceramic compositions

    International Nuclear Information System (INIS)

    Meena, P.L.; Sreenivas, K.; Singh, M.R.; Kumar, Ashok; Singh, S.P.; Kumar, Ravi

    2016-01-01

    We report structural and magnetic properties of spinel Co_3_−_xMn_xO_4 (x=0.1–1.0) synthesized by solid state reaction technique. Rietveld refinement analysis of X-ray diffraction (XRD) data, revealed the formation of polycrystalline single phase Co_3_−_xMn_xO_4 without any significant structural change in cubic crystal symmetry with Mn substitution, except change in lattice parameter. Temperature dependent magnetization data show changes in magnetic ordering temperature, indicating formation of antiferromagnetic (AFM) and ferrimagnetic (FM) phase at low Mn concentration (x≤0.3) and well-defined FM phase at high Mn concentration (x≥0.5). The isothermal magnetization records established an AFM/FM mixed phase for composition ranging 0.1 0.5. - Highlights: • Synthesis of single phase polycrystalline Co_3_−_xMn_xO_4 ceramic. • Change in magnetic ordering with varying Mn concentration. • The complex spin distribution is contributing to FM ordering with higher Mn.

  13. Thermally-induced electronic relaxation in structurally-modified Cu0.1Ni0.8Co0.2Mn1.9O4 spinel ceramics

    International Nuclear Information System (INIS)

    Shpotyuk, O.; Balitska, V.; Brunner, M.; Hadzaman, I.; Klym, H.

    2015-01-01

    Thermally-induced electronic relaxation in structurally-modified Cu 0.1 Ni 0.8 Co 0.2 Mn 1.9 O 4 spinel ceramics is shown to be adequately described by stretched exponential function on time. This kinetics is defined by microsctructure perfectness of the relaxing media, showing obvious onset to stretched exponential behaviour with non-exponentionality index attaining close to 0.43 values for high-monolith ceramics and smaller ones in fine-grained ceramics. Percolation threshold in relaxation-degradation kinetics is detected for ceramics with 10% of NiO extractions, showing the smallest but most prolonged single-path degradation effect. This finding is treated in terms of Phillips’ axiomatic diffusion-to-trap model, where only one of two relaxation channels (caused by operative short-range forces) occurs to be effective, while additional non-operative channels contribute to electronic relaxation in fine-grained ceramics

  14. Nickel stabilization efficiency of aluminate and ferrite spinels and their leaching behavior.

    Science.gov (United States)

    Shih, Kaimin; White, Tim; Leckie, James O

    2006-09-01

    Stabilization efficiencies of spinel-based construction ceramics incorporating simulated nickel-laden waste sludge were evaluated and the leaching behavior of products investigated. To simulate the process of immobilization, nickel oxide was mixed alternatively with gamma-alumina, kaolinite, and hematite. These tailoring precursors are commonly used to prepare construction ceramics in the building industry. After sintering from 600 to 1480 degrees C at 3 h, the nickel aluminate spinel (NiAl204) and the nickel ferrite spinel (NiFe204) crystallized with the ferrite spinel formation commencing about 200-300 degrees C lower than for the aluminate spinel. All the precursors showed high nickel incorporation efficiencies when sintered at temperatures greater than 1250 degrees C. Prolonged leach tests (up to 26 days) of product phases were carried out using a pH 2.9 acetic acid solution, and the spinel products were invariably superior to nickel oxide for immobilization over longer leaching periods. The leaching behavior of NiAl2O4 was consistent with congruent dissolution without significant reprecipitation, but for NiFe2O4, ferric hydroxide precipitation was evident. The major leaching reaction of sintered kaolinite-based products was the dissolution of cristobalite rather than NiAl2O4. This study demonstrated the feasibility of transforming nickel-laden sludge into spinel phases with the use of readily available and inexpensive ceramic raw materials, and the successful reduction of metal mobility under acidic environments.

  15. Preparation of LiMn2O4 Graphene Hybrid Nanostructure by Combustion Synthesis and Their Electrochemical Properties

    Directory of Open Access Journals (Sweden)

    Dinesh Rangappa

    2014-10-01

    Full Text Available The LiMn2O4 graphene hybrid cathode material has been synthesized by spray drying combustion process. The spinel structure cubic phase LiMn2O4 graphene hybrid material was prepared by spray drying process at 120 ℃ and subsequent heat treatment at 700 ℃ for 1 hour. The result indicates that the spinel shaped LiMn2O4 particles wrapped with graphene sheets were formed with particle size in the range of 60-70 nm. The charge-discharge measurement indicates that the LiMn2O4 graphene hybrid material shows an improved discharge capacity of 139 mAh/g at 0.1C rate. The pristine LiMn2O4 nano crystals present only about 132 mAh/g discharge capacity. The LiMn2O4 graphene hybrid samples show good cyclic performance with only 13% of capacity fading in 30 cycles when compared to the pristine LiMn2O4 that shows 22% of capacity fading in 30 cycles. The capacity retention of the LiMn2O4 graphene hybrid samples is about 10% higher than the pristine cycle after 30 cycles.

  16. Synthesis and Characterization of Polyol-Assisted Nano Cu0.2Ni0.2Sn0.2Ba0.4 Fe2O4 by a Wet Hydroxyl Route

    Science.gov (United States)

    Pavithradevi, S.; Suriyanarayanan, N.; Boobalan, T.; Velumani, S.; Chandramohan, M.; Manivel Raja, M.

    2017-08-01

    Nanocrystalline spinel ferrite of composition Cu0.2Ni0.2Sn0.2Ba0.4 Fe2O4 has been synthesized by a wet hydroxyl chemical route in ethylene glycol as chelating agent and sodium hydroxide as precipitator at pH 8. Ethylene glycol has been used as the medium which serves as the solvent as well as a complexing agent. The synthesized particles are annealed at temperatures of 350°C, 700°C, and 1050°C. Thermogravimetric (TG) analysis confirms that at 240°C, ethylene glycol has evaporated completely, and a stable phase is formed above 670°C. Fourier transform infrared (FT-IR) spectroscopy of mixed Cu0.2Ni0.2Sn0.2Ba0.4 ferrite nanoparticles like as synthesized and annealed at 1050°C are recorded between 400 cm-1 and 4000 cm-1. FT-IR appraises the structural formation of Cu0.2Ni0.2Sn0.2Ba0.4 Fe2O4 between the as-synthesized sample and the sample annealed at 1050°C. Structural characterizations of all the samples are carried out by x-ray diffraction (XRD) technique. XRD reveals that the particle size increases with the increase in annealing temperatures. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) confirms that the particles are flaky and spherical with the crystallite size in the range of 11-27 nm. The decrement of dielectric properties, like dielectric constant and dielectric loss, with the increment of frequency as seen in all the samples is an usual dielectric behavior of spinel ferrites. The lack of net magnetization is noticed immediately when the applied magnetic field is removed which prompts superparamagnetic behavior, as seen in all the samples.

  17. Chemical vs. electrochemical extraction of lithium from the Li-excess Li(1.10)Mn(1.90)O4 spinel followed by NMR and DRX techniques.

    Science.gov (United States)

    Martinez, S; Sobrados, I; Tonti, D; Amarilla, J M; Sanz, J

    2014-02-21

    Lithium extraction from the Li-excess Li1.10Mn1.90O4 spinel has been performed by chemical and electrochemical methods in aqueous and in organic media, respectively. De-lithiated samples have been investigated by XRD, SEM, TG, (7)Li and (1)H MAS-NMR techniques. The comparative study has allowed demonstrating that the intermediate de-intercalated samples prepared during the chemical extraction by acid titration are similar to those prepared by the electrochemical way in a non-aqueous electrolyte. LiMn2O4 based spinel with a tailored de-lithiation degree can be prepared as a single phase by controlling the pH used in chemical extraction. (7)Li MAS-NMR spectroscopy has been used to follow the influence of the manganese oxidation state on tetra and octahedral Li-signals detected in Li-extracted samples. The oxidation of Mn(III) ions goes parallel to the partial dissolution of the spinel, following Hunter's mechanism. Based on this mechanism, a generalized chemical reaction has been proposed to explain the formation of intermediate Li(+) de-intercalated samples during acid treatment in aqueous media. By the (1)H MAS NMR study, no evidence of Li-H topotactic exchange in the bulk of the acid treated material was found.

  18. Degradation of polychlorinated biphenyls using mesoporous iron-based spinels

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Linyan; Su, Guijin, E-mail: gjsu@rcees.ac.cn; Zhang, Aiqian; Shi, Yali; Xia, Chaobo; Lu, Huijie; Li, Liewu; Liu, Sha; Zheng, Minghui

    2013-10-15

    Highlights: • The NiFe{sub 2}O{sub 4} had the highest activity in degradation of CB-209, followed by Fe{sub 3}O{sub 4}. • Hydroxyl species, organic acids, PCBs and chlorobenzenes were identified as products. • Three degradation reactions and one combination reaction competitively occurred. • Hydrodechlorination of CB-209 was more favored over Fe{sub 3}O{sub 4} than NiFe{sub 2}O{sub 4}. • Oxidation reaction of CB-209 was more favored over NiFe{sub 2}O{sub 4} than Fe{sub 3}O{sub 4}. -- Abstract: A series of mesoporous iron-based spinel materials were synthesized to degrade polychlorinated biphenyls (PCBs), with CB-209 being used as a model compound. The materials were characterized by X-ray powder diffraction (XRD), pore structure analysis, and X-ray photoelectron spectroscopy (XPS). A comparison of the dechlorination efficiencies (DEs) of the materials revealed that NiFe{sub 2}O{sub 4} had the highest DE, followed by Fe{sub 3}O{sub 4}. Newly produced polychlorinated biphenyls, chlorinated benzenes, hydroxyl species and organic acids were detected by gas chromatography–mass spectrometry, high performance liquid chromatography–mass spectrometry and ion chromatograph. Identification of the intermediate products indicates that three degradation pathways, hydrodechlorination, the breakage of C-C bridge bond and oxidative reaction, accompanied by one combination reaction, are competitively occurring over the iron-based spinels. The relative amounts of produced three NoCB isomers were illustrated by the C-Cl BDEs of CB-209 at meta-, para- and ortho-positions, and their energy gap between HOMO and LUMO. The consumption of the reactive oxygen species caused by the transformation of Fe{sub 3}O{sub 4} into Fe{sub 2}O{sub 3} in the Fe{sub 3}O{sub 4} reaction system, and the existence of the highly reactive O{sub 2}{sup −}· species in the NiFe{sub 2}O{sub 4} reaction system, could provide a reason why the oxidation reaction was more favored over NiFe{sub 2}O

  19. Structural, magnetic, and dielectric properties of multiferroic Co1-xMgxCr2O4 nanoparticles

    Science.gov (United States)

    Kamran, M.; Ullah, A.; Rahman, S.; Tahir, A.; Nadeem, K.; Anis ur Rehman, M.; Hussain, S.

    2017-07-01

    We examined the structural, magnetic, and dielectric properties of Co1-xMgxCr2O4 nanoparticles with composition x = 0, 0.2, 0.4, 0.5, 0.6, 0.8 and 1 in detail. X-ray diffraction (XRD) revealed normal spinel structure for all the samples. Rietveld refinement fitting results of the XRD showed no impurity phases which signifies the formation of single phase Co1-xMgxCr2O4 nanoparticles. The average crystallite size showed a peak behaviour with maxima at x = 0.6. Raman and Fourier transform infrared (FTIR) spectroscopy also confirmed the formation of single phase normal spinel for all the samples and exhibited dominant vibrational changes for x ≥ 0.6. For x = 0 (CoCr2O4), zero field cooled/field cooled (ZFC/FC) magnetization curves showed paramagnetic (PM) to ferrimagnetic (FiM) transition at Tc = 97 K and a conical spiral magnetic order at Ts = 30 K. The end members CoCr2O4 (x = 0) and MgCr2O4 (x = 1) are FiM and antiferromagnetic (AFM), respectively. Tc and Ts showed decreasing trend with increasing x, followed by an additional AFM transition at TN = 15 K for x = 0.6. The system finally stabilized and changed to highly frustrated AFM structure at x = 1 due to formation of pure MgCr2O4. High field FC curves (5T) depicted nearly no effect on spiral magnetic state, which is attributed to strong exchange B-B magnetic interactions at low temperatures. Dielectric parameters showed a non-monotonous behaviour with Mg concentration and were explained with the help of Maxwell-Wagner model and Koop's theory. Dielectric properties were improved for nanoparticles with x = 0.6 and is attributed to their larger average crystallite size. In summary, Mg doping has significantly affects the structural, magnetic, and dielectric properties of CoCr2O4 nanoparticles, which can be attributed to variations in local magnetic exchange interactions and variation in average crystallite size of these chromite nanoparticles.

  20. Preparation of submicrocrystal LiMn2O4 used Mn3O4 as precursor and its electrochemical performance for lithium ion battery

    International Nuclear Information System (INIS)

    Liu, Bao-Sheng; Wang, Zhen-Bo; Zhang, Yin; Yu, Fu-Da; Xue, Yuan; Ke, Ke; Li, Fang-Fei

    2015-01-01

    Graphical abstract: Spinal LiMn 2 O 4 particles synthesized at 800 °C for 12 h has the best crystallinity with a submicron size and smallest cation disorder, resulting in a superior capacity retention ratio of 90.4% after 200 cycles at 1 °C at room temperature, which possesses an initial capacity of 106.8 mA h/g. - Highlights: • High purity spinel LiMn 2 O 4 was synthesized from industrial grade raw materials. • LiMn 2 O 4 prepared by optimal conditions has the smallest cation mixing. • Optimized LiMn 2 O 4 has the highest initial capacity with 112.9 mA h/g. • Capacity retention of optimized LiMn 2 O 4 is 90.4% after 200 cycles at 1 °C. - Abstract: Spinel LiMn 2 O 4 has been synthesized by solid state reaction with industrial grade Mn 3 O 4 and Li 2 CO 3 as precursors without purification, and its electrochemical performance for lithium ion battery has been investigated by CR2025 coin cell. The results of X-ray diffraction (XRD) patterns and scanning electron microscope (SEM) images show that the size of LiMn 2 O 4 particles grow up with increasing temperature of calcination, and the sample synthesized at 800 °C for 12 h has the best crystallinity with a submicron size. It can deliver initial capacity of 112.9 mA h/g with capacity retention ratio of 89.1% after 200 cycles at charge/discharge rate of 1 C. The results of cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) also show that it has the highest electrochemical activity and lowest charge transfer impedance

  1. Cations in Octahedral Sites: A Descriptor for Oxygen Electrocatalysis on Transition-Metal Spinels

    Energy Technology Data Exchange (ETDEWEB)

    Wei, Chao; Feng, Zhenxing; Scherer, Günther G.; Barber, James; Shao-Horn, Yang; Xu, Zhichuan J. (Nanyang); (ICL); (Oregon State U.); (TUM-CREATE); (MIT)

    2017-04-10

    Exploring efficient and low-cost electrocatalysts for the oxygen-reduction reaction (ORR) and oxygen-evolution reaction (OER) is critical for developing renewable energy technologies such as fuel cells, metal–air batteries, and water electrolyzers. A rational design of a catalyst can be guided by identifying descriptors that determine its activity. Here, a descriptor study on the ORR/OER of spinel oxides is presented. With a series of MnCo2O4, the Mn in octahedral sites is identified as an active site. This finding is then applied to successfully explain the ORR/OER activities of other transition-metal spinels, including MnxCo3-xO4 (x = 2, 2.5, 3), LixMn2O4 (x = 0.7, 1), XCo2O4 (X = Co, Ni, Zn), and XFe2O4 (X = Mn, Co, Ni). A general principle is concluded that the eg occupancy of the active cation in the octahedral site is the activity descriptor for the ORR/OER of spinels, consolidating the role of electron orbital filling in metal oxide catalysis.

  2. Experimental and ab initio investigations on textured Li–Mn–O spinel thin film cathodes

    Energy Technology Data Exchange (ETDEWEB)

    Fischer, J., E-mail: Julian.Fischer@kit.edu [Karlsruhe Institute of Technology (KIT), Institute for Applied Materials (IAM), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Music, D. [RWTH Aachen University, Materials Chemistry, Kopernikusstrasse 10, 52074 Aachen (Germany); Bergfeldt, T.; Ziebert, C.; Ulrich, S.; Seifert, H.J. [Karlsruhe Institute of Technology (KIT), Institute for Applied Materials (IAM), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany)

    2014-12-01

    This paper describes the tailored preparation of nearly identical lithium–manganese–oxide thin film cathodes with different global grain orientations. The thin films were synthesized by rf magnetron sputtering from a LiMn{sub 2}O{sub 4}-target in a pure argon plasma. Under appropriate processing conditions, thin films with a cubic spinel structure and a nearly similar density and surface topography but different grain orientation, i.e. (111)- and (440)-textured films, were achieved. The chemical composition was determined by inductively coupled plasma optical emission spectroscopy and carrier gas hot extraction. The constitution- and microstructure were evaluated by X-ray diffraction and Raman spectroscopy. The surface morphology and roughness were investigated by scanning electron and atomic force microscopy. The differently textured films represent an ideal model system for studying potential effects of grain orientation on the lithium ion diffusion and electrochemical behavior in LiMn{sub 2}O{sub 4}-based thin films. They are nearly identical in their chemical composition, atomic bonding behavior, surface-roughness, morphology and thickness. Our initial ab initio molecular dynamics data indicate that Li ion transport is faster in (111)-textured structure than in (440)-textured one. - Highlights: • Thin film model system of differently textured cubic Li–Mn–O spinels. • Investigation of the Li–Mn–O thin film mass density by X-ray reflectivity. • Ab initio molecular dynamics simulation on Li ion diffusion in LiMn{sub 2}O{sub 4}.

  3. Experimental and ab initio investigations on textured Li–Mn–O spinel thin film cathodes

    International Nuclear Information System (INIS)

    Fischer, J.; Music, D.; Bergfeldt, T.; Ziebert, C.; Ulrich, S.; Seifert, H.J.

    2014-01-01

    This paper describes the tailored preparation of nearly identical lithium–manganese–oxide thin film cathodes with different global grain orientations. The thin films were synthesized by rf magnetron sputtering from a LiMn 2 O 4 -target in a pure argon plasma. Under appropriate processing conditions, thin films with a cubic spinel structure and a nearly similar density and surface topography but different grain orientation, i.e. (111)- and (440)-textured films, were achieved. The chemical composition was determined by inductively coupled plasma optical emission spectroscopy and carrier gas hot extraction. The constitution- and microstructure were evaluated by X-ray diffraction and Raman spectroscopy. The surface morphology and roughness were investigated by scanning electron and atomic force microscopy. The differently textured films represent an ideal model system for studying potential effects of grain orientation on the lithium ion diffusion and electrochemical behavior in LiMn 2 O 4 -based thin films. They are nearly identical in their chemical composition, atomic bonding behavior, surface-roughness, morphology and thickness. Our initial ab initio molecular dynamics data indicate that Li ion transport is faster in (111)-textured structure than in (440)-textured one. - Highlights: • Thin film model system of differently textured cubic Li–Mn–O spinels. • Investigation of the Li–Mn–O thin film mass density by X-ray reflectivity. • Ab initio molecular dynamics simulation on Li ion diffusion in LiMn 2 O 4

  4. Urea-nitrate combustion synthesis of MgO/MgAl2O4 nanocatalyst used in biodiesel production from sunflower oil: Influence of fuel ratio on catalytic properties and performance

    International Nuclear Information System (INIS)

    Rahmani Vahid, Behgam; Haghighi, Mohammad

    2016-01-01

    Graphical abstract: As a base catalyst for biodiesel production, MgAl 2 O 4 spinel was successfully synthesized by combustion method with MgO, as the active phase, dispersed on the catalyst surface. The nanocatalysts were characterized by XRD, FESEM, EDX, BET-BJH, TGA and FTIR analyses, so as to optimize the concentration of urea (as fuel) in the combustion synthesis. Analyzing the effect of fuel ratio on the combustion synthesized MgAl 2 O 4 , it was revealed that the synthesized base catalyst with a fuel ratio of 1.5 was of the best specifications for biodiesel production process. Future researches may investigate the catalyst reusability and mild reaction conditions, so as to achieve more economical production of biodiesel. - Highlights: • Efficient synthesis of MgAl 2 O 4 spinel by solution combustion method. • Improvement of catalytic activity and stability by optimum ratio fuel. • Enhanced dispersion of MgO over MgAl 2 O 4 spinel. • Production of biodiesel over MgO/MgAl 2 O 4 at relatively mild reaction conditions. - Abstract: MgO/MgAl 2 O 4 nanocatalyst was synthesized by a simple, cost-effective and rapid method and used in biodiesel production from sunflower oil. MgAl 2 O 4 was synthesized by combustion method at different fuel ratios and then active phase of MgO was dispersed on the samples by impregnation method. The nanocatalysts were characterized by XRD, FESEM, EDX, BET-BJH, TGA and FTIR analyses, so as to optimize the concentration of urea (as fuel) in the combustion synthesis. The physicochemical properties of the nanocatalyst confirmed the sample synthesized with fuel ratio of 1.5 has high surface area, effective morphology and texture properties. Finally, in order to evaluate catalytic activity of the samples in biodiesel production, the transesterification reaction was performed. The results indicated the catalyst prepared by combustion synthesis with a fuel ratio of 1.5 was optimum specifications for biodiesel production. Using this

  5. Microscopic origin of the mobility enhancement at a spinel/perovskite oxide heterointerface revealed by photoemission spectroscopy

    DEFF Research Database (Denmark)

    Schuetz, P.; Christensen, Dennis Valbjørn; Borisov, V.

    2017-01-01

    The spinel/perovskite heterointerface γ−Al2O3/SrTiO3 hosts a two-dimensional electron system (2DES) with electron mobilities exceeding those in its all-perovskite counterpart LaAlO3/SrTiO3 by more than an order of magnitude, despite the abundance of oxygen vacancies which act as electron donors a...

  6. γ-irradiation induced zinc ferrites and their enhanced room-temperature ammonia gas sensing properties

    Science.gov (United States)

    Raut, S. D.; Awasarmol, V. V.; Ghule, B. G.; Shaikh, S. F.; Gore, S. K.; Sharma, R. P.; Pawar, P. P.; Mane, R. S.

    2018-03-01

    Zinc ferrite (ZnFe2O4) nanoparticles (NPs), synthesized using a facile and cost-effective sol-gel auto-combustion method, were irradiated with 2 and 5 kGy γ-doses using 60Co as a radioactive source. Effect of γ-irradiation on the structure, morphology, pore-size and pore-volume and room-temperature (300 K) gas sensor performance has been measured and reported. Both as-synthesized and γ-irradiated ZnFe2O4 NPs reveal remarkable gas sensor activity to ammonia in contrast to methanol, ethanol, acetone and toluene volatile organic gases. The responses of pristine, 2 and 5 kGy γ-irradiated ZnFe2O4 NPs are respectively 55%, 66% and 81% @100 ppm concentration of ammonia, signifying an importance of γ-irradiation for enhancing the sensitivity, selectivity and stability of ZnFe2O4 NPs as ammonia gas sensors. Thereby, due to increase in surface area and crystallinity on γ-doses, the γ-irradiation improves the room-temperature ammonia gas sensing performance of ZnFe2O4.

  7. Self-propagating high temperature synthesis, structural morphology and magnetic interactions in rare earth Ho{sup 3+} doped CoFe{sub 2}O{sub 4} nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Lohar, K.S. [Materials Research Laboratory, Srikrishna Mahavidyalaya Gunjoti, Omerga, Osmanabad 413 613, MS (India); Pachpinde, A.M.; Langade, M.M. [Department of Chemistry, Jawahar Art Science and Commerce College Andur, Osmanabad, MS (India); Kadam, R.H. [Materials Research Laboratory, Srikrishna Mahavidyalaya Gunjoti, Omerga, Osmanabad 413 613, MS (India); Shirsath, Sagar E., E-mail: shirsathsagar@hotmail.com [Spin Device Technology Center, Department of Information Engineering, Shinshu University, Nagano 380-8553 (Japan)

    2014-08-01

    Highlights: • Rare earth Ho{sup 3+} substituted CoFe{sub 2}O{sub 4.} • XRD and IR spectra reveal the spinel structure. • Magnetization and coercivity increased with Ho{sup 3+} substitution. - Abstract: Substitution effect of rare earth trivalent Ho{sup 3+} ions on the composition, Ho{sub x}CoFe{sub 2−x}O{sub 4}, with x varying from 0.0 to 0.1 in steps of 0.025 using sol–gel auto combustion route has been investigated. Examination of X-ray diffraction (XRD) patterns shows that all the samples consisted of ferrite phases of typical spinel cubic structure, and when Ho{sup 3+} ion content was x ⩾ 0.075, orthoferrite–HoFeO{sub 3} phase was detected. The micro and nanostructure of the synthesized Ho doped CoFe{sub 2}O{sub 4} ferrites were investigated by scanning and transmission electron microscopy respectively. With increasing doping content of Ho{sup 3+} ions, the lattice constant, particle size and bulk density increased, and after an increase to its maximum value, the sample particle size and density dropped down. Cation distribution estimated from XRD patter revealed that the Co{sup 2+} and Ho{sup 3+} ions prefer to occupy octahedral B-site whereas Fe{sup 3+} ions are distributed over tetra- and octa-hedral site. Oxygen positional parameter shows larger values than its ideal value. The analysis of magnetic properties revealed that the saturation magnetization and coercivity of CoFe{sub 2}O{sub 4} increased with the rare earth Ho{sup 3+} substitution.

  8. Phase purity of NiCo2O4, a catalyst candidate for electrolysis of water

    Science.gov (United States)

    Singer, J.; Fielder, W. L.; Garlick, R. G.; Negas, T.

    1987-01-01

    NiCo2O4 is shown to be difficult to obtain as a pure phase, and may never have been so obtained. High resolution x-ray diffractometry is required for its precise characterization. Film XRD is not likely to show the asymmetry in the spinel diffraction lines, caused by poorly crystallized NiO, as seen in diffractometer traces. The Co3O4 which is expected to accompany NiO as an impurity in NiCo2O4 syntheses has the same diffraction pattern as the binary oxide. Firings of the co-precipitated hydroxides at 300, 350, and 400 C, including one in pure O2, failed to produce single phase cobaltate. Scanning electron microscopy showed all the sintered products to range over several orders of magnitude in agglomerate/particle size. Surface areas by BET were all in the range 40 to 110 m sq/g, equivalent to particles of 200 to 100 Angstrom diameter. The spinel diffraction line breadths were compatible with those approximate dimensions.

  9. Effect of Gd"3"+ substitution on structural, magnetic, dielectric and optical properties of nanocrystalline CoFe_2O_4

    International Nuclear Information System (INIS)

    Joshi, Seema; Kumar, Manoj; Chhoker, Sandeep; Kumar, Arun; Singh, Mahavir

    2017-01-01

    Nanoparticles of CoGd_xFe_2_−_xO_4 with x=0.0, 0.03, 0.05, 0.07, 0.10 and 0.15 were synthesized by co-precipitation method. Gd"3"+ substitution effect on different properties of nanocrystalline CoFe_2O_4 has been studied. X-ray diffraction and Raman spectroscopy confirmed the formation of single phase cubic mixed spinel structure. Cation distribution has been proposed from Rietveld refined data. Mössbauer spectra at room temperature showed two ferrimagnetic Zeeman sextets with one superparamagnetic doublet. Mössbauer parameters suggested that Gd"3"+ ions occupy the octahedral site in CoFe_2O_4. Room temperature magnetic measurements exhibited that the saturation magnetization decreased from 91 emu/gm to 54 emu/gm for x=0.0 to 0.15 samples. The coercivity decreased from 1120 Oe to 340 Oe for x=0.0 to 0.07 samples and increased from 400 Oe to 590 Oe for x=0.10 and 0.15 samples, respectively. Raman analysis showed that the degree of inversion with Gd"3"+ substitution supporting the variation of coercivity. Electron spin resonance spectra revealed the dominancy of superexchange interactions in these samples. Optical band gap measurement suggested that all samples are indirect band gap materials and band gap has been decreased with Gd"3"+ substitution. Both dielectric constant and dielectric loss is found to decrease because of the decrease in hopping rate with the Gd"3"+ substitution for Fe"3"+ at the octahedral sites. Low dielectric loss suggested the applicability of Gd"3"+ doped CoFe_2O_4 nanoparticles for high frequency microwave device applications. - Highlights: • Gd"3"+ ions were successfully added in to the spinel lattice of CoFe_2O_4. • Magnetic hysteresis loss is influenced by Gd"3"+ doping. • All doped samples exhibit normal dielectric dispersion behaviour of spinel ferrites. • UV–vis diffuse spectroscopy concludes band gap is reduced by Gd"3"+ doping.

  10. Neutron Powder Diffraction Measurements of the Spinel MgGa2O4:Cr3+ - A Comparative Study between the High Flux Diffractometer D2B at the ILL and the High Resolution Powder Diffractometer Aurora at IPEN

    International Nuclear Information System (INIS)

    Da Silva, M A F M; Sosman, L P; Yokaichiya, F; Henry, P F; Bordallo, H N; Mazzocchi, V L; Parente, C B R; Mestnik-Filho, J

    2012-01-01

    Optical materials that emit from the visible to the near-infrared spectral region are of great interest due to their possible application as tunable radiation sources, as signal transmission, display, optoelectronics signal storage, cellulose industry as well as in dosimetry. One important family of such systems are the spinel compounds doped with Cr 3+ , in which the physical the properties are related to the insertion of punctual defects in the crystalline structure. The purpose of our work is two fold. First, we compare the luminescence of the MgGa 2 O 4 -Ga 2 O 3 system with the single phase Ga 2 O 3 and MgGa 2 O 4 and relate structural changes observed in MgGa 2 O 4 -Ga 2 O 3 system to the optical properties, and secondly, to compare the neutron powder diffraction results obtained using two diffractometers: D2B located at the ILL (Grenoble, France) and Aurora located at IPEN (São Paulo, Brazil). In the configuration chosen, Aurora shows an improved resolution, which is related to the design of its silicon focusing monochromator.

  11. Inhomogeneous magnetic phase in Co–Al–O spinel nanocrystals

    Energy Technology Data Exchange (ETDEWEB)

    Sato, K., E-mail: sato.koichi@nims.go.jp [National Institute for Materials Science, 2-1-1 Sengen, Tsukuba, Ibaraki 305-0047 (Japan); Naka, T., E-mail: naka.takashi@nims.go.jp [National Institute for Materials Science, 2-1-1 Sengen, Tsukuba, Ibaraki 305-0047 (Japan); Nakane, T. [National Institute for Materials Science, 2-1-1 Sengen, Tsukuba, Ibaraki 305-0047 (Japan); Rangappa, D. [International Advanced Research Centre for Powder Metallurgy and New Materials, Balapur PO, Hyderabad 500-005 (India); Takami, S. [Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai, Miyagi 980-8577 (Japan); Ohara, S. [Joining and Welding Research Institute, Osaka University, 11-1 Mihogaoka, Ibaraki, Osaka 567-0047 (Japan); Adschiri, T. [WPI, Advanced Institute for Materials Research, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai, Miyagi 980-8577 (Japan)

    2014-01-15

    We report on the crystallographic structure and magnetism of 5-nm Co–Al–O spinel nanocrystals synthesized under supercritical hydrothermal conditions. Structural examination using powder X-ray diffraction and chemical analysis showed the composition of the sample to be Co{sub 0.47}Al{sub 2.36}O{sub 4} rather than the stoichiometric composition of CoAl{sub 2}O{sub 4}. The site occupancy of Co on the A-site forming the diamond lattice was 0.47, which is slightly larger than the site percolation limit. Magnetization measurements showed that magnetic clusters emerged below 40 K. At temperatures below 40 K, a Griffiths-phase-like inhomogeneous state appeared in the sample in which magnetic clusters and paramagnetic spins coexisted. The dc-paramagnetic and ac-susceptibilities exhibited an anomaly below 7 K. - Highlights: • The synthesized sample had an Al-rich structure described by Co{sub 0.47}Al{sub 2.36}O{sub 4}. • The site occupancy of Co at the A-site is larger than the site percolation limit of the A-site. • The non-linearity of the magnetization appeared at T<40 K. • The paramagnetic component showed a peak at 7 K. • An inhomogeneous state is established in our Co–Al oxide nanocrystals.

  12. Neutron Powder Diffraction Measurements of the Spinel MgGa 2 O 4 :Cr 3+ - A Comparative Study between the High Flux Diffractometer D2B at the ILL and the High Resolution Powder Diffractometer Aurora at IPEN

    DEFF Research Database (Denmark)

    Silva, M A F M da; Sosman, L P; Yokaichiya, F

    2012-01-01

    Optical materials that emit from the visible to the near-infrared spectral region are of great interest due to their possible application as tunable radiation sources, as signal transmission, display, optoelectronics signal storage, cellulose industry as well as in dosimetry. One important family...... of such systems are the spinel compounds doped with Cr 3+ , in which the physical the properties are related to the insertion of punctual defects in the crystalline structure. The purpose of our work is two fold. First, we compare the luminescence of the MgGa 2 O 4 -Ga 2 O 3 system with the single phase Ga 2 O 3...

  13. Amplification of the discharge current density of lithium-ion batteries with spinel phase Li(PtAu)0.02Mn1.98O4 nano-materials

    CSIR Research Space (South Africa)

    Ross, N

    2014-05-01

    Full Text Available -ion batteries (LIB) was synthesized by incorporation of the Pt-Au (1:1) nanoparticles onto the spinel phase LiMn(sub2)O(sub4). Ultra-low scan rate (0.01 mV (sups-1)) cyclic voltammetry of the cathode material in 1 M LiPF(sub6) (in 1:1 EC:DMC), showed four sets...

  14. SYNTHESIS OF M–Nd DOPED Fe3O4 NANOPARTICLES (M = Co ...

    African Journals Online (AJOL)

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    nanoparticles were spherical shaped with inverse spinel structure. ... To obtain nano sized spinel ferrite particles, various preparation techniques have been ... SEM images of (a) Fe3O4, (b) Fe3O4 doped with Nd3+ and Co2+, (c) Fe3O4 doped with. Nd3+ .... Nayar, S.; Mir, A.; Ashok, A.; Sharma, A. J. Bionic Eng. 2010, 7, 29.

  15. NiCo2O4-Based Supercapacitor Nanomaterials

    OpenAIRE

    Chenggang Wang; E Zhou; Weidong He; Xiaolong Deng; Jinzhao Huang; Meng Ding; Xianqi Wei; Xiaojing Liu; Xijin Xu

    2017-01-01

    In recent years, the research on supercapacitors has ushered in an explosive growth, which mainly focuses on seeking nano-/micro-materials with high energy and power densities. Herein, this review will be arranged from three aspects. We will summarize the controllable architectures of spinel NiCo2O4 fabricated by various approaches. Then, we introduce their performances as supercapacitors due to their excellent electrochemical performance, including superior electronic conductivity and electr...

  16. The effect of defects and disorder on the electronic properties of ZnIr{sub 2}O{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Ramo, David Muñoz, E-mail: dm586@cam.ac.uk; Bristowe, Paul D., E-mail: pdb1000@cam.ac.uk [Department of Materials Science and Metallurgy, University of Cambridge, 27 Charles Babbage Road, Cambridge CB3 0FS (United Kingdom)

    2014-08-28

    We analyze by means of ab initio calculations the role of imperfections on the electronic structure of ZnIr{sub 2}O{sub 4}, ranging from point defects in the spinel phase to the fully amorphous phase. We find that interstitial defects and anion vacancies in the spinel have large formation energies, in agreement with the trends observed in other spinels. In contrast, cation vacancies and antisites have lower formation energies. Among them, the zinc antisite and the zinc vacancy are the defects with the lowest formation energy. They are found to act as acceptors, and may be responsible for the spontaneous hole doping in the material. They may also induce optical transitions that would reduce the transparency of the material. Amorphization of ZnIr{sub 2}O{sub 4} leads a large decrease of the band gap and appearance of localized states at the edges of the band gap region, which may act as charge traps and prevent amorphous ZnIr{sub 2}O{sub 4} from being a good hole conductor.

  17. Spin Filtering in Epitaxial Spinel Films with Nanoscale Phase Separation

    KAUST Repository

    Li, Peng

    2017-05-08

    The coexistence of ferromagnetic metallic phase and antiferromagnetic insulating phase in nanoscaled inhomogeneous perovskite oxides accounts for the colossal magnetoresistance. Although the model of spin-polarized electron transport across antiphase boundaries has been commonly employed to account for large magnetoresistance (MR) in ferrites, the magnetic anomalies, the two magnetic phases and enhanced molecular moment, are still unresolved. We observed a sizable MR in epitaxial spinel films (NiCo2O4-δ) that is much larger than that commonly observed in spinel ferrites. Detailed analysis reveals that this MR can be attributed to phase separation, in which the perfect ferrimagnetic metallic phase and ferrimagnetic insulating phase coexist. The magnetic insulating phase plays an important role in spin filtering in these phase separated spinel oxides, leading to a sizable MR effect. A spin filtering model based on Zeeman effect and direct tunneling is developed to account for MR of the phase separated films.

  18. Cation disorder in high-dose, neutron-irradiated spinel

    International Nuclear Information System (INIS)

    Sickafus, K.E.; Larson, A.C.; Yu, N.; Nastasi, M.; Hollenberg, G.W.; Garner, F.A.; Bradt, R.C.

    1994-08-01

    The objective of this effort is to determine whether MgAl 2 O 4 spinel is a suitable ceramic for fusion applications. Here, the crystal structures of MgAl 2 O 4 spinel single crystals irradiated to high neutron fluences [>5·10 26 n/m 2 (E n > 0.1 MeV)] were examined by neutron diffraction. Crystal structure refinement of the highest dose sample indicated that the average scattering strength of the tetrahedral crystal sites decreased by ∼ 20% while increasing by ∼ 8% on octahedral sites. Since the neutron scattering length for Mg is considerably larger than for Al, this results is consistent with site exchange between Mg 2+ ions on tetrahedral sites and Al 3+ ions on octahedral sites. Least-squares refinements also indicated that, in all irradiated samples, at least 35% of Mg 2+ and Al 3+ ions in the crystal experienced disordering replacements. This retained dpa on the cation sublattices is the largest retained damage ever measured in an irradiated spinel material

  19. Synthesis, structure and electrochemistry of Ag-modified LiMn2O4 cathode materials for lithium-ion batteries

    International Nuclear Information System (INIS)

    Zhou Wenjia; He Benlin; Li Hulin

    2008-01-01

    Spinel lithium manganese oxide was prepared by sol-gel method and a series of Ag/LiMn 2 O 4 composites with different Ag additive contents were prepared by thermal decomposition of AgNO 3 added to the pure LiMn 2 O 4 powders. X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive analysis of X-ray (EDAX) and various electrochemical measurement methods were used to examine the structural and electrochemical characteristics of the Ag/LiMn 2 O 4 composite powders. Phase analysis showed that Ag particles were dispersed on the surface of LiMn 2 O 4 instead of entering the spinel structure. According to the electrochemical tests results, it is clearly to see that Ag additives efficiently improved the cycling stability, reversibility and high-rate discharge capacity of pristine LiMn 2 O 4 by increasing the electrical conductivity between LiMn 2 O 4 particles, decreasing the polarization of cathode and reducing the dissolution of Mn. Meanwhile the influence of the Ag additive contents on the electrochemical properties of the Ag/LiMn 2 O 4 composites is also investigated in detail

  20. LaCrO3/CuFe2O4 Composite-Coated Crofer 22 APU Stainless Steel Interconnect of Solid Oxide Fuel Cells

    Science.gov (United States)

    Hosseini, Seyedeh Narjes; Enayati, Mohammad Hossein; Karimzadeh, Fathallah; Dayaghi, Amir Masoud

    2017-07-01

    Rapidly rising contact resistance and cathode Cr poisoning are the major problems associated with unavoidable chromia scale growth on ferritic stainless steel (FSS) interconnects of solid oxide fuel cells. This work investigates the performance of the novel screen-printed composite coatings consisting of dispersed conductive LaCrO3 particles in a CuFe2O4 spinel matrix for Crofer 22 APU FSS, with emphasis on the oxidation behavior and electrical conductivity of these coatings. The results show that the presence of protective spinel coating, accompanied by the effective role of LaCrO3 particle incorporation, prevents the Cr2O3 subscale growth as well as chromium migration into the coating surface at the end of 400 hours of oxidation at 1073 K (800 °C) in air. In addition, the composite coatings decreased the area specific resistance (ASR) from 51.7 and 13.8 mΩ cm2 for uncoated and spinel-coated samples, respectively, to a maximum of 7.7 mΩ cm2 for composite-coated samples after 400 hours of oxidation.

  1. High-Pressure Phase Relations and Crystal Structures of Postspinel Phases in MgV2O4, FeV2O4, and MnCr2O4: Crystal Chemistry of AB2O4 Postspinel Compounds.

    Science.gov (United States)

    Ishii, Takayuki; Sakai, Tsubasa; Kojitani, Hiroshi; Mori, Daisuke; Inaguma, Yoshiyuki; Matsushita, Yoshitaka; Yamaura, Kazunari; Akaogi, Masaki

    2018-06-04

    We have investigated high-pressure, high-temperature phase transitions of spinel (Sp)-type MgV 2 O 4 , FeV 2 O 4 , and MnCr 2 O 4 . At 1200-1800 °C, MgV 2 O 4 Sp decomposes at 4-7 GPa into a phase assemblage of MgO periclase + corundum (Cor)-type V 2 O 3 , and they react at 10-15 GPa to form a phase with a calcium titanite (CT)-type structure. FeV 2 O 4 Sp transforms to CT-type FeV 2 O 4 at 12 GPa via decomposition phases of FeO wüstite + Cor-type V 2 O 3 . MnCr 2 O 4 Sp directly transforms to the calcium ferrite (CF)-structured phase at 10 GPa and 1000-1400 °C. Rietveld refinements of CT-type MgV 2 O 4 and FeV 2 O 4 and CF-type MnCr 2 O 4 confirm that both the CT- and CF-type structures have frameworks formed by double chains of edge-shared B 3+ O 6 octahedra (B 3+ = V 3+ and Cr 3+ ) running parallel to one of orthorhombic cell axes. A relatively large A 2+ cation (A 2+ = Mg 2+ , Fe 2+ , and Mn 2+ ) occupies a tunnel-shaped space formed by corner-sharing of four double chains. Effective coordination numbers calculated from eight neighboring oxygen-A 2+ cation distances of CT-type MgV 2 O 4 and FeV 2 O 4 and CF-type MnCr 2 O 4 are 5.50, 5.16, and 7.52, respectively. This implies that the CT- and CF-type structures practically have trigonal prism (six-coordinated) and bicapped trigonal prism (eight-coordinated) sites for the A 2+ cations, respectively. A relationship between cation sizes of VIII A 2+ and VI B 3+ and crystal structures (CF- and CT-types) of A 2+ B 2 3+ O 4 is discussed using the above new data and available previous data of the postspinel phases. We found that CF-type A 2+ B 2 3+ O 4 crystallize in wide ionic radius ranges of 0.9-1.4 Å for VIII A 2+ and 0.55-1.1 Å for VI B 3+ , whereas CT-type phases crystallize in very narrow ionic radius ranges of ∼0.9 Å for VIII A 2+ and 0.6-0.65 Å for VI B 3+ . This would be attributed to the fact that the tunnel space of CT-type structure is geometrically less flexible due to the smaller coordination

  2. Effect of chitosan coating on the structural and magnetic properties of MnFe2O4 and Mn0.5Co0.5Fe2O4 nanoparticles

    Science.gov (United States)

    Mdlalose, W. B.; Mokhosi, S. R.; Dlamini, S.; Moyo, T.; Singh, M.

    2018-05-01

    We report the influence of polymer coatings on structural and magnetic properties of MnFe2O4 and Mn0.5Co0.5Fe2O4 nanoferrites synthesized by glycol thermal technique and then coated with chitosan viz. CHI-MnFe2O4 and CHI-Mn0.5Co0.5Fe2O4. The compounds were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), high-resolution scanning electron microscopy (HRSEM), Mössbauer spectroscopy and magnetization measurements. The powder XRD patterns of naked nanoferrites confirmed single-phase spinel cubic structure with an average crystallite size of 13 nm, while the coated samples exhibited an average particle size of 15 nm. We observed a reduction in lattice parameters with coating. HRTEM results correlated well with XRD results. 57Fe Mössbauer spectra showed ordered magnetic spin states in both nanoferrites. This study shows that coatings have significant effects on the structural and magnetic properties of Mn-nanoferrites. Magnetization studies performed at room temperature in fields up to 14 kOe revealed the superparamagnetic nature of both naked and coated nanoparticles with spontaneous magnetizations at room temperature of 49.2 emu/g for MnFe2O4, 23.6 emu/g for coated CHI-MnFe2O4 nanoparticles, 63.2 emu/g for Mn0.5Co0.5Fe2O4 and 33.2 emu/g for coated CHI-Mn0.5Co0.5Fe2O4 nanoparticles. We observed reduction in coercive fields due to coating. Overall, chitosan-coated manganese and manganese-cobalt nanoferrites present as suitable candidates for biomedical applications owing to physicochemical, and magnetic properties exhibited.

  3. Effect of Precursor Synthesis on Catalytic Activity of Co3O4 in N2O Decomposition.

    Czech Academy of Sciences Publication Activity Database

    Chromčáková, Ž.; Obalová, L.; Kovanda, F.; Legut, D.; Titov, A.; Ritz, M.; Fridrichová, D.; Michalik, S.; Kustrowski, P.; Jirátová, Květa

    2015-01-01

    Roč. 257, Part 1 (2015), s. 18-25 ISSN 0920-5861. [AWPAC2014 - International Symposium on Air & Water Pollution Abatement Catalysis. Krakow, 01.09.2014-05.09.2014] R&D Projects: GA ČR GA14-13750S Institutional support: RVO:67985858 Keywords : cobalt spinel * Co3O4 * N2O decomposition * precursor synthesis Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 4.312, year: 2015

  4. Hierarchical CuCo2O4 nanobelts as a supercapacitor electrode with high areal and specific capacitance

    International Nuclear Information System (INIS)

    Vijayakumar, Subbukalai; Lee, Seong-Hun; Ryu, Kwang-Sun

    2015-01-01

    Highlights: • First time we report the synthesis of CuCo 2 O 4 nanobelts using hydrothermal method. • The spinel CuCo 2 O 4 nanobelts exhibit maximum areal capacitance of 2.42 F cm −2 . • After 1800 cycles, 127% of the initial specific capacitance was retained. - Abstract: One dimensional hierarchical CuCo 2 O 4 nanobelt like architecture was synthesized via hydrothermal method. The synthesized nanomaterial was characterized using X-ray diffraction (XRD) analysis, field emission scanning electron microscopy (FESEM), and transmission electron microscopy (TEM). The TEM image clearly shows the nanobelt like architecture of CuCo 2 O 4 . The supercapacitor properties of CuCo 2 O 4 nanobelts electrode were tested using cyclic voltammetry, charge-discharge and electrochemical impedance spectroscopy. The spinel CuCo 2 O 4 nanobelts exhibit maximum areal and specific capacitance of 2.42 F cm −2 (809 F g −1 ). After 1800 continuous charge-discharge cycles, 127% of the initial capacitance was retained. This superior electrochemical supercapacitor property is mainly due to increased surface area and ion transport of nanobelt like architecture. The charge transfer resistance (R ct ) value of CuCo 2 O 4 nanobelt electrode is 3.85 Ω. This high capacitance and cyclic stability demonstrate that the prepared CuCo 2 O 4 nanobelts are a promising candidate for supercapacitors.

  5. Efficient one-pot sonochemical synthesis of thickness-controlled silica-coated superparamagnetic iron oxide (Fe3O4/SiO2) nanospheres

    Science.gov (United States)

    Abbas, Mohamed; Abdel-Hamed, M. O.; Chen, Jiangang

    2017-12-01

    A facile and eco-friendly efficient sonochemical approach was designed for the synthesis of highly crystalline Fe3O4 and Fe3O4/SiO2 core/shell nanospheres in single reaction. The generated physical properties (shock waves, microjets, and turbulent flows) from ultrasonication as a consequence of the collapse of microbubbles and polyvinylpyrrolidone (PVP) as a chemical linker were found to play a crucial role in the successful formation of the core/shell NPs within short time than the previously reported methods. Transmission electron microscopy revealed that a uniform SiO2 shell is successfully coated over Fe3O4 nanospheres, and the thickness of the silica shell could be easily controlled in the range from 5 to 15 nm by adjusting the reaction parameters. X-ray diffraction data were employed to confirm the formation of highly crystalline and pure phase of a cubic inverse spinel structure for magnetite (Fe3O4) nanospheres. The magnetic properties of the as-synthesized Fe3O4 and Fe3O4/SiO2 core/shell nanospheres were measured at room temperature using vibrating sample magnetometer, and the results demonstrated a high magnetic moment values with superparamagnetic properties.

  6. Annealing temperature dependent structural and magnetic properties of MnFe{sub 2}O{sub 4} nanoparticles grown by sol-gel auto-combustion method

    Energy Technology Data Exchange (ETDEWEB)

    Bhandare, S.V. [Department of Physics, Gulbarga University, Gulbarga 585106 (India); Kumar, R.; Anupama, A.V.; Choudhary, H.K. [Materials Research Centre, Indian Institute of Science, Bangalore 560012 (India); Jali, V.M., E-mail: vmjali@gmail.com [Department of Physics, Gulbarga University, Gulbarga 585106 (India); Sahoo, B., E-mail: bsahoo@mrc.iisc.ernet.in [Materials Research Centre, Indian Institute of Science, Bangalore 560012 (India)

    2017-07-01

    Highlights: • Phase pure MnFe{sub 2}O{sub 4} samples were prepared by sol-gel auto-combustion method. • Annealing MnFe{sub 2}O{sub 4} below ∼500 °C, two spinel phases were observed indicating partial oxidation of Mn{sup 2+} to Mn{sup 3+}. • Oxidation of Mn{sup 2+} to Mn{sup 3+} results in decrease in lattice parameter of the spinel lattice. • Annealing at ≥ 600 °C, MnFe{sub 2}O{sub 4} decomposes into crystalline α-Mn{sub 2}O{sub 3} and α-Fe{sub 2}O{sub 3} along with amorphous-FeO phase. - Abstract: Manganese ferrite (MnFe{sub 2}O{sub 4}) nanoparticles were synthesized by sol-gel auto-combustion method using manganese nitrate and ferric nitrate as precursors and citric acid as a fuel. Scanning electron micrographs show irregularly shaped morphology of the particles. The as-prepared samples were annealed at 400, 500, 600 and 800 °C for 2 h in air. The phase identification and structural characterizations were performed using powder X-ray diffraction technique along with Mössbauer spectroscopy. Magnetization loops and {sup 57}Fe Mössbauer spectra were measured at RT. After annealing the sample at or below ∼ 500 °C, we observed two different spinel phases corresponding to two different lattice parameters. This is originating due to the partial oxidation of Mn{sup 2+} to Mn{sup 3+}. At high annealing temperatures (∼ 600 °C or above) the spinel MnFe{sub 2}O{sub 4} phase decomposes into crystalline α-Mn{sub 2}O{sub 3} and α-Fe{sub 2}O{sub 3} phases, and amorphous FeO phase.

  7. Performance assessment of the catalyst ZnAl{sub 2}O{sub 4} and Cu/ZnAl{sub 2}O{sub 4} esterification reaction fatty acid in biodiesel; Avaliacao do desempenho do catalisador ZnAl{sub 2}O{sub 4} e Cu/ZnAl{sub 2}O{sub 4} na reacao de estereficacao de acidos graxos em biodiesel

    Energy Technology Data Exchange (ETDEWEB)

    Feitosa, A.C.; Dantas, J.; Costa, A.C.M.F., E-mail: alexcaval2@hotmail.com [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Departamento de Engenharia de Materiais; Barbosa, D.C.; Meneghetti, S.M.P. [Universidade Federal de Alagoas (UFAL), Maceio, AL (Brazil). Dept. de Quimica

    2012-07-01

    This study aims to evaluate the performance of the Cu/ZnAl{sub 2}O{sub 4} and ZnAl{sub 2}O{sub 4} methyl esterification of fatty acids of soybean oil into biodiesel. The ZnAl{sub 2}O{sub 4} was synthesized by combustion reaction and then the sample was wet impregnated with a copper source. The samples were characterized by XRD, SEM, textural analysis and catalytic tests bench. The characterization results showed that the samples showed characteristic diffraction peaks spinel, with the characteristic of mesoporous material (10-250 Å), particles in the form of blocks and slabs of hard point. The results showed that the conversion impregnation of copper has increased by 17% conversion to biodiesel. (author)

  8. MOCVD growth of transparent conducting Cd2SnO4 thin films

    International Nuclear Information System (INIS)

    Metz, A.W.; Poeppelmeier, K.R.; Marks, T.J.; Lane, M.A.; Kannewurt, C.R.

    2004-01-01

    The first preparation of transparent conducting Cd 2 SnO 4 thin films by a simple MOCVD process is described. As-deposited films using Cd(hfa) 2 (TMEDA) (Figure), at 365 C are found to be highly crystalline with a relatively wide range of grain size of 100-300 nm. XRD indicates a cubic spinel Cd 2 SnO 4 crystal structure and the possible presence of a small amount of CdO. The films exhibit conductivities of 2170 S/cm and a bandgap of 3.3 eV, rivaling those of commercial tin-doped indium oxide. (Abstract Copyright [2004], Wiley Periodicals, Inc.)

  9. The influence of CeO2 on the microstructure and electrical behaviour of ZnO-Bi2O3 based varistors

    International Nuclear Information System (INIS)

    Lei Ming; Li Shengtao; Jiao Xiaodong; Li Jianying; Alim, Mohammad A

    2004-01-01

    The processing-microstructure-property relations have been studied in order to understand the role of the addition of CeO 2 (up to 0.9 mole%) in the ZnO-Bi 2 O 3 based varistor recipe. The microstructural investigation suggests that CeO 2 is segregated at the corners of the ZnO grains in addition to the existence of the Zn 7 Sb 2 O 12 spinel phase. However, the α -spinel phase was observed instead of the β -spinel phase that is usually found in most commercial and laboratory ZnO-Bi 2 O 3 based varistors. The α -spinel phase is more stable than the β -spinel phase and does not transform to the pyrochlore phase during the cooling process. The most significant effect of the CeO 2 particles is the ZnO grain refinement owing to the pinning effect of the grain growth. The average grain size decreases from 7.8 to 5.7 μm when compared to the 0.9 mole% CeO 2 -added sample against the CeO 2 -free sample. This grain refinement results in a significantly enhanced breakdown field when compared to the CeO 2 -free sample. The coefficient of nonlinearity of the current-voltage (I-V) characteristics is found to be nearly identical for the CeO 2 added varistor materials. However, when a slower cooling cycle (1 deg. C min -1 instead of 4 deg. C min -1 ) is used in the sintering process, these varistor materials exhibited a high nonlinear coefficient (α = 29 ± 5) as extracted from the I-V behaviour

  10. Conformal spinel/layered heterostructures of Co3O4 shells grown on single-crystal Li-rich nanoplates for high-performance lithium-ion batteries

    Science.gov (United States)

    Xin, Yue; Lan, Xiwei; Chang, Peng; Huang, Yaqun; Wang, Libin; Hu, Xianluo

    2018-07-01

    Lithium-rich layered materials have received much attention because of their high specific capacity and high energy density. Unfortunately, they suffer from irreversible capacity loss, low initial Coulombic efficiency and poor cyclability. Here we report a facile co-precipitation method to synthesize uniform single-crystal Li-rich Li[Li0.2Mn0.54Ni0.13Co0.13]O2 nanoplates without using any template. Subsequently, a Co3O4 shell is in situ grown on the Li-rich nanoplates through a hydrothermal method, leading to spinel/layered heterostructures. The electrode made of conformal heterostructured Li-rich/Co3O4 nanoplates delivers a high discharge capacity of 296 mA h g-1 at 0.1 C with an initial Coulombic efficiency of 84%. The capacity retention reaches 83.2% with a discharge capacity of 223 mA h g-1 after 160 cycles at 0.2 C during the potential window ranging from 2.0 to 4.8 V. The enhanced electrochemical performance of the resulting Li-rich/Co3O4 nanoplates benefits from the unique conformal heterostructure as well as the electrochemically active LixCoOy generated between the reaction of Co3O4 shells and the extracted Li2O during charging/discharging processes.

  11. Synthesis and characterization of nanocomposite NiFe2O4 ...

    African Journals Online (AJOL)

    In this work, nano ferrite spinel NiFe2O4 was synthesized by sol-gel method and characterized by SEM, XRD, FT-IR, and VSM. In second step Schiff base made from salicylaldehyde and amino propyl triethoxy silane was used for modification of the synthesized nano ferrit. In the third step removal of Ni(II) was done using ...

  12. Impact of larger rare earth Pr{sup 3+} ions on the physical properties of chemically derived Pr{sub x}CoFe{sub 2−x}O{sub 4} nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Pachpinde, A.M.; Langade, M.M. [Department of Chemistry, Jawahar Art Science and Commerce College Andur, Osmanabad, MS (India); Lohar, K.S.; Patange, S.M. [Materials Research Laboratory, Srikrishna Mahavidyalaya Gunjoti, Omerga, Osmanabad 413 613, MS (India); Shirsath, Sagar E., E-mail: shirsathsagar@hotmail.com [Spin Device Technology Center, Department of Information Engineering, Shinshu University, Nagano 380 8553 (Japan)

    2014-01-31

    Highlights: • Rare earth Pr{sup 3+} substituted CoFe{sub 2}O{sub 4}. • Sol–gel auto combustion synthesis. • XRD and IR spectra reveal the spinel structure. • Magnetization and coercivity increased with Pr{sup 3+} substitution. - Abstract: Rare earth Pr{sup 3+} ions with its larger ionic radii substituted CoFe{sub 2}O{sub 4} nanoparticles with x ranging from 0.0 to 0.1 were synthesized by sol–gel auto-combustion chemical method. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared spectroscopy (IR) and vibrating sample magnetometer (VSM) were employed to characterize the physical properties of these ferrite nanoparticles. XRD pattern reveals the formation of cubic spinel ferrite with the signature of PrFeO{sub 3} phases for x ⩾ 0.05. SEM images show that the synthesized samples are in good homogeneity with uniformly distributed grain. The results of IR spectroscopy analysis indicated that the functional groups of cobalt spinel ferrite were formed during the sol–gel process. The cations distribution between the tetrahedral (A-site) and octahedral sites (B-site) has been estimated by XRD analysis. Room temperature magnetic measurement shows saturation magnetization and coercivity increased from 54.7 to 64.2 emu/g and 644 to 1013 Oe, respectively with the increasing Pr{sup 3+} substitution.

  13. Neutron diffraction analysis and electrochemical performance of spinel Ni(Mn{sub 2−x}Co{sub x})O{sub 4} as anode materials for lithium ion battery

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Hu; Liu, Lei; Hu, Zhongbo [College of Materials Science and Opto-Electronic Technology, University of Chinese Academy of Sciences, Beijing 100049 (China); Sun, Limei, E-mail: sunlm@ciae.ac.cn [Department of Nuclear and Physics, China Institute of Atomic Energy, Beijing 102413 (China); Han, Songbai; Liu, Yuntao; Chen, Dongfeng [Department of Nuclear and Physics, China Institute of Atomic Energy, Beijing 102413 (China); Liu, Xiangfeng, E-mail: liuxf@ucas.ac.cn [College of Materials Science and Opto-Electronic Technology, University of Chinese Academy of Sciences, Beijing 100049 (China)

    2016-05-15

    Highlights: • The reversible capacity and cyclability of Ni(Mn{sub 2−x}Co{sub x})O{sub 4} first increases and then decreases with increasing Co content. • Neutron diffraction and Rielveld refinements are applied to analyze the site occupancies of Mn, Co, O and Ni. • Excessive Co ions in 8a and 16d sites reduce the structure stability leading to poor electrochemical performance. - Abstract: The effects of Co substitution on the structure and electrochemical performances of spinel Ni(Mn{sub 2−x}Co{sub x})O{sub 4} (x = 0, 0.5, and 1.0) have been investigated. With the increase of Co content the lattice parameters decrease owing to the smaller ion radius of Co than Mn. The reversible capacity and cyclability of Ni(Mn{sub 2−x}Co{sub x})O{sub 4} first increase and then decrease with the increase of Co content and NiMn{sub 1.5}Co{sub 0.5}O{sub 4} shows the best electrochemical performance in compared to the other two samples. Neutron diffraction and Rielveld refinement are further applied to analyze the site occupancies of the elements of Mn, Co, O and Ni. A certain amount of Co ions substitution are favorable to enhance the electrochemical performance, but excessive Co ions in 8a and 16d sites reduce the stability of host structure which leads to the poor electrochemical performance.

  14. Study of the crystallographic and magnetic properties of cubic manganite spinels NiMn{sub 2}O{sub 4}; Etude des proprietes cristallographiques et magnetiques des manganites spinelles cubiques NiMn{sub 2}O{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Boucher, B [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1969-07-01

    We study the variation of the crystallographic properties (inversion degree, position parameters and short range order) of the cubic spinel Mn{sub {nu}}Ni{sub 1-{nu}}[Mn{sub 2{nu}}Ni{sub {nu}}]O{sub 4}, as a function of the thermal treatment applied to the sample. {nu} lies between 0. 74 and 0. 93; the slower the sample is cooled the more inverse it is. We show, in a molecular field theory, that a system of three magnetic sublattices can afford a 'star' configuration. We establish the conditions of stability of such a structure and its evolution as a function of temperature is foreseen. Neutron diffraction measurements show that the magnetic structure of NiMn{sub 2}O{sub 4} at 4.2 K is a 'star' configuration and that with increasing temperature it becomes a collinear structure in agreement with the theory. Furthermore, we find an anomaly in the value of specific heat at the transition temperature between 'star' and collinear structures. (author) [French] On etudie la variation des proprietes cristallographiques (inversion, parametre de position, ordre a courte distance) du spinelle cubique Mn{sub {nu}}Ni{sub 1-{nu}}[Mn{sub 2{nu}}Ni{sub {nu}}]O{sub 4}, en fonction du traitement thermique que subit l'echantillon, {nu} est compris entre 0,74 et 0,93; plus le corps est refroidi lentement, plus il est inverse. On montre, dans le cadre d'une theorie de champ moleculaire, qu'un systeme a trois sous-reseaux magnetiques peut presenter une configuration en ''etoile''. On etablit les conditions de stabilite d'une telle structure et on prevoit son evolution en fonction de la temperature. Les mesures de diffraction de neutrons montrent que la structure magnetique de NiMn{sub 2}O{sub 4} a 4,2 K est du type ''en etoile'' et qu'elle evolue en fonction de la temperature vers une structure colineaire comme le prevoit la theorie. De plus on observe une anomalie de chaleur specifique a la temperature de la transition entre la structure ''en etoile'' et la structure colineaire. (auteur)

  15. Structural characterization and electrochemical behaviour of Li{sub (4−x)/3}Ti{sub (5−2x)/3}Mn{sub x}O{sub 4} solid solution with spinel-structure

    Energy Technology Data Exchange (ETDEWEB)

    Martín, P., E-mail: pmartinp@quim.ucm.es; López, M.L.; Pico, C.; Veiga, M.L.

    2013-07-15

    A series of new oxides Li{sub (4−x)/3}Ti{sub (5−2x)/3}Mn{sub x}O{sub 4} (0.1 ≤ x ≤ 0.9) have been synthesized by solid state reactions and characterized by thermal analysis and X-ray and neutron diffraction. In all phases, Li{sup +} cations mainly occupy tetrahedral sites and transition metals cations are located on the octahedral ones. These phases show a structural disorder–order transition associated to the proportion of manganese in the samples and to its oxidation state. All these factors have a marked influence on the electrochemical properties and the phase x = 0.1 shows the best characteristics to be used as anode in a solid state battery. - Highlights: • Lithium spinels anodes in batteries. • Influence of Ti/Mn ratio in the electrochemical behaviour. • Li{sub 1.3}Ti{sub 1.6}Mn{sub 0.1}O{sub 4}: a promising zero-strain material. • Influence of disorder–order transitions on the physical properties.

  16. A novel approach for the synthesis of ultrathin silica-coated iron oxide nanocubes decorated with silver nanodots (Fe3O4/SiO2/Ag) and their superior catalytic reduction of 4-nitroaniline

    Science.gov (United States)

    Abbas, Mohamed; Torati, Sri Ramulu; Kim, Cheolgi

    2015-07-01

    A novel sonochemical approach was developed for the synthesis of different core/shell structures of Fe3O4/SiO2/Ag nanocubes and SiO2/Ag nanospheres. The total reaction time of the three sonochemical steps for the synthesis of Fe3O4/SiO2/Ag nanocubes is shorter than that of the previously reported methods. A proposed reaction mechanism for the sonochemical functionalization of the silica and the silver on the surface of magnetic nanocubes was discussed in detail. Transmission electron microscopy revealed that the surface of Fe3O4/SiO2 nanocubes was decorated with small Ag nanoparticles of approximately 10-20 nm in size, and the energy dispersive spectroscopy mapping analysis confirmed the morphology of the structure. Additionally, X-ray diffraction data were used to confirm the formation of both phases of a cubic inverse spinel structure for Fe3O4 and bcc structures for Ag in the core/shell structure of the Fe3O4/SiO2/Ag nanocubes. The as-synthesized Fe3O4/SiO2/Ag nanocubes showed a high efficiency in the catalytic reduction reaction of 4-nitroaniline to 4-phenylenediamine and a better performance than both Ag and SiO2/Ag nanoparticles. The grafted silver catalyst was recycled and reused at least fifteen times without a significant loss of catalytic efficiency.A novel sonochemical approach was developed for the synthesis of different core/shell structures of Fe3O4/SiO2/Ag nanocubes and SiO2/Ag nanospheres. The total reaction time of the three sonochemical steps for the synthesis of Fe3O4/SiO2/Ag nanocubes is shorter than that of the previously reported methods. A proposed reaction mechanism for the sonochemical functionalization of the silica and the silver on the surface of magnetic nanocubes was discussed in detail. Transmission electron microscopy revealed that the surface of Fe3O4/SiO2 nanocubes was decorated with small Ag nanoparticles of approximately 10-20 nm in size, and the energy dispersive spectroscopy mapping analysis confirmed the morphology of the

  17. Microwave synthesis of high-quality and uniform 4 nm ZnFe2O4 nanocrystals for application in energy storage and nanomagnetics

    Directory of Open Access Journals (Sweden)

    Christian Suchomski

    2016-09-01

    Full Text Available Magnetic nanocrystals with a narrow size distribution hold promise for many applications in different areas ranging from biomedicine to electronics and energy storage. Herein, the microwave-assisted sol–gel synthesis and thorough characterization of size-monodisperse zinc ferrite nanoparticles of spherical shape is reported. X-ray diffraction, 57Fe Mössbauer spectroscopy and X-ray photoelectron spectroscopy all show that the material is both chemically and phase-pure and adopts a partially inverted spinel structure with Fe3+ ions residing on tetrahedral and octahedral sites according to (Zn0.32Fe0.68tet[Zn0.68Fe1.32]octO4±δ. Electron microscopy and direct-current magnetometry confirm the size uniformity of the nanocrystals, while frequency-dependent alternating-current magnetic susceptibility measurements indicate the presence of a superspin glass state with a freezing temperature of about 22 K. Furthermore, as demonstrated by galvanostatic charge–discharge tests and ex situ X-ray absorption near edge structure spectroscopy, the as-prepared zinc ferrite nanocrystals can be used as a high-capacity anode material for Li-ion batteries, showing little capacity fade – after activation – over hundreds of cycles. Overall, in addition to the good material characteristics, it is remarkable that the microwave-based synthetic route is simple, easily reproducible and scalable.

  18. Photocatalytic degradation of methylene blue on magnetically separable MgFe2O4 under visible light irradiation

    KAUST Repository

    Shahid, Muhammad

    2013-05-01

    A magnetically separable single-phase MgFe2O4 photocatalyst with a spinel crystal structure was synthesized by using the solid-state reaction method. The formation of spinel structure is confirmed by X-ray diffraction and Fourier transform infrared spectroscopy. The magnetic measurements showed that the photocatalyst material can be separated from water when an external magnetic field is added and redispersed into water solution after the external magnetic field is eliminated. It is one of the promising photocatalysts for waste water treatment. The photocatalytic activity of MgFe2O4 was investigated by using the photo-decomposition of methylene blue dye under visible light. The photoelectrochemical property of the MgFe2O4 was studied by measuring their photocurrent-potential behavior in 1 M NaOH electrolyte under AM 1.5100 mW cm-2 illumination. © 2013 Elsevier B.V. All rights reserved.

  19. Thermal expansion of spinel-type Si3N4

    DEFF Research Database (Denmark)

    Paszkowics, W.; Minkikayev, R.; Piszora, P.

    2004-01-01

    The lattice parameter and thermal expansion coefficient (TEC) for the spinel-type Si3N4 phase prepared under high-pressure and high-temperature conditions are determined for 14 K......The lattice parameter and thermal expansion coefficient (TEC) for the spinel-type Si3N4 phase prepared under high-pressure and high-temperature conditions are determined for 14 K...

  20. Electronic structure of dimerized spinel ZnV2O4

    International Nuclear Information System (INIS)

    Baldomir, D.; Pardo, V.; Blanco-Canosa, S.; Rivadulla, F.; Khomskii, D.I.; Wu, Hua; Pineiro, A.; Arias, J.E.; Rivas, J.

    2009-01-01

    Electronic structure calculations were performed for ZnV 2 O 4 , a material close to a metal-insulator transition. Structural optimization leads to the formation of V-V dimers along the off-plane chains. A strong spin-lattice coupling is expected close to the transition to itinerancy. No orbital ordering is observed in such a structure, and the experimentally found magnetic structure is naturally explained

  1. Crystallization and magnetic properties of a 10Li{sub 2}O–9MnO{sub 2}–16Fe{sub 2}O{sub 3}–25CaO–5P{sub 2}O{sub 5}–35SiO{sub 2} glass

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Moo-Chin, E-mail: mcwang@kmu.edu.tw [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China); Cheng, Huy-Zu [Department of Materials Science and Engineering, I-Shou University, 1 123456789Hsueh-Cheng Road, Section 1, Ta-Hsu, Kaohsiung 84001, Taiwan (China); Lin, Huey-Jiuan [Department of Materials Science and Engineering, National United University, 1 Lien-Da Road, Kung-Ching Li, Miao-Li 36003, Taiwan (China); Wang, Chien-Fu [Department of Materials Science and Engineering, I-Shou University, 1 123456789Hsueh-Cheng Road, Section 1, Ta-Hsu, Kaohsiung 84001, Taiwan (China); Hsi, Chi-Shiung, E-mail: chsi@nuu.edu.tw [Department of Materials Science and Engineering, National United University, 1 Lien-Da Road, Kung-Ching Li, Miao-Li 36003, Taiwan (China)

    2013-06-15

    The crystallization behavior and magnetic properties of 10Li{sub 2}O–9MnO{sub 2}–16Fe{sub 2}O{sub 3}–25CaO–5P{sub 2}O{sub 5}–35SiO{sub 2} (10LFS) glass have been studied using differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDS), transmission electron microscopy (TEM) and selected area electron diffraction (SAED) to observe the crystallization behavior and a superconducting quantum interference device (SQUID) for measurements of the magnetic properties. The DTA shows that the 10LFS glass has one broad exothermic peak at approximately 674 °C and one sharp (the highest) exothermic peak at 764 °C. When the 10LFS glass crystallized at 850 °C for 4 h, the crystalline phases identified by XRD were lithium silicate (Li{sub 2}SiO{sub 3}), β-wollastonite (β-CaSiO{sub 3}), lithium orthophosphate (Li{sub 3}PO{sub 4}), magnetite (FeFe{sub 2}O{sub 4}) and triphylite (Li(Mn{sub 0.5}Fe{sub 0.5})PO{sub 4}). The SEM surface analysis revealed that the β-wollastonite and lithium silicate have a lath morphology. The TEM microstructure examination showed that the largest FeFe{sub 2}O{sub 3} particles have a size of approximately 0.3 μm. When the 10LFS glass was heat treated at 850 °C for 16 h and a magnetic field of 1000 Oe was applied, a very small remnant magnetic induction of 0.01 emu g{sup −1} and a coercive force of 50 Oe were obtained, which revealed an inverse spinel structure. - Highlights: ► The phases formed at 850 °C in the 10LFS glass-ceramics are LiSiO{sub 3}, β-CaSiO{sub 3}, Li{sub 3}PO{sub 4}, FeFe{sub 2}O{sub 4} and Li(Mn{sub 0.5}Fe{sub 0.5})PO{sub 4}. ► The β-wollastonite and lithium silicate have a lath morphology. ► When 10LFS glass-ceramics applied magnetic field showing the ferromagnetic behavior of an inverse spinel structure.

  2. Reduction under hydrogen of ferrite MFe{sub 2}O{sub 4} (M: Fe, Co, Ni) nanoparticles obtained by hydrolysis in polyol medium: A novel route to elaborate CoFe{sub 2}, Fe and Ni{sub 3}Fe nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Ballot, N.; Schoenstein, F.; Mercone, S.; Chauveau, T.; Brinza, O. [Laboratoire des Sciences des Procedes et des Materiaux, CNRS, LSPM - UPR 3407, Universite Paris 13, PRES Sorbonne-Paris-Cite, 99 Avenue J.-B. Clement, 93430 Villetaneuse (France); Jouini, N., E-mail: jouini@univ-paris13.fr [Laboratoire des Sciences des Procedes et des Materiaux, CNRS, LSPM - UPR 3407, Universite Paris 13, PRES Sorbonne-Paris-Cite, 99 Avenue J.-B. Clement, 93430 Villetaneuse (France)

    2012-09-25

    Highlights: Black-Right-Pointing-Pointer Spinels nano-particles MFe{sub 2}O{sub 4} (M: Co, Fe or Ni) are obtained by hydrolysis in polyol medium. Black-Right-Pointing-Pointer Gentle reduction under hydrogen flow of spinel nano-particles yields metal and alloy nanoparticles. Black-Right-Pointing-Pointer TEM and X-ray analysis show that CoFe{sub 2}, Fe and Ni{sub 3}Fe nano-particles are monocrystalline particles with size less than 160 nm. Black-Right-Pointing-Pointer Iron with size of 150 nm presents ferromagnetic behavior. Black-Right-Pointing-Pointer CoFe{sub 2} alloy with size of 55 nm could be considered as a superparamagnetic material. - Abstract: A novel method to process metal and various alloy particles of nanometric size is described. The first step consists in the elaboration of MFe{sub 2}O{sub 4} (M: Fe, Ni or Co) spinel nanoparticles in polyol medium via hydrolysis and the second one in gently reducing these latter under hydrogen at 300 Degree-Sign C. X-ray diffraction analysis shows that pure Fe and CoFe{sub 2} alloy are well obtained by reducing Fe{sub 3}O{sub 4} and CoFe{sub 2}O{sub 4}, respectively. This is not the case when we try to reduce NiFe{sub 2}O{sub 4}. A mixture of Fe and Ni{sub 3}Fe is observed. TEM analysis reveals that the size of metal particles stays within the range of a few tenths of nm up to 150 nm, while the precursors (MFe{sub 2}O{sub 4}) never exceed 5 nm. Our results show that the formation of metal particles occurs via two main steps: (i) reduction of the spinel oxide nanoparticles into metal ones and (ii) aggregation of the latter, leading to larger metal nanoparticles. Magnetic measurements indicate that the as-obtained metallic materials have good magnetic properties mainly affected by the sizes of the nanoparticles and the purity of the reduced phases.

  3. Synthesis on spinel behaviour under irradiation

    International Nuclear Information System (INIS)

    Chauvin, N.; Dodane, C.; Noirot, J.; Konings, R.J.M.; Matzke, H.J.; Wiss, T.; Conrad, R.

    2001-01-01

    The spinel MgAl 2 O 4 is one of the materials able to be used in reactor for the transmutation of the minor actinides stemming from the back-end of the fuel cycle. It has been studied under irradiation since many years. Indeed, one of the first uses considered is to be employed as material for fusion reactors. Otherwise, it was shown that spinel presents nuclear and physico-chemical properties suitable for an utilization as nuclear inert matrix that loaded with an actinide phase constitutes a target devoted to the heterogeneous recycling in reactor. In order to improve the knowledge on spinel behaviour under irradiation, an assessment of the former studies must be done. The objective of this paper is to gather all the results of the spinel irradiations and to take out synthetic conclusion on the opportunity to use this material for the transmutation programme. (author)

  4. On the Utility of Spinel Oxide Hosts for Magnesium-Ion Batteries.

    Science.gov (United States)

    Knight, James C; Therese, Soosairaj; Manthiram, Arumugam

    2015-10-21

    There is immense interest to develop Mg-ion batteries, but finding suitable cathode materials has been a challenge. The spinel structure has many advantages for ion insertion and has been successfully used in Li-ion batteries. We present here findings on the attempts to extract Mg from MgMn2O4-based spinels with acid (H2SO4) and with NO2BF4. The acid treatment was able to fully remove all Mg from MgMn2O4 by following a mechanism involving the disproportionation of Mn(3+), and the extraction rate decreased with increasing cation disorder. Samples with additional Mg(2+) ions in the octahedral sites (e.g., Mg1.1Mn1.9O4 and Mg1.5Mn1.5O4) also exhibit complete or near complete demagnesiation due to an additional mechanism involving ion exchange of Mg(2+) by H(+), but no Mg could be extracted from MgMnAlO4 due to the disruption of Mn-Mn interaction/contact across shared octahedral edges. In contrast, no Mg could be extracted with the oxidizing agent NO2BF4 from MgMn2O4 or Mg1.5Mn1.5O4 as the electrostatic repulsion between the divalent Mg(2+) ions prevents Mg(2+) diffusion through the 16c octahedral sites, unlike Li(+) diffusion, suggesting that spinels may not serve as potential hosts for Mg-ion batteries. The ability to extract Mg with acid in contrast to that with NO2BF4 is attributed to Mn dissolution from the lattice and the consequent reduction in electrostatic repulsion. The findings could provide insights toward the design of Mg hosts for Mg-ion batteries.

  5. Thin-Film Photoluminescent Properties and the Atomistic Model of Mg2TiO4 as a Non-rare Earth Matrix Material for Red-Emitting Phosphor

    Science.gov (United States)

    Huang, Chieh-Szu; Chang, Ming-Chuan; Huang, Cheng-Liang; Lin, Shih-kang

    2016-12-01

    Thin-film electroluminescent devices are promising solid-state lighting devices. Red light-emitting phosphor is the key component to be integrated with the well-established blue light-emitting diode chips for stimulating natural sunlight. However, environmentally hazardous rare-earth (RE) dopants, e.g. Eu2+ and Ce2+, are commonly used for red-emitting phosphors. Mg2TiO4 inverse spinel has been reported as a promising matrix material for "RE-free" red light luminescent material. In this paper, Mg2TiO4 inverse spinel is investigated using both experimental and theoretical approaches. The Mg2TiO4 thin films were deposited on Si (100) substrates using either spin-coating with the sol-gel process, or radio frequency sputtering, and annealed at various temperatures ranging from 600°C to 900°C. The crystallinity, microstructures, and photoluminescent properties of the Mg2TiO4 thin films were characterized. In addition, the atomistic model of the Mg2TiO4 inverse spinel was constructed, and the electronic band structure of Mg2TiO4 was calculated based on density functional theory. Essential physical and optoelectronic properties of the Mg2TiO4 luminance material as well as its optimal thin-film processing conditions were comprehensively reported.

  6. Moessbauer study of iron-cobalt-rhodium spinels

    Energy Technology Data Exchange (ETDEWEB)

    Spencer, C D; Smith, P A; Karnes, C M; Shepard, W A [Ithaca Coll., NY (USA). Dept. of Physics

    1980-01-01

    Moessbauer source and absorber studies have been carried out on the spinel system CoFesub(x)Rhsub(2-x)O/sub 4/ for x 0.005, 0.3, 0.5, 1.0, 1.2 and 1.5. For 0.005 =< x =< 1.2, the cation distribution is normal with Co/sup 2 +/ on A sites. At x = 1.5, the distribution is nearly inverse. In the cases x = 0.005 and 0.3, iron on the B sites does not produce a quadrupole doublet indicating that the B sites are cubic which is contrary to the usual case in spinels.

  7. Influence of the cation substitution on the magnetic properties of LiCo2O4 and Li(Me,Co2O4 spinels

    Directory of Open Access Journals (Sweden)

    Gautier, J. L.

    2004-08-01

    Full Text Available Lithium-based cells LiCo2O4 have been characterized by magnetic techniques, looking at the influence of the partial substitution of cobalt by 3d or 4d transition metal elements (Fe, Ni, Cu, Cr, Mo. The non-substituted compound LiCo2O4 behaves as an antiferromagnet, with a Néel temperature TN of 30 K, although antiferromagnetic interactions are much more important, as suggested by a Weiss parameter Θ of the order of ‑225 K. In the solid solution Li(NixCo2‑xO4 the Weiss parameter Θ changes with x(Ni, reaching large positive values (e.g., Θ ~ +230 K, for x = 0.5. This phenomenon suggests the existence of a canted‑antiferromagnetic or ferrimagnetic structures with large ferromagnetic components. Substitution of cobalt by other 3d or 4d transition metals in the LiMe0.5Co1.5O4 series shows dramatic effects with respect to the non-substituted LiCo2O4 compound : copper completely suppresses the magnetic order, while iron increases TN to almost room temperature. No modifications are observed when molybdenum substitutes cobalt, while chromium transforms the AF order in a ferromagnetic one, with Tc of about 90 K.Se ha caracterizado por técnicas magnéticas, el efecto de la sustitución parcial de Co por elementos de transición 3d o 4d (Fe, Ni, Cu, Cr, Mo en celdas LiCo2O4 a base de litio. El compuesto no sustituído LiCo2O4, se comporta como un antiferromagneto de temperatura de Néel TN de 30 K, aunque existen interacciones antiferromagnéticas mucho más importantes, como lo indica un parámetro de Weiss Θ del orden de -225K. En la solución sólida Li(NixCo2‑xO4, el parámetro de Weiss Θ cambia con x(Ni, alcanzando valores positivos altos (e.g., Θ ~ +230K, para x=0.5. Este fenómeno sugiere la existencia de una estructura antiferromagnética inclinada (“AF-canted” o de una estructura ferrimagnética, donde predominan componentes ferromagnéticas importantes. La sustitución del cobalto por otros elementos de transición 3d o 4d en

  8. Jahn-teller domains and magnetic domains in Mn2FeO4

    NARCIS (Netherlands)

    Kub, J.; Brabers, V.A.M.; Novák, P.; Gemperle, R.; Simsova, J.

    2000-01-01

    Elastic (Jahn–Teller) domains and magnetic domains in the tetragonal spinel Mn2FeO4 were studied using X-ray double-crystal topography, X-ray diffractometry and the colloid-SEM method. The Jahn–Teller domains of the measured samples are tetragonal with the [0 0 1] c-axis alternating perpendicularly

  9. Strongly reduced band gap in NiMn2O4 due to cation exchange

    International Nuclear Information System (INIS)

    Huang, Jhih-Rong; Hsu, Han; Cheng, Ching

    2014-01-01

    NiMn 2 O 4 is extensively used as a basis material for temperature sensors due to its negative temperature coefficient of resistance (NTCR), which is commonly attributed to the hopping mechanism involving coexisting octahedral-site Mn 4+ and Mn 3+ . Using density-functional theory + Hubbard U calculations, we identify a ferrimagnetic inverse spinel phase as the collinear ground state of NiMn 2 O 4 . By a 12.5% cation exchange, a mixed phase with slightly higher energy can be constructed, accompanied by the formation of an impurity-like band in the original 1 eV band gap. This impurity-like band reduces the gap to 0.35 eV, suggesting a possible source of NTCR. - Highlights: • Density functional based calculations were used to study collinear phase of NiMn 2 O 4 . • The ground-state structure is a ferrimagnetic inverse spinel phase. • The tetrahedral and octahedral Mn cations have ferromagnetic interactions. • A 12.5% cation exchange introduces an impurity-like band in the original 1 eV gap. • The 0.35 eV gap suggests a source of negative temperature coefficient of resistance

  10. Checkerboard deposition of lithium manganese oxide spinel (LiMn2O4) by RF magnetron sputtering on a stainless steel in all-solid-state thin film battery

    Science.gov (United States)

    Hsueh, T. H.; Yu, Y. Q.; Jan, D. J.; Su, C. H.; Chang, S. M.

    2018-03-01

    All-solid-state thin film lithium batteries (TFLBs) are the most competitive low-power sources to be applied in various kinds of micro-electro-mechanical systems and have been draw a lot of attention in academic research. In this paper, the checkerboard deposition of all-solid-state TFLB was composed of thin film lithium metal anode, lithium phosphorus oxynitride (LiPON) solid electrolyte, and checkerboard deposition of lithium manganese oxide spinel (LiMn2O4) cathode. The LiPON and LiMn2O4 were deposited by a radio frequency magnetron sputtering system, and the lithium metal was deposited by a thermal evaporation coater. The electrochemical characterization of this lithium battery showed the first discharge capacity of 107.8 μAh and the capacity retention was achieved 95.5% after 150 charge-discharge cycles between 4.3V and 3V at a current density of 11 μA/cm2 (0.5C). Obviously, the checkerboard of thin film increased the charge exchange rate; also this lithium battery exhibited high C-rate performance, with better capacity retention of 82% at 220 μA/cm2 (10C).

  11. Structure, magnetic ordering, and spin filtering efficiency of NiFe{sub 2}O{sub 4}(111) ultrathin films

    Energy Technology Data Exchange (ETDEWEB)

    Matzen, S.; Moussy, J.-B., E-mail: jean-baptiste.moussy@cea.fr [CEA, IRAMIS, SPCSI, F-91191 Gif-sur-Yvette (France); Wei, P. [Francis Bitter Magnet Laboratory, Massachusetts Institute of Technology, Cambridge, Massachusetts 02139 (United States); Gatel, C. [CEMES-CNRS, F-31055 Toulouse (France); Cezar, J. C. [ESRF, F-38043 Grenoble (France); Arrio, M. A.; Sainctavit, Ph. [IMPMC, F-75015 Paris (France); Moodera, J. S. [Francis Bitter Magnet Laboratory, Massachusetts Institute of Technology, Cambridge, Massachusetts 02139 (United States); Physics Department, Massachusetts Institute of Technology, Cambridge, Massachusetts 02139 (United States)

    2014-05-05

    NiFe{sub 2}O{sub 4}(111) ultrathin films (3–5 nm) have been grown by oxygen-assisted molecular beam epitaxy and integrated as effective spin-filter barriers. Structural and magnetic characterizations have been performed in order to investigate the presence of defects that could limit the spin filtering efficiency. These analyses have revealed the full strain relaxation of the layers with a cationic order in agreement with the inverse spinel structure but also the presence of antiphase boundaries. A spin-polarization up to +25% has been directly measured by the Meservey-Tedrow technique in Pt(111)/NiFe{sub 2}O{sub 4}(111)/γ-Al{sub 2}O{sub 3}(111)/Al tunnel junctions. The unexpected positive sign and relatively small value of the spin-polarization are discussed, in comparison with predictions and previous indirect tunnelling magnetoresistance measurements.

  12. Inverse spinel transition metal oxides for lithium-ion storage with different discharge/charge conversion mechanisms

    International Nuclear Information System (INIS)

    Wang, Jiawei; Ren, Yurong; Huang, Xiaobing; Ding, Jianning

    2016-01-01

    Highlights: • Inverse spinel structure relieves the irreversible phase transition of electrodes. • Anodes with the same structure show different discharge/charge conversion mechanisms. • High reversible capacity confirms the potential feasibility of composites. - Abstract: Inverse spinel transition metal oxides (Fe 3 O 4 , MnFe 2 O 4 , Fe 3 O 4 /reduced graphene oxide and MnFe 2 O 4 /reduced graphene oxide) are prepared by a facile ethylene-glycol-assisted hydrothermal method. The stability of inverse spinel structure and the high specific surface area of nanoscale provide transition metal oxides with high specific capacity. And the surface modification with reduced graphene oxide improves the poor conductivity of pristine transition metal oxides. Pristine Fe 3 O 4 and MnFe 2 O 4 deliver the high initial discharge capacity of 1137.1 and 1088.9 mAh g −1 , respectively. Fe 3 O 4 /reduced graphene oxide and MnFe 2 O 4 /reduced graphene oxide get the reversible capacity of 645.8 and 720 mAh g −1 , respectively, even after 55 cycles. The different discharge/charge conversion mechanisms make them different capacity stability. The great electrochemical performances of composites offer electrodes with suitable characteristics for high-performance energy storage application.

  13. Synthesis and electrochemical study of Mg{sub 1.5}MnO{sub 3}: A defect spinel cathode for rechargeable magnesium battery

    Energy Technology Data Exchange (ETDEWEB)

    Saha, Partha [Department of Bioengineering, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); US Department of Energy, National Energy Technology Laboratory, Morgantown, WV 26507 (United States); Jampani, Prashanth H., E-mail: pjampani@pitt.edu [Department of Bioengineering, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); Hong, DaeHo [Department of Bioengineering, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); Gattu, Bharat [Mechanical Engineering and Materials Science, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); Poston, James A.; Manivannan, Ayyakkannu [US Department of Energy, National Energy Technology Laboratory, Morgantown, WV 26507 (United States); Datta, Moni Kanchan [Department of Bioengineering, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); US Department of Energy, National Energy Technology Laboratory, Morgantown, WV 26507 (United States); Kumta, Prashant N., E-mail: pkumta@pitt.edu [Department of Bioengineering, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); US Department of Energy, National Energy Technology Laboratory, Morgantown, WV 26507 (United States); Mechanical Engineering and Materials Science, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); Chemical and Petroleum Engineering, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); School of Dental Medicine, University of Pittsburgh, PA 15261 (United States); Center for Complex Engineered Multifunctional Materials, University of Pittsburgh, Pittsburgh, PA 15261 (United States)

    2015-12-15

    Graphical abstract: Mg{sub 1.5}MnO{sub 3}, a defect oxide spinel derived by the Pechini route, was tested as cathode for rechargeable magnesium battery. TEM and XRD analyses of Mg{sub 1.5}MnO{sub 3} shows the formation of ∼100 nm sized nano particles in the cubic defect spinel structure (space group: Fd3m; unit cell: 0.833294 nm). Cyclic voltammetry illustrates a reversible reaction occurring between 0.3 and 1.5 V versus magnesium. Galvanostatic cycling of the Mg{sub 1.5}MnO{sub 3} cathode exhibits a low capacity of ∼12.4 mAh/g up to 20 cycle with ∼99.9% Coulombic efficiency when cycled at a current rate of ∼C/27. XPS (X-ray photoelectron spectroscopy) surface probe of magnesiated/de-magnesiated electrodes confirm a change in the redox center of Mn-ions during intercalation/de-intercalation of Mg-ion from the Mg{sub 1.5}MnO{sub 3} electrode. The low capacity of Mg{sub 1.5}MnO{sub 3} electrode mainly stem from the kinetic limitation of Mg-ion removal from the defect oxide spinel as the electrochemical impedance spectroscopy results of electrodes after 1st and 2nd cycle show that charge transfer resistance, R{sub e}, increases post charge state whereas interfacial resistance, R{sub i}, increases after discharge state, respectively. - Highlights: • Pechini process yields 100 nm sized particles of the defect cubic spinel Mg{sub 1.5}MnO{sub 3}. • Stable capacity of ∼12.4 mAh/g obtained at C/27 rate and 99.9% Coulombic efficiency. • XPS shows change in valence state of Mn{sup 3+}/Mn{sup 4+} center with cycling. • Low capacity stems from increase in charge-transfer and interfacial resistances with cycling. - Abstract: Mg{sub 1.5}MnO{sub 3}, a defect oxide spinel (space group: Fd3m; unit cell: 0.833294 nm) of particle size ∼100 nm derived by the Pechini route was tested as a cathode for rechargeable magnesium battery. Cyclic voltammetry illustrates a reversible reaction occurring in the 0.3–2.0 V potential window versus magnesium. The spinel however

  14. Structural, morphological and magnetic properties of Eu-doped CoFe2O4 nano-ferrites

    Directory of Open Access Journals (Sweden)

    Aiman Zubair

    Full Text Available Europium (Eu doped spinel cobalt ferrites having composition CoEuxFe2−xO4 where x = 0.00, 0.03, 0.06, 0.09, 0.12 were fabricated by co-precipitation route. In order to observe the phase development of the ferrite samples, thermo-gravimetric analysis was carried out. The synthesized samples were subjected to X-ray diffraction analysis for structural investigation. All the samples were found to constitute face centered cubic (FCC spinel structure belonging to Fd3m space group. Scanning electron microscopy revealed the formation of nanocrystalline grains with spherical shape. Energy dispersive X-ray spectra confirmed the presence of Co, Eu, Fe and O elements with no existence of any impurity. The magnetic hysteresis curves measured at room temperature exhibited ferrimagnetic behavior with maximum saturation magnetization (Ms of 65 emu/g and coercivity (Hc of 966 Oe. The origin of ferrimagnetism in Eu doped cobalt ferrites was discussed in detail with reverence to the allocation of Co2+ and Fe3+ ions within the spinel lattice. The overall coercivity was increased (944–966 Oe and magnetization was decreased (65–46 emu/g with the substitution of Eu3+. The enhancement of former is ascribed to the transition from multi domain to single domain state and reduction in lateral is attributed to the incorporation of nonmagnetic Eu ions for Fe, resulting in weak superexchange interactions. Keywords: Europium doped cobalt ferrites, Co-precipitation, X-ray diffraction, Scanning electron microscopy, Magnetic properties

  15. Double channel electrode flow cell application to the study of HO2- production on Mn xCo3-xO4 (0 ≤ x ≤ 1) spinel films

    International Nuclear Information System (INIS)

    Rios, E.; Reyes, H.; Ortiz, J.; Gautier, J.L.

    2005-01-01

    We conducted a study on the electroreduction of O 2 in alkaline solution at room temperature on pure thin oxide electrodes of composition Mn x Co 3-x O 4 (0 ≤ x ≤ 1) using the double channel electrode flow cell (DCEFC). The oxides were prepared at 150 deg. C and deposited by spray pyrolysis onto titanium substrates. The oxygen reduction reaction (orr) occurs through 'interactive' and 'parallel' pathways, and the ratio of O 2 molecules reduced to OH - ions with respect to those reduced to HO 2 - ions depends on the oxide stoichiometry and on the applied overpotential. The formation of HO 2 - increases when the manganese concentration increases. The results obtained for the orr show that the number of electrons transferred per O 2 molecule decreases from 3 to 2 and the ratio k 1 /k 2 (the rate constants for direct reduction to OH - and indirect reduction to HO 2 - ) increases, respectively, in the overpotential studied range (-0.05 to -0.6 V). The Mn 3+ ions placed in the B-sites of the spinel structure seem to be the active centres, where hydrogen peroxide is formed

  16. Lattice vibrations of materials for lithium rechargeable batteries II. Lithium extraction-insertion in spinel structures

    International Nuclear Information System (INIS)

    Julien, C.M.; Camacho-Lopez, M.A.

    2004-01-01

    Lithiated spinel manganese oxides with various amounts of lithium have been prepared through solid-state reaction and electrochemical intercalation and deintercalation. Local structure of the samples are studied using Raman scattering and Fourier transform infrared spectroscopy. We report vibrational spectra of lithiated manganese oxides Li x Mn 2 O 4 as a function of lithium concentration in the range 0.1≤x≤2.0. Raman and Fourier transform infrared (FTIR) spectral results indicated multiple-phase reactions when the lithium content is modified in the spinel lattice. Lattice dynamics of lithiated spinel manganese oxides have been interpreted using either a classical factor-group analysis or a local environment model. The structural modifications have been studied on the basis of vibrations of LiO 4 tetrahedral and MnO 6 octahedral units when Li/Mn≤0.5, and LiO 4 , LiO 6 , and MnO 6 structural units when Li/Mn>0.5

  17. Investigation of positive electrode materials based on MnO2 for lithium batteries

    International Nuclear Information System (INIS)

    Le, My Loan Phung; Lam, Thi Xuan Binh; Pham, Quoc Trung; Nguyen, Thi Phuong Thoa

    2011-01-01

    Various composite materials of MnO 2 /C have been synthesized by electrochemical deposition and then used for the synthesis of lithium manganese oxide (LiMn 2 O 4 ) spinel as a cathode material for lithium ion batteries. The structure and electrochemical properties of electrode materials based on MnO 2 /C, spinel LiMn 2 O 4 and doped spinel LiNi 0.5 Mn 1.5 O 4 have been studied. The influence of synthesis conditions on the structural and electrochemical properties of synthesized materials was investigated by x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electronic microscopy (TEM) and charge–discharge experiments. Some of the studied materials exhibit good performance of cycling and discharge capacity

  18. Electronic structure and physical properties of the spinel-type phase of BeP2N4 from all-electron density functional calculations

    International Nuclear Information System (INIS)

    Ching, W. Y.; Aryal, Sitram; Rulis, Paul; Schnick, Wolfgang

    2011-01-01

    Using density-functional-theory-based ab initio methods, the electronic structure and physical properties of the newly synthesized nitride BeP 2 N 4 with a phenakite-type structure and the predicted high-pressure spinel phase of BeP 2 N 4 are studied in detail. It is shown that both polymorphs are wide band-gap semiconductors with relatively small electron effective masses at the conduction-band minima. The spinel-type phase is more covalently bonded due to the increased number of P-N bonds for P at the octahedral sites. Calculations of mechanical properties indicate that the spinel-type polymorph is a promising superhard material with notably large bulk, shear, and Young's moduli. Also calculated are the Be K, P K, P L 3 , and N K edges of the electron energy-loss near-edge structure for both phases. They show marked differences because of the different local environments of the atoms in the two crystalline polymorphs. These differences will be very useful for the experimental identification of the products of high-pressure syntheses targeting the predicted spinel-type phase of BeP 2 N 4 .

  19. Photocatalytic degradation of methylene blue on magnetically separable MgFe2O4 under visible light irradiation

    International Nuclear Information System (INIS)

    Shahid, Muhammad; Jingling, Liu; Ali, Zahid; Shakir, Imran; Warsi, Muhammad Farooq; Parveen, Riffat; Nadeem, Muhammad

    2013-01-01

    A magnetically separable single-phase MgFe 2 O 4 photocatalyst with a spinel crystal structure was synthesized by using the solid-state reaction method. The formation of spinel structure is confirmed by X-ray diffraction and Fourier transform infrared spectroscopy. The magnetic measurements showed that the photocatalyst material can be separated from water when an external magnetic field is added and redispersed into water solution after the external magnetic field is eliminated. It is one of the promising photocatalysts for waste water treatment. The photocatalytic activity of MgFe 2 O 4 was investigated by using the photo-decomposition of methylene blue dye under visible light. The photoelectrochemical property of the MgFe 2 O 4 was studied by measuring their photocurrent–potential behavior in 1 M NaOH electrolyte under AM 1.5100 mW cm −2 illumination. - Graphical abstract: Highly efficient magnetically separable MgFe 2 O 4 photocatalyst for organic based impurities decomposition as well as for the production of H 2 gas was synthesized and characterized successfully (a) MgFe 2 O 4 photocatalyst in polluted water, (b) The photocatalyst (MgFe 2 O 4 ) is being attracted toward magnetic field for separation, (c) Hysteresis loop of MgFe 2 O 4 showing magnetic behavior. Highlights: ► New photocatalyst working in the visible range have been synthesized by facile cheap route. ► MgFe 2 O 4 photocatalyst showed well defined magnetically separable behavior. ► Excellent water splitting characteristics to produce H 2 was observed under visible light irradiation

  20. Incorporation of zinc for fabrication of low-cost spinel-based composite ceramic membrane support to achieve its stabilization.

    Science.gov (United States)

    Li, Lingling; Dong, Xinfa; Dong, Yingchao; Zhu, Li; You, Sheng-Jie; Wang, Ya-Fen

    2015-04-28

    In order to reduce environment risk of zinc, a spinel-based porous membrane support was prepared by the high-temperature reaction of zinc and bauxite mineral. The phase evolution process, shrinkage, porosity, mechanical property, pore size distribution, gas permeation flux and microstructure were systematically studied. The XRD results, based on a Zn/Al stoichiometric composition of 1/2, show a formation of ZnAl2O4 structure starting from 1000°C and then accomplished at 1300°C. For spinel-based composite membrane, shrinkage and porosity are mainly influenced by a combination of an expansion induced by ZnAl2O4 formation and a general densification due to amorphous liquid SiO2. The highest porosity, as high as 44%, is observed in ZnAl4 membrane support among all the investigated compositions. Compared with pure bauxite (Al), ZnAl4 composite membrane support is reinforced by ZnAl2O4 phase and inter-locked mullite crystals, which is proved by the empirical strength-porosity relationships. Also, an increase in average pore diameter and gas flux can be observed in ZnAl4. A prolonged leaching experiment reveals the zinc can be successfully incorporated into ceramic membrane support via formation of ZnAl2O4, which has substantially better resistance toward acidic attack. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Thermoluminescence of Stoichiometric Magnesium-Aluminium Spinel Defects

    International Nuclear Information System (INIS)

    Kobyakov, V.A.; Gritsina, V.T.; Kazarinov, Yu.G.; Volokitin, V.N.

    2005-01-01

    The investigations of thermoluminescence of spinel single crystals MgAl 2 O 4 after UV- and X-ray irradiation was provided by using method of self consisting heating. It was shown, that observed maxima at temperatures of ∼360 and ∼530 K in UV- and green ranges of spectra, respectively, are complex and consist of several strongly overlapping partial maxima. By using method of self consisting heating we have revealed the approximate position of partial maxima, which are included in maxima of ∼360 and ∼530 K, and for some partial maxima there was obtained the order of kinetics, activation energies, and frequency factors

  2. The Influence of Doping with Transition Metal Ions on the Structure and Magnetic Properties of Zinc Oxide Thin Films

    Directory of Open Access Journals (Sweden)

    Jenica Neamtu

    2014-01-01

    Full Text Available Zn1−xNixO (x=0.03÷0.10 and Zn1−xFexO (x=0.03÷0.15 thin films were synthesized by sol-gel method. The structure and the surface morphology of zinc oxide thin films doped with transition metal (TM ions have been investigated by X-ray diffraction (XRD and atomic force microscopy (AFM. The magnetic studies were done using vibrating sample magnetometer (VSM at room temperature. Experimental results revealed that the substitution of Ni ions in ZnO wurtzite lattice for the contents x=0.03÷0.10 (Ni2+ leads to weak ferromagnetism of thin films. For Zn1-xFexO with x=0.03÷0.05, the Fe3+ ions are magnetic coupling by superexchange interaction via oxygen ions in wurtzite structure. For x=0.10÷0.15 (Fe3+ one can observe the increasing of secondary phase of ZnFe2O4 spinel. The Zn0.9Fe0.1O film shows a superparamagnetic behavior due to small crystallite sizes and the net spin magnetic moments arisen from the interaction between the iron ions through an oxygen ion in the spinel structure.

  3. Impact of Nd{sup 3+} in CoFe{sub 2}O{sub 4spinel ferrite nanoparticles on cation distribution, structural and magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Yadav, Raghvendra Singh, E-mail: yadav@fch.vutbr.cz [Materials Research Centre, Brno University of Technology, Purkyňova 464/118, 61200 Brno (Czech Republic); Havlica, Jaromir; Masilko, Jiri; Kalina, Lukas; Wasserbauer, Jaromir; Hajdúchová, Miroslava; Enev, Vojtěch [Materials Research Centre, Brno University of Technology, Purkyňova 464/118, 61200 Brno (Czech Republic); Kuřitka, Ivo; Kožáková, Zuzana [Centre of Polymer Systems, University Institute, Tomas Bata University in Zlín, Nad Ovčírnou 3685, 760 01 Zlín (Czech Republic)

    2016-02-01

    Nd{sup 3+} doped cobalt ferrite nanoparticles have been synthesized by starch-assisted sol–gel auto-combustion method. The significant role played by Nd{sup 3+} added to cobalt ferrite in changing cation distribution and further in influencing structural and magnetic properties, was explored and reported. The crystal structure formation and crystallite size were studied from X-ray diffraction studies. The microstructural features were investigated by field emission scanning electron microscopy and transmission electron microscopy that demonstrates the nanocrystalline grain formation with spherical morphology. An infrared spectroscopy study shows the presence of two absorption bands related to tetrahedral and octahedral group complexes within the spinel ferrite lattice system. The change in Raman modes in synthesized ferrite system were observed with Nd{sup 3+} substitution, particle size and cation redistribution. The impact of Nd{sup 3+} on cation distribution of Co{sup 2+} and Fe{sup 3+} at octahedral and tetrahedral sites in spinel ferrite cobalt ferrite nanoparticles was investigated by X-ray photoelectron spectroscopy. Room temperature magnetization measurements showed that the saturation magnetization and coercivity increase with addition of Nd{sup 3+} substitution in cobalt ferrite. - Highlights: • Nd{sup 3+} doped CoFe{sub 2}O{sub 4} nanoparticles by starch-assisted sol–gel auto-combustion method. • The change in Raman modes with Nd{sup 3+} substitution. • Presence of absorption infrared bands related to octahedral and tetrahedral site. • The impact of Nd{sup 3+} on cation distribution at octahedral and tetrahedral sites. • Influence of Nd{sup 3+} substitution in cobalt ferrite on magnetic properties.

  4. Dielectric studies of Co3-xMnxO4 (x=0.1-1.0) cubic spinel multiferroic

    Science.gov (United States)

    Meena, P. L.; Kumar, Ravi; Prajapat, C. L.; Sreenivas, K.; Gupta, Vinay

    2009-07-01

    A series of Co3-xMnxO4 (x =0.1-1.0) multiferroic cubic spinel ceramics were prepared to study the effect of Mn substitution at Co site on the crystal structures and dielectric properties. No significant change in the structural symmetry was observed with increasing x up to 1.0. A linear increase in lattice parameter with x is attributed to the substitution of Co3+ by Mn3+ (large ionic radii) at the octahedral sites. An antiferromagnetic-type ordering of Co3O4 changes to ferrimagnetic-type order after incorporation of Mn. The effect of Mn substitution on the dielectric constant and loss tangent was studied over a wide range of frequency (75 kHz-5 MHz) and temperature of 150-450 K. The measured value of room temperature ac conductivity at 1.0 MHz was found to increase from 2.0×10-6 to 4.4×10-4 Ω-1 cm-1 and follows power law (σac=Aωs) behavior. The dielectric constant ɛ'(ω) shows a weak frequency dispersion and small temperature dependence below 250 K for all ceramic samples. However, a strong temperature and frequency dependence on ɛ'(ω) was observed at higher temperature (>250 K). The temperature dependent ɛ'(ω) data show the existence of room temperature ferroelectricity in all prepared samples.

  5. Synthesis, characterization and photocatalytic activity of cubic-like CuCr2O4 for dye degradation under visible light irradiation

    International Nuclear Information System (INIS)

    Yuan, Wenhui; Liu, Xiaoxia; Li, Li

    2014-01-01

    Graphical abstract: Hydrothermal synthesis method was applied for preparation of cubic-like CuCr 2 O 4 spinel nanoparticles without template. The synthesized cubic-like CuCr 2 O 4 shows excellent photocatalytic activity for degradation of RhB and MB cationic dyes but not for MO anionic dye in the presence of H 2 O 2 under visible light irradiation. - Highlights: • The cubic-like CuCr 2 O 4 spinel nanoparticles were successfully synthesized via the hydrothermal synthesis method. • The calcination temperature has a great influence on the morphology, particle size and photocatalytic activity of CuCr 2 O 4 . • The pH at the point of zero charge (pH pzc ) of the CuCr 2 O 4 calcined at 600 °C is about 4.52. • The cubic-like CuCr 2 O 4 calcined at 600 °C exhibits excellent photocatalytic activity for RhB and MB in the presence of H 2 O 2 under visible-light irradiation. - Abstract: CuCr 2 O 4 nanoparticles with cubic-like morphology were prepared via hydrothermal synthesis method without template. The CuCr 2 O 4 samples were characterized by thermogravimetry and differential scanning calorimetry (TG–DSC), X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV–vis diffuse reflectance spectra (DRS) and Zeta potentials, respectively. The results indicated that cubic-like CuCr 2 O 4 could be successfully synthesized by calcining the precursor at 600 °C, and the calcination temperature greatly influenced the morphology and optical performance of CuCr 2 O 4 . The pH at the point of zero charge (pH pzc ) of the CuCr 2 O 4 calcined at 600 °C was about 4.52. The photocatalytic activity of CuCr 2 O 4 was evaluated for degradation of rhodamine B (RhB), methylene blue (MB), and methyl orange (MO) in the presence of H 2 O 2 under visible light irradiation and the effects of the calcination temperature, dosage of photocatalyst, etc., on photocatalytic activity were studied in detail. The photocatalytic results

  6. Preparation, characterization and photocatalytic activity of visible-light-driven plasmonic Ag/AgBr/ZnFe2O4 nanocomposites

    International Nuclear Information System (INIS)

    Li, Xiaojuan; Tang, Duanlian; Tang, Fan; Zhu, Yunyan; He, Changfa; Liu, Minghua; Lin, Chunxiang; Liu, Yifan

    2014-01-01

    Highlights: • A plasmonic Ag/AgBr/ZnFe 2 O 4 photocatalyst has been successfully synthesized. • Ag/AgBr/ZnFe 2 O 4 nanocomposites exhibit high visible light photocatalytic activity. • Ag/AgBr/ZnFe 2 O 4 photocatalyst is stable and magnetically separable. - Abstract: A visible-light-driven plasmonic Ag/AgBr/ZnFe 2 O 4 nanocomposite has been successfully synthesized via a deposition–precipitation and photoreduction through a novel one-pot process. X-ray diffraction spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy and UV–vis diffuse reflectance spectroscopy were employed to investigate the crystal structure, chemical composition, morphology, and optical properties of the as-prepared nanocomposites. The photocatalytic activities of the nanocomposites were evaluated by photodegradation of Rhodamine B (RhB) and phenol under visible light. The results demonstrated that the obtained Ag/AgBr/ZnFe 2 O 4 nanocomposites exhibited higher photocatalytic activity as compared to pure ZnFe 2 O 4 . In addition, the sample photoreduced for 20 min and calcined at 500 °C achieved the highest photocatalytic activity. Furthermore, the Ag/AgBr/ZnFe 2 O 4 nanocomposite has high stability under visible light irradiation and could be conveniently separated by using an external magnetic field

  7. Ferri-magnetic order in Mn induced spinel Co{sub 3−x}Mn{sub x}O{sub 4} (0.1≤x≤1.0) ceramic compositions

    Energy Technology Data Exchange (ETDEWEB)

    Meena, P.L., E-mail: plmeena@gmail.com [Department of Physics, Deen Dayal Upadhyaya College (University of Delhi), Shivaji Marg, Karampura, New Delhi 110015 (India); Sreenivas, K. [Department of Physics and Astrophysics, University of Delhi, North Campus, Delhi 110007 (India); Singh, M.R. [Technical Physics and Prototype Engineering Division, Bhabha Atomic Research Centre, Mumbai, Maharashtra 400085 (India); Kumar, Ashok; Singh, S.P. [National Physical Laboratory, Dr. K.S. Krishnan Marg, New Delhi 110012 (India); Kumar, Ravi [Beant College of Engineering and Technology, Gurdaspur, Punjab 143521 (India)

    2016-04-01

    We report structural and magnetic properties of spinel Co{sub 3−x}Mn{sub x}O{sub 4} (x=0.1–1.0) synthesized by solid state reaction technique. Rietveld refinement analysis of X-ray diffraction (XRD) data, revealed the formation of polycrystalline single phase Co{sub 3−x}Mn{sub x}O{sub 4} without any significant structural change in cubic crystal symmetry with Mn substitution, except change in lattice parameter. Temperature dependent magnetization data show changes in magnetic ordering temperature, indicating formation of antiferromagnetic (AFM) and ferrimagnetic (FM) phase at low Mn concentration (x≤0.3) and well-defined FM phase at high Mn concentration (x≥0.5). The isothermal magnetization records established an AFM/FM mixed phase for composition ranging 0.10.5. - Highlights: • Synthesis of single phase polycrystalline Co{sub 3−x}Mn{sub x}O{sub 4} ceramic. • Change in magnetic ordering with varying Mn concentration. • The complex spin distribution is contributing to FM ordering with higher Mn.

  8. Magnetic, hyperthermic and structural properties of zn substituted CaFe2O4 powders

    Science.gov (United States)

    Kheradmand, Abbas; Vahidi, Omid; Masoudpanah, S. M.

    2018-03-01

    In the present study, we have synthesized single phase Ca1 - x Zn x Fe2O4 powders by hydrothermal method. The cation distribution between the tetrahedral and octahedral sites in the spinel structure and the magnetic properties as a function of the zinc substitution have been investigated by X-ray diffraction (XRD), infrared spectroscopy and vibrating sample magnetometer methods. The obtained XRD pattern indicated that the synthesized particles had single phase cubic spinel structure with no impurity. The magnetic measurements showed that the saturation magnetization increased from 83 to 98 emu/g with the addition of zinc due to the decrease of inversity. The particle size observed by electron microscopy decreased from 1.38 to 0.97 µm with the increase of zinc addition. The Ca0.7Zn0.3Fe2O4 powders exhibited appropriate heating capability for hyperthermia applications with the maximum AC heating temperature of 20 °C and specific loss power of 9.29 W/g.

  9. Structural and magnetic properties of [001] CoCr2O4 thin films

    NARCIS (Netherlands)

    Guzman, Roger; Heuver, Jeroen; Matzen, Sylvia; Magen, Cesar; Noheda, Beatriz

    2017-01-01

    The spinel CoCr2O4 (CCO) is one of the few bulk multiferroics with net magnetic moment. However, studies on the properties of CCO thin films are scarce. Here, we investigate the interplay between microstructure and magnetism of a series of CCO epitaxial thin films by means of x-ray diffraction,

  10. Structure and cation distribution of (Mn0.5Zn0.5)Fe2O4 thin films on SrTiO3(001)

    Science.gov (United States)

    Welke, M.; Brachwitz, K.; Lorenz, M.; Grundmann, M.; Schindler, K.-M.; Chassé, A.; Denecke, R.

    2017-06-01

    A comprehensive study on growth of ferrimagnetic manganese zinc ferrite (Mn0.5Zn0.5Fe2O4) films on single crystalline strontium titanate(001) (SrTiO3) substrates was carried out. Under the optimized conditions, a thin film with a layer thickness of 200 nm was deposited, and the structural properties were investigated. Contrary to data published in literature, no buffer layer was necessary to achieve epitaxial growth of a poorly lattice-matched layer. This was confirmed for Mn0.5Zn0.5Fe2O4(001) on SrTiO3(001) by x-ray diffraction and the adjoined phi scans, which also revealed a lattice compression of 1.2% of the manganese zinc ferrite film in the out-of-plane direction. Using x-ray photoelectron spectroscopy, the near surface stoichiometry of the film could be shown to agree with the intended one within the uncertainty of the method. X-ray absorption spectroscopy showed an electronic structure close to that published for bulk samples. Additional x-ray magnetic circular dichroism investigations were performed to answer detailed structural questions by a comparison of experimental data with the calculated ones. The calculations took into account ion sites (tetrahedral vs. octahedral coordination) as well as the charge of Fe ions (Fe2+ vs. Fe3+). Contrary to the expectation for a perfect normal spinel that only Fe3+ ions are present in octahedral sites, hints regarding the presence of additional Fe2+ in octahedral sites as well as Fe3+ ions in tetrahedral sites have been obtained. Altogether, the layer could be shown to be mostly in a normal spinel configuration.

  11. Surface modification of spinel λ-MnO2 and its lithium adsorption properties from spent lithium ion batteries

    International Nuclear Information System (INIS)

    Li, Li; Qu, Wenjie; Liu, Fang; Zhao, Taolin; Zhang, Xiaoxiao; Chen, Renjie; Wu, Feng

    2014-01-01

    Highlights: • A method is designed to synthesize a λ-MnO 2 ion-sieve for lithium ions adsorption. • Ultrasonic treatment with acid is highly efficient for lithium ions extraction. • Surface modification by CeO 2 is used to improve the adsorption capacity. • A 0.5 wt.% CeO 2 -coated ion-sieve shows the best adsorption properties. • λ-MnO 2 ion-sieves are promising for recovering scarce lithium resources. - Abstract: Spinel λ-MnO 2 ion-sieves are promising materials because of their high selectivity toward lithium ions, and this can be applied to the recovery of lithium from spent lithium ion batteries. However, manganese dissolution loss during the delithiation of LiMn 2 O 4 causes a decrease in adsorption capacity and poor cycling stability for these ion-sieves. To improve the lithium adsorption properties of λ-MnO 2 ion-sieves, surface modification with a CeO 2 coating was studied using hydrothermal-heterogeneous nucleation. The structure, morphology and composition of the synthesized materials were determined by XRD, SEM, TEM and EDS. The effect of hydrothermal synthesis conditions and the amount of CeO 2 coating on the adsorption performance of λ-MnO 2 were also investigated. A 0.5 wt.% CeO 2 -coated ion-sieve was synthesized by heating at 120 °C for 3 h and it had better adsorption properties than the bare samples. The effect of ultrasonic treatment on the lithium extraction ratio from LiMn 2 O 4 upon acid treatment at various temperatures was studied and the results were compared with conventional mechanical stirring. We found that ultrasonic treatment at lower temperature gave almost the same maximum lithium extraction ratio and was more efficient and economic

  12. Synthesis and electrochemical properties of LiNi0.4Mn1.5Cr0.1O4 and Li4Ti5O12

    CSIR Research Space (South Africa)

    Liu, GQ

    2011-08-01

    Full Text Available Spinel compound LiNi0.4Mn1.5Cr0.1O4 (LNMCO) and Li4Ti5O12 (LTO) were synthesized by the sol-gel method and the solid-state method, respectively. The particle sizes of the products LiNi0.4Mn1.5Cr0.1O4 and Li4Ti5O12 were 0.5 to 2 um and 0.5 to 0.8 um...

  13. The effect of dolomite type and Al2O3 content on the phase composition in aluminous cements containing spinel

    Directory of Open Access Journals (Sweden)

    R. Naghizadeh

    2011-06-01

    Full Text Available In this paper, the effect of dolomite type and Al2O3 content on the phase composition in aluminous cements containing MA spinel is investigated. For this reason, the raw and calcined dolomites are used as raw materials along with calcined alumina in the preparation of the cement. Then, different compositions are prepared at 1350°C using the sintering method and their mineralogical compositions are investigated using the diffractometric technique. Also, their microstructures arre evaluated. The results indicate that raw materials used have great effect on the type and amount of formed phases in cement composition. Independently of the dolomite type used, a mixed phase product consisting of spinel accompanied by CA and CA2 is obtained. The content of CA phase in the cement composition is decreased with increasing of Al2O3 in the raw materials composition. On the other hand, the content of CA2 phase is increased with the addition of Al2O3. In addition, the results show that the formation of C12A7 is favored by use of calcined dolomite.

  14. Mechanism of γ-irradiation induced phase transformations in nanocrystalline Mn{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} ceramics

    Energy Technology Data Exchange (ETDEWEB)

    Jagadeesha Angadi, V. [Department of Physics, Bangalore University, Bangalore, Karnataka 560056 (India); Anupama, A.V.; Choudhary, Harish K.; Kumar, R. [Materials Research Centre, Indian Institute of Science, Bangalore, 560012 (India); Somashekarappa, H.M. [Center for Application of Radioisotopes and Radiation Technology, Mangalore University, Mangalore 574199 (India); Mallappa, M. [Department of Chemistry, Government Science College, Bangalore 560001 (India); Rudraswamy, B. [Department of Physics, Bangalore University, Bangalore, Karnataka 560056 (India); Sahoo, B., E-mail: bsahoo@mrc.iisc.ernet.in [Materials Research Centre, Indian Institute of Science, Bangalore, 560012 (India)

    2017-02-15

    The structural, infrared absorption and magnetic property transformations in nanocrystalline Mn{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} samples irradiated with different doses (0, 15, 25 and 50 kGy) of γ-irradiation were investigated in this work and a mechanism of phase transformation/decomposition is provided based on the metastable nature of the Mn-atoms in the spinel lattice. The nano-powder sample was prepared by solution combustion route and the pellets of the sample were exposed to γ-radiation. Up to a dose of 25 kGy of γ-radiation, the sample retained the single phase cubic spinel (Fd-3m) structure, but the disorder in the sample increased. On irradiating the sample with 50 kGy γ-radiation, the spinel phase decomposed into new stable phases such as α-Fe{sub 2}O{sub 3} and ZnFe{sub 2}O{sub 4} phases along with amorphous MnO phase, leading to a change in the surface morphology of the sample. Along with the structural transformations the magnetic properties deteriorated due to breakage of the ferrimagnetic order with higher doses of γ-irradiation. Our results are important for the understanding of the stability, durability and performance of the Mn-Zn ferrite based devices used in space applications. - Graphical abstract: The nanocrystalline Mn{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} ceramic sample transforms to crystalline α-Fe{sub 2}O{sub 3} and ZnFe{sub 2}O{sub 4} phases (and amorphous MnO phase) at a γ-irradiation dose of 50 kGy, as MnO goes out of the spinel lattice. The high energy γ-irradiation causes structural damage to the nanomaterials leading to change in morphology of the sample as seen in the SEM images. - Highlights: • Mn atoms are more unstable in the Mn-Zn ferrite spinel lattice than Zn-atoms. • Displacement of Mn atoms by γ-radiation from the lattice renders phase transformation. • In Mn{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4}, Mn-ferrite cell transforms to crystalline α-Fe{sub 2}O{sub 3} and amorphous MnO. • The stable ZnFe{sub 2}O

  15. Modified voltammetric, impedimetric and optical behavior of polymer- assisted sol-gel MgFe2O4 nanostructured thin films

    International Nuclear Information System (INIS)

    Bazhan, Z.; Ghodsi, F.E.; Mazloom, J.

    2017-01-01

    Highlights: •Electrochemical properties of spinel PEG/PVP MgFe 2 O 4 thin films prepared by spin coating technique have been investigated. •PSD analysis indicated that spectral roughness of films decreased by polymer incorporation. •Optical calculations exhibited a blue shift on optical band gap by polymer addition. •CV curves revealed that ion storage capacitance of PEG/MgFe 2 O 4 is two times higher than MgFe 2 O 4 thin films. •EIS analysis confirmed that incorporation of appropriate amount of PEG reduced the charge transfer resistance. -- Abstract: The effect of polyethylene glycol (PEG) and polyvinylpyrrolidone (PVP) on physical properties of sol-gel prepared magnesium ferrite (MF) thin films was investigated. The X-ray diffraction (XRD) results showed the formation of cubic spinel magnesium ferrite for all samples. The surface morphology of films changed and average surface roughness decreased by polymer addition. The height-height correlation function and fractal dimension were evaluated using cube counting and triangulation methods from atomic force microscopy (AFM) images. The refractive index and extinction coefficient of MF thin films decreased by adding polymer while the band gap value increased from 2.24 to 2.72 eV. The PEG addition enhanced the electrochemical performance while PVP addition didn’t have significant effect on cyclic voltammetry (CV) of magnesium ferrite thin films. The sample with highest value of PEG showed the maximum specific capacitance (68.5 mF cm −2 ) and the smallest charge transfer resistance (565 Ω) among all samples.

  16. Negative and anomalous T-dependent magnetization trend in CoCr2O4 nanoparticles

    Science.gov (United States)

    Kamran, M.; Nadeem, K.; Mumtaz, M.

    2017-10-01

    We studied the temperature dependent magnetic properties of cobalt chromite (CoCr2O4) nanoparticles. X-ray diffraction revealed the cubic spinel structure of the nanoparticles and average crystallite size was about 42 nm. Raman and Fourier transform infrared spectroscopy confirmed the formation of single phase spinel structure. ZFC/FC curves revealed a paramagnetic (PM) to ferromagnetic (FiM) transition at TC = 100 K with conical spiral state at TS = 27 K and lock-in state at TL = 13 K. Negative magnetization is observed in the ZFC curve under 50 Oe applied field, which gets suppressed upon the application of higher field. The TC was shifted towards higher temperature with the application of higher field, while TS and TL remain unaffected. M-H loops showed FiM behavior below 100 K and nearly PM at TC = 100 K. Below 75 K, an abnormal decrease in MS is observed down to 5 K, which may be due to presence of stiffed/strong conical spin spiral and lock in states at low temperatures. Modified Kneller's law showed a good fit for temperature dependent Hc at higher temperature and deviated at low temperature (disordered surface spins. Nanoparticles showed slow spin relaxation in both ZFC and FC protocols at 5 K, which signifies the presence of spin-glass like behavior at low temperatures. Both curves were fitted with stretched exponential law and the value of β lies in the spin-glass regime. In summary, CoCr2O4 nanoparticles showed anomalous decrease of MS with decreasing temperature, negative magnetization at low field and rather stiffed/strong conical spin spiral and lock-in states in combination with spin-glass behavior at the low temperatures.

  17. Thin film fabrication and transport properties of the heavy Fermion oxide LiV{sub 2}O{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Niemann, Ulrike [Max Planck Institute for Solid State Research, Stuttgart (Germany); Hirai, Daigorou [University of Tokyo, Tokyo (Japan); Takagi, Hidenori [Max Planck Institute for Solid State Research, Stuttgart (Germany); University of Tokyo, Tokyo (Japan); Institute for Functional Matter and Quantum Technologies, University of Stuttgart, Stuttgart (Germany)

    2016-07-01

    The spinel compound LiV{sub 2}O{sub 4} is well-known for its heavy fermion behaviour, although it contains no f-electron bands. This unexpected behaviour has been a subject of several studies, but the origin of it is still not fully understood. In this study, we successfully fabricated single crystalline epitaxial thin film of LiV{sub 2}O{sub 4} on SrTiO{sub 3}, LSAT and MgO substrates, using a pulsed laser deposition technique. By changing film thickness and substrate materials, dimensionality and epitaxial strain was controlled. The formation of an epitaxially grown LiV{sub 2}O{sub 4} phase has been confirmed by X-ray diffraction measurements. LiV{sub 2}O{sub 4} films on MgO were found to be strained, due to the small lattice mismatch, in contrast to fully relaxed films on SrTiO{sub 3}.The heavy fermion behaviour of bulk LiV{sub 2}O{sub 4} at low temperatures is well reproduced in thick enough (∼ 7 nm) films on SrTiO{sub 3} substrates. In contrast, an insulating phase was found in strained LiV{sub 2}O{sub 4} thin films on MgO substrates, revealing the key role of the lattice in stabilising the metallic ground state. In this presentation, we discuss the thin film fabrication and the effect of epitaxial strain on heavy fermion behaviour in LiV{sub 2}O{sub 4}.

  18. Examination of the magnetic hyperthermia and other magnetic properties of CoFe2O4@MgFe2O4 nanoparticles using external field Mössbauer spectroscopy

    Science.gov (United States)

    Park, Jeongho; Choi, Hyunkyung; Kim, Sam Jin; Kim, Chul Sung

    2018-05-01

    CoFe2O4@MgFe2O4 core/shell nanoparticles were synthesized by high temperature thermal decomposition with seed-mediated growth. The crystal structure and magnetic properties of the nanoparticles were investigated using X-ray diffractometry (XRD), vibrating sample magnetometry (VSM), and Mössbauer spectrometry. The magnetic hyperthermia properties were investigated using a MagneTherm device. Analysis of the XRD patterns showed that CoFe2O4@MgFe2O4 had a cubic spinel crystal structure with space group Fd-3m and a lattice constant (a0) of 8.3686 Å. The size and morphology of the CoFe2O4@MgFe2O4 nanoparticles were confirmed by HR-TEM. The VSM measurements showed that the saturation magnetization (MS) of CoFe2O4@MgFe2O4 was 77.9 emu/g. The self-heating temperature of CoFe2O4@MgFe2O4 was 37.8 °C at 112 kHz and 250 Oe. The CoFe2O4@MgFe2O4 core/shell nanoparticles showed the largest saturation magnetization value, while their magnetic hyperthermia properties were between those of the CoFe2O4 and MgFe2O4 nanoparticles. In order to investigate the hyperfine interactions of CoFe2O4, MgFe2O4, and CoFe2O4@MgFe2O4, we performed Mössbauer spectrometry at various temperatures. In addition, Mössbauer spectrometry of CoFe2O4@MgFe2O4 was performed at 4.2 K with applied fields of 0-4.5 T, and the results were analyzed with sextets for the tetrahedral A-site and sextets for the octahedral B-site.

  19. Fabrication and spectroscopic properties of Co:MgAl2O4 transparent ceramics by the HIP post-treatment

    Science.gov (United States)

    Luo, Wei; Ma, Peng; Xie, Tengfei; Dai, Jiawei; Pan, Yubai; Kou, Huamin; Li, Jiang

    2017-07-01

    Cobalt-doped magnesium aluminate spinel (Co:MgAl2O4) is one of the most important saturable absorbers for the passive Q-switching of solid-state lasers operating at eye-safe wavelength of 1.5 μm. In this work, highly transparent Co:MgAl2O4 ceramics were fabricated by vacuum sintering combined with hot isostatic pressing (HIP) post-treatment, using the mixture of the commercial spinel and the lab-made Co:MgAl2O4 powder as the raw materials. The densification mechanism of Co:MgAl2O4 transparent ceramics was discussed. The microstructure and optical properties of the samples were investigated. The ground state absorption cross section (σGSA) was calculated from the fitted curve of the absorption coefficient spectrum. The results show that Co:MgAl2O4 ceramics fabricated by vacuum sintering at 1500 °C for 5 h and then HIP post-treatment at 1650 °C for 3 h perform good transparency, whose in-line transmittance exceeds 80% at 2500 nm. Moreover, the ground state absorption cross section of 0.02 at.% Co:MgAl2O4 ceramics is calculated to be 3.35 × 10-19 cm2 at the wavelength of 1540 nm, which is promising for the application to the passive Q-switching of solid-state laser operating in the near infrared region (NIR).

  20. Surface Modification of LiMn2O4 for Lithium Batteries by Nanostructured LiFePO4 Phosphate

    Directory of Open Access Journals (Sweden)

    B. Sadeghi

    2012-01-01

    Full Text Available LiMn2O4 spinel cathode materials have been successfully synthesized by solid-state reaction. Surface of these particles was modified by nanostructured LiFePO4 via sol gel dip coating method. Synthesized products were characterized by thermally analyzed thermogravimetric and differential thermal analysis (TG/DTA, X-ray diffraction (XRD, scanning electron microscopy (SEM, transmission electron microscopy (TEM, and energy dispersive X-ray spectroscopy (EDX. The results of electrochemical tests showed that the charge/discharge capacities improved and charge retention of battery enhanced. This improved electrochemical performance is caused by LiFePO4 phosphate layer on surfaces of LiMn2O4 cathode particles.

  1. Ni doped Fe3O4 magnetic nanoparticles.

    Science.gov (United States)

    Larumbe, S; Gómez-Polo, C; Pérez-Landazábal, J I; García-Prieto, A; Alonso, J; Fdez-Gubieda, M L; Cordero, D; Gómez, J

    2012-03-01

    In this work, the effect of nickel doping on the structural and magnetic properties of Fe3O4 nanoparticles is analysed. Ni(x)Fe(3-x)O4 nanoparticles (x = 0, 0.04, 0.06 and 0.11) were obtained by chemical co-precipitation method, starting from a mixture of FeCl2 x 4H2O and Ni(AcO)2 x 4H2O salts. The analysis of the structure and composition of the synthesized nanoparticles confirms their nanometer size (main sizes around 10 nm) and the inclusion of the Ni atoms in the characteristic spinel structure of the magnetite Fe3O4 phase. In order to characterize in detail the structure of the samples, X-ray absorption (XANES) measurements were performed on the Ni and Fe K-edges. The results indicate the oxidation of the Ni atoms to the 2+ state and the location of the Ni2+ cations in the Fe2+ octahedral sites. With respect to the magnetic properties, the samples display the characteristic superparamagnetic behaviour, with anhysteretic magnetic response at room temperature. The estimated magnetic moment confirms the partial substitution of the Fe2+ cations by Ni2+ atoms in the octahedral sites of the spinel structure.

  2. Structural and magnetic anisotropy in the epitaxial FeV2O4 (110) spinel thin films

    Science.gov (United States)

    Shi, Xiaolan; Wang, Yuhang; Zhao, Kehan; Liu, Na; Sun, Gaofeng; Zhang, Liuwan

    2015-11-01

    The epitaxial 200-nm-thick FeV2O4(110) films on (110)-oriented SrTiO3, LaAlO3 and MgAl2O4 substrates were fabricated for the first time by pulsed laser deposition, and the structural, magnetic, and magnetoresistance anisotropy were investigated systematically. All the films are monoclinic, whereas its bulk is cubic. Compared to FeV2O4 single crystals, films on SrTiO3 and MgAl2O4 are strongly compressively strained in [001] direction, while slightly tensily strained along normal [110] and in-plane [ 1 1 ¯ 0 ] directions. In contrast, films on LaAlO3 are only slightly distorted from cubic. The magnetic hard axis is in direction, while the easier axis is along normal [110] direction for films on SrTiO3 and MgAl2O4, and in-plane [ 1 1 ¯ 0 ] direction for films on LaAlO3. Magnetoresistance anisotropy follows the magnetization. The magnetic anisotropy is dominated by the magnetocrystalline energy, and tuned by the magneto-elastic coupling.

  3. Cation-substituted spinel oxide and oxyfluoride cathodes for lithium ion batteries

    Science.gov (United States)

    Manthiram, Arumugam; Choi, Wonchang

    2010-05-18

    The present invention includes compositions and methods of making cation-substituted and fluorine-substituted spinel cathode compositions by firing a LiMn2-y-zLiyMzO4 oxide with NH4HF2 at low temperatures of between about 300 and 700.degree. C. for 2 to 8 hours and a .eta. of more than 0 and less than about 0.50, mixed two-phase compositions consisting of a spinel cathode and a layered oxide cathode, and coupling them with unmodified or surface modified graphite anodes in lithium ion cells.

  4. Sol-gel route of synthesis of nanoparticles of MgFe2O4 and XRD, FTIR and VSM study

    International Nuclear Information System (INIS)

    Pradeep, A.; Priyadharsini, P.; Chandrasekaran, G.

    2008-01-01

    Nanoparticles of MgFe 2 O 4 are synthesized using sol-gel autocombustion method. Structural studies are carried out using X-ray diffraction (XRD). The XRD pattern of MgFe 2 O 4 provides information about single-phase formation of spinel structure with cubic symmetry. The grain size and lattice constant are obtained using XRD data. The cation distribution is also proposed theoretically. The change in site preference of cations in nano-MgFe 2 O 4 is compared with its bulk counterpart. The structural morphology of the nanoparticles is studied using Scanning Electron Microscopy (SEM). Formation of spinel structure is conformed using Fourier transform infrared spectroscopy (FTIR), which also lends support for the cation distribution proposed using XRD data. The effect of nanoregime on parameters such as bond length, vibration frequency and force constant are discussed with the help of FTIR data. The M-H loop of MgFe 2 O 4 has been traced using the Vibrating Sample Magnetometer (VSM) and magnetic parameters such as saturation magnetization (M S ), coercivity (H C ) and retentivity (M R ) are obtained from VSM data

  5. Synthesis of magnesium aluminate spinel by periclase and alumina chlorination

    International Nuclear Information System (INIS)

    Orosco, Pablo; Barbosa, Lucía; Ruiz, María del Carmen

    2014-01-01

    Highlights: • Use of chlorination for the synthesis of magnesium aluminate spinel. • The reagents used were alumina, periclase and chlorine. • Isothermal and non-isothermal assays were performed in air and Cl 2 –N 2 flows. • The chlorination produced magnesium aluminate spinel at 700 °C. • Selectivity of the chlorination reaction to obtain spinel is very high. - Abstract: A pyrometallurgical route for the synthesis of magnesium aluminate spinel by thermal treatment of a mechanical mixture containing 29 wt% MgO (periclase) and 71 wt% Al 2 O 3 (alumina) in chlorine atmosphere was developed and the results were compared with those obtained by calcining the same mixture of oxides in air atmosphere. Isothermal and non-isothermal assays were performed in an experimental piece of equipment adapted to work in corrosive atmospheres. Both reagents and products were analyzed by differential thermal analysis (DTA), X-ray diffraction (XRD) and X-ray fluorescence (XRF). Thermal treatment in Cl 2 atmosphere of the MgO–Al 2 O 3 mixture produces magnesium aluminate spinel at 700 °C, while in air, magnesium spinel is generated at 930 °C. The synthesis reaction of magnesium aluminate spinel was complete at 800 °C

  6. Synthesis and characterization of multilayered BaTiO3/NiFe2O4 thin films

    Directory of Open Access Journals (Sweden)

    Branimir Bajac

    2013-03-01

    Full Text Available Presented research was focused on the fabrication of multiferroic thin film structures, composed of ferrielectric barium titanate perovskite phase and magnetostrictive nickel ferrite spinel phase. The applicability of different, solution based, deposition techniques (film growth from solution, dip coating and spin coating for thefabrication of multilayered BaTiO3 /NiFe2O4 thin films was investigated. It was shown that only spin coating produces films of desired nanostructure, thickness and smooth and crackfree surfaces.

  7. Microwave-assisted optimization of the manganese redox states for enhanced capacity and capacity retention of LiAl(subx)Mn(sub2-x)O(sub4) (x = 0 and 0.3) spinel materials

    CSIR Research Space (South Africa)

    Nkosi, FP

    2015-03-01

    Full Text Available -assisted optimization of the manganese redox states for enhanced capacity and capacity retention of LiAlxMn2-xO4 (x = 0 and 0.3) spinel materials Funeka P. Nkosi1,2, Charl J. Jafta2, Mesfin Kebede2, Lukas le Roux2, Mkhulu K. Mathe2, and Kenneth I. Ozoemena,1... polypropylene-based membrane separator soaked in non-aqueous electrolyte. A 1 M LiPF6 in EC/DC/DMC in 1:1:1 volume ratio solution was used as the electrolyte. LiPF6 in EC-DMC-DEC has increased ion mobility and high ionic conductivity compared to a commercial...

  8. Comparative studies of the dielectric properties of (1−x)BiFeO{sub 3}-xNi{sub 0.8}Zn{sub 0.2}Fe{sub 2}O{sub 4} (x=0.0, 0.2, 0.5, 0.8, 1.0) multiferroic nanocomposite with their single phase BiFeO{sub 3} and Ni{sub 0.8}Zn{sub 0.2}Fe{sub 2}O{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Mani, Angom Devadatta, E-mail: angomdevadattamani@gmail.com; Soibam, Ibetombi

    2017-02-15

    BiFeO{sub 3} (BFO) and nickel zinc ferrite Ni{sub 0.8}Zn{sub 0.2}Fe{sub 2}O{sub 4} (NZFO) were prepared by sol gel and auto combustion route respectively. Stoichiometric proportions were mixed to obtain the multiferroic nanocomposites having the compositional formula (1−x)BiFeO{sub 3}-x Ni{sub 0.8}Zn{sub 0.2}Fe{sub 2}O{sub 4} (x=0.0, 0.2, 0.5, 0.8, 1.0). The phases were confirmed by XRD analyses. SEM micrographs showed the agglomerated nature of the particles with continuous grain growth in all directions. Elemental compositions were confirmed from EDAX studies. FTIR studies showed the stretching and bending vibrations of the various bonds present in the samples. The dielectric properties such as dielectric constant, ε′ and dielectric loss tangent, tanδ were studied for the spinel, perovskite and nanocomposite ferrites. Experimental result shows an increasing trend in the value of dielectric constant in going from spinel to perovskite phase. The frequency dependence of tanδ showed minimum loss for x=0.5 nanocomposite. Possible mechanisms explaining the above results were being discussed.

  9. Magnetic phase diagram of Co(Cr1-xA lx) 2O4 (x = 0.0-1.0)

    Science.gov (United States)

    Padam, R.; Sarkar, T.; Mathieu, R.; Thota, S.; Pal, D.

    2017-08-01

    We report the role of Al substitution in the magnetic properties of spinel CoCr2O4 by means of temperature dependent dc and ac magnetization and heat capacity measurements. Various compositions (0.0 ≤ x ≤ 1.0) of polycrystalline Co(Cr1-xAlx)2O4 samples have been prepared by sol-gel processing and their crystal structure was investigated by X-ray diffraction which was found to crystallize in the normal cubic spinel structure. For x ≤ 0.1, the system exhibits multiple magnetic orderings (long range ferrimagnetic ordering TC, spin-spiral ordering TS, and lock-in transition TL), similar to that of the parent compound, CoCr2O4. However, all the compositions between x = 0.1 and 0.5 exhibit long range ferrimagnetic ordering below TC and also a short range order at low temperature. Spin-glass like ordering was noticed between x = 0.6 and 0.8 due to the diluted B-site occupancy, whereas the end compound CoAl2O4 (x = 1.0) shows antiferromagnetic behavior. On the basis of these results, we propose a magnetic phase diagram for the Co(Cr1-xAlx)2O4 series as a function of the Al content (x) and measuring temperature (T).

  10. Magnetic behavior of the oxide spinels

    Indian Academy of Sciences (India)

    ... Refresher Courses · Symposia · Live Streaming. Home; Journals; Pramana – Journal of Physics; Volume 58; Issue 5-6. Magnetic behavior of the oxide spinels: Li0.5Fe2.5-2AlCrO4. U N Trivedi K B Modi H H Joshi. Colossal Magnetoresistance & Other Materials Volume 58 Issue 5-6 May-June 2002 pp 1031-1034 ...

  11. Microstructure, crystal structure and electrical properties of Cu0.1Ni0.8Co0.2Mn1.9O4 ceramics obtained at different sintering conditions

    International Nuclear Information System (INIS)

    Bodak, O.; Akselrud, L.; Demchenko, P.; Kotur, B.; Mrooz, O.; Hadzaman, I.; Shpotyuk, O.; Aldinger, F.; Seifert, H.; Volkov, S.; Pekhnyo, V.

    2002-01-01

    Details of the formation of Cu 0.1 Ni 0.8 Co 0.2 Mn 1.9 O 4 ceramics under different sintering conditions have been studied by optical microscopy, scanning electron microscopy (SEM), electron probe and energy dispersive spectroscopy (EDX) microanalyses, X-ray diffraction (XRD) and electrical resistivity measurements. Microstructure studies of samples sintered at 1170 deg. C for 1 h indicated the presence of a secondary phase besides the main spinel phase with modified composition. XRD measurements showed that the spinel phase exhibits a tetragonally distorted spinel structure (space group I4 1 /amd, a=5.9410(5) A, c=8.4196(15) A). The secondary phase (solid solution based on NiO) crystallizes with the NaCl-type structure (space group Fm3-bar m, a=4.1872(3) A). The content of the secondary phase in ceramics is 10.61 mass%. For NiMn 2 O 4 ceramics, prepared under the same sintering conditions, the decomposition with Ni 1-x Mn x O solid solution (NaCl-type structure) and spinel phase formation have been observed. The tetragonal modification of the spinel phase for NiMn 2 O 4 ceramics is more preferable (space group I4 1 /amd, a=5.9764(5) A, c=8.4201(8) A). The distribution of atoms in the structure has been proposed for both ceramics. According to XRD results the Cu 0.1 Ni 0.8 Co 0.2 Mn 1.9 O 4 ceramic samples, sintered at 920 deg. C for 8 h (program 1), at 920 deg. C for 8 h and at 750 deg. C for 24 h (program 2), at 920 deg. C for 8 h, at 1200 deg. C for 1 h and at 920 deg. C for 24 h (program 3) and at 920 deg. C for 8 h, at 1200 deg. C for 1 h, at 920 deg. C for 24 h and at 750 deg. C for 48 h (program 4), contain a single phase with the cubic spinel structure (space group Fd3-bar m). Small residuals of the secondary phase for the ceramics, prepared via programs 3 and 4, have been observed by SEM investigations. The structure transformations of the spinel phase for Cu 0.1 Ni 0.8 Co 0.2 Mn 1.9 O 4 ceramics sintered at 1170 deg. C are attributed to a Jahn

  12. Spin-Coating and Characterization of Multiferroic MFe{sub 2}O{sub 4} (M=Co, Ni) / BaTiO{sub 3} Bilayers

    Energy Technology Data Exchange (ETDEWEB)

    Quandt, Norman [Institute of Chemistry, Martin Luther University Halle-Wittenberg, Kurt-Mothes-Straße 2, 06120 Halle (Germany); Roth, Robert [Institute of Physics, Martin Luther University Halle-Wittenberg, Von-Danckelmann-Platz 3, 06120 Halle (Germany); Syrowatka, Frank [Interdisciplinary Center of Materials Science, Martin Luther University Halle-Wittenberg, Heinrich-Damerow-Straße 4, 06120 Halle (Germany); Steimecke, Matthias [Institute of Chemistry, Martin Luther University Halle-Wittenberg, Von-Danckelmann-Platz 4, 06120 Halle (Germany); Ebbinghaus, Stefan G., E-mail: stefan.ebbinghaus@chemie.uni-halle.de [Institute of Chemistry, Martin Luther University Halle-Wittenberg, Kurt-Mothes-Straße 2, 06120 Halle (Germany)

    2016-01-15

    Bilayer films of MFe{sub 2}O{sub 4} (M=Co, Ni) and BaTiO{sub 3} were prepared by spin coating of N,N-dimethylformamide/acetic acid solutions on platinum coated silicon wafers. Five coating steps were applied to get the desired thickness of 150 nm for both the ferrite and perovskite layer. XRD, IR and Raman spectroscopy revealed the formation of phase-pure ferrite spinels and BaTiO{sub 3}. Smooth surfaces with roughnesses in the order of 3 to 5 nm were found in AFM investigations. Saturation magnetization of 347 emu cm{sup −3} for the CoFe{sub 2}O{sub 4}/BaTiO{sub 3} and 188 emu cm{sup −3} for the NiFe{sub 2}O{sub 4}/BaTiO{sub 3} bilayer, respectively were found. For the CoFe{sub 2}O{sub 4}/BaTiO{sub 3} bilayer a strong magnetic anisotropy was observed with coercivity fields of 5.1 kOe and 3.3 kOe (applied magnetic field perpendicular and parallel to film surface), while for the NiFe{sub 2}O{sub 4}/BaTiO{sub 3} bilayer this effect is less pronounced. Saturated polarization hysteresis loops prove the presence of ferroelectricity in both systems. - Graphical abstract: The SEM image of the CoFe{sub 2}O{sub 4}/BaTiO{sub 3} bilayer on Pt–Si-substrate (left), magnetization as a function of the magnetic field perpendicular and parallel to the film plane (right top) and P–E and I–V hysteresis loops of the bilayer at room temperature. - Highlights: • Ferrite and perovskite oxides grown on platinum using spin coating technique. • Columnar growth of cobalt ferrite particle on the substrate. • Surface investigation showed a homogenous and smooth surface. • Perpendicular and parallel applied magnetic field revealed a magnetic anisotropy. • Switching peaks and saturated P–E hysteresis loops show ferroelectricity.

  13. Growth of InN films on spinel substrates by pulsed laser deposition

    Energy Technology Data Exchange (ETDEWEB)

    Mitamura, K. [Institute of Industrial Science (IIS), The University of Tokyo, 4-6-1 Komaba, Megruro-ku, Tokyo 153-8505 (Japan); Ohta, J.; Fujioka, H. [Institute of Industrial Science (IIS), The University of Tokyo, 4-6-1 Komaba, Megruro-ku, Tokyo 153-8505 (Japan); Kanagawa Academy of Science and Technology (KAST), 3-2-1 Sakado, Takatsu-ku, Kanagawa 213-0012 (Japan); Oshima, M. [Department of Applied Chemistry, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656 (Japan)

    2007-10-15

    We have grown InN films on MgAl{sub 2}O{sub 4}(111) substrates with atomically flat surfaces using pulsed laser deposition (PLD) and compared their structural properties with those grown on (Mn,Zn)Fe{sub 2}O{sub 4}(111) substrates. It has been revealed that InN(0001) films grow on MgAl{sub 2}O{sub 4}(111) with an in-plane epitaxial relationship of InN[1 anti 100]//MgAl{sub 2}O{sub 4}[1 anti 10], achieving a lattice mismatch minimum. The InN films exhibited a clear sixfold rotational symmetry, without 30 rotational domains and with a full width at half maximum value of the InN 0002 rocking curve being 17.5 arcmin. Comparison between InN films grown on MgAl{sub 2}O{sub 4} and those on (Mn,Zn)Fe{sub 2}O{sub 4} led us to conclude that suppression of the interfacial reactions between the InN films and the substrate is inherently important to obtain high quality InN on substrates with a spinel structure. (copyright 2007 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  14. Atomic Structure of a Spinel-like Transition Al2O3 (100) Surface

    DEFF Research Database (Denmark)

    Jensen, Thomas Nørregaard; Meinander, Kristoffer; Helveg, Stig

    2014-01-01

    We study a crystalline epitaxial alumina thin film with the characteristics of a spinel-type transition Al2O3(100) surface by using atom-resolved noncontact atomic force microscopy and density functional theory. It is shown that the films are terminated by an Al-O layer rich in Al vacancies......, exhibiting a strong preference for surface hydroxyl group formation in two configurations. The transition alumina films are crystalline and perfectly stable in ambient atmospheres, a quality which is expected to open the door to new fundamental studies of the surfaces of transition aluminas....

  15. Synthesis and photocatalytic activity of CuY{sub y}Fe{sub 2-y}O{sub 4}-CuCo{sub 2}O{sub 4} nanocomposites for H{sub 2} evolution under visible light irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Yan, Jianhui; Yang, Haihua; Yao, Maohai; Han, Yong [Department of Chemistry and Chemical Engineering, Hunan Institute of Science and Technology, Shuyuan Load, Yueyang, Hunan 414000 (China); College of Chemistry and Chemical Engineering, Central South University, Changsha, Hunan 410083 (China); Tang, Yougen; Lu, Zhouguang [College of Chemistry and Chemical Engineering, Central South University, Changsha, Hunan 410083 (China); Zheng, Shuqin [Department of Chemistry and Chemical Engineering, Hunan Institute of Science and Technology, Shuyuan Load, Yueyang, Hunan 414000 (China)

    2009-11-15

    Spinel-type CuY{sub y}Fe{sub 2-y}O{sub 4}-CuCo{sub 2}O{sub 4} nanocomposites have been successfully synthesized via a facile citric acid (CA)-assisted sol-gel method. And the as-synthesized nanocomposites have been characterized by techniques of X-ray diffraction (XRD), nitrogen adsorption BET method, and transmission electron microscopy (TEM). The samples are composed of primary ultrafine nanoparticles with nearly spherical morphology and mean particle size of about 80 nm. Moreover, the photocatalytic H{sub 2} evolution activity of the as-obtained samples has been evaluated from aqueous oxalic acid solution under visible light irradiation. The influence of photocatalyst type, calcination temperature, Y{sup 3+} doping content, and the durability of the as-obtained photocatalyst have been investigated in detail. The best photocatalytic H{sub 2} evolution activity was obtained over the as-synthesized CuY{sub 0.08}Fe{sub 1.92}O{sub 4}-CuCo{sub 2}O{sub 4} nanocomposite. (author)

  16. Structural, magnetic, and dielectric properties of multiferroic Co{sub 1−x}Mg{sub x}Cr{sub 2}O{sub 4} nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Kamran, M.; Ullah, A. [Nanomagnetism and Nanotechnology Laboratory, International Islamic University, Islamabad 44000 (Pakistan); Rahman, S. [Department of Material Science and Engineering, University of Science and Technology of China Hefei, Anhui 230026 (China); Tahir, A. [Department of Physics, Quaid-e-Azam University, Islamabad 44000 (Pakistan); Nadeem, K., E-mail: kashif.nadeem@iiu.edu.pk [Nanomagnetism and Nanotechnology Laboratory, International Islamic University, Islamabad 44000 (Pakistan); Beijing National Laboratory for Condensed Matter Physics, National Laboratory for Superconductivity, Institute of Physics, Chinese Academy of Sciences, P.O. Box 603, Beijing 100190 (China); Anis ur Rehman, M. [Applied Thermal Physics Laboratory, Department of Physics, COMSATS Institute of Information Technology, Islamabad 44000 (Pakistan); Hussain, S. [Magnetism Laboratory, Department of Physics, COMSATS Institute of Information Technology, Islamabad 44000 (Pakistan)

    2017-07-01

    Highlights: • Properties of multiferroic Co{sub 1−x}Mg{sub x}Cr{sub 2}O{sub 4} nanoparticles have been studied. • XRD showed that CoCr{sub 2}O{sub 4} and MgCr{sub 2}O{sub 4} are cubic normal spinel structure. • Rietveld refinement of XRD showed no impurity phases. • T{sub c} and T{sub s} showed decreasing trend with increasing Mg concentration. • Dielectric properties were improved for x = 0.6 Mg concentration. - Abstract: We examined the structural, magnetic, and dielectric properties of Co{sub 1−x}Mg{sub x}Cr{sub 2}O{sub 4} nanoparticles with composition x = 0, 0.2, 0.4, 0.5, 0.6, 0.8 and 1 in detail. X-ray diffraction (XRD) revealed normal spinel structure for all the samples. Rietveld refinement fitting results of the XRD showed no impurity phases which signifies the formation of single phase Co{sub 1−x}Mg{sub x}Cr{sub 2}O{sub 4} nanoparticles. The average crystallite size showed a peak behaviour with maxima at x = 0.6. Raman and Fourier transform infrared (FTIR) spectroscopy also confirmed the formation of single phase normal spinel for all the samples and exhibited dominant vibrational changes for x ≥ 0.6. For x = 0 (CoCr{sub 2}O{sub 4}), zero field cooled/field cooled (ZFC/FC) magnetization curves showed paramagnetic (PM) to ferrimagnetic (FiM) transition at T{sub c} = 97 K and a conical spiral magnetic order at T{sub s} = 30 K. The end members CoCr{sub 2}O{sub 4} (x = 0) and MgCr{sub 2}O{sub 4} (x = 1) are FiM and antiferromagnetic (AFM), respectively. T{sub c} and T{sub s} showed decreasing trend with increasing x, followed by an additional AFM transition at T{sub N} = 15 K for x = 0.6. The system finally stabilized and changed to highly frustrated AFM structure at x = 1 due to formation of pure MgCr{sub 2}O{sub 4}. High field FC curves (5T) depicted nearly no effect on spiral magnetic state, which is attributed to strong exchange B-B magnetic interactions at low temperatures. Dielectric parameters showed a non-monotonous behaviour with

  17. Simple synthetic route to manganese-containing nanowires with the spinel crystal structure

    Energy Technology Data Exchange (ETDEWEB)

    Yu, Lei; Zhang, Yan; Hudak, Bethany M.; Wallace, Damon K.; Kim, Doo Young; Guiton, Beth S.

    2016-08-15

    This report describes a new route to synthesize single-crystalline manganese-containing spinel nanowires (NWs) by a two-step hydrothermal and solid-state synthesis. Interestingly, a nanowire or nanorod morphology is maintained during conversion from MnO{sub 2}/MnOOH to CuMn{sub 2}O{sub 4}/Mg{sub 2}MnO{sub 4}, despite the massive structural rearrangement this must involve. Linear sweep voltammetry (LSV) curves of the products give preliminary demonstration that CuMn{sub 2}O{sub 4} NWs are catalytically active towards the oxygen evolution reaction (OER) in alkaline solution, exhibiting five times the magnitude of current density found with pure carbon black. - Highlights: • Synthesis of single-crystalline manganese-containing spinel nanowires. • Binary oxide nanowire converted to ternary oxide wire through solid state reaction. • Approach to structure conversion with shape retention could be generally applicable. • Copper and Manganese display multiple oxidation states with potential for catalysis. • CuMn{sub 2}O{sub 4} nanowires show promise as catalysts for the oxygen evolution reaction.

  18. Synthesis and optical property of zinc aluminate spinel cryogels

    Directory of Open Access Journals (Sweden)

    Lifen Su

    2016-06-01

    Full Text Available Zinc aluminate spinel cryogels with various molar ratio of Al/Zn are synthesized by sol–gel technology followed by vacuum freeze drying. The structures and optical properties are both found to be affected by the molar ratios of Al/Zn and annealed temperatures. The peaks of zinc oxide (ZnO and zinc dialuminum oxide (ZnAl2O4 are both obtained for the samples with more Zn content annealed at 750 °C or upward. The composites have a large surface area (137 m2/g with mesoporous structure after annealing at 750 °C. The SEM images reveal that the ZnAl2O4 crystals formed a multilayer structure with redundant ZnO particles which deposited on it. Furthermore, the maximum infrared reflectance is about 80% with an improvement of 35% in the infrared region after annealing at 950 °C compared with that of 450 °C, which indicates that these porous cryogels have a potential application as thermal insulating materials at a high temperature.

  19. Flotation Behaviors of Perovskite, Titanaugite, and Magnesium Aluminate Spinel Using Octyl Hydroxamic Acid as the Collector

    Directory of Open Access Journals (Sweden)

    Weiqing Wang

    2017-08-01

    Full Text Available The flotation behaviors of perovskite, titanaugite, and magnesium aluminate spinel (MA-spinel, using octyl hydroxamic acid (OHA as the collector, were investigated using microflotation experiments, zeta-potential measurements, Fourier transform infrared (FT-IR analyses, X-ray photoelectron spectroscopy (XPS analyses, and flotation experiments on artificially mixed minerals. The microflotation experiments show that the floatability of perovskite is clearly better than titanaugite and MA-spinel at around pH 5.5, while titanaugite possesses certain floatability at pH 6.0–6.5, and MA-spinel displays good floatability at pH > 8.0. The results of the FT-IR and XPS analyses show that OHA mainly interacts with Ti, resulting in perovskite flotation, and that the Al on titanaugite, as well as the Mg and Al on the MA-spinel surface, chemically react with OHA under acidic conditions. However, OHA mainly reacts with the Ti and Ca on the perovskite surface, Ca and Mg on the titanaugite surface, and Mg and Al on the MA-spinel surface under alkaline conditions. The results of the artificially mixed mineral flotation experiment show that the concentrate of TiO2 grade increased from 19.73% to 30.18% at pH 5.4, which indicates that a weakly acidic solution is the appropriate condition for the flotation separation of perovskite from titanaugite and MA-spinel. The results of the modified slag flotation experiments show that the TiO2 grade of concentrate increased from 18.13% to 23.88% at pH 5.4, through the open circuit test of “one roughing and one cleaning”. OHA displays selectivity toward perovskite in the modified slag flotation, but the consumption of H2SO4 is very high. The CaSO4 precipitate covered on the mineral surfaces results in poor TiO2 grade and recovery.

  20. Synthesis, structure and magnetic properties of CoFe_2O_4 nanomaterial by coprecipitation method

    International Nuclear Information System (INIS)

    Nguyen Anh Tien; Hoang Thi Tuyet

    2015-01-01

    CoFe_2O_4 spinel nanomaterial has been synthesized by coprecipitation method through the hydrolysis of Co(II) and Fe(III) cations in boiling water. The results of DTA/TGA/DrTGA, XRD, TEM methods showed that CoFe_2O_4 crystals formed after a calcination at 700 °C exhibited structure of cubic with the particles size of 30-50 nm, H_c = 1526.89 Oe, M_s = 41.703 emu/g, M_r = 19.545 emu/g. (author)

  1. Versatile electronic behavior of the Li{sub x}Mn{sub 3−x−y}Fe{sub y}O{sub 4} spinels

    Energy Technology Data Exchange (ETDEWEB)

    Alonso-Domínguez, D. [Departamento de Química Inorgánica, Facultad de Ciencias Químicas, Universidad Complutense de Madrid, Avda. Complutense s/n, 28040 Madrid (Spain); CEI Moncloa, UCM-UPM, Madrid (Spain); Álvarez-Serrano, I., E-mail: ias@quim.ucm.es [Departamento de Química Inorgánica, Facultad de Ciencias Químicas, Universidad Complutense de Madrid, Avda. Complutense s/n, 28040 Madrid (Spain); López, M.L.; Veiga, M.L.; Pico, C. [Departamento de Química Inorgánica, Facultad de Ciencias Químicas, Universidad Complutense de Madrid, Avda. Complutense s/n, 28040 Madrid (Spain); Mompeán, F.; García-Hernández, M. [Instituto de Ciencia de Materiales, CSIC, Cantoblanco, 28049 Madrid (Spain); Cuello, G.J. [Institut Laue-Langevin, 6 rue Jules Horowitz, F-38042 Grenoble (France)

    2013-11-15

    Highlights: •The Li{sub x}Mn{sub 3−x−y}Fe{sub y}O{sub 4} spinels show a versatile electronic behavior. •Optimal compositional ranges for different application fields are proposed. •Frustrated ferromagnetic response is compositionally driven. •High ε′ values are obtained when B sites are occupied by both Mn and Fe cations. •High lithium contents are linked to the electrochemical behavior. -- Abstract: The detailed structural and electronic characterization of microcrystalline powders of new spinels Li{sub x}Mn{sub 3−x−y}Fe{sub y}O{sub 4} (0.4 ⩽ x ⩽ 1.33; 0 ⩽ y ⩽ 1.30), obtained by the “liquid mix” method, is reported. Compositional characterization was carried out by means of thermogravimetric analysis, energy-dispersive X-ray spectroscopy and electron energy loss spectroscopy, and their structure was refined from neutron and X-ray diffraction showing a cubic symmetry between 5 and 550 K, Space Group Fd3{sup ¯}m. However, at temperatures above ca. 950 K, a reversible transformation, probably implying the formation of an ordered vacant phase, has been detected. The magnetic behavior, analyzed from neutron diffraction data and magnetization measurements, is interpreted considering an “incomplete” ferrimagnetic response, due to magnetic frustration in the B sites. Potential applications have been evaluated from the magnetocaloric, electrochemical and dielectric behavior in selected compositional ranges.

  2. Structural and transport properties of nanocrystalline MnFe/sub 2/O/sub 4/ synthesized by co-precipitation method

    International Nuclear Information System (INIS)

    Akhtar, M.J.; Younas, M.

    2012-01-01

    The nanocrystalline ferrites with spinel structures have been the focus of scientific investigation and received continuous interest in recent decades. The structural and electrical properties of these materials have become an important area of research and are attracting considerable interest due to broad range of applications. Spinel ferrites have been shown to exhibit interesting dielectric properties in the nanocrystalline form in comparison to the corresponding bulk materials. Structural and electrical properties of nanocrystalline MnFe/sub 2/O/sub 4/ were investigated. X-ray diffraction and X-ray absorption fine structure spectroscopy results showed that nanocrystalline MnFe/sub 2/O/sub 4/ had cubic symmetry with 80% inversion. shows the X-ray absorption near edge structure (XANES) spectra of MnFe/sub 2/O/sub 4/ and Zn/sub 1-x/Ni/sub x/Fe/sub 2/O/sub 4/, used as model compounds. The electrical transport properties were investigated by employing impedance spectroscopy. It was observed that the dielectric constant decreased with the increase in frequency. The effects of frequency on dielectric properties were more prominent in the low frequency region, where dielectric constant increased as temperature was increased. (Orig./A.B.)

  3. Spinel–rock salt transformation in LiCoMnO4−δ

    Science.gov (United States)

    Reeves-McLaren, Nik; Sharp, Joanne; Beltrán-Mir, Héctor; Rainforth, W. Mark; West, Anthony R.

    2016-01-01

    The transformation on heating LiCoMnO4, with a spinel structure, to LiCoMnO3, with a cation-disordered rock salt structure, accompanied by loss of 25% of the oxygen, has been followed using a combination of diffraction, microscopy and spectroscopy techniques. The transformation does not proceed by a topotactic mechanism, even though the spinel and rock salt phases have a similar, cubic close-packed oxygen sublattice. Instead, the transformation passes through two stages involving, first, precipitation of Li2MnO3, leaving behind a Li-deficient, Co-rich non-stoichiometric spinel and, second, rehomogenization of the two-phase assemblage, accompanied by additional oxygen loss, to give the homogeneous rock salt final product; a combination of electron energy loss spectroscopy and X-ray absorption near edge structure analyses showed oxidation states of Co2+ and Mn3+ in LiCoMnO3. Subsolidus phase diagram determination of the Li2O-CoOx-MnOy system has established the compositional extent of spinel solid solutions at approximately 500°C. PMID:26997883

  4. CO 2-rich komatiitic melt inclusions in Cr-spinels within beach sand from Gorgona Island, Colombia

    Science.gov (United States)

    Shimizu, Kenji; Shimizu, Nobumichi; Komiya, Tsuyoshi; Suzuki, Katsuhiko; Maruyama, Shigenori; Tatsumi, Yoshiyuki

    2009-10-01

    The volatile content of komatiite is a key to constrain the thermal and chemical evolution of the deep Earth. We report the volatile contents with major and trace element compositions of ~ 80 melt inclusions in chromian spinels (Cr-spinels) from beach sands on Gorgona Island, Colombia. Gorgona Island is a ~ 90 Ma volcanic island, where picrites and the youngest komatiites known on the Earth are present. Melt inclusions are classified into three types on the basis of their host Cr-spinel compositions: low Ti (P type), high Ti with high Cr # (K1 type) and high Ti with low Cr # (K2 type). Chemical variations of melt inclusions in the Cr-spinels cover all of the island's lava types. P-type inclusions mainly occur in the picrites, K1-type in high-TiO 2 komatiites (some enriched basalts: E-basalts) and K2-type in low-TiO 2 komatiites. The H 2O and CO 2 contents of melt inclusions within Cr-spinels from the beach sand are highly variable (H 2O: 0.03-0.9 wt.%; CO 2: 40-4000 ppm). Evaluation of volatile content is not entirely successful because of compositional alterations of the original melt by degassing, seawater/brine assimilation and post-entrapment modification of certain elements and volatiles. However, the occurrence of many melt inclusions with low H 2O/K 2O ratios indicates that H 2O/K 2O of Gorgona komatiite is not much different from that of modern mid-oceanic ridge basalt (MORB) or oceanic island basalt. Trend of CO 2/Nb and Zr/Y ratios, accounted for by two-component mixing between the least degassed primary komatiite and low-CO 2/Nb evolved basalt, allow us to estimate a primary CO 2/Nb ratio of 4000 ± 2200 or a CO 2 content of 0.16 ± 0.09 wt.%. The determined CO 2/Nb ratio is unusually high, compared to that of MORB (530). Although the presence of CO 2 in the Gorgona komatiite does not affect the magma generation temperature, CO 2 degassing may have contributed to the eruption of high-density magmas. High CO 2/Nb and the relatively anhydrous nature of

  5. Phase evaluation of Li{sup +} substituted CoFe{sub 2}O{sub 4} nanoparticles, their characterizations and magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Kadam, R.H. [Materials Science Research Lab, Shrikrishna Mahavidyalaya Gunjoti, Osmanabad, Maharashtra (India); Alone, Suresh T. [Department of Physics, RS Art' s, Science and Commerce College, Pathri, Aurangabad, Maharashtra (India); Mane, Maheshkumar L. [Department of Physics, Rajarshi Shahu Mahavidyalaya, Latur, Maharashtra (India); Biradar, A.R. [Materials Science Research Lab, Shrikrishna Mahavidyalaya Gunjoti, Osmanabad, Maharashtra (India); Shirsath, Sagar E., E-mail: shirsathsagar@hotmail.com [Spin Device Technology Center, Department of Information Engineering, Shinshu University, Nagano 380-8553 (Japan)

    2014-04-15

    Li{sup +} substituted CoFe{sub 2}O{sub 4} with the chemical formula Li{sub 3x}CoFe{sub 2−x}O{sub 4} were synthesized by sol–gel auto combustion method. The synthesized samples were annealed at 600 °C for 4 h. X-ray diffraction data were used to evaluate the structure of the prepared samples. Spinel ferrite phase of CoFe{sub 2}O{sub 4} changes to ordered like lithium ferrite phase with increase in L{sup i+} substitution. Lattice constant increases whereas particle size found to decrease with Li{sup +} substitution. Infrared spectroscopy also confirmed the phase transition of CoFe{sub 2}O{sub 4} after the incorporation of lithium ions. Substitution of Li{sup +} ions for Fe{sup 3+} caused a decrease in the saturation magnetization from 69.59 emu/g to 47.71 emu/g and the coercivity increased from 647 Oe to 802 Oe. Resistivity and dielectric properties shows inverse relation to each other. - Highlights: • Li{sup +} ion substituted CoFe{sub 2}O{sub 4}. • Single phase cubic spinel structure changes with Li{sup +} substitution. • Magnetization decreases whereas coercivity increases with increasing Li{sup +}. • Resistivity decreases with Li{sup +} substitution.

  6. Effect of Gd{sup 3+} substitution on structural, magnetic, dielectric and optical properties of nanocrystalline CoFe{sub 2}O{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Joshi, Seema [Department of Physics and Materials Science and Engineering, Jaypee Institute of Information Technology, Noida 201307 (India); Kumar, Manoj, E-mail: mkumar.phy@gmail.com [Department of Physics and Materials Science and Engineering, Jaypee Institute of Information Technology, Noida 201307 (India); Chhoker, Sandeep [Department of Physics and Materials Science and Engineering, Jaypee Institute of Information Technology, Noida 201307 (India); Kumar, Arun; Singh, Mahavir [Department of Physics, Himachal Pradesh University, Shimla 5 (India)

    2017-03-15

    Nanoparticles of CoGd{sub x}Fe{sub 2−x}O{sub 4} with x=0.0, 0.03, 0.05, 0.07, 0.10 and 0.15 were synthesized by co-precipitation method. Gd{sup 3+} substitution effect on different properties of nanocrystalline CoFe{sub 2}O{sub 4} has been studied. X-ray diffraction and Raman spectroscopy confirmed the formation of single phase cubic mixed spinel structure. Cation distribution has been proposed from Rietveld refined data. Mössbauer spectra at room temperature showed two ferrimagnetic Zeeman sextets with one superparamagnetic doublet. Mössbauer parameters suggested that Gd{sup 3+} ions occupy the octahedral site in CoFe{sub 2}O{sub 4}. Room temperature magnetic measurements exhibited that the saturation magnetization decreased from 91 emu/gm to 54 emu/gm for x=0.0 to 0.15 samples. The coercivity decreased from 1120 Oe to 340 Oe for x=0.0 to 0.07 samples and increased from 400 Oe to 590 Oe for x=0.10 and 0.15 samples, respectively. Raman analysis showed that the degree of inversion with Gd{sup 3+} substitution supporting the variation of coercivity. Electron spin resonance spectra revealed the dominancy of superexchange interactions in these samples. Optical band gap measurement suggested that all samples are indirect band gap materials and band gap has been decreased with Gd{sup 3+} substitution. Both dielectric constant and dielectric loss is found to decrease because of the decrease in hopping rate with the Gd{sup 3+} substitution for Fe{sup 3+} at the octahedral sites. Low dielectric loss suggested the applicability of Gd{sup 3+} doped CoFe{sub 2}O{sub 4} nanoparticles for high frequency microwave device applications. - Highlights: • Gd{sup 3+} ions were successfully added in to the spinel lattice of CoFe{sub 2}O{sub 4}. • Magnetic hysteresis loss is influenced by Gd{sup 3+} doping. • All doped samples exhibit normal dielectric dispersion behaviour of spinel ferrites. • UV–vis diffuse spectroscopy concludes band gap is reduced by Gd{sup 3+} doping.

  7. Near white light emitting ZnAl2O4:Dy3+ nanocrystals: Sol–gel synthesis and luminescence studies

    International Nuclear Information System (INIS)

    Kumar, Mithlesh; Gupta, Santosh K.; Kadam, R.M.

    2016-01-01

    Highlights: • ZnAl 2 O 4 :Dy 3+ spinel synthesized using sol–gel method. • Characterized by XRD, SEM and PL spectroscopy. • Investigations of emission, excitation and lifetime properties. • Evaluation of defect centers and trap parameters of the system. • Evaluation of CIE indices of near white light emitting phosphor. - Abstract: ZnAl 2 O 4 :Dy 3+ nanoparticles were synthesized using citrate sol–gel method and characterized systematically using X-ray diffraction, scanning electron microscopy and photoluminescence spectroscopy. Emission spectrum of pure ZnAl 2 O 4 shows intense violet blue emission under ultra violet irradiation. Based on electron paramagnetic resonance (EPR) results; it was attributed to presence of singly ionized oxygen vacancy centres in ZnAl 2 O 4 . On doping Dy 3+ in ZnAl 2 O 4 , complete host–dopant energy transfer does not take place. Local structural investigation and lifetime measurements reveal that dysprosium ion is distributed between both Zn 2+ and Al 3+ sites. Near white light from ZnAl 2 O 4 :Dy 3+ is attributed to combined host and dopant luminescence. The trap parameters such as activation energy (E) and frequency factor (s) for TSL glow peak 165 °C were determined using different heating rate method. Thermally stimulated emission showed the presence of oxygen related defect centre.

  8. Microstructural and optical properties of spinel oxide M{sub x}Co{sub 2−x}MnO{sub 4} (M = Ni, Zn or Cu; 0 < x < 1) thin films prepared by inorganic polycondensation and dip-coating methods

    Energy Technology Data Exchange (ETDEWEB)

    Le, Thi Ly; Guillemet-Fritsch, Sophie; Dufour, Pascal; Tenailleau, Christophe, E-mail: tenailleau@chimie.ups-tlse.fr

    2016-08-01

    Spinel oxide nanoparticles of M{sub x}Co{sub 2−x}MnO{sub 4} (M = Ni, Zn, Cu; 0 < x < 1) were prepared at 120 °C by the inorganic polycondensation method. Phase composition and microstructure of each sample powder thus obtained were characterized by X-ray diffraction, X-ray fluorescence and scanning electron microscopy. Nanoparticles are well crystallized and uniformly distributed in both shape and size. Colloidal dispersions were stabilized in a low cost and environmentally friendly solvent solution. Spinel oxide thin films were then deposited on glass substrates by using the dip-coating technique. Their optical properties were measured in the 300–1100 nm wavelength range. Thin films show extremely good absorbance in the ultra-violet and blue regions. The highest absorbance observed in the red region was for x = 0.15 in zinc. A smaller direct band gap was determined when a low amount of doping M element was introduced in the cobalt and manganese spinel oxide material. - Highlights: • Pure complex spinel oxide nanoparticles synthesis at low T • Low cost method used to stabilize colloidal dispersions • Preparation of homogenous light absorber thin films by dip-coating • Adjustable optical properties and band gaps with the dopants.

  9. Thermal decomposition study of Mn doped Fe3O4 nanoparticles

    Science.gov (United States)

    Malek, Tasmira J.; Chaki, S. H.; Tailor, J. P.; Deshpande, M. P.

    2016-05-01

    Fe3O4 is an excellent magnetic material among iron oxides. It has a cubic inverse spinel structure exhibiting distinguished electric and magnetic properties. In this paper the authors report the synthesis of Mn doped Fe3O4 nanoparticles by wet chemical reduction technique at ambient temperature and its thermal characterization. Ferric chloride hexa-hydrate (FeCl3•6H2O), manganese chloride tetra-hydrate (MnCl24H2O) and sodium boro-hydrate (NaBH4) were used for synthesis of Fe3O4 nanoparticles at ambient temperature. The elemental composition of the as-synthesized Mn doped Fe3O4 nanoparticles were determined by energy dispersive analysis of X-rays (EDAX) technique. Thermogravimetric (TG) and differential thermal analysis (DTA) were carried out on the Mn doped Fe3O4 nanoparticles in the temperature range of ambient to 1124 K. The thermo-curves revealed that the particles decompose by four steps. The kinetic parameters were evaluated using non-mechanistic equations for the thermal decomposition.

  10. Crystallographic and magnetic properties of the spinel-type ferrites ZnxCo1-xFe2O4 (0.0 ≤ x ≤ 0.75)

    Science.gov (United States)

    Azad, A. K.; Zakaria, A. K. M.; Jewel, Md. Yusuf; Khan, Abu Saeed; Yunus, S. M.; Kamal, I.; Datta, T. K.; Eriksson, S.-G.

    2015-05-01

    Ultrahigh frequencies (UHF) have applications in signal and power electronics to minimize product sizes, increase production quantity and lower manufacturing cost. In the UHF range of 300 MHz to 3 GHz, ferrimagnetic iron oxides (ferrites) are especially useful because they combine the properties of a magnetic material with that of an electrical insulator. Ferrites have much higher electrical resistivity than metallic ferromagnetic materials, resulting in minimization of the eddy current losses, and total penetration of the electromagnetic (EM) field. Hence ferrites are frequently applied as circuit elements, magnetic storage media like read/write heads, phase shifters and Faraday rotators. The electromagnetic properties of ferrites are affected by operating conditions such as field strength, temperature and frequency. The spinel system ZnxCo1-xFe2O4 (x=0.0, 0.25, 0.50 and 0.75) has been prepared by the standard solid state sintering method. X-ray and neutron powder diffraction measurements were performed at room temperature. Neutron diffraction data analysis confirms the cubic symmetry corresponding to the space group Fd3m. The distribution of three cations Zn2+, Co2+ and Fe3+ over the spinel lattice and other crystallographic parameters like lattice constant, oxygen position parameter, overall temperature factor and occupancies of different ions in different lattice sites for the samples have been determined from the analysis of neutron diffraction data. The lattice constant increases with increasing Zn content in the system. The magnetic structure was found to be ferrimagnetic for the samples with x≤0.50. Magnetization measurements show that with the increase of Zn content in the system the value of saturation magnetization first increases and then decreases. The variation of the magnetic moment with Zn substitution has been discussed in terms of the distribution of magnetic and non-magnetic ions over the A and B sub-lattices and their exchange coupling.

  11. Role of 3d-ions for radiation defect production in MgO and MgAl2O4

    International Nuclear Information System (INIS)

    Mironova, N.A.; Grinvald, G.A.; Skvortsova, V.N.

    1985-01-01

    Optical properties of MgO and MgAl 2 O 4 crystals containing chromium and manganese impurity ions were studied by exposure to but all types of radiation. Complicated defects of the ''impurity-intrinsic matrix defect'' type were preferably considered. It has been shown that different symmetry center forming chromium ions in MgO:Crsup(3+) change their valency with various efficiency being exposed to external action. Besides, the compensating vacancy does not participate in the hole center formation. For MgOxAl 2 O 3 single crystals the presence of octahedrally coordinated manganese ions suppresses the hole center creation by gamma-irradiation. Studying luminescence spectra of Crsup(3+) ions in MgAl 2 O 4 it has been states that neutron irradiation increases the degree of inversion for the magnesium-aluminium spinel

  12. Cu4Pr6(MoO4)11-Pr2(MoO4)3 system

    International Nuclear Information System (INIS)

    Arzumanyan, G.A.

    1982-01-01

    Existence boundaries and Dalton compositions (CuPr(MoO 4 ) 2 , CuPr 3 (MoO 4 ) 5 ) of solid solutions that in the mojority are of shcheelite dsitored structure have been determined in the Cu 4 Pr 6 (MoO 4 ) 11 -Pr 2 (MoO 4 ) 3 system. It has been revealed that regions of homogeneity near the CuPr(MoO 4 ) 2 composition have a horseshoeshaped profile

  13. A facile route to synthesize multiporous MnCo2O4 and CoMn2O4 spinel quasi-hollow spheres with improved lithium storage properties

    Science.gov (United States)

    Li, Jingfa; Xiong, Shenglin; Li, Xiaowei; Qian, Yitai

    2013-02-01

    A facile and general way for the synthesis of porous and hollow complex oxides is highly desirable owing to their significant applications for energy storage and other fields. In this contribution, uniform Mn0.33Co0.67CO3 and Co0.33Mn0.67CO3 microspheres are firstly fabricated solvothermally just by tuning the molar ratio of Mn and Co. Subsequently, the growth of multiporous MnCo2O4 and CoMn2O4 quasi-hollow microspheres by topotactic chemical transformation from the corresponding precursors are realized through a non-equilibrium heat treatment process. Topotactic conversion further demonstrated that the much larger CoMn2O4 pores than those of MnCo2O4 are possibly due to the longer transfer distance of ions. When evaluated as anode materials for LIBs (lithium ion batteries), after 25 cycles at a current density of 200 mA g-1, the resultant MnCo2O4 and CoMn2O4 quasi-hollow microspheres possessed reversible capacities of 755 and 706 mA h g-1, respectively. In particular, the MnCo2O4 samples could deliver a reversible capacity as high as 610 mA h g-1 even at a higher current density of 400 mA g-1 with excellent electrochemical stability after 100 cycles of testing, indicating its potential application in LIBs. We believe that such good performance results from the appropriate pore size and quasi-hollow nature of MnCo2O4 microspheres, which can effectively buffer the large volume variation of anodes based on the conversion reaction during Li+ insertion/extraction. The present strategy is simple but very effective, and due to its versatility, it can be extended to other binary, even ternary complex metal oxides with high-performance in LIBs.A facile and general way for the synthesis of porous and hollow complex oxides is highly desirable owing to their significant applications for energy storage and other fields. In this contribution, uniform Mn0.33Co0.67CO3 and Co0.33Mn0.67CO3 microspheres are firstly fabricated solvothermally just by tuning the molar ratio of Mn and Co

  14. Structural and magnetic properties of Co substituted Li{sub 0.5}Fe{sub 2.5}O{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Patil, R.P., E-mail: raj_rbm_raj@yahoo.co.in [Department of Chemistry, M.H. Shinde Mahavidyalaya, Tisangi 416206, MH (India); Patil, S.B. [Department of Physics, Krantisinh Nana Patil College Walwa, Sangli 416313, MH (India); Jadhav, B.V. [Department of Chemistry, Changu Kana Thakur Arts, Commerce and Science College, New Panvel 400035, MH (India); Delekar, S.D.; Hankare, P.P. [Department of Chemistry, Shivaji University, Kolhapur 416004, MH (India)

    2016-03-01

    Nanocrystalline Li{sub 0.5}Fe{sub 2.5−x}Co{sub x}O{sub 4} (2.5≥x≥0) system was prepared by sol–gel route. Formation of single phase cubic spinel structure for all the compositions was confirmed from their X-ray diffraction studies. These ferrite samples existed as homogenous and uniform grains as observed from Scanning Electron Microscopy technique. The magnetic studies indicated that, the ferrimagnetic behavior decreases with Cobalt substitution. In general, the substitution of cobalt plays an important role in changing the structural and magnetic properties of these ferrites. - Highlights: • Novel Co doped Li{sub 0.5}Fe{sub 2.5}O{sub 4} system. • Sol–gel method synthesized Co–Lithium ferrites. • Single Phase Cubic spinel structure. • Homogenous and uniform grain size of samples. • Ferrimagnetic behavior for all the samples.

  15. Transverse acoustic phonon anomalies at intermediate wave vectors in MgV2O4

    Science.gov (United States)

    Weber, T.; Roessli, B.; Stock, C.; Keller, T.; Schmalzl, K.; Bourdarot, F.; Georgii, R.; Ewings, R. A.; Perry, R. S.; Böni, P.

    2017-11-01

    Magnetic spinels (with chemical formula A X2O4 , with X a 3 d transition metal ion) that also have an orbital degeneracy are Jahn-Teller active and hence possess a coupling between spin and lattice degrees of freedom. At high temperatures, MgV2O4 is a cubic spinel based on V3 + ions with a spin S =1 and a triply degenerate orbital ground state. A structural transition occurs at TOO=63 K to an orbitally ordered phase with a tetragonal unit cell followed by an antiferromagnetic transition of TN=42 K on cooling. We apply neutron spectroscopy in single crystals of MgV2O4 to show an anomaly for intermediate wave vectors at TOO associated with the acoustic phonon sensitive to the shear elastic modulus (C11-C12)/2 . On warming, the shear mode softens for momentum transfers near close to half the Brillouin zone boundary, but recovers near the zone center. High resolution spin-echo measurements further illustrate a temporal broadening with increased temperature over this intermediate range of wave vectors, indicative of a reduction in phonon lifetime. A subtle shift in phonon frequencies over the same range of momentum transfers is observed with magnetic fields. We discuss this acoustic anomaly in context of coupling to orbital and charge fluctuations.

  16. Spinel and orthopyroxene exsolved from clinopyroxene in the Haladala pluton in the middle Tianshan (Xinjiang, China)

    Science.gov (United States)

    Zhu, Yongfeng; Chen, Jing; Xue, Yunxin; Feng, Wanyi; Jiang, Jiuyang

    2017-12-01

    The Haladala pluton, consisting of troctolite, olivine gabbro and gabbro with zircon SHRIMP U-Pb age of 309 ± 2 Ma (MSWD = 0.72), intruded the Devonian-Carboniferous arc segments in the middle Tianshan. Amphibole, coexisting with magnetite, amphibole, and phlogopite, crystallized in a magma chamber at depth of 20 km (6.9-7.4 kbar, 934-943 °C) based on various thermobaramoters. Two kinds of exsolution textures (spinel rods in clinopyroxene, orthopyroxene lamellae in clinopyroxene) occur in troctolite and olivine gabbro. We describe oriented spinel rods and orthopyroxene lamellae exsolved from the host clinopyroxene based on optical and high-resolution transmission electron microscope (HRTEM) observations. The spinel rods (100) are parallel to their host clinopyroxene (010). Orthopyroxene lamellae (010) are coherent and strictly parallel to their host clinopyroxene (010). Exsolution of spinel rods from the host clinopyroxene is controlled by the reaction of (Ca0.5M2+ 0.5)Fe3+[AlSiO6]in clinopyroxene → (Ca0.86-0.17M2+ 0.14-0.17)(M2 + 1.00-0.96Al0-0.04)[Al0.17-0.10Si1.83-1.90O6] + Fe3O4 + O2.

  17. An infrared study of the surface chemistry of lithium titanate spinel (Li4Ti5O12)

    International Nuclear Information System (INIS)

    Snyder, Mark Q.; DeSisto, William J.; Tripp, Carl P.

    2007-01-01

    While there are numerous studies examining the performance of lithium titanate spinel (LTS) as a lithium-ion battery, little is known about the surface chemistry of this material. In this paper, diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy spectroscopy was used to study the type of surface groups present on LTS as a function of temperature. The surface was found to contain isolated and hydrogen-bonded TiOH groups and the dehydroxylation behavior with thermal treatment was similar to that of TiO 2 . In addition, hexamethyldisilazane (HMDZ) and pyridine were used to probe the reactivity of surface hydroxyl groups and the presence of Lewis acid sites, respectively. The reaction of HMDZ occurred with both LiOH and TiOH groups to form Li-O-Si and Ti-O-Si. In addition, the reaction of gaseous CO 2 with the Li + ions resulted in the formation of surface carbonate ions. The carbonate ions are removed by heating at 400 deg. C in air

  18. Neutron diffraction study of the reduction of NiAl2O4

    International Nuclear Information System (INIS)

    Ustundag, E.; Clausen, B.; Bourke, M. A. M.

    2000-01-01

    The reduction of a solid NiAl 2 O 4 cylinder to a metal-ceramic composite consisting of Ni particles in an Al 2 O 3 matrix was monitored in situ at 1220 degree sign C with neutron powder diffraction. The reaction kinetics was determined with a time resolution of 30 min. The reduction is associated with a volume shrinkage. A comparison of finite element calculations and the changes in the measured lattice parameters suggests that creep has relaxed the residual strains that would otherwise result from the volume shrinkage. The data also indicate that structural evolution in unreduced NiAl 2 O 4 via a change in the cationic sublattice towards inverse spinel occurred and that led to a variation in lattice parameters. (c) 2000 American Institute of Physics

  19. Structural and magnetic properties of Ni0.8M0.2Fe2O4 (M = Cu, Co) nano-crystalline ferrites

    Science.gov (United States)

    Vijaya Babu, K.; Satyanarayana, G.; Sailaja, B.; Santosh Kumar, G. V.; Jalaiah, K.; Ravi, M.

    2018-06-01

    Nano-crystalline nickel ferrites are interesting materials due to their large physical and magnetic properties. In the present work, two kinds of spinel ferrites Ni0.8M0.2Fe2O4 (M = Cu, Co) are synthesized by using sol-gel auto-combustion method and the results are compared with NiFe2O4. The structural properties of synthesized ferrites are determined by using X-ray powder diffraction; scanning electron microscope and Fourier transform infrared spectroscopy. The cation distribution obtained from X-ray diffraction show that cobalt/copper occupies only tetrahedral site in spinel lattice. The lattice constant increases with the substitution of cobalt/copper. The structural parameters like bond lengths, tetrahedral and octahedral edges have been varied with the substitution. The microstructural study is carried out by using SEM technique and the average grain size is increased with nickel ferrite. The initial permeability (μi) is improving with the substitution. The observed g-value from ESR is approximately equal to standard value.

  20. RHEED oscillations in spinel ferrite epitaxial films grown by conventional planar magnetron sputtering

    Science.gov (United States)

    Ojima, T.; Tainosho, T.; Sharmin, S.; Yanagihara, H.

    2018-04-01

    Real-time in situ reflection high energy electron diffraction (RHEED) observations of Fe3O4, γ-Fe2O3, and (Co,Fe)3O4 films on MgO(001) substrates grown by a conventional planar magnetron sputtering was studied. The change in periodical intensity of the specular reflection spot in the RHEED images of three different spinel ferrite compounds grown by two different sputtering systems was examined. The oscillation period was found to correspond to the 1/4 unit cell of each spinel ferrite, similar to that observed in molecular beam epitaxy (MBE) and pulsed laser deposition (PLD) experiments. This suggests that the layer-by-layer growth of spinel ferrite (001) films is general in most physical vapor deposition (PVD) processes. The surfaces of the films were as flat as the surface of the substrate, consistent with the observed layer-by-layer growth process. The observed RHEED oscillation indicates that even a conventional sputtering method can be used to control film thickness during atomic layer depositions.

  1. RHEED oscillations in spinel ferrite epitaxial films grown by conventional planar magnetron sputtering

    Directory of Open Access Journals (Sweden)

    T. Ojima

    2018-04-01

    Full Text Available Real-time in situ reflection high energy electron diffraction (RHEED observations of Fe3O4, γ-Fe2O3, and (Co,Fe3O4 films on MgO(001 substrates grown by a conventional planar magnetron sputtering was studied. The change in periodical intensity of the specular reflection spot in the RHEED images of three different spinel ferrite compounds grown by two different sputtering systems was examined. The oscillation period was found to correspond to the 1/4 unit cell of each spinel ferrite, similar to that observed in molecular beam epitaxy (MBE and pulsed laser deposition (PLD experiments. This suggests that the layer-by-layer growth of spinel ferrite (001 films is general in most physical vapor deposition (PVD processes. The surfaces of the films were as flat as the surface of the substrate, consistent with the observed layer-by-layer growth process. The observed RHEED oscillation indicates that even a conventional sputtering method can be used to control film thickness during atomic layer depositions.

  2. Synthesis and characterization of CdS/CuAl2O4 core-shell: application to photocatalytic eosin degradation

    Science.gov (United States)

    Bellal, B.; Trari, M.; Afalfiz, A.

    2015-08-01

    The advantages of the hetero-junction CdS/CuAl2O4 for the photocatalytic eosin degradation are reported. Composite semiconductors are elaborated by co-precipitation of CdS on the spinel CuAl2O4 giving a core-shell structure with a uniform dispersion and intimate contact of the spinel nanoparticles inside the hexagonal CdS. The Mott-Schottky plots ( C -2- V) of both materials show linear behaviors from which flat band potentials are determined. The photoactivity increases with increasing the mass of the sensitizer CdS and the best performance is achieved on CdS/CuAl2O4 (85 %/15 %). The pH has a strong influence on the degradation and the photoactivity peaks at pH 7.78. The dark adsorption eosin is weak (~4 %), hence the change in the eosin concentration is attributed to the photocatalytic process. The degradation follows a zero-order kinetic with a rate constant of 5.2 × 10-8 mol L-1 mn-1 while that of the photolysis is seven times lower (0.75 × 10-8 mol L-1 mn-1).

  3. Thermally-induced electronic relaxation in structurally-modified Cu{sub 0.1}Ni{sub 0.8}Co{sub 0.2}Mn{sub 1.9}O{sub 4} spinel ceramics

    Energy Technology Data Exchange (ETDEWEB)

    Shpotyuk, O., E-mail: shpotyuk@novas.lviv.ua [Institute of Materials, Scientific Research Company “Carat”, 202, Stryjska Street, Lviv 79031 (Ukraine); Institute of Physics, Jan Dlugosz University, 13/15, al. Armii Krajowej, Czestochowa 42200 Poland (Poland); Balitska, V. [Institute of Materials, Scientific Research Company “Carat”, 202, Stryjska Street, Lviv 79031 (Ukraine); Lviv State University of Vital Activity Safety, 35, Kleparivska Street, Lviv 79007 (Ukraine); Brunner, M. [Fachhochschule Köln/University of Applied Sciences, 2, Betzdorfer Strasse, Köln 50679 (Germany); Hadzaman, I. [Institute of Materials, Scientific Research Company “Carat”, 202, Stryjska Street, Lviv 79031 (Ukraine); Drohobych Ivan Franko State Pedagogical University, 24, I. Franko Street, Drohobych 82100 (Ukraine); Klym, H. [Institute of Materials, Scientific Research Company “Carat”, 202, Stryjska Street, Lviv 79031 (Ukraine); Lviv Polytechnic National University, 12, Bandera Street, Lviv 79013 (Ukraine)

    2015-02-15

    Thermally-induced electronic relaxation in structurally-modified Cu{sub 0.1}Ni{sub 0.8}Co{sub 0.2}Mn{sub 1.9}O{sub 4} spinel ceramics is shown to be adequately described by stretched exponential function on time. This kinetics is defined by microsctructure perfectness of the relaxing media, showing obvious onset to stretched exponential behaviour with non-exponentionality index attaining close to 0.43 values for high-monolith ceramics and smaller ones in fine-grained ceramics. Percolation threshold in relaxation-degradation kinetics is detected for ceramics with 10% of NiO extractions, showing the smallest but most prolonged single-path degradation effect. This finding is treated in terms of Phillips’ axiomatic diffusion-to-trap model, where only one of two relaxation channels (caused by operative short-range forces) occurs to be effective, while additional non-operative channels contribute to electronic relaxation in fine-grained ceramics.

  4. Irradiation effects and behaviour of fission products in zirconia and spinel

    International Nuclear Information System (INIS)

    Gentils, A.

    2003-10-01

    Crystalline oxides, such as zirconia (ZrO 2 ) and spinel (MgAl 2 O 4 ), are promising inert matrices for the transmutation of plutonium and minor actinides. This work deals with the study of the physico-chemical properties of these matrices, more specifically their behaviour under irradiation and their capacity to retain fission products. Irradiations at low energy and incorporation of stable analogs of fission products (Cs, I, Xe) into yttria-stabilized zirconia and magnesium-aluminate spinel single crystals were performed by using the ion implanter IRMA (CSNSM-Orsay). Irradiations at high energy were made on several heavy ion accelerators (GANIL-Caen, ISL-Berlin, HIL-Warsaw). The damage induced by irradiation and the release of fission products were monitored by in situ Rutherford Backscattering Spectrometry experiments. Transmission electron microscopy was also used in order to determine the nature of the damage induced by irradiation. The results show that irradiation of ZrO 2 and MgAl 2 O 4 with heavy ions (about hundred keV and about hundred MeV) induces a huge structural damage in crystalline matrices. Total disorder (amorphization) is however never reached in zirconia, contrary to what is observed in the case of spinel. The results also emphasize the essential role played by the concentration of implanted species on their retention capacity. A dramatic release of fission products was observed when the concentration exceeds a threshold of a few atomic percent. Irradiation of implanted samples with medium-energy noble-gas ions leads to an enhancement of the fission product release. The exfoliation of spinel crystals implanted at high concentration of Cs ions is observed after a thermal treatment at high temperature. (author)

  5. Effect of gamma irradiation on the structural and magnetic properties of Co–Zn spinel ferrite nanoparticles

    International Nuclear Information System (INIS)

    Raut, Anil V.; Kurmude, D.V.; Shengule, D.R.; Jadhav, K.M.

    2015-01-01

    Highlights: • Co–Zn ferrite nanoparticles were examined before and after γ-irradiation. • Single phase cubic spinel structure of Co–Zn was confirmed by XRD data. • The grain size was reported in the range of 52–62 nm after γ-irradiation. • Ms, Hc, n B were reported to be increased after gamma irradiation. - Abstract: In this work, the structural and magnetic properties of Co 1−x Zn x Fe 2 O 4 (0.0 ≤ x ≤ 1.0) ferrite nanoparticles were studied before and after gamma irradiation. The as-synthesized samples of Co–Zn ferrite nanoparticles prepared by sol–gel auto-combustion technique were analysed by XRD which suggested the single phase; cubic spinel structure of the material. Crystal defects produced in the spinel lattice were studied before and after Co 60 γ-irradiation in a gamma cell with a dose rate of 0.1 Mrad/h in order to report the changes in structural and magnetic properties of the Co–Zn ferrite nanoparticles. The average crystallite size (t), lattice parameter (α) and other structural parameters of gamma-irradiated and un-irradiated Co 1−x Zn x Fe 2 O 4 spinel ferrite system was calculated from XRD data. The morphological characterizations were performed using scanning electron microscopy (SEM). The magnetic properties were measured using pulse field hysteresis loop tracer by applying magnetic field of 1000 Oe, and the analysis of data obtained revealed that the magnetic property such as saturation magnetization (Ms), coecivity (Hc), magneton number (n B ) etc. magnetic parameters were increased after irradiation

  6. Microstructural changes and effect of variation of lattice strain on positron annihilation lifetime parameters of zinc ferrite nanocomposites prepared by high enegy ball-milling

    Directory of Open Access Journals (Sweden)

    Abhijit Banerjee

    2012-12-01

    Full Text Available Zn-ferrite nanoparticles were synthesized at room temperature by mechanical alloying the stoichiometric (1:1 mol% mixture of ZnO and α-Fe2O3 powder under open air. Formation of both normal and inverse spinel ferrite phases was noticed after 30 minutes and 2.5 hours ball milling respectively and the content of inverse spinel phase increased with increasing milling time. The phase transformation kinetics towards formation of ferrite phases and microstructure characterization of ball milled ZnFe2O4 phases was primarily investigated by X-ray powder diffraction pattern analysis. The relative phase abundances of different phases, crystallite size, r.m.s. strain, lattice parameter change etc. were estimated from the Rietveld powder structure refinement analysis of XRD data. Positron annihilation lifetime spectra of all ball milled samples were deconvoluted with three lifetime parameters and their variation with milling time duration was explained with microstructural changes and formation of different phases with increase of milling time duration.

  7. Determination of milling parameters to obtain mechanosynthesized ZnFe2O4

    International Nuclear Information System (INIS)

    Jean, Malick; Nachbaur, Virginie

    2008-01-01

    In this work, the mechanosynthesis of zinc ferrite in WC vials is studied. Millings are performed under air, with a planetary ball-milling, starting from elemental oxides α-Fe 2 O 3 and ZnO. As-milled powders are structurally and magnetically characterized by X-ray diffraction and Moessbauer spectroscopy. Milling parameters as rotational speeds of main disc and vials are particularly discussed in terms of influence on the obtaining of a pure zinc ferrite phase. These parameters have a strong influence on injected power, on radial and tangential components of the impact force. Friction phenomenon, associated with injected power, have been found to be the governing parameters of the end product

  8. True atomic-scale imaging of a spinel Li{sub 4}Ti{sub 5}O{sub 12}(111) surface in aqueous solution by frequency-modulation atomic force microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Kitta, Mitsunori, E-mail: m-kitta@aist.go.jp; Kohyama, Masanori [Research Institute for Ubiquitous Energy Devices, National Institute of Advanced Industrial Science and Technology, 1-8-31 Midorigaoka, Ikeda, Osaka 563-8577 (Japan); Onishi, Hiroshi [Department of Chemistry, Graduate School of Science, Kobe University 1-1 Rokkodai, Nada, Kobe 657-8501 (Japan)

    2014-09-15

    Spinel-type lithium titanium oxide (LTO; Li{sub 4}Ti{sub 5}O{sub 12}) is a negative electrode material for lithium-ion batteries. Revealing the atomic-scale surface structure of LTO in liquid is highly necessary to investigate its surface properties in practical environments. Here, we reveal an atomic-scale image of the LTO(111) surface in LiCl aqueous solution using frequency-modulation atomic force microscopy. Atomically flat terraces and single steps having heights of multiples of 0.5 nm were observed in the aqueous solution. Hexagonal bright spots separated by 0.6 nm were also observed on the flat terrace part, corresponding to the atomistic contrast observed in the ultrahigh vacuum condition, which suggests that the basic atomic structure of the LTO(111) surface is retained without dramatic reconstruction even in the aqueous solution.

  9. Phase formation in the Li2MoO4–Rb2MoO4–Fe2(MoO4)3 system and crystal structure of a novel triple molybdate LiRb2Fe(MoO4)3

    International Nuclear Information System (INIS)

    Khal'baeva, Klara M.; Solodovnikov, Sergey F.; Khaikina, Elena G.; Kadyrova, Yuliya M.; Solodovnikova, Zoya A.; Basovich, Olga M.

    2013-01-01

    X-ray investigation of solid state interaction of the components in the Li 2 MoO 4 –Rb 2 MoO 4 –Fe 2 (MoO 4 ) 3 system was carried out, and a subsolidus phase diagram of the said system was constructed. The subsystem Rb 2 MoO 4 –LiRbMoO 4 –RbFe(MoO 4 ) 2 was shown to be non-quasiternary. Formation of a novel triple molybdate LiRb 2 Fe(MoO 4 ) 3 was established, conditions of solid state synthesis and crystallization of the compound were found. Its crystal structure (orthorhombic, space group Pnma, Z=4, a=24.3956(6), b=5.8306(1), c=8.4368(2) Å) represents a new structure type and includes infinite two-row ribbons ([Fe(MoO 4 ) 3 ] 3− ) ∞ parallel to the b axis and composed of FeO 6 octahedra, terminal Mo(3)O 4 tetrahedra, and bridge Mo(1)O 4 and Mo(2)O 4 tetrahedra connecting two or three FeO 6 octahedra. The ribbons are connected to form 3D framework via corner-sharing LiO 4 tetrahedra. Rubidium cations are 11- and 13-coordinated and located in cavities of this heterogeneous polyhedral framework. - Graphical abstract: Exploring the Li 2 MoO 4 –Rb 2 MoO 4 –Fe 2 (MoO 4 ) 3 system showed its partial non-quasiternarity and revealed a new compound LiRb 2 Fe(MoO 4 ) 3 which was structurally studied. - Highlights: • The Li 2 MoO 4 –Rb 2 MoO 4 –Fe 2 (MoO 4 ) 3 system study revealed a new compound LiRb 2 Fe(MoO 4 ) 3 . • Its structure of a new type includes ribbons of FeO 6 octahedra and MoO 4 tetrahedra. • The ribbons are connected into a 3D framework via corner-sharing LiO 4 tetrahedra

  10. High pressure in-situ X-ray diffraction study on Zn-doped magnetite nanoparticles

    Science.gov (United States)

    Ferrari, S.; Bilovol, V.; Pampillo, L. G.; Grinblat, F.; Errandonea, D.

    2018-03-01

    We have performed high pressure synchrotron X-ray powder diffraction experiments on two different samples of Zn-doped magnetite nanoparticles (formula Fe(3-x)ZnxO4; x = 0.2, 0.5). The structural behavior of then a noparticles was studied up to 13.5 GPa for x = 0.2, and up to 17.4 GPa for x = 0.5. We have found that both systems remain in the cubic spinel structure as expected for this range of applied pressures. The analysis of the unit cell volume vs. pressure results in bulk modulus values lower than in both end-members, magnetite (Fe3O4) and zinc ferrite (ZnFe2O4), suggesting that chemical disorder may favor compressibility, which is expected to improve the increase of the Neel temperature under compression.

  11. Modification of Alumina and Spinel Inclusions by Calcium in Liquid Steel

    Science.gov (United States)

    Verma, Neerav

    2011-12-01

    samples were characterized for inclusion shape, size and chemistry through scanning electron microscopy (SEM). Automated inclusion analysis tools (like ASCAT [59, 91, 92], INCA-GSR [126]; Please refer section 6.4., page number 68) were employed to generate statistical information of the inclusions. Thermodynamic database software FACTSAGE [62] was used to determine thermochemistry of reactions, ternary phase diagrams (Ca-Al-S and Ca-Al-Mg systems). The compositions of the inclusions were tracked before and after calcium treatment to determine the effectiveness of calcium treatment. Extraction of inclusions through dissolution of iron in bromine-methanol solution was employed to reveal 3-D geometry of inclusions and analyze inclusions through EDS (Energy-dispersive X-ray spectroscopy) without any matrix effects. Various industrial samples were also analyzed to confirm the feasibility of various reaction mechanisms deduced through experiments. Successful modification of alumina and spinel inclusions by calcium was demonstrated [85, 86]. It was observed that these modification mechanisms proceed through transient phase (CaO, CaS) formation. In the case of spinels, preferential reduction of MgO part was also observed during calcium modification of spinels. The magnesium after MgO reduction by calcium can enter back into the melt or leave the melt in vapor form. The inclusion area fraction decreased after calcium treatment, but the inclusion concentration (number of inclusions per cm2) increased because inclusions shifted to a smaller size distribution after calcium treatment. Severe matrix effects during EDS analysis of inclusions were observed, due to which inclusion composition analyses can be significantly affected. *Please refer to dissertation for footnotes.

  12. Exchange coupling behavior in bimagnetic CoFe{sub 2}O{sub 4}/CoFe{sub 2} nanocomposite

    Energy Technology Data Exchange (ETDEWEB)

    Leite, G.C.P. [Instituto de Fisica, Universidade Federal de Mato Grosso, 78060-900 Cuiaba-MT (Brazil); Chagas, E.F., E-mail: efchagas@fisica.ufmt.br [Instituto de Fisica, Universidade Federal de Mato Grosso, 78060-900 Cuiaba-MT (Brazil); Pereira, R.; Prado, R.J. [Instituto de Fisica, Universidade Federal de Mato Grosso, 78060-900 Cuiaba-MT (Brazil); Terezo, A.J. [Departamento de Quimica, Universidade Federal do Mato Grosso, 78060-900 Cuiaba-MT (Brazil); Alzamora, M.; Baggio-Saitovitch, E. [Centro Brasileiro de Pesquisas Fisicas, Rua Xavier Sigaud 150 Urca, Rio de Janeiro (Brazil)

    2012-09-15

    In this work we report a study of the magnetic behavior of ferrimagnetic oxide CoFe{sub 2}O{sub 4} and ferrimagnetic oxide/ferromagnetic metal CoFe{sub 2}O{sub 4}/CoFe{sub 2} nanocomposite. The latter compound is a good system to study hard ferrimagnet/soft ferromagnet exchange coupled. Two steps were followed to synthesize the bimagnetic CoFe{sub 2}O{sub 4}/CoFe{sub 2} nanocomposite: (i) first, preparation of CoFe{sub 2}O{sub 4} nanoparticles using a simple hydrothermal method, and (ii) second, reduction reaction of cobalt ferrite nanoparticles using activated charcoal in inert atmosphere and high temperature. The phase structures, particle sizes, morphology, and magnetic properties of CoFe{sub 2}O{sub 4} nanoparticles were investigated by X-Ray diffraction (XRD), Mossbauer spectroscopy (MS), transmission electron microscopy (TEM), and vibrating sample magnetometer (VSM) with applied field up to 3.0 kOe at room temperature and 50 K. The mean diameter of CoFe{sub 2}O{sub 4} particles is about 16 nm. Mossbauer spectra revealed two sites for Fe{sup 3+}. One site is related to Fe in an octahedral coordination and the other one to the Fe{sup 3+} in a tetrahedral coordination, as expected for a spinel crystal structure of CoFe{sub 2}O{sub 4}. TEM measurements of nanocomposite showed the formation of a thin shell of CoFe{sub 2} on the cobalt ferrite and indicate that the nanoparticles increase to about 100 nm. The magnetization of the nanocomposite showed a hysteresis loop that is characteristic of exchange coupled systems. A maximum energy product (BH){sub max} of 1.22 MGOe was achieved at room temperature for CoFe{sub 2}O{sub 4}/CoFe{sub 2} nanocomposites, which is about 115% higher than the value obtained for CoFe{sub 2}O{sub 4} precursor. The exchange coupling interaction and the enhancement of product (BH){sub max} in nanocomposite CoFe{sub 2}O{sub 4}/CoFe{sub 2} are discussed. - Highlights: Black-Right-Pointing-Pointer CoFe{sub 2}O{sub 4}/CoFe{sub 2} nanocomposite

  13. Effect of Sulfur on Liquidus Temperatures in the ZnO-"FeO"-Al2O3-CaO-SiO2-S System in Equilibrium with Metallic Iron

    Science.gov (United States)

    Zhao, Baojun; Hayes, Peter C.; Jak, Evgueni

    2011-10-01

    The phase equilibria in the ZnO-"FeO"-Al2O3-CaO-SiO2-S system have been determined experimentally in equilibrium with metallic iron. A pseudoternary section of the form ZnO-"FeO"-(Al2O3+CaO+SiO2) for CaO/SiO2 = 0.71 (weight), (CaO+SiO2)/Al2O3 = 5.0 (weight), and fixed 2.0 wt pct S concentration has been constructed. It was found that the addition of 2.0 wt pct S to the liquid extends the spinel primary phase field significantly and decreases the size of the wustite primary phase field. The liquidus temperature in the wustite primary phase field is decreased by approximately 80 K and the liquidus temperature in the spinel primary phase field is decreased by approximately 10 K with addition of 2.0 wt pct S in the composition range investigated. It was also found that iron-zinc sulfides are present in some samples in the spinel primary phase field, which are matte appearing at low zinc concentrations and sphalerite (Zn,Fe)S at higher zinc concentrations. The presence of sulfur in the slag has a minor effect on the partitioning of ZnO between the wustite and liquid phases but no effect on the partitioning of ZnO between the spinel and liquid phases.

  14. Effect of mulitivalent cation dopants on lithium manganese spinel cathodes

    CSIR Research Space (South Africa)

    De Kock, A

    1998-02-01

    Full Text Available The aim of this investigation is to determine optimised spinel cathode compositions that can be used in lithium cells. The cycling stability of 4 V LixMn2O4 electrodes in lithium, flooded electrolyte glass cells has been improved by the addition...

  15. Sol-Gel Synthesis and Characterization of Selected Transition Metal Nano-Ferrites

    Directory of Open Access Journals (Sweden)

    Aurelija GATELYTĖ

    2011-09-01

    Full Text Available In the present work, the sinterability and formation of nanosized yttrium iron garnet (Y3Fe5O12, yttrium perovskite ferrite (YFeO3, cobalt, nickel and zinc iron spinel (CoFe2O4, NiFe2O4 and ZnFe2O4, respectively powders by an aqueous sol-gel processes are investigated. The metal ions, generated by dissolving starting materials of transition metals in the diluted acetic acid were complexed by 1,2-ethanediol to obtain the precursors for the transition metal ferrite ceramics. The phase purity of synthesized nano-compounds was characterized by infrared spectroscopy (IR and powder X-ray diffraction analysis (XRD. The microstructural evolution and morphological features of obtained transition metal ferrites were studied by scanning electron microscopy (SEM.http://dx.doi.org/10.5755/j01.ms.17.3.598

  16. Synthesis, structural, optical, electrical and Mössbauer spectroscopic studies of Co substituted Li{sub 0.5}Fe{sub 2.5}O{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Sharma, Parul [School of Physics & Materials Science, Shoolini University, Solan, HP (India); Thakur, Preeti, E-mail: preetithakur@shooliniuniversity.com [School of Physics & Materials Science, Shoolini University, Solan, HP (India); Mattei, Jean Luc; Queffelec, Patrick [Laboratoire des Sciences et Techniques, de l’Information, de la Communication et de la Connaissance, UMR CNRS 6285, 6 av. Le Gorgeu, CS 93837, 29238 BREST CEDEX 3 (France); Thakur, Atul [School of Physics & Materials Science, Shoolini University, Solan, HP (India); Nanotechnology Wing, Innovative Science Research Society, Shimla 171001 (India)

    2016-06-01

    A series of cobalt substituted lithium ferrite Li{sub 0.5}Co{sub x}Fe{sub 2.5−x}O{sub 4} with x=0, 0.2, 0.4 was prepared by a chemical technique called citrate precursor method. In this technique citric acid was used as a reducing agent. Structural, morphological, topographical, optical, electrical, and magnetic properties were studied by using X-Ray Diffractometer (XRD), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Fourier Transform Infrared Spectroscopy (FTIR), Raman Spectroscopy, DC resistivity, Mössbauer Spectroscopy. XRD patterns showed characteristic (2 2 0), (3 1 1), (4 0 0), (4 2 2), (5 1 1), (4 4 0) peaks which confirmed the inverse spinel phase. SEM and TEM support the formation of cubic nanoparticles. FTIR studies reported the ferrite peaks between 400 cm{sup −1} and 800 cm{sup −1} confirming the inverse spinel structure. Five optical Raman modes (A{sub 1g}+E{sub g}+3F{sub 2g}), characteristics of the cubic spinel structure with (P4{sub 3}32) space group are also observed. Electrical DC resistivity studied from room temperature to 300 °C showed the semiconducting behavior of lithium ferrite. Porosity, transition temperature and activation energy are found to decrease with cobalt ion concentration. The room temperature Mössbauer spectra of all the samples showed normal Zeeman Splitting sextets supporting the formation of ferromagnetic phase. With increase in cobalt content, the value of hyperfine field at A site is found to vary from 53.15 to 54.96 T whereas at B site it vary from 54.79 to 52.82 T. The obtained results have been explained based on possible mechanisms, models and theories. - Highlights: • XRD studies confirmed the spinel structure. • In FTIR studies, two frequency metal oxide bands are observed. • Raman spectra confirmed the symmetric and anti-symmetric band position. • Mössbauer spectroscopy reveals the two magnetic sextets.

  17. Mechanical behaviour of Zn-Fe alloy coated mild steel

    International Nuclear Information System (INIS)

    Panagopoulos, C.N.; Georgiou, E.P.; Agathocleous, P.E.; Giannakopoulos, K.I.

    2009-01-01

    Zinc alloy coatings containing various amounts of Fe were deposited by electrodeposition technique on a mild steel substrate. The concentration of Fe in the produced alloy coatings ranged from 0 to 14 wt.%, whereas the thickness of the coatings was about 50 μm. Structural and metallurgical characterization of the produced coatings was performed with the aid of X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) techniques. This study aims in investigating the mechanical behaviour of Zn-Fe coated mild steel specimens, as no research investigation concerning the tensile behaviour of Zn alloy coated ferrous alloys has been reported in the past. The experimental results indicated that the ultimate tensile strength of the Zn-Fe coated mild steel was lower than the bare mild steel. In addition, the ductility of the Zn-Fe coated mild steel was found to decrease significantly with increasing Fe content in the coating.

  18. Frequency domain kinetic of positron-electron annihilation in the MgO-Al2O3 spinel-type ceramics

    Science.gov (United States)

    Fl'unt, Orest; Klym, Halyna; Ingram, Adam

    2018-03-01

    In this work, the kinetic of positron-electron annihilation in the MgO-Al2O3 spinel-type ceramics sintered at different temperatures (1100, 1200 and 1400 °C) has been calculated and analyzed in a frequency domain. The spectra of real (in-phase) and imaginary (quadrature) components of positron-electron annihilation kinetic have been obtained numerically from usual temporal characteristics using integral Fourier transform. The numerical calculations were carried out using cubic spline interpolation of the pulse characteristics of MgO-Al2O3 ceramics in time domain with following analytical calculations of integrals. The obtained spectra as real so imaginary part of MgO-Al2O3 ceramics in frequency domain almost good obey a Debye law denying correlation between elementary positron annihilation processes. Complex diagrams of frequency domain responses of as-prepared samples have a shape of semicircles with close characteristic frequencies. Some deviation on low-frequency side of the semicircles is observed confirming an availability of longer time kinetic processes. Sintering temperature dependencies of the relaxation times and characteristic frequencies of positron-electron annihilation processes have been obtained. It is shown that position of large maxima on the frequency dependencies of imaginary part corresponds to fast average relaxation lifetime representing the most intensive interaction process of positrons with small cavity traps in solids.

  19. Topotactic synthesis of Co3O4 nanoboxes from Co(OH)2 nanoflakes

    International Nuclear Information System (INIS)

    Tian Li; Huang Kelong; Liu Younian; Liu Suqin

    2011-01-01

    Hollow nanocubes of spinel Co 3 O 4 with the dimension of 20 nm were successfully prepared via a facile and reproducible solvothermal route. The structure and morphology of Co 3 O 4 nanoboxes were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and high-resolution transmission electron microscope (HRTEM) techniques. And a possible growth mechanism of Co 3 O 4 nanoboxes were suggested that solid Co 3 O 4 nanocubes nucleate in-situ and grow epitaxially from hexagonal β-Co(OH) 2 precursors with the structural matching relationship of [0 0 1] β-Co(OH) 2 //[1 1 1] Co 3 O 4 , and then solid Co 3 O 4 nanocubes gradually hollow and convert to single-crystal nanoboxes owing to Ostwald ripening. - Graphical abstract: The formation mechanism of Co 3 O 4 nanoboxes can be expressed as epitaxial growth of Co 3 O 4 nanocubes from β-Co(OH) 2 nanoflakes due to a topotactic transformation and hollowing process owing to Ostwald ripening. Highlights: → Co 3 O 4 nanoboxes were prepared by a convenient, economical and controllable hydrothermal route. → Morphology and structure of Co 3 O 4 nanoboxes were characterized by XRD, SEM, and TEM techniques. → Co 3 O 4 nanoboxes grow epitaxially from Co(OH) 2 by topotactic transformation was suggested.

  20. P-type zinc oxide spinels: application to transparent conductors and spintronics

    International Nuclear Information System (INIS)

    Stoica, Maria; S Lo, Cynthia

    2014-01-01

    We report on the electronic and optical properties of two theoretically predicted stable spinel compounds of the form ZnB 2 O 4 , where B = Ni or Cu; neither compound has been previously synthesized, so we compare them to the previously studied p-type ZnCo 2 O 4 spinel. These new materials exhibit spin polarization, which is useful for spintronics applications, and broad conductivity maxima near the valence band edge that indicate good p-type dopability. We show that 3d electrons on the octahedrally coordinated Zn atom fall deep within the valence band and do not contribute significantly to the electronic structure near the band edge of the material, while the O 2p and tetrahedrally coordinated B 3d electrons hybridize broadly in the shallow valence states, resulting in increasing curvature (i.e., decreased electron effective mass) of valence bands near the band edge. In particular, ZnCu 2 O 4 exhibits high electrical conductivities in the p-doping region near the valence band edge that, at σ=2×10 4  S cm −1 , are twice the maximum found for ZnCo 2 O 4 , a previously synthesized compound in this class of materials. This material also exhibits ferromagnetism in all of its most stable structures, which makes it a good candidate for further study as a dilute magnetic semiconductor. (paper)

  1. Phase formation in the Li2MoO4–K2MoO4–In2(MoO4)3 system and crystal structures of new compounds K3InMo4O15 and LiK2In(MoO4)3

    International Nuclear Information System (INIS)

    Khal’baeva, Klara M.; Solodovnikov, Sergey F.; Khaikina, Elena G.; Kadyrova, Yuliya M.; Solodovnikova, Zoya A.; Basovich, Olga M.

    2012-01-01

    XRD study of solid-phase interaction in the Li 2 MoO 4 –K 2 MoO 4 –In 2 (MoO 4 ) 3 system was performed. The boundary K 2 MoO 4 –In 2 (MoO 4 ) 3 system is an non-quasibinary join of the K 2 O–In 2 O 3 –MoO 3 system where a new polymolybdate K 3 InMo 4 O 15 isotypic to K 3 FeMo 4 O 15 was found. In the structure (a=33.2905(8), b=5.8610(1), c=15.8967(4) Å, β=90.725(1)°, sp. gr. C2/c, Z=8, R(F)=0.0407), InO 6 octahedra, Mo 2 O 7 diortho groups and MoO 4 tetrahedra form infinite ribbons {[In(MoO 4 ) 2 (Mo 2 O 7 )] 3− } ∞ along the b-axis. Between the chains, 8- to 10-coordinate potassium cations are located. A subsolidus phase diagram of the Li 2 MoO 4 –K 2 MoO 4 –In 2 (MoO 4 ) 3 system was constructed and a novel triple molybdate LiK 2 In(MoO 4 ) 3 was revealed. Its crystal structure (a=7.0087(2), b=9.2269(3), c=10.1289(3) Å, β=107.401(1)°, sp. gr. P2 1 , Z=2, R(F)=0.0280) contains an open framework of vertex-shared MoO 4 tetrahedra, InO 6 octahedra and LiO 5 tetragonal pyramids with nine- and seven-coordinate potassium ions in the framework channels. - Graphical abstract: Exploring the Li 2 MoO 4 –K 2 MoO 4 –In 2 (MoO 4 ) 3 system showed its partial non-quasibinarity and revealed new compounds K 3 InMo 4 O 15 (isotypic to K 3 FeMo 4 O 15 ) and LiK 2 In(MoO 4 ) 3 which were structurally studied. An open framework of the latter is formed by vertex-shared MoO 4 tetrahedra, InO 6 octahedra and LiO 5 tetragonal pyramids. Highlights: ► Subsolidus phase relations in the Li 2 MoO 4 –K 2 MoO 4 –In 2 (MoO 4 ) 3 system were explored. ► The K 2 MoO 4 –In 2 (MoO 4 ) 3 system is a non-quasibinary join of the K 2 O–In 2 O 3 –MoO 3 system. ► New compounds K 3 InMo 4 O 15 and LiK 2 In(MoO 4 ) 3 were obtained and structurally studied. ► K 3 InMo 4 O 15 is isotypic to K 3 FeMo 4 O 15 and carries bands of InO 6 , MoO 4 and Mo 2 O 7 units. ► An open framework of LiK 2 In(MoO 4 ) 3 is formed by polyhedra MoO 4 , InO 6 and LiO 5 .

  2. Preparation and luminescence of green-emitting ZnAl{sub 2}O{sub 4}:Mn{sup 2+} phosphor thin films

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Ing-Bang [Department of Materials Science and Engineering, National Formosa University, Huwei, Yunlin 632, Taiwan (China); Chang, Yee-Shin [Department of Electronic Engineering, National Formosa University, Huwei, Yunlin 632, Taiwan (China); Chen, Hao-Long [Department of Electronic Engineering, Kao Yuan University, Lujhu, Kaohsiung 821, Taiwan (China); Hwang, Ching Chiang [Department of Biotechnology, Mingdao University, Chang-Hua 52345, Taiwan (China); Jian, Chen-Jhu; Chen, Yu-Shiang [Department of Materials Science and Engineering, National Formosa University, Huwei, Yunlin 632, Taiwan (China); Tsai, Mu-Tsun, E-mail: mttsai@ms23.hinet.net [Department of Materials Science and Engineering, National Formosa University, Huwei, Yunlin 632, Taiwan (China)

    2014-11-03

    Nanocrystalline Mn{sup 2+}-doped zinc spinel (ZnAl{sub 2}O{sub 4}:Mn{sup 2+}) green-emitting phosphor films were deposited on silicon substrate by sol–gel spin coating and subsequent heat treatment up to 1000 °C. The effects of dopant concentration and heat treatment on the optical and structural properties were investigated. The variations in sol viscosity with time, film thickness with number of layers were also examined. Thin films were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, energy-dispersive X-ray microscopy, atomic force microscopy, and photoluminescence spectrum. Single-phase ZnAl{sub 2}O{sub 4} started to crystallize at around 600 °C, with a normal spinel structure. On annealing at 1000 °C, the films had smooth surfaces with a nanocrystalline structure. Under UV or visible light excitation, the phosphor films exhibited an intense green emission band peaking at around 512 nm, corresponding to the typical {sup 4}T{sub 1} → {sup 6}A{sub 1} transition of tetrahedral Mn{sup 2+} ions. The most intense green emission was obtained by exciting at 456 nm. The emission intensity of films was highly dependent upon the excitation wavelength, crystallinity, dopant content, and deposition conditions. The results show that the ZnAl{sub 2}O{sub 4}:Mn{sup 2+} films have good potential for use as a green phosphor for displays and/or white light-emitting diodes. - Highlights: • ZnAl2O4:Mn2 + thin film phosphors have been synthesized by a sol–gel process. • The most intense green emission was obtained by exciting at 456 nm. • Photoluminescence is highly dependent on the crystallinity and doping content. • Emission intensity can also be modulated by controlling the film thickness.

  3. Origin of spinel lamella and/or inclusions in olivine of harzburgite form the Pauza ultramafic rocks from the Kurdistan region, northeastern Iraq

    Science.gov (United States)

    Mohammad, Y.; Maekawa, H.; Karim, K.

    2009-04-01

    Exsolution lamellae and octahedral inclusions of chromian spinel occur in olivine of harzburgite of the Pauza ultramafic rocks, Kurdistan region, northeastern Iraq. The lamella is up to 80μm long and up to 50 μm wide. The lamellae and octahedral inclusions of chromian spinel are distributed heterogeneously in the host olivine crystal. They are depleted in Al2O3 relative to the subhedral spinel grains in the matrix and spinel lamella in orthopyroxene. Olivine (Fo92 - 93) with spinel lamellae occurs as fine-grained crystals around orthopyroxene, whereas olivine (Fo90-91) free from spinel is found in matrix. Based on back-scattered images analyses, enrichments of both Cr # and Fe+3 in the chromian spinel lamella in olivine (replacive olivine) relative to that in adjacent orthopyroxene. As well as the compositions of chromian spinel lamellae host olivine are more Mg-rich than the matrix olivine. Furthermore the restriction of olivine with spinel lamellae and octahedral inclusions on around orthopyroxene, and the similarity of spinel lamella orientations in both olivine and adjacent orthopyroxene. This study concludes that the spinel inclusions in olivine are remnant (inherited from former orthopyroxene) spinel exsolution lamella in orthopyroxene, that has been formed in upper mantle conditions ( T = 1200 °C, P = 2.5 GPa ). Replacive olivine are formed by reaction of ascending silica poor melt and orthopyroxene in harzburgite as pressure decrease the solubility of silica-rich phase (orthopyroxene) in the system increase, therefore ascending melt dissolve pyroxene with spinel exsolution lamella and precipitate replacive olivine with spinel inclusions. We can conclude that the olivines with spinel lamella are not necessary to be original and presenting ultrahigh-pressure and/or ultra deep-mantle conditions as previously concluded. It has been formed by melting of orthopyroxene (orthopyroxene with spinel exsolution lamella = olivine with spinel lamellae and octahedral

  4. NiFe{sub 2}O{sub 4}/activated carbon nanocomposite as magnetic material from petcoke

    Energy Technology Data Exchange (ETDEWEB)

    Briceño, Sarah, E-mail: sbriceno@ivic.gob.ve [Laboratorio de Física de la Materia Condensada, Centro de Física, Instituto Venezolano de Investigaciones Científicas IVIC, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); Brämer-Escamilla, W., E-mail: wbramer@ivic.gob.ve [Laboratorio de Física de la Materia Condensada, Centro de Física, Instituto Venezolano de Investigaciones Científicas IVIC, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); Silva, P. [Laboratorio de Física de la Materia Condensada, Centro de Física, Instituto Venezolano de Investigaciones Científicas IVIC, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); García, J.; Del Castillo, H.; Villarroel, M. [Laboratorio de Cinética y Catálisis, Departamento de Química, Facultad de Ciencias, Universidad de Los Andes ULA, Mérida 5101-A (Venezuela, Bolivarian Republic of); Rodriguez, J.P. [Laboratorio de Microscopia Electrónica. Instituto de Estudios Científicos y Tecnológicos IDECYT. Apartado 47925 - Caracas 1041-A (Venezuela, Bolivarian Republic of); Ramos, M.A.; Morales, R. [Instituto Zuliano de Investigaciones Tecnológicas INZIT. Apdo. Postal 331. La Cañada-Maracaibo (Venezuela, Bolivarian Republic of); Diaz, Y. [Centro de Química, Instituto Venezolano de Investigaciones Científicas IVIC, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of)

    2014-06-01

    Nickel ferrite (NiFe{sub 2}O{sub 4}) was supported on activated carbon (AC) from petroleum coke (petcoke). Potassium hydroxide (KOH) was employed with petcoke to produce activated carbon. NiFe{sub 2}O{sub 4} were synthesized using PEG-Oleic acid assisted hydrothermal method. The structural and magnetic properties were determined using thermogravimetric and differential thermal analysis (TGA–DTA), X-ray diffraction (XRD), Fourier Transform Infrared (IR-FT), surface area (BET), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM). XRD analysis revealed the cubic spinel structure and ferrite phase with high crystallinity. IR-FT studies showed that chemical modification promoted the formation of surface oxygen functionalities. Morphological investigation by SEM showed conglomerates of spherical nanoparticles with an average particle size of 72 nm and TEM showed the formation of NiFe{sub 2}O{sub 4}/carbon nanofibers. Chemical modification and activation temperature of 800 °C prior to activation dramatically increased the BET surface area of the resulting activated carbon to 842.4 m{sup 2}/g while the sulfur content was reduced from 6 to 1%. Magnetic properties of nanoparticles show strong dependence on the particle size. - Highlights: • TEM showed the formation of NiFe{sub 2}O{sub 4}/carbon nanofibers. • Nanoparticles were supported on the activated carbon from petcoke. • Activation dramatically increased the BET surface area to 842 m{sup 2}/g. • Magnetic properties show strong dependence on the particle size. • Sulphur content was reduced from 6 to 1% with the petcoke activation.

  5. Microstructure and magnetic properties of MFe2O4 (M = Co, Ni, and Mn) ferrite nanocrystals prepared using colloid mill and hydrothermal method

    Science.gov (United States)

    Wang, Wei; Ding, Zui; Zhao, Xiruo; Wu, Sizhu; Li, Feng; Yue, Ming; Liu, J. Ping

    2015-05-01

    Three kinds of spinel ferrite nanocrystals, MFe2O4 (M = Co, Ni, and Mn), are synthesized using colloid mill and hydrothermal method. During the synthesis process, a rapid mixing and reduction of cations with sodium borohydride (NaBH4) take place in a colloid mill then through a hydrothermal reaction, a slow oxidation and structural transformation of the spinel ferrite nanocrystals occur. The phase purity and crystal lattice parameters are estimated by X-ray diffraction studies. Scanning electron microscopy and transmission electron microscopy images show the morphology and particle size of the as-synthesized ferrite nanocrystals. Raman spectrum reveals active phonon modes at room temperature, and a shifting of the modes implies cation redistribution in the tetrahedral and octahedral sites. Magnetic measurements show that all the obtained samples exhibit higher saturation magnetization (Ms). Meanwhile, experiments demonstrate that the hydrothermal reaction time has significant effects on microstructure, morphologies, and magnetic properties of the as-synthesized ferrite nanocrystals.

  6. Spinel FeCo2S4 nanoflower arrays grown on Ni foam as novel binder-free electrodes for long-cycle-life supercapacitors

    Science.gov (United States)

    Deng, Cuifen; Yang, Lishan; Yang, Chunming; Shen, Ping; Zhao, Liping; Wang, Zhiyu; Wang, Chunhui; Li, Junhua; Qian, Dong

    2018-01-01

    Spinel FeCo2S4 nanoflower arrays grown on Ni foam (FeCo2S4@Ni) have been successfully fabricated via a facile hydrothermal sulfurization of the corresponding FeCo2O4 precursor. The results of X-ray diffraction and X-ray photoelectron spectroscopy characterizations affirm that partial Co2+/Co3+ ions in Co3S4 have been substituted by Fe2+/Fe3+ ions to form FeCo2S4. The obtained FeCo2S4@Ni exhibits an ultrahigh specific capacitance (1644.07 mF cm-2 at 50 mA cm-2) and a supreme cycling stability (∼100% after 10,000 cycles at 50 mA cm-2) as binder-free electrodes for supercapacitors. The cycling stability of the fabricated product is the highest among the documented ternary metallic sulfides so far. The excellent supercapacitive performance of FeCo2S4@Ni emanates from the unique architectures of Fe2Co2S4 nanoflower arrays constituted by ultrathin nanoflakes, three-dimensional porous and conductive Ni foam, and solid skeleton of Ni foam for robust connections to the Fe2Co2S4.

  7. Pressure-induced structural and semiconductor-semiconductor transitions in C o0.5M g0.5C r2O4

    Science.gov (United States)

    Rahman, S.; Saqib, Hajra; Zhang, Jinbo; Errandonea, D.; Menéndez, C.; Cazorla, C.; Samanta, Sudeshna; Li, Xiaodong; Lu, Junling; Wang, Lin

    2018-05-01

    The effect of pressure on the structural, vibrational, and electronic properties of Mg-doped Cr bearing spinel C o0.5M g0.5C r2O4 was studied up to 55 GPa at room-temperature using x-ray diffraction, Raman spectroscopy, electrical transport measurements, and ab initio calculations. We found that the ambient-pressure phase is cubic (spinel-type, F d 3 ¯m ) and underwent a pressure-induced structural transition to a tetragonal phase (space group I 4 ¯m 2 ) above 28 GPa. The ab initio calculation confirmed this first-order phase transition. The resistivity of the sample decreased at low pressures with the existence of a low-pressure (LP) phase and started to increase with the emergence of a high-pressure (HP) phase. The temperature dependent resistivity experiments at different pressures illustrated the wide band gap semiconducting nature of both the LP and HP phases with different activation energies, suggesting a semiconductor-semiconductor transition at HP. No evidence of chemical decomposition or a semiconductor-metal transition was observed in our studies.

  8. Microstructure, crystal structure and electrical properties of Cu{sub 0.1}Ni{sub 0.8}Co{sub 0.2}Mn{sub 1.9}O{sub 4} ceramics obtained at different sintering conditions

    Energy Technology Data Exchange (ETDEWEB)

    Bodak, O.; Akselrud, L.; Demchenko, P.; Kotur, B.; Mrooz, O.; Hadzaman, I.; Shpotyuk, O.; Aldinger, F.; Seifert, H.; Volkov, S.; Pekhnyo, V

    2002-12-16

    Details of the formation of Cu{sub 0.1}Ni{sub 0.8}Co{sub 0.2}Mn{sub 1.9}O{sub 4} ceramics under different sintering conditions have been studied by optical microscopy, scanning electron microscopy (SEM), electron probe and energy dispersive spectroscopy (EDX) microanalyses, X-ray diffraction (XRD) and electrical resistivity measurements. Microstructure studies of samples sintered at 1170 deg. C for 1 h indicated the presence of a secondary phase besides the main spinel phase with modified composition. XRD measurements showed that the spinel phase exhibits a tetragonally distorted spinel structure (space group I4{sub 1}/amd, a=5.9410(5) A, c=8.4196(15) A). The secondary phase (solid solution based on NiO) crystallizes with the NaCl-type structure (space group Fm3-bar m, a=4.1872(3) A). The content of the secondary phase in ceramics is 10.61 mass%. For NiMn{sub 2}O{sub 4} ceramics, prepared under the same sintering conditions, the decomposition with Ni{sub 1-x}Mn{sub x}O solid solution (NaCl-type structure) and spinel phase formation have been observed. The tetragonal modification of the spinel phase for NiMn{sub 2}O{sub 4} ceramics is more preferable (space group I4{sub 1}/amd, a=5.9764(5) A, c=8.4201(8) A). The distribution of atoms in the structure has been proposed for both ceramics. According to XRD results the Cu{sub 0.1}Ni{sub 0.8}Co{sub 0.2}Mn{sub 1.9}O{sub 4} ceramic samples, sintered at 920 deg. C for 8 h (program 1), at 920 deg. C for 8 h and at 750 deg. C for 24 h (program 2), at 920 deg. C for 8 h, at 1200 deg. C for 1 h and at 920 deg. C for 24 h (program 3) and at 920 deg. C for 8 h, at 1200 deg. C for 1 h, at 920 deg. C for 24 h and at 750 deg. C for 48 h (program 4), contain a single phase with the cubic spinel structure (space group Fd3-bar m). Small residuals of the secondary phase for the ceramics, prepared via programs 3 and 4, have been observed by SEM investigations. The structure transformations of the spinel phase for Cu{sub 0.1}Ni{sub 0.8}Co

  9. μSR Study of the Unusual Magnetic Ordering in the Frustrated Antiferromagnet Zn(CrxGa1-x)2O4

    International Nuclear Information System (INIS)

    Kikuchi, H.; Fukushima, H.; Higemoto, W.; Nishiyama, K.

    2001-01-01

    μSR spectra on the spin frustrating spinel antiferromagnet Zn(Cr x Ga 1-x ) 2 O 4 (x=0.9,1.0) have been measured. For x=1.0 compound, both the relaxation rate and the initial asymmetry showed distinct anomalies at the Neel temperature. The magnetic susceptibility for the x=0.9 compound was known to have a faint peak at around 12 K, whose origin was not clear so far. Our μSR study revealed that this temperature is the onset temperature of development of the magnetic correlation accompanied by appreciable spin fluctuations.

  10. Synthesis, characterization and adsorption capability for Congo red of CoFe2O4 ferrite nanoparticles

    International Nuclear Information System (INIS)

    Ding, Zui; Wang, Wei; Zhang, Yajun; Li, Feng; Liu, J. Ping

    2015-01-01

    Highlights: • CoFe 2 O 4 ferrite nanoparticles are synthesized by an ethanol-assisted hydrothermal method. • Suitable amount of ethanol can reduce the particle size and increase BET surface area. • The introduction of ethanol leads to the cation redistribution. • Using ethanol/water mixed solution greatly enhances their adsorption capacity for CR dyes. - Abstract: CoFe 2 O 4 ferrite nanoparticles are synthesized by an ethanol-assisted hydrothermal method, where the ethanol is mixed with water as the solution. In this synthesis, a rapid mixing of reducible metal cations with reducing agent and a simultaneous reduction process take place in a colloid mill. Synthesized ferrite samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), vibrating sample magnetometer (VSM) and Raman spectroscopy. XRD patterns reveal the formation of CoFe 2 O 4 ferrites with single spinel phase. SEM and TEM images show that the as-synthesized samples are with narrow size distribution. Raman spectroscopy studies clearly indicate the cation distribution in nanosized particles. Here, it is worthy to note that, with increasing ethanol content in ethanol–water mixed solution, an obvious superparamagnetic behavior of as-synthesized nanoparticles at room temperature is observed. The adsorption capability of the as-synthesized ferrite nanoparticles for Congo Red (CR) is examined. Enhancement of adsorption capability for CR with adding ethanol as the mixing solution is shown. The adsorption mechanism is discussed. This investigation reveals that the composition of ethanol/water mixed solution has great effects on the microstructure and magnetic properties as well as adsorption capacity of Congo Red (CR) dye of the as-synthesized CoFe 2 O 4 ferrite samples

  11. Structural and magnetic properties of Mg-Zn ferrites (Mg1−xZnxFe2O4) prepared by sol-gel method

    International Nuclear Information System (INIS)

    Reyes-Rodríguez, Pamela Yajaira; Cortés-Hernández, Dora Alicia; Escobedo-Bocardo, José Concepción; Almanza-Robles, José Manuel; Sánchez-Fuentes, Héctor Javier; Jasso-Terán, Argentina; De León-Prado, Laura Elena; Méndez-Nonell, Juan; Hurtado-López, Gilberto Francisco

    2017-01-01

    In this study, the Mg 1−x Zn x Fe 2 O 4 nanoparticles (x=0–0.9) were prepared by sol-gel method. These ferrites exhibit an inverse spinel structure and the lattice parameter increases as the substitution of Zn 2+ ions is increased. At lower Zn content (0.1≤x≤0.5), saturation magnetization (Ms) increases, while it decreases at higher Zn content (x≥6). The remnant magnetization (0.17–2.0 emu/g) and coercive field (6.0–60 Oe) indicate a ferrimagnetic behavior. The average core diameter of selected ferrites is around 15 nm and the nanoparticles morphology is quasi spherical. The heating ability of some Mg 0.9 Zn 0.1 Fe 2 O 4 and Mg 0.7 Zn 0.3 Fe 2 O 4 aqueous suspensions indicates that the magnetic nanoparticles can increase the medium temperature up to 42 °C in a time less than 10 min - Highlights: • Magnetic nanoparticles of Mg 1−x Zn x Fe 2 O 4 were synthesized by sol-gel method. • Nanoparticles showing a single spinel crystalline structure were obtained. • Aqueous suspensions of Mg 0.7 Zn 0.3 Fe 2 O 4 and Mg 0.9 Zn 0.1 Fe 2 O 4 show heating ability.

  12. Determination of transition metal ion distribution in cubic spinel Co1.5Fe1.5O4 using anomalous x-ray diffraction

    Directory of Open Access Journals (Sweden)

    M. N. Singh

    2015-08-01

    Full Text Available We report anomalous x-ray diffraction studies on Co ferrite with composition Co1.5Fe1.5O4 to obtain the distribution of transition metal ions in tetrahedral and octahedral sites. We synthesize spinel oxide (Co1.5Fe1.5O4 through co-precipitation and subsequent annealing route. The imaginary part (absorption of the energy dependent anomalous form factor is measured and the real part is calculated theoretically through Kramers–Krönig transformation to analyze anomalous x-ray diffraction peak intensities. Fe and Co K-edge x-ray absorption near edge structure (XANES spectra are used to estimate charge states of transition metals. Our analysis, within experimental errors, suggests 44% of the tetrahedral sites contain Co in +2 oxidation state and the rest 56% sites contain Fe in +2 and +3 oxidation states. Similarly, 47% of the octahedral sites contain Fe in +3 oxidation states, whereas, the rest of the sites contain Co in +2 and +3 oxidation states. While a distinct pre-edge feature in the Fe K-edge XANES is observed, Co pre-edge remains featureless. Implications of these results to magnetism are briefly discussed.

  13. Fast reactor irradiation effects on fracture toughness of Si_3N_4 in comparison with MgAl_2O_4 and yttria stabilized ZrO_2

    International Nuclear Information System (INIS)

    Tada, K.; Watanabe, M.; Tachi, Y.; Kurishita, H.; Nagata, S.; Shikama, T.

    2016-01-01

    Fracture toughness of silicon nitride (Si_3N_4), magnesia-alumina spinel (MgAl_2O_4) and yttria stabilized zirconia (8 mol%Y_2O_3–ZrO_2) was evaluated by the Vickers-indentation technique after the fast reactor irradiation up to 55 dpa (displacement per atom) at about 700 °C in the Joyo. The change of the fracture toughness by the irradiation was correlated with nanostructural evolution by the irradiation, which was examined by transmission electron microscopy. The observed degradation of fracture toughness in Si_3N_4 is thought to be due to the relatively high density of small-sized of the irradiation induced defects, which should be resulted from a large amount of transmutation gases of hydrogen and helium. Observed improvement of fracture toughness in MgAl_2O_4 was due to the blocking of crack propagation by the antiphase boundaries. The radiation effects affected the fracture toughness of yttria stabilized zirconia at 55 dpa, suggesting that the generated high density voids would affect the propagation of cracks. - Highlights: • Si_3N_4, MgAl_2O_4 and YSZ were neutron irradiated up to 55dpa around 700 °C in the Joyo. • They are candidate ceramics for the inert matrices of nuclear fuels in the fast reactors. • The irradiation enhanced the fracture toughness of MgAl_2O_4 and YSZ, while degraded that of Si_3N_4. • The toughness changes were correlated with radiation induced defects and transmutation gases.

  14. Effect of gamma irradiation on the structural and magnetic properties of Co–Zn spinel ferrite nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Raut, Anil V., E-mail: nano9993@gmail.com [Vivekanand Arts, Sardar Dalipsingh Commerce and Science College, Aurangabad 431004, (M.S.) India (India); Kurmude, D.V. [Milind College of Science, Aurangabad 431004, (M.S.) India (India); Shengule, D.R. [Vivekanand Arts, Sardar Dalipsingh Commerce and Science College, Aurangabad 431004, (M.S.) India (India); Jadhav, K.M. [Department of Physics, Dr. Babasaheb Ambedkar Marathwada University, Aurangabad 431004, (M.S.) India (India)

    2015-03-15

    Highlights: • Co–Zn ferrite nanoparticles were examined before and after γ-irradiation. • Single phase cubic spinel structure of Co–Zn was confirmed by XRD data. • The grain size was reported in the range of 52–62 nm after γ-irradiation. • Ms, Hc, n{sub B} were reported to be increased after gamma irradiation. - Abstract: In this work, the structural and magnetic properties of Co{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} (0.0 ≤ x ≤ 1.0) ferrite nanoparticles were studied before and after gamma irradiation. The as-synthesized samples of Co–Zn ferrite nanoparticles prepared by sol–gel auto-combustion technique were analysed by XRD which suggested the single phase; cubic spinel structure of the material. Crystal defects produced in the spinel lattice were studied before and after Co{sup 60} γ-irradiation in a gamma cell with a dose rate of 0.1 Mrad/h in order to report the changes in structural and magnetic properties of the Co–Zn ferrite nanoparticles. The average crystallite size (t), lattice parameter (α) and other structural parameters of gamma-irradiated and un-irradiated Co{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} spinel ferrite system was calculated from XRD data. The morphological characterizations were performed using scanning electron microscopy (SEM). The magnetic properties were measured using pulse field hysteresis loop tracer by applying magnetic field of 1000 Oe, and the analysis of data obtained revealed that the magnetic property such as saturation magnetization (Ms), coecivity (Hc), magneton number (n{sub B}) etc. magnetic parameters were increased after irradiation.

  15. Effect of surfactant amount on the morphology and magnetic properties of monodisperse ZnFe{sub 2}O{sub 4} nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Haitao, E-mail: zht95711lunwen@163.com; Liu, Ruiping; Zhang, Qiang; Wang, Qiao

    2016-03-15

    Graphical abstract: Polyol process to monodisperse ZnFe{sub 2}O{sub 4} nanoparticles. - Highlights: • An one-step, facile and inexpensive synthetic route to monodisperse ZnFe{sub 2}O{sub 4} nanoparticles is described. • The sodium citrate stabilized ZnFe{sub 2}O{sub 4} nanoparticles with a diameter in the 5–8 nm size range can be easily dispersed in water. • The synthesis is very robust in terms of variations of experimental parameters. • ZnFe{sub 2}O{sub 4} nanoparticles present ferrimagnetic behavior at room temperature with a small hysteresis. - Abstract: The spinel ZnFe{sub 2}O{sub 4} ferrites with sodium citrate as a surfactant were fabricated by polyol process. The effect of surfactant amount on the structure, morphology and magnetic properties of ZnFe{sub 2}O{sub 4} ferrites were investigated by X-ray diffraction(XRD), transmission electron microscope (TEM), thermogravimetric and differential scanning calorimetry (TG–DSC) and vibrating sample magnetometry (VSM), respectively. The results indicate that the structure of ZnFe{sub 2}O{sub 4} ferrites is a pure cubic spinel structure with a particle size of 5–8 nm. The dispersion of the synthesized ZnFe{sub 2}O{sub 4} is enhanced when the mole ratio of Fe(acac){sub 3} to sodium citrate decreases. The synthesized particles present ferrimagnetic behavior with a small hysteresis at room temperature. The increase of surfactant amount conversely leads to the decrease in the saturation magnetization value (Ms) especially when the mole ratio of Fe(acac){sub 3} to sodium citrate decreases to 8:3. Its Ms value is drastically reduced to 18.97 emu/g.

  16. Improving the fast discharge performance of high-voltage LiNi{sub 0.5}Mn{sub 1.5}O{sub 4} spinel by Cu{sup 2+}, Al{sup 3+}, Ti{sup 4+} tri-doping

    Energy Technology Data Exchange (ETDEWEB)

    Deng, Jicheng [Electronic Materials Research Laboratory, Key Laboratory of the Ministry of Education & International Center for Dielectric Research, Xi' an Jiaotong University, Xi' an (China); Shaanxi Engineering Research Center of Advanced Energy Materials & Devices, Xi' an Jiaotong University, Xi' an (China); Xu, Youlong, E-mail: ylxuxjtu@mail.xjtu.edu.cn [Electronic Materials Research Laboratory, Key Laboratory of the Ministry of Education & International Center for Dielectric Research, Xi' an Jiaotong University, Xi' an (China); Shaanxi Engineering Research Center of Advanced Energy Materials & Devices, Xi' an Jiaotong University, Xi' an (China); Xiong, Lilong; Li, Liang [Electronic Materials Research Laboratory, Key Laboratory of the Ministry of Education & International Center for Dielectric Research, Xi' an Jiaotong University, Xi' an (China); Sun, Xiaofei [Shaanxi Engineering Research Center of Advanced Energy Materials & Devices, Xi' an Jiaotong University, Xi' an (China); Zhang, Yuan [Electronic Materials Research Laboratory, Key Laboratory of the Ministry of Education & International Center for Dielectric Research, Xi' an Jiaotong University, Xi' an (China)

    2016-08-25

    The sluggish Li{sup +} ion diffusion coefficient at ∼4.7 V (vs. Li{sup +}/Li) greatly impairs the fast discharge performance of LiMn{sub 1.5}Ni{sub 0.5}O{sub 4} cathode material. Herein, a tri-doping strategy is proposed where Cu{sup 2+}, Al{sup 3+}, Ti{sup 4+} ions are partially substituted for Ni{sup 2+} and Mn{sup 4+}. Cu{sup 2+}, Al{sup 3+}, Ti{sup 4+} tri-doping effectively suppresses the Li{sub x}Ni{sub 1−x}O impurity phase, increases the cation mixing in the octahedral B-site in the spinel, enlarges the electronic conductivity, and enhances the structural stability. Most importantly, the Li{sup +} diffusion coefficients show a peculiar boost at 4.7 V by two orders of magnitude after tri-doping. Compared to the pristine LiMn{sub 1.5}Ni{sub 0.5}O{sub 4} (denoted P-LNM), the tri-doped Li[Ni{sub 0.455}Cu{sub 0.03}Al{sub 0.03}Mn{sub 1.455}Ti{sub 0.03}]O{sub 4} (denoted TD-LNM) exhibits much better fast discharge performance, delivering a specific capacity of ∼101 mAh g{sup −1} at 100 C discharge rate. - Graphical abstract: For the LiMn{sub 1.5}Ni{sub 0.5}O{sub 4} cathode material, the sluggish Li{sup +} ion diffusion coefficient around the ∼4.7 V (vs. Li{sup +}/Li) plateau greatly impair its fast discharge performance, which therefore limit its application in electric vehicles. Herein, a tri-doping strategy is proposed where Cu{sup 2+}, Al{sup 3+}, Ti{sup 4+} ions are partially substituted for Ni{sup 2+} and Mn{sup 4+}. After tri-doping, the Li{sup +} diffusion coefficient at 4.7 V (vs. Li{sup +}/Li) is boosted by two orders of magnitude. Compared to the pristine LiMn{sub 1.5}Ni{sub 0.5}O{sub 4} (denoted P-LNM), the tri-doped Li[Ni{sub 0.455}Cu{sub 0.03}Al{sub 0.03}Mn{sub 1.455}Ti{sub 0.03}]O{sub 4} (denoted TD-LNM) exhibits much better fast discharge performance, delivering a capacity of ∼101 mAh·g{sup −1} at 100 C discharge rate. - Highlights: • Cu, Al, Ti Tri-doping improves electronic conductivity of LiNi{sub 0.5}Mn{sub 1.5}O{sub 4}. • Cu

  17. Synthesis of nanocrystalline nickel-zinc ferrite (Ni0.8Zn0.2Fe2O4) thin films by chemical bath deposition method

    International Nuclear Information System (INIS)

    Pawar, D.K.; Pawar, S.M.; Patil, P.S.; Kolekar, S.S.

    2011-01-01

    Graphical abstract: Display Omitted Research highlights: → We have successfully synthesized nickel-zinc ferrite (Ni 0.8 Zn 0.2 Fe 2 O 4 ) thin films on stainless steel substrates using a low temperature chemical bath deposition method. → The surface morphological study showed the compact flakes like morphology. → The as-deposited thin films are hydrophilic (10 o o ) whereas the annealed thin films are super hydrophilic (θ o ) in nature. → Ni 0.8 Zn 0.2 Fe 2 O 4 thin films could be used in supercapacitor. - Abstract: The nickel-zinc ferrite (Ni 0.8 Zn 0.2 Fe 2 O 4 ) thin films have been successfully deposited on stainless steel substrates using a chemical bath deposition method from alkaline bath. The films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), static water contact angle and cyclic voltammetry measurements. The X-ray diffraction pattern shows that deposited Ni 0.8 Zn 0.2 Fe 2 O 4 thin films were oriented along (3 1 1) plane. The FTIR spectra showed strong absorption peaks around 600 cm -1 which are typical for cubic spinel crystal structure. SEM study revealed compact flakes like morphology having thickness ∼1.8 μm after air annealing. The annealed films were super hydrophilic in nature having a static water contact angle (θ) of 5 o .The electrochemical supercapacitor study of Ni 0.8 Zn 0.2 Fe 2 O 4 thin films has been carried out in 6 M KOH electrolyte. The values of interfacial and specific capacitances obtained were 0.0285 F cm -2 and 19 F g -1 , respectively.

  18. Structural modifications of spinels under radiation

    International Nuclear Information System (INIS)

    Quentin, A.

    2010-12-01

    This work is devoted to the study of spinel structure materials under radiation. For that purpose, samples of polycrystalline ZnAl 2 O 4 and monocrystalline MgAl 2 O 4 were irradiated by different heavy ions with different energies. Samples of ZnAl 2 O 4 were studied par electron transmission microscopy, and by grazing incidence X-Ray diffraction and Rietveld analysis. Samples of MgAl 2 O 4 were studied by optical spectroscopy. Most of the results concern amorphization and crystalline structure modification of ZnAl 2 O 4 especially the inversion. We were able to determine a stopping power threshold for amorphization, between 11 keV/nm and 12 keV/nm, and also the amorphization process, which is a multiple impacts process. We studied the evolution of the amorphous phase by TEM and showed a nano-patterning phenomenon. Concerning the inversion, we determined that it did happen by a single impact process, and the saturation value did not reach the random cation distribution value. Inversion and amorphization have different, but close, stopping power threshold. However, amorphization seems to be conditioned by a pre-damage of the material which consists in inversion. (author)

  19. Canted spin structure and the first order magnetic transition in CoFe{sub 2}O{sub 4} nanoparticles coated by amorphous silica

    Energy Technology Data Exchange (ETDEWEB)

    Lyubutin, I.S. [Shubnikov Institute of Crystallography, Russian Academy of Sciences, Moscow 119333 (Russian Federation); Starchikov, S.S., E-mail: sergey.s.starchikov@gmail.com [Shubnikov Institute of Crystallography, Russian Academy of Sciences, Moscow 119333 (Russian Federation); Gervits, N.E.; Korotkov, N.Yu.; Dmitrieva, T.V. [Shubnikov Institute of Crystallography, Russian Academy of Sciences, Moscow 119333 (Russian Federation); Lin, Chun-Rong, E-mail: crlinspin@gmail.com [Department of Applied Physics, National Pingtung University, Pingtung County 90003, Taiwan (China); Tseng, Yaw-Teng [Department of Applied Physics, National Pingtung University, Pingtung County 90003, Taiwan (China); Shih, Kun-Yauh [Department of Applied Chemistry, National Pingtung University, Pingtung County 90003, Taiwan (China); Lee, Jiann-Shing [Department of Applied Physics, National Pingtung University, Pingtung County 90003, Taiwan (China); Wang, Cheng-Chien [Department of Chemical and Materials Engineering, Southern Taiwan University of Science and Technology, Tainan 710, Taiwan (China)

    2016-10-01

    The functional polymer (PMA-co-MAA) latex microspheres were used as a core template to prepare magnetic hollow spheres consisting of CoFe{sub 2}O{sub 4}/SiO{sub 2} composites. The spinel type crystal structure of CoFe{sub 2}O{sub 4} ferrite is formed under annealing, whereas the polymer cores are completely removed after annealing at 450 °C. Magnetic and Mössbauer spectroscopy measurements reveal very interesting magnetic properties of the CoFe{sub 2}O{sub 4}/SiO{sub 2} hollow spheres strongly dependent on the particle size which can be tuned by the annealing temperature. In the ground state of low temperatures, the CoFe{sub 2}O{sub 4} nanoparticles are in antiferromagnetic state due to the canted magnetic structure. Under heating in the applied field, the magnetic structure gradually transforms from canted to collinear, which increases the magnetization. The Mössbauer data revealed that the small size CoFe{sub 2}O{sub 4}/SiO{sub 2} particles (2.24.3 nm) do not show superparamagnetic behavior but transit from the magnetic to the paramagnetic state by a jump-like magnetic transition of the first order This effect is a specific property of the magnetic nanoparticles isolated by inert material, and can be initiated by internal pressure creating at the particle surface. The suggested method of synthesis can be modified with various bio-ligands on the silane surface, and such materials can find many applications in diagnostics and bio-separation. - Highlights: • CoFe{sub 2}O{sub 4}/SiO{sub 2} nanocomposites in shell of hollow microcapsules designed for biomedical applications • The CoFe{sub 2}O{sub 4} particle size and magnetic properties can be tuned by thermal treatment • Canted spin structure in the CoFe{sub 2}O{sub 4} nanoparticles coated by SiO{sub 2} • The first order magnetic transition in the CoFe{sub 2}O{sub 4} nanoparticles coated by silica.

  20. Moessbauer spectroscopy study of the synthesis of SnFe2O4 by high energy ball milling (HEBM) of SnO and α-Fe2O3

    International Nuclear Information System (INIS)

    Uwakweh, Oswald N C; Perez Moyet, Richard; Mas, Rita; Morales, Carolyn; Vargas, Pedro; Silva, Josue; Rossa, Angel; Lopez, Neshma

    2010-01-01

    The formation of single phase nanoparticles of spinel structured ferrite, SnFe 2 O 4 , by mechanochemical syntheses using HEBM of stoichiometric amounts of solid SnO and α-Fe 2 O 3 with acetone as surfactant was achieved progressively as function of ball milling time. Single phase SnFe 2 O 4 formation commenced from five hours of continuous ball milling, and reached completion after 22 hours, thereby yielding a material with a lattice parameter of 8.543 A, and particle size of 10.91 nm. The coercivity was 4.44 mT, magnetic saturation value of 17.75 Am 2 /kg, and remanent magnetizations of 1.50 Am 2 /kg, correspondingly. The nanosized particles exhibited superparamagnetic behavior phenomenon based on Moessbauer spectroscopy measurements. The kinetic analyses based on the modified Kissinger method yielded four characteristic stages during the thermal evolution of the 22 hours milled state with activation energies of 0.23 kJ/mol, 2.52 kJ/mol, 0.024 kJ/mol, and 1.57 kJ/mol respectively.

  1. Photocatalytic reduction of Cr(VI) on the new hetero-system CuAl{sub 2}O{sub 4}/TiO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Gherbi, R. [Laboratory of Reaction Engineering, Faculty of Mechanic and Engineering Processes, USTHB, BP 32, 16111 Algiers (Algeria); Nasrallah, N. [Laboratory of Reaction Engineering, Faculty of Mechanic and Engineering Processes, USTHB, BP 32, 16111 Algiers (Algeria); Equipe chimie et Ingenierie des procedes, UMR CNRS 6226, E.N.S.C.R., Avenue du General Leclerc, CS 50837, 35708 Rennes Cedex 7 (France); Amrane, A. [Equipe chimie et Ingenierie des procedes, UMR CNRS 6226, E.N.S.C.R., Avenue du General Leclerc, CS 50837, 35708 Rennes Cedex 7 (France); Maachi, R. [Laboratory of Reaction Engineering, Faculty of Mechanic and Engineering Processes, USTHB, BP 32, 16111 Algiers (Algeria); Trari, M., E-mail: solarchemistry@gmail.com [Laboratory of Storage and Valorization of Renewable Energies, Faculty of Chemistry, USTHB, BP 32, 16111 Algiers (Algeria)

    2011-02-28

    Visible light driven HCrO{sub 4}{sup -} reduction was successfully achieved over the new hetero-system CuAl{sub 2}O{sub 4}/TiO{sub 2}. The spinel, elaborated by nitrate route, was characterized photo electrochemically. The optical gap was found to be 1.70 eV and the transition is directly allowed. The conduction band (-1.05 V{sub SCE}) is located below that of TiO{sub 2}, more negative than the HCrO{sub 4}{sup -}/Cr{sup 3+} level (+0.58 V{sub SCE}) yielding a thermodynamically feasible chromate reduction upon visible illumination. CuAl{sub 2}O{sub 4} is stable against photo corrosion by holes consumption reaction involving salicylic acid which favors the charges separation. There is a direct correlation between the dark adsorption and the photo activity. A reduction of more than 95% of chromate was achieved after 3 h irradiation at pH 2 with an optimal mass ratio (CuAl{sub 2}O{sub 4}/TiO{sub 2}) equal to 1/3. The reduction follows a first order kinetic with a half life of {approx}1 h and a quantum yield of 0.11% under polychromatic light. Prolonged illumination was accompanied by a deceleration of the Cr(VI) reduction thanks to the competitive water discharge. The hydrogen evolution, an issue of energetic concern, took place with a rate of 3.75 cm{sup 3} (g catalyst){sup -1} h{sup -1}.

  2. Elucidation of structural, vibrational and dielectric properties of transition metal (Co2+) doped spinel Mg-Zn chromites

    Science.gov (United States)

    Choudhary, Pankaj; Varshney, Dinesh

    2018-05-01

    Co2+ doped Mg-Zn spinel chromite compositions Mg0.5Zn0.5-xCoxCr2O4 (0.0 ≤ x ≤ 0.5) have been synthesized by the high-temperature solid state method. Synchrotron and X-ray diffraction (XRD) studies show single-phase crystalline nature. The structural analysis is validated by Rietveld refinement confirms the cubic structure with space group Fd3m. Crystallite size is estimated from Synchrotron XRD which was found to be 30-34 nm. Energy dispersive analysis confirms stoichiometric Mg0.5Zn0.5-xCoxCr2O4 composition. Average crystallite size distribution is estimated from imaging software (Image - J) of SEM is in the range of 100-250 nm. Raman spectroscopy reveals four active phonon modes, and a pronounced red shift is due to enhanced Co2+ concentration. Increased Co2+ concentration in Mg-Zn chromites shows a prominent narrowing of band gap from 3.46 to 2.97 eV. The dielectric response is attributed to the interfacial polarization, and the electrical modulus study supports non-Debye type of dielectric relaxation. Ohmic junctions (minimum potential drop) at electrode interface are active at lower levels of doping (x transformer applications at high frequencies.

  3. Chemical, structural, and electrochemical characterization of 5 V spinel and complex layered oxide cathodes of lithium ion batteries

    Science.gov (United States)

    Tiruvannamalai Annamalai, Arun Kumar

    2007-12-01

    Lithium ion batteries have revolutionized the portable electronics market since their commercialization first by Sony Corporation in 1990. They are also being intensively pursued for electric and hybrid electric vehicle applications. Commercial lithium ion cells are currently made largely with the layered LiCoO 2 cathode. However, only 50% of the theoretical capacity of LiCoO 2 can be utilized in practical cells due to the chemical and structural instabilities at deep charge as well as safety concerns. These drawbacks together with the high cost and toxicity of Co have created enormous interest in alternative cathodes. In this regard, spinel LiMn2O4 has been investigated widely as Mn is inexpensive and environmentally benign. However, LiMn 2O4 exhibits severe capacity fade on cycling, particularly at elevated temperatures. With an aim to overcome the capacity fading problems, several cationic substitutions to give LiMn2-yMyO 4 (M = Cr, Fe, Co, Ni, and Cu) have been pursued in the literature. Among the cation-substituted systems, LiMn1.5Ni0.5O 4 has become attractive as it shows a high capacity of ˜ 130 mAh/g (theoretical capacity: 147 mAh/g) at around 4.7 V. With an aim to improve the electrochemical performance of the 5 V LiMn 1.5Ni0.5O4 spinel oxide, various cation-substituted LiMn1.5-yNi0.5-zMy+zO4 (M = Li, Mg, Fe, Co, and Zn) spinel oxides have been investigated by chemical lithium extraction. The cation-substituted LiMn1.5-yNi0.5-zM y+zO4 spinel oxides exhibit better cyclability and rate capability in the 5 V region compared to the unsubstituted LiMn1.5Ni 0.5O4 cathodes although the degree of manganese dissolution does not vary significantly. The better electrochemical properties of LiMn 1.5-yNi0.5-zMy+zO4 are found to be due to a smaller lattice parameter difference among the three cubic phases formed during the charge-discharge process. In addition, while the spinel Li1-xMn1.58Ni0.42O4 was chemically stable, the spinel Li1-xCo2O4 was found to exhibit both

  4. Structural and physical property study of sol-gel synthesized CoFe2-xHoxO4 nano ferrites

    Science.gov (United States)

    Patankar, K. K.; Ghone, D. M.; Mathe, V. L.; Kaushik, S. D.

    2018-05-01

    CoFe2-xHoxO4 (x = 0.00, 0.05, 0.10, 0.15, 0.20) ferrites were prepared by the suitably modified Sol-Gel technique. X-ray diffraction (XRD) analysis revealed that the substituted samples show phase pure formation till 10% substitution, which is far higher phase pure than the earlier reports. Upon further substitution an inevitable secondary phase of HoFeO3 along with the spinel phase despite regulating synthesis parameters in the sol-gel reaction route. These results are further corroborated more convincingly by room temperature neutron diffraction. Morphological features of the ferrites were studied by Scanning Electron Microscopy (SEM). The magnetic parameters viz. the saturation magnetization (Ms), coercivity (Hc) and remanence (Mr) were determined from room temperature isothermal magnetization. These parameters were found to decrease with increase in Ho substitution. The decrease in magnetization is analyzed in the light of exchange interactions between rare earth and transition metal ions. Magnetostriction measurements revealed interesting results and the presence of a secondary phase was found to be responsible for decreased measu-red magnetostriction values. The solubility limit of Ho in CoFe2O4 lattice is also reflected from the X-ray and neutron diffraction analysis and magnetostriction studies.

  5. Some clues about the interphase reaction between ZnO and MnO2 oxides

    International Nuclear Information System (INIS)

    Rubio-Marcos, F.; Quesada, A.; Garcia, M.A.; Banares, M.A.; Fierro, J.L.G.; Martin-Gonzalez, M.S.; Costa-Kraemer, J.L.; Fernandez, J.F.

    2009-01-01

    Raman spectroscopy is used to evidence both the nature of the interphase reaction between ZnO and MnO 2 particles and its kinetic evolution. Zn cations migrate from the ZnO grains during oxygen vacancies formation process and diffuse into the MnO 2 particles leading to an interphase region with an intermediate valence Mn +3 -O-Mn +4 . Large amounts of desorbed Zn cations promote the formation of ZnMn 2 O 4 structure, in addition to the intermediate valence state. The system evolves towards complete formation of the spinel phase at higher thermal treatment times. The reactivity of the ZnO plays an important role in the formation of this interphase. Low-reactivity ZnO powder, in which the oxygen vacancies are previously produced, shows a stabilization of the intermediate valence state with very limited formation of the spinel phase. A clear correlation between the amount of the intermediate state interphase and the magnetic properties has been established. - Graphical abstract: Recently new room temperature interphase magnetism has been reported to appear in ZnO-MnO 2 system. Raman spectroscopy is used to evidence both the nature of the interphase reaction and the kinetic. The interphase evolved towards complete formation of the spinel phase. The reactivity of the ZnO plays an important role in the formation of this interphase. Finally, a clear correlation between the amount of the intermediate valence state and the interphase magnetic properties has been established.

  6. Rapid and efficient visible light photocatalytic dye degradation using AFe2O4 (A = Ba, Ca and Sr) complex oxides

    International Nuclear Information System (INIS)

    Vijayaraghavan, T.; Suriyaraj, S.P.; Selvakumar, R.; Venkateswaran, R.; Ashok, Anuradha

    2016-01-01

    Highlights: • Alkaline earth ferrites AFe 2 O 4 (A = Ba, Ca and Sr) were synthesized by sol–gel method. • Visible light photocatalytic activity of these ferrites were studied using congo red dye degradation. • BaFe 2 O 4 exhibited the best photocatalytic activity under visible light (xenon lamp) irradiation; CaFe 2 O 4 was the best photocatalyst under natural sun light irradiation. - Abstract: Photocatalytic activity of spinel type complex oxides has been investigated in this study. Alkaline earth ferrites AFe 2 O 4 (A = Ba, Ca, Sr) were synthesized by sol–gel method. Structural characterizations reveal that the synthesized ferrites have orthorhombic crystal structures with different space groups and cell dimensions when they have different alkaline earth metals in their A site. All the synthesized ferrites exhibited their bandgap in the range 2.14–2.19 eV. Their photocatalytic activities were studied using congo red dye under sunlight and xenon lamp radiation. The substitution of Ba, Ca and Sr at A site of these ferrites had varying impact on dye degradation process. Under xenon lamp irradiation, BaFe 2 O 4 exhibited the highest percentage of dye degradation (92% after 75 min). However, CaFe 2 O 4 showed the fastest degradation of the dye (70% within 15 min). In the absence of irradiation, SrFe 2 O 4 showed the highest dye adsorption (44% after 75 min).

  7. Enhanced electrochemical performance of LiMn2O4 by constructing a stable Mn2+-rich interface

    Science.gov (United States)

    Lu, Zhongpei; Lu, Xiaojun; Ding, Jingjing; Zhou, Ting; Ge, Tao; Yang, Gang; Yin, Fan; Wu, Mingfang

    2017-12-01

    Spinel LiMn2O4 has drawn continuous attentions due to its low cost, good electrochemical performance, environmental friendliness and natural abundant resources. In view of its severe capacity fading, some types of manganese-based compounds with different Mn oxidation states are selected to protect bare LiMn2O4 by constructing a stable coating layer. In this work, LiMn2O4@LiMnPO4 composite, spherical LiMn2O4 (LMO) as core and Mn2+-rich phase of LiMnPO4 (LMP) as shell, is designed and synthesized. Two composites of LiMn2O4 particles coated with 3 wt% and 10 wt% LiMnPO4 have been compared studied. After 100 cycles at 0.5C rate, the two samples deliver capacity retentions of 96.63% and 93.23% of their initial capacities. Moreover, LMO coated by 3 wt% LiMnPO4 delivers 100.3 mAh g-1 after 200 cycles at 10C rate and 76.3 mAh g-1 after 1000 cycles at 20C rate, much higher than bare LiMn2O4 with 90 mAh g-1 and 45.8 mAh g-1, respectively. This core-shell structure with Mn2+-rich phase as a coating layer effectively enhance the material's cycling performance and rate capacity by reducing the contact of LiMn2O4 with electrolyte.

  8. Improved electrochemical performances of oxygen plasma treated LiMn2O4 thin films

    International Nuclear Information System (INIS)

    Chen, C C; Chiu, K-F; Lin, K M; Lin, H C; Yang, C-R; Wang, F M

    2007-01-01

    LiMn 2 O 4 spinel thin films were deposited by radio frequency (rf) magnetron sputtering followed by annealing at 600 0 C in air.The films were then post-treated with an rf driven oxygen plasma. The crystallization and surface morphology of LiMn 2 O 4 thin films were seen to change with rf power. The treated samples were tested under harsh conditions such as deep discharge to 1.5 V and cycling at elevated temperature of 60 0 C to verify the electrochemical performances of LiMn 2 O 4 cathodes. The oxygen plasma treatments improved the electrochemical properties of LiMn 2 O 4 thin films significantly. As the cells were cycled in the range of 4.5-2.0 V at 60 0 C, the samples treated at a proper rf power of 50 W exhibited an initial capacity greater than ∼400 mAh g -1 with reasonable cycling stability. The results were attributed to the change of morphology and the formation of a surface layer induced by the oxygen plasma irradiation

  9. Electronic and optical properties of the SiB{sub 2}O{sub 4} (B=Mg, Zn, and Cd) spinel oxides: An ab initio study with the Tran–Blaha-modified Becke–Johnson density functional

    Energy Technology Data Exchange (ETDEWEB)

    Allali, D. [Laboratory for Developing New Materials and their Characterization, University of Setif 1, 19000 Setif (Algeria); Bouhemadou, A., E-mail: a_bouhemadou@yahoo.fr [Laboratory for Developing New Materials and their Characterization, University of Setif 1, 19000 Setif (Algeria); Safi, E. Muhammad Abud Al [Department of Physics and Astronomy, College of Science, King Saud University, P.O. Box 2455, Riyadh 11451 (Saudi Arabia); Bin-Omran, S. [Department of Physics and Astronomy, College of Science, King Saud University, P.O. Box 2455, Riyadh 11451 (Saudi Arabia); Department of Physics, Faculty of Science and Humanitarian Studies, Salman Bin Abdalaziz University, Alkharj 11942 (Saudi Arabia); Chegaar, M. [Department of Physics, Faculty of Science, University of Setif 1, 19000 Setif (Algeria); Khenata, R. [Laboratoire de Physique Quantique et de Modélisation Mathématique (LPQ3M), Département de Technologie, Université de Mascara, 29000 Mascara (Algeria); Reshak, A.H. [New Technologies-Research Center, University of West Bohemia, Univerzitni 8, 306 14 Pilson (Czech Republic); Center of Excellence Geopolymer and Green Technology, School of Material Engineering, University Malaysia Perlis, 01007 Kangar, Perlis (Malaysia)

    2014-06-15

    We report ab initio density functional theory calculations of the structural, electronic and optical properties of the spinel oxides SiMg{sub 2}O{sub 4}, SiZng{sub 2}O{sub 4}, and SiCd{sub 2}O{sub 4} using the full-potential linearized augmented plane-wave method. The structural parameters calculated using both the local density and generalized gradient approximations to the exchange-correlation potential are consistent with the literature data. To calculate the electronic properties, the exchange-correlation potential is treated with various functionals, and we find that the newly developed Tran–Blaha-modified Becke–Johnson functional significantly improves the band gap. We predict a direct band gap in all of the considered SiB{sub 2}O{sub 4} compounds, and the band gaps continuously decrease as the atomic size of the B element increases. The decrease in the fundamental direct band gap (Γ–Γ) from SiMg{sub 2}O{sub 4} to SiZn{sub 2}O{sub 4} to SiCd{sub 2}O{sub 4} can be attributed to p–d mixing in the upper valence bands of SiZn{sub 2}O{sub 4} and SiCd{sub 2}O{sub 4}. The lowest conduction band is well dispersive, similar to that found for transparent conducting oxides such as ZnO. This band is mainly defined by the s and p electrons of the Si and B (B=Mg, Zn, Cd) atoms. The topmost valence band is considerably less dispersive and is defined by O-2p and B–d electrons. The charge-carrier effective masses are evaluated at the topmost valence band and at the bottommost conduction band that were calculated. The frequency-dependent complex dielectric function, absorption coefficient, refractive index, extinction coefficient, reflectivity and electron energy loss function were estimated. We find that the value of the zero-frequency limit of the dielectric function ε(0) increases as the band gap decreases. The origins of the peaks and structures in the optical spectra are determined in terms of the calculated energy band structures.

  10. Preparation and characterization of self-assembled percolative BaTiO3–CoFe2O4 nanocomposites via magnetron co-sputtering

    Directory of Open Access Journals (Sweden)

    Qian Yang

    2014-04-01

    Full Text Available BaTiO3–CoFe2O4 composite films were prepared on (100 SrTiO3 substrates by using a radio-frequency magnetron co-sputtering method at 750 °C. These films contained highly (001-oriented crystalline phases of perovskite BaTiO3 and spinel CoFe2O4, which can form a self-assembled nanostructure with BaTiO3 well-dispersed into CoFe2O4 under optimized sputtering conditions. A prominent dielectric percolation behavior was observed in the self-assembled nanocomposite. Compared with pure BaTiO3 films sputtered under similar conditions, the nanocomposite film showed higher dielectric constants and lower dielectric losses together with a dramatically suppressed frequency dispersion. This dielectric percolation phenomenon can be explained by the 'micro-capacitor' model, which was supported by measurement results of the electric polarization and leakage current.

  11. The MgO-Al2O3-SiO2 system - Free energy of pyrope and Al2O3-enstatite. [in earth mantle formation

    Science.gov (United States)

    Saxena, S. K.

    1981-01-01

    The model of fictive ideal components is used to determine Gibbs free energies of formation of pyrope and Al2O3-enstatite from the experimental data on coexisting garnet and orthopyroxene and orthopyroxene and spinel in the temperature range 1200-1600 K. It is noted that Al2O3 forms an ideal solution with MgSiO3. These thermochemical data are found to be consistent with the Al2O3 isopleths that could be drawn using most recent experimental data and with the reversed experimental data on the garnet-spinel field boundary.

  12. Effect of Cu-doping on structural and electrical properties of Ni0.4-xCu0.3+xMg0.3Fe2O4 ferrites prepared using sol-gel method

    Science.gov (United States)

    Dhaou, Mohamed Houcine

    2018-06-01

    Ni0.4-xCu0.3+xMg0.3Fe2O4 spinel ferrites were prepared by sol-gel technique. X-ray diffraction results indicate that ferrite samples have a cubic spinel-type structure with ? space group. The electrical properties of the studied samples using complex impedance spectroscopy technique have been investigated as a function of frequency at different temperatures. We found that the addition of copper in Ni0.4-xCu0.3+xMg0.3Fe2O4 ferrite system can improve its conductivity. Dielectric properties have been discussed in terms of hopping of charge carriers between Fe2+ and Fe3+ ions. For all samples, frequency dependence of the imaginary part of impedance (Z") shows the existence of relaxation phenomenon. The appropriate equivalent circuit configuration for modeling the Nyquist plots of impedance is of the type of (Rg + Rgb//Cgb).

  13. Modified structural and magnetic properties of nanocrystalline MnFe{sub 2}O{sub 4} by pH in capping agent free co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Iranmanesh, P., E-mail: p.iranmanesh@vru.ac.ir [Department of Physics, Vali-e-Asr University of Rafsanjan, 77139-36417 Rafsanjan (Iran, Islamic Republic of); Saeednia, S. [Department of Chemistry, Vali-e-Asr University of Rafsanjan, 77139-36417 Rafsanjan (Iran, Islamic Republic of); Mehran, M.; Dafeh, S. Rashidi [Department of Physics, Vali-e-Asr University of Rafsanjan, 77139-36417 Rafsanjan (Iran, Islamic Republic of)

    2017-03-01

    Nano-sized manganese ferrite (MnFe{sub 2}O{sub 4}) particles were prepared using co-precipitation method in two different pH (9 and 11). The structural, morphological, optical and magnetic properties of as-synthesized nanoparticles were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM), UV–vis absorption and vibrating sample magnetometer (VSM). The FTIR spectra revealed two strong peaks at about 600 and 400 cm{sup −1} that can be attributed to the vibration mode of octahedral and tetrahedral sites of spinel structure of MnFe{sub 2}O{sub 4}, respectively. The XRD results showed that the nanocrystalline MnFe{sub 2}O{sub 4} has pure cubic spinel crystal structure with average crystallite size of 11 nm. The cation distribution of these nanoparticles was estimated by X-ray analysis data. The blue shift was observed in the band gap when compared with bulk sample which is due to the quantum size effect. The absence of hysteresis for MnFe{sub 2}O{sub 4} nanoparticles indicated the superparamagnetic behaviour, as expected for single domain nanoparticles. The obtained value for saturation magnetization being less than its value of bulk ones and larger pH is due to surface effects. The calculated magnetic particle size was smaller than crystallite size estimated from the XRD results; which indicate the presence of dead layer on particle surface. - Highlights: • We study effect of pH on the size and magnetic properties of MnFe{sub 2}O{sub 4} nanoparticles. • MnFe{sub 2}O{sub 4} were synthesized by co-precipitation method without any capping agent. • The physical properties are affected by cation contribution and surface effects. • The smaller nanoparticles with larger pH show a red shift in the band gap energy. • The M{sub s} is less than its value of bulk ones due to surface effects.

  14. Electrospun PVDF fibers and a novel PVDF/CoFe2O4 fibrous composite as nanostructured sorbent materials for oil spill cleanup

    Science.gov (United States)

    Dorneanu, Petronela Pascariu; Cojocaru, Corneliu; Olaru, Niculae; Samoila, Petrisor; Airinei, Anton; Sacarescu, Liviu

    2017-12-01

    In this work, pure polyvinylidene fluoride (PVDF) and PVDF/cobalt ferrite (CoFe2O4) magnetic fibrous composite were successfully prepared by electrospinning method for oil spill sorption applications. The pure spinel phase of CoFe2O4 and PVDF/CoFe2O4 composites were confirmed by X-ray diffraction analysis (XRD). Electrospun sorbent materials were characterized by scanning and transmission electron microscopy (SEM and TEM) as well as by contact angle measurements. In addition, the composite sorbent (PVDF/CoFe2O4) was characterized by magnetic measurements. It revealed good magnetic properties that are of real interest to facilitate the separation of the oil-loaded sorbent under the external magnetic field. Finally, the produced electrospun sorbents were tested for sorption of oily liquids, such as: decane, dodecane and commercial motor oils. We obtained good oil sorption capacity (between 9.751-23.615 g/g of pure PVDF) and (8.133-18.074 g/g for the magnetic composite) depending on the nature of oil tested. The present electrospun magnetic PVDF/CoFe2O4 fibrous composite could be potentially useful for the efficient removal of oil in water and recovery of sorbent material.

  15. Vibrational spectra of Cs2Cu(SO4)2·6H2O and Cs2Cu(SeO4)2·nH2O (n = 4, 6) with a crystal structure determination of the Tutton salt Cs2Cu(SeO4)2·6H2O

    Science.gov (United States)

    Wildner, M.; Marinova, D.; Stoilova, D.

    2016-02-01

    The solubility in the three-component systems Cs2SO4-CuSO4-H2O and Cs2SeO4-CuSeO4-H2O have been studied at 25 °C. The experimental results show that double salts, Cs2Cu(SO4)2·6H2O and Cs2Cu(SeO4)2·4H2O, crystallize from the ternary solutions within large concentration ranges. Crystals of Cs2Cu(SeO4)2·6H2O were synthesized at somewhat lower temperatures (7-8 °C). The thermal dehydration of the title compounds was studied by TG, DTA and DSC methods and the respective dehydration schemes are proposed. The calculated enthalpies of dehydration (ΔHdeh) have values of: 434.2 kJ mol-1 (Cs2Cu(SeO4)2·6H2O), 280.9 kJ mol-1 (Cs2Cu(SeO4)2·4H2O), and 420.2 kJ mol-1 (the phase transition of Cs2Cu(SO4)2·6H2O into Cs2Cu(SO4)2·H2O). The crystal structure of Cs2Cu(SeO4)2ṡ6H2O was determined from single crystal X-ray diffraction data. It belongs to the group of Tutton salts, crystallizing isotypic to the respective sulfate in a monoclinic structure which is characterized by isolated Cu(H2O)6 octahedra and SeO4 tetrahedra, interlinked by hydrogen bonds and [9]-coordinated Cs+ cations. Infrared spectra of the cesium copper compounds are presented and discussed with respect to both the normal modes of the tetrahedral ions and the water molecules. The analysis of the infrared spectra of the double compounds reveals that the distortion of the selenate tetrahedra in Cs2Cu(SeO4)2·4H2O is stronger than those in Cs2Cu(SeO4)2·6H2O in agreement with the structural data. Matrix-infrared spectroscopy was applied to confirm this claim - Δν3 for SO4 2 - ions matrix-isolated in Cs2Cu(SeO4)2·6H2O has a value of 35 cm-1 and that of the same ions included in Cs2Cu(SeO4)2·4H2O - 84 cm-1. This spectroscopic finding is due to the formation of strong covalent bands Cu-OSO3 on one hand, and on the other to the stronger deformation of the host SeO4 2 - tetrahedra in Cs2Cu(SeO4)2·4H2O as compared to those in Cs2Cu(SeO4)2·6H2O. The strength of the hydrogen bonds as deduced from the

  16. Characterization of MgMnxFe2-xO4 as a possible cathode material for electrochemical reduction of NOx

    DEFF Research Database (Denmark)

    Bræstrup, Frantz Radzik; Kammer Hansen, Kent

    2009-01-01

    Spinel-type oxides of MgMn x Fe2−x O4, x = 0.0, 0.2, 0.4, 0.6, 0.8, 1.0, were synthesized as a solid state reaction and characterized with dilatometry and resistivity measurements up to 1000 °C. Results showed a general decrease of the linear expansion and an increase in conductivity as a function...

  17. Formation of the ZnFe{sub 2}O{sub 4} phase in an electric arc furnace off-gas treatment system

    Energy Technology Data Exchange (ETDEWEB)

    Suetens, T., E-mail: thomas.suetens@mtm.kuleuven.be; Guo, M., E-mail: muxing.guo@mtm.kuleuven.be; Van Acker, K., E-mail: karel.vanacker@lrd.kuleuven.be; Blanpain, B., E-mail: bart.blanpain@mtm.kuleuven.be

    2015-04-28

    Highlights: • EAF dust was characterized with particle size analysis, XRF, and EPMA. • Slag particles showed no sign of reaction with Zn vapor. • Fe{sub 2}O{sub 3} particles showed different degrees of reaction based on their size. • The thermodynamic stability of Zn vapor in EAF off-gas ducts was reevaluated. • In presence of Fe{sub 2}O{sub 3}, Zn vapor reacts to form ZnFe{sub 2}O{sub 4} and ZnO. - Abstract: To better understand the phenomena of ZnFe{sub 2}O{sub 4} spinel formation in electric arc furnace dust, the dust was characterized with particle size analysis, X-ray fluorescence (XRF), electron backscatter diffraction (EBSD), and electron probe micro-analysis (EPMA). Different ZnFe{sub 2}O{sub 4} formation reaction extents were observed for iron oxide particles with different particle sizes. ZnO particles were present as both individual particles and aggregated on the surface of larger particles. Also, the slag particles found in the off-gas were shown not to react with the zinc vapor. After confirming the presence of a ZnFe{sub 2}O{sub 4} formation reaction, the thermodynamic feasibility of in-process separation – a new electric arc furnace dust treatment technology – was reevaluated. The large air intake and the presence of iron oxide particles in the off-gas were included into the thermodynamic calculations. The formation of the stable ZnFe{sub 2}O{sub 4} spinel phase was shown to be thermodynamically favorable in current electric arc furnace off-gas ducts conditions even before reaching the post combustion chamber.

  18. High-pressure phase transition and properties of spinel ZnMn2O4

    DEFF Research Database (Denmark)

    Åbrink, S.; Waskowska, A.; Gerward, Leif

    1999-01-01

    to normal pressure. The c/a ratio reduces from 1.62 to 1.10 above P-c and remains nearly pressure independent in the high-pressure phase. The transition is attributed to the changes in electron configuration of the Mn3+ ions. According to the crystal field theory, the e(g) electron of octahedrally......-pressure behavior of ZnMn2O4 was investigated up to 52 GPa using the energy-dispersive x-ray diffraction technique and synchrotron radiation. The structural first-order phase transition from the body-centered to primitive-tetragonal cell takes place at P-c = 23 GPa. The high-pressure phase is metastable down...... coordinated Mn3+ is either in the d(z)(2) orbital or in the d(x2-y2). In the first configuration the MnO6 octahedron will be elongated and this is the case at normal pressure, while the second configuration gives the flattened octahedron. In the high-pressure phase some proportion of the e(g) electrons...

  19. Microstructure and magnetic properties of MFe{sub 2}O{sub 4} (M = Co, Ni, and Mn) ferrite nanocrystals prepared using colloid mill and hydrothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Wei, E-mail: wangwei@mail.buct.edu.cn; Ding, Zui; Zhao, Xiruo [State Key Laboratory of Chemical Resource Engineering and School of Science, Beijing University of Chemical Technology, Beijing 100029 (China); Beijing Key Laboratory of Environmentally Harmful Chemical Analysis, Beijing University of Chemical Technology, Beijing 100029 (China); Wu, Sizhu [State Key Laboratory of Organic–Inorganic Composites, Beijing University of Chemical Technology, Beijing 100029 (China); Li, Feng [State Key Laboratory of Chemical Resource Engineering and School of Science, Beijing University of Chemical Technology, Beijing 100029 (China); Yue, Ming [College of Materials Science and Engineering, Beijing University of Technology, Beijing 100022 (China); Liu, J. Ping [Department of Physics, University of Texas at Arlington, Arlington, Texas 76019 (United States)

    2015-05-07

    Three kinds of spinel ferrite nanocrystals, MFe{sub 2}O{sub 4} (M = Co, Ni, and Mn), are synthesized using colloid mill and hydrothermal method. During the synthesis process, a rapid mixing and reduction of cations with sodium borohydride (NaBH{sub 4}) take place in a colloid mill then through a hydrothermal reaction, a slow oxidation and structural transformation of the spinel ferrite nanocrystals occur. The phase purity and crystal lattice parameters are estimated by X-ray diffraction studies. Scanning electron microscopy and transmission electron microscopy images show the morphology and particle size of the as-synthesized ferrite nanocrystals. Raman spectrum reveals active phonon modes at room temperature, and a shifting of the modes implies cation redistribution in the tetrahedral and octahedral sites. Magnetic measurements show that all the obtained samples exhibit higher saturation magnetization (M{sub s}). Meanwhile, experiments demonstrate that the hydrothermal reaction time has significant effects on microstructure, morphologies, and magnetic properties of the as-synthesized ferrite nanocrystals.

  20. Micromagnetic simulations of spinel ferrite particles

    International Nuclear Information System (INIS)

    Dantas, Christine C.; Gama, Adriana M.

    2010-01-01

    This paper presents the results of simulations of the magnetization field ac response (at 2-12 GHz) of various submicron ferrite particles (cylindrical dots). The ferrites in the present simulations have the spinel structure, expressed here by M 1 - n Zn n Fe 2 O 4 (where M stands for a divalent metal), and the parameters chosen were the following: (a) for n=0: M={Fe, Mn, Co, Ni, Mg, Cu }; (b) for n=0.1: M = {Fe, Mg} (mixed ferrites). These runs represent full 3D micromagnetic (one-particle) ferrite simulations. We find evidences of confined spin waves in all simulations, as well as a complex behavior nearby the main resonance peak in the case of the M = {Mg, Cu} ferrites. A comparison of the n=0 and n=0.1 cases for fixed M reveals a significant change in the spectra in M = Mg ferrites, but only a minor change in the M=Fe case. An additional larger scale simulation of a 3 by 3 particle array was performed using similar conditions of the Fe 3 O 4 (magnetite; n=0, M = Fe) one-particle simulation. We find that the main resonance peak of the Fe 3 O 4 one-particle simulation is disfigured in the corresponding 3 by 3 particle simulation, indicating the extent to which dipolar interactions are able to affect the main resonance peak in that magnetic compound.

  1. Optical properties of Ni-doped MgGa2O4 single crystals grown by floating zone method

    International Nuclear Information System (INIS)

    Suzuki, Takenobu; Hughes, Mark; Ohishi, Yasutake

    2010-01-01

    The single crystal growth conditions and spectroscopic characterization of Ni-doped MgGa 2 O 4 with inverse-spinel structure crystal family are described. Single crystals of this material have been grown by floating zone method. Ni-doped MgGa 2 O 4 single crystals have broadband fluorescence in the 1100-1600 nm wavelength range, 1.6 ms room temperature lifetime, 56% quantum efficiency and 1.05x10 -21 cm 2 stimulated emission cross section at the emission peak. This new material is very promising for tunable laser applications covering the important optical communication and eye safe wavelength region.

  2. Petrology of spinel lherzolite xenoliths in alkali basalts from Liri ...

    African Journals Online (AJOL)

    Al2O3), and Al-rich spinel occur in alkali basalts from Liri, South of the ... these spinel lherzolite xenoliths are reported, along with the analyses of ...... erupted in the Liri region. .... and temperatures with controlled activities of water, carbon.

  3. Dielectric relaxation behavior and impedance studies of Cu2+ ion doped Mg - Zn spinel nanoferrites

    Science.gov (United States)

    Choudhary, Pankaj; Varshney, Dinesh

    2018-03-01

    Cu2+ substituted Mg - Zn nanoferrites is synthesized by low temperature fired sol gel auto combustion method. The spinel nature of nanoferrites was confirmed by lab x-ray technique. Williamson - Hall (W-H) analysis estimate the average crystallite size (22.25-29.19 ± 3 nm) and micro strain induced Mg0.5Zn0.5-xCuxFe2O4 (0.0 ≤ x ≤ 0.5). Raman scattering measurements confirm presence of four active phonon modes. Red shift is observed with enhanced Cu concentration. Dielectric parameters exhibit a non - monotonous dispersion with Cu concentration and interpreted with the support of hopping mechanism and Maxwell-Wagner type of interfacial polarization. The ac conductivity of nanoferrites increases with raising the frequency. Complex electrical modulus reveals a non - Debye type of dielectric relaxation present in nanoferrites. Reactive impedance (Z″) detected an anomalous behavior and is related with resonance effect. Complex impedance demonstrates one semicircle corresponding to the intergrain (grain boundary) resistance and also explains conducting nature of nanoferrites. For x = 0.2, a large semicircle is observed revealing the ohmic nature (minimum potential drop at electrode surface). Dielectric properties were improved for nanoferrites with x = 0.2 and is due to high dielectric constant, conductivity and minimum loss value (∼0.009) at 1 MHz.

  4. Mechanistic studies of mercury adsorption and oxidation by oxygen over spinel-type MnFe{sub 2}O{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Yingju [State Key Laboratory of Coal Combustion, School of Energy and Power Engineering, Huazhong University of Science and Technology, Wuhan 430074 (China); Liu, Jing, E-mail: liujing27@mail.hust.edu.cn [State Key Laboratory of Coal Combustion, School of Energy and Power Engineering, Huazhong University of Science and Technology, Wuhan 430074 (China); Shenzhen Institute of Huazhong University of Science and Technology, Shenzhen 518000 (China); Zhang, Bingkai; Liu, Feng [State Key Laboratory of Coal Combustion, School of Energy and Power Engineering, Huazhong University of Science and Technology, Wuhan 430074 (China)

    2017-01-05

    Highlights: • Hg adsorption and oxidation mechanisms on MnFe{sub 2}O{sub 4} were studied using DFT method. • Hg{sup 0} adsorption on Mn-terminated MnFe{sub 2}O{sub 4} (100) surface is a chemisorption process. • HgO shows high chemical reactivity for its adsorption on MnFe{sub 2}O{sub 4} surface. • The reaction between adsorbed Hg and surface oxygen is the rate-determining step. - Abstract: MnFe{sub 2}O{sub 4} has been regarded as a very promising sorbent for mercury emission control in coal-fired power plants because of its high adsorption capacity, magnetic, recyclable and regenerable properties. First-principle calculations based on density functional theory (DFT) were used to elucidate the mercury adsorption and oxidation mechanisms on MnFe{sub 2}O{sub 4} surface. DFT calculations show that Mn-terminated MnFe{sub 2}O{sub 4} (1 0 0) surface is much more stable than Fe-terminated surface. Hg{sup 0} is physically adsorbed on Fe-terminated MnFe{sub 2}O{sub 4} (1 0 0) surface. Hg{sup 0} adsorption on Mn-terminated MnFe{sub 2}O{sub 4} (1 0 0) surface is a chemisorption process. The partial density of states (PDOS) analysis indicates that Hg atom interacts strongly with surface Mn atoms through the orbital hybridization. HgO is adsorbed on the MnFe{sub 2}O{sub 4} surface in a chemical adsorption manner. The small HOMO–LUMO energy gap implies that HgO molecular shows high chemical reactivity for HgO adsorption on MnFe{sub 2}O{sub 4} surface. The energy barriers of Hg{sup 0} oxidation by oxygen on Fe- and Mn-terminated MnFe{sub 2}O{sub 4} surfaces are 206.37 and 76.07 kJ/mol, respectively. Mn-terminated surface is much more favorable for Hg{sup 0} oxidation than Fe-terminated surface. In the whole Hg{sup 0} oxidation process, the reaction between adsorbed mercury and surface oxygen is the rate-determining step.

  5. Synthesis of high-surface-area spinel-type MgAl2O4 nanoparticles by

    Indian Academy of Sciences (India)

    2Institute of Chemical Technologies, Iranian Research Organization for Science and Technology, Tehran ... on synthesis and textural properties of magnesium aluminate nanopowders. .... −1 over temper- ature range of 10–900. ◦. C, in air atmosphere. XRD patterns ..... assigned to two phases of MgAl2O4 (JCPDS PDF no.

  6. Microstructure and Electrical Properties of Fe,Cu Substituted (Co,Mn)3O4 Thin Films

    DEFF Research Database (Denmark)

    Szymczewska, Dagmara; Molin, Sebastian; Hendriksen, Peter Vang

    2017-01-01

    In this work, thin films (~1000 nm) of a pure MnCo2O4 spinel together with its partially substituted derivatives (MnCo1.6Cu0.2Fe0.2O4, MnCo1.6Cu0.4O4, MnCo1.6Fe0.4O4) were prepared by spray pyrolysis and were evaluated for electrical conductivity. Doping by Cu increases the electrical conductivit...

  7. Synthesis, characterization and electrochemical performance of Al-substituted Li_2MnO_3

    International Nuclear Information System (INIS)

    Torres-Castro, Loraine; Shojan, Jifi; Julien, Christian M.; Huq, Ashfia; Dhital, Chetan; Paranthaman, Mariappan Parans; Katiyar, Ram S.; Manivannan, Ayyakkannu

    2015-01-01

    Graphical abstract: Comparison of the cycling performances for pure Li_2MnO_3 and Al-substituted Li_2MnO_3 compounds at a current density of 10 mAh g"−"1 for 100 cycles. Al-substitution increases the spinel phase and hence improves the cycling behavior. - Highlights: • Pure and Al-doped Li_2MnO_3 compounds were synthesized by a Pechini method. • Presence of monoclinic and spinel phases confirmed by Raman and Neutron diffraction. • Al substitution occurs at both Mn and Li sites in Li_2MnO_3 structure. • Al substitution reduces Mn valence state and promotes spinel phase formation. • Stable cycling capacity of 70 mAh g"−"1 was observed for nominal Li_0_._5Al_0_._5MnO_3. - Abstract: Li_2MnO_3 is known to be electrochemically inactive due to Mn in tetravalent oxidation state. Several compositions such as Li_2MnO_3, Li_1_._5Al_0_._1_7MnO_3, Li_1_._0Al_0_._3_3MnO_3 and Li_0_._5Al_0_._5MnO_3 were synthesized by a sol–gel Pechini method. All the samples were characterized with XRD, Raman, XPS, SEM, Tap density and BET analyzer. XRD patterns indicated the presence of monoclinic phase for pristine Li_2MnO_3 and mixed monoclinic/spinel phases (Li_2_−_xMn_1_−_yAl_x_+_yO_3_+_z) for Al-substituted Li_2MnO_3 compounds. The Al substitution seems to occur both at Li and Mn sites, which could explain the presence of spinel phase. XPS analysis for Mn 2p orbital reveals a significant decrease in binding energy for Li_1_._0Al_0_._3_3MnO_3 and Li_0_._5Al_0_._5MnO_3 compounds. Cyclic voltammetry, charge/discharge cycles and electrochemical impedance spectroscopy were also performed. A discharge capacity of 24 mAh g"−"1 for Li_2MnO_3, 68 mAh g"−"1 for Li_1_._5Al_0_._1_7MnO_3, 58 mAh g"−"1 for Li_1_._0Al_0_._3_3MnO_3 and 74 mAh g"−"1 for Li_0_._5Al_0_._5MnO_3 were obtained. Aluminum substitutions increased the formation of spinel phase which is responsible for cycling.

  8. Structure and electrochemical impedance of LiNi_xMn_2_-_xO_4

    International Nuclear Information System (INIS)

    Ta Anh Tan; Nguyen Si Hieu; Le Ha Chi; Pham Duy Long; Dang Tran Chien; Le Dinh Trong

    2016-01-01

    Ni-substitution spinel LiNi_xMn_2_-_xO_4 (x = 0, 0.1, 0.2) materials were synthesized by the sol--gel method. The structure and morphology of the samples were characterized by the X-ray diffraction (XRD) and the scanning electron microscopy. The ac conduction of the materials was investigated by electrochemical impedance spectroscopy (EIS) measurements. The refinement results showed that the substitution of Ni decreased the lattice constant and Mn--O distance, while increased Li--O bond length and 16c octahedral volume. The EIS results confirmed the decrease of conductivity with increasing Ni substitution content. Based on XRD and EIS results, the relationship between the crystal structure and electrochemical behavior of the materials was discussed and explained. (author)

  9. Phenomenological analysis of densification mechanism during spark plasma sintering of MgAl2O4

    Science.gov (United States)

    Bernard-Granger, Guillaume; Benameur, Nassira; Addad, Ahmed; Nygren, Mats; Guizard, Christian; Deville, Sylvain

    2009-05-01

    Spark plasma sintering (SPS) of MgAl2O4 powder was investigated at temperatures between 1200 and 1300{\\deg}C. A significant grain growth was observed during densification. The densification rate always exhibits at least one strong minimum, and resumes after an incubation period. Transmission electron microscopy investigations performed on sintered samples never revealed extensive dislocation activity in the elemental grains. The densification mechanism involved during SPS was determined by anisothermal (investigation of the heating stage of a SPS run) and isothermal methods (investigation at given soak temperatures). Grain-boundary sliding, accommodated by an in-series {interface-reaction/lattice diffusion of the O$^2$-anions} mechanism controlled by the interface-reaction step, governs densification. The zero-densification-rate period, detected for all soak temperatures, arise from the difficulty of annealing vacancies, necessary for the densification to proceed. The detection of atomic ledges at grain boundaries and the modification of the stoichiometry of spinel during SPS could be related to the difficulty to anneal vacancies at temperature soaks.

  10. Moessbauer studies of superexchange interactions in NiFe sub 2 O sub 4

    CERN Document Server

    Kim, S J; Kim, C S; Lee, S W

    2000-01-01

    NiFe sub 2 O sub 4 has been studied using Moessbauer spectroscopy and X-ray diffraction. The crystal was found to have a inverse cubic spinel structure with the lattice constant a sub 0 =8.326+-0.003 A. Moessbauer spectra of NiFe sub 2 O sub 4 was obtained at various absorber temperatures from 13 K to the Neel temperature. The Moessbauer spectra consisted of two sets of six lines corresponding to Fe sup + sup 3 at the tetrahedral (A) and the octahedral (B) sites. The temperature dependence of the magnetic hyperfine fields at sup 5 sup 7 Fe nuclei at the tetrahedral (A) and the octahedral (B) sites was analyzed by the Neel theory of ferrimagnetism. The intersublattice A-O-B and intrasublattice A-O-A superexchange interactions were found to be antiferromagnetic with strengths of J sub A sub - sub B =-25.0 k sub B and J sub A sub - sub A =-4.0 K sub B , respectively, while the intrasublattice B-O-B superexchange interaction is ferromagnetic with a strength J sub B sub - sub B =4.2 k sub B.

  11. Effect of Feed Melting, Temperature History and Minor Component Addition on Spinel Crystallization in High-Level Waste Glass

    International Nuclear Information System (INIS)

    Izak, Pavel; Hrma, Pavel R.; Arey, Bruce W.; Plaisted, Trevor J.

    2001-01-01

    This study was undertaken to help design mathematical models for high-level waste (HLW) glass melter that simulate spinel behavior in molten glass. Spinel, (Fe,Ni,Mn) (Fe,Cr)2O4, is the primary solid phase that precipitates from HLW glasses containing Fe and Ni in sufficient concentrations. Spinel crystallization affects the anticipated cost and risk of HLW vitrification. To study melting reactions, we used simulated HLW feed, prepared with co-precipitated Fe, Ni, Cr, and Mn hydroxides. Feed samples were heated up at a temperature-increase rate (4C/min) close to that which the feed experiences in the HLW glass melter. The decomposition, melting, and dissolution of feed components (such as nitrates, carbonates, and silica) and the formation of intermediate crystalline phases (spinel, sodalite (Na8(AlSiO4)6(NO2)2), and Zr-containing minerals) were characterized using evolved gas analysis, volume-expansion measurement, optical microscope, scanning electron microscope, thermogravimetric analysis, differential scanning calorimetry, and X-ray diffraction. Nitrates and quartz, the major feed components, converted to a glass-forming melt by 880C. A chromium-free spinel formed in the nitrate melt starting from 520C and Sodalite, a transient product of corundum dissolution, appeared above 600C and eventually dissolved in glass. To investigate the effects of temperature history and minor components (Ru,Ag, and Cu) on the dissolution and growth of spinel crystals, samples were heated up to temperatures above liquidus temperature (TL), then subjected to different temperature histories, and analyzed. The results show that spinel mass fraction, crystals composition, and crystal size depend on the chemical and physical makeup of the feed and temperature history

  12. Size-controlled synthesis of NiFe2O4 nanospheres via a PEG assisted hydrothermal route and their catalytic properties in oxidation of alcohols by periodic acid

    International Nuclear Information System (INIS)

    Paul, Bappi; Purkayastha, Debraj Dhar; Dhar, Siddhartha Sankar

    2016-01-01

    Graphical abstract: - Highlights: • Hydrothermal synthesis of NiFe 2 O 4 NPs with (C 4 H 9 ) 3 N as hydroxylating agent. • PEG 4000 was used as surfactant to control sizes of NPs. • The TEM images revealed the material to be spherical in shape with sizes 2–10 nm. • NiFe 2 O 4 was used as recyclable catalyst for oxidation of alcohols by periodic acid. - Abstract: A novel and facile approach for synthesis of spinel nickel ferrites (NiFe 2 O 4 ) nanoparticles (NPs) employing homogeneous chemical precipitation followed by hydrothermal heating is reported. The synthesis involves use of tributylamine (TBA) as a hydroxylating agent in synthesis of nickel ferrites. Polyethylene glycol (PEG) 4000 was used as surfactant. As-synthesized NiFe 2 O 4 NPs were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), N 2 adsorption–desorption isotherm (BET) and vibrating sample magnetometry (VSM). The XRD pattern revealed formation of cubic face-centered NiFe 2 O 4 and TEM image showed spherical particles of sizes 2–10 nm. These NiFe 2 O 4 NPs were used as magnetically recoverable catalyst in oxidation of cyclic alcohols to their corresponding aldehydes by periodic acid. This eco-friendly procedure affords products in very high yield and selectivity. The reusability of the catalyst is proved to be noteworthy as the material exhibits no significant changes in its catalytic activity even after five cycles of reuse.

  13. Synthesis and electrochemical properties of Li4Ti5O12

    CSIR Research Space (South Africa)

    Liu, GQ

    2011-06-01

    Full Text Available The spinel compound Li4Ti5O12 was synthesized by a solid state method. In this synthesizing process, anatase TiO2 and Li2CO3 were used as reactants. The influences of reaction temperature and calcination time on the properties of products were...

  14. Structural parameters and resistive switching phenomenon study on Cd0.25Co0.75Fe2O4 ferrite thin film

    International Nuclear Information System (INIS)

    Chhaya, U.V.; Gadhvi, M.R.; Mistry, B.V.; Bhavsar, K.H.; Joshi, U.S.; Lakhani, V.K.; Modi, K.B.

    2011-01-01

    Cadmium substituted cobalt ferrite thin film with nominal composition Cd 0.25 Co 0.75 Fe 2 O 4 , has been grown on quartz substrate by chemical solution deposition and their structural and electrical properties have been investigated. Grazing incidence X-ray diffraction (XRD) confirmed single phase spine) structure with nanometer grain size. Atomic force microscopic analysis revealed uniform nano structured growth of about 70 nm average crystallite size. The XRD data have been used to determine the distribution of cations among the tetrahedral and octahedral sites of the spinel lattice and various structural parameters. The cation distribution determined from X-ray diffraction line intensity calculations revealed, 60% octahedral sites occupancy of Cd 2+ -ions in the composition. Four terminal I-V measurements show hysteretic curves, suggesting high resistance state (HRS) and low resistance state (LRS) in the film with polarity dependence. Maximum resistance ratio, R high /R low of 57% was observed at room temperature in the Ag/Cd 0.25 Co 0.75 Fe 2 O 4 /Ag planar structure. Observed resistance switching is attributed to combined effects, viz., in the LRS, the major fraction of cadmium occupation and electron exchange between Fe 3+ and Fe 2+ at the B-sites, whereas the HRS shows Schottky-like conduction mechanism at the Ag/Cd 0.25 Co 0.75 Fe 2 O 4 interface. (author)

  15. Fuel effect on solution combustion synthesis of Co(Cr,Al)2O4 pigments

    International Nuclear Information System (INIS)

    Gilabert, J.; Palacios, M.D.; Sanz, V.; Mestre, S.

    2017-01-01

    The fuel effect on the synthesis of a ceramic pigment with a composition CoCr22ΨAl2ΨO4 (0≤Ψ≤1) by means of solution combustion synthesis process (SCS) has been studied. Three different fuels were selected to carry out the synthesis (urea, glycine and hexamethylentetramine (HMT)). Highly foamy pigments with very low density were obtained. Fd-3m spinel-type structure was obtained in all the experiments. Nevertheless, crystallinity and crystallite size of the spinels show significant differences with composition and fuel. The use of glycine along with the chromium-richest composition favours ion rearrangement to obtain the most ordered structure. Lattice parameter does not seem to be affected by fuel, although it evolves with Ψ according to Vegard's law. Colouring power in a transparent glaze shows important variations with composition. On the other hand, fuel effect presents a rather low influence since practically the same shades are obtained. However, it exerts certain effect on luminosity (L*). [es

  16. Sintering of (Ni,Mg)(Al,Fe)2O4 Materials and their Corrosion Process in Na3AlF6-AlF3-K3AlF6 Electrolyte

    Science.gov (United States)

    Xu, Yibiao; Li, Yawei; Yang, Jianhong; Sang, Shaobai; Wang, Qinghu

    2017-06-01

    The application of ledge-free sidewalls in the Hall-Héroult cells can potentially reduce the energy requirement of aluminum production by about 30 pct (Nightingale et al. in J Eur Ceram, 33:2761-2765, 2013). However, this approach poses great material challenges since such sidewalls are in direct contact with corrosive electrolyte. In the present paper, (Ni,Mg)(Al,Fe)2O4 materials were prepared using fused magnesia, reactive alumina, nickel oxide, and iron oxide powders as the starting materials. The sintering behaviors of specimens as well as their corrosion resistance to molten electrolyte have been investigated by means of X-ray diffraction and scanning electron microscope. The results show that after firing at temperature ranging from 1673 K (1400 °C) up to 1873 K (1600 °C), all the specimens prepared are composed of single-phase (Ni,Mg)(Al,Fe)2O4 composite spinel, the lattice parameter of which increases with increasing Fe3+ ion concentration. Increasing the iron oxide content enhances densification of the specimens, which is accompanied by the formation of homogeneously distributed smaller pores in the matrix. The corrosion tests show that corrosion layers consist of fluoride and Ni(Al,Fe)2O4 composite spinel grains are produced in specimens with Fe/Al mole ratio no more than 1, whereas dense Ni(Al,Fe)2O4 composite spinel layers are formed on the surface of the specimens with Fe/Al mole ratio more than 1. The dense Ni(Al,Fe)2O4 composite spinel layers formed improve the corrosion resistance of the specimens by inhibiting the infiltration of electrolyte and hindering the chemical reaction between the specimen and electrolyte.

  17. Growth and in-plane magnetic anisotropy of inverse spinel Co{sub 2}MnO{sub 4} thin films

    Energy Technology Data Exchange (ETDEWEB)

    Koo, Taeyeong; Kim, Jaeyeong [Pohang University of Science and Technology, Pohang (Korea, Republic of); Song, Jonghyun [Chungnam National University, Daejeon (Korea, Republic of)

    2014-11-15

    Epitaxial Co{sub 2}MnO{sub 4} thin films were grown on Nb(0.1wt.)-doped SrTiO{sub 3} single-crystal substrates with (100) and (110) crystal orientations by using pulsed laser deposition. Their crystal structures and magnetic properties were investigated. Both samples exhibited ferrimagnetic transitions with enhanced transition temperatures. Isotropic M-H loops were observed on the in-plane surface of Co{sub 2}MnO{sub 4}(00l) grown on Nb(0.1wt)-doped SrTiO{sub 3}(100). Strong magnetic anisotropy was observed on the in-plane surface for Co{sub 2}MnO{sub 4} (ll0) grown on Nb(0.1wt)-doped SrTiO{sub 3}(110). A magnetic easy axis existed along the elongated tetragonal direction. This was attributed to the strong interplay between the spin and lattice degrees of freedom in the Co{sub 2}MnO{sub 4} thin film.

  18. Correlação entre dados estruturais e bandas de vibração no infravermelho para a fase espinélio Zn7-xNi xSb2O12 Correlation between structural data and infraved vibrational bands of the Zn7-xNi xSb2O12 spinel phase

    Directory of Open Access Journals (Sweden)

    L. Gama

    2000-12-01

    Full Text Available A fase espinélio Zn7-xNi xSb2O12 tem apresentado propriedades magnéticas importantes, comportando-se como spin-glass. Desde que estas propriedades são fortemente dependentes da configuração precisa dos átomos nesta estrutura, foram utilizados neste trabalho, com o intuito de clarificar essa configuração, a espectroscopia de infravermelho, aliada ao refinamento de estruturas pelo método de Rietveld. O espectro de infravermelho mostra nas condições de contorno estudadas a presença de três das quatro bandas ativas comuns aos espinélios. Conforme resultados do refinamento pelo método de Rietveld, o níquel substitui o zinco primeiramente no sítio octaédrico e, em altas concentrações (x > ou = 3, migra para o sítio tetraédrico. Essa migração é indicada pelo "splitting", em torno de 520 cm-1, para (x > ou = 3, apresentado no espectro de infravermelho quando a banda n2 é afetada pela mudança do cátion bivalente.The Zn7-xNi xSb2O12 spinel phase shows important magnetic properties with a spin-glass behavior. As these properties are strongly dependent on the atomic configuration in the spinel structure, infrared spectroscopy and the structure refining by the Rietveld analysis have been studied. The infrared spectrum presents three to four of the common spinel active modes. The Rietveld analysis shows that Ni firstly substitutes for Zn in the octahedral site and, for large (x > or = 3 concentrations, migrates to the tetrahedral site. The indication of that migration is the splitting at approximately 520 cm-1, shown in the infrared spectrum when the nu 2 band is modified by the substitution of the divalent cation.

  19. Synthesis and Electrochemical Performance of LixMn2-yCoyO4-dCld Cathode Material

    Science.gov (United States)

    2016-06-13

    Synthesis and Electrochemical Performance of LixMn2-yCoyO4-dCld Cathode Material Terrill B. Atwater, Paula C. Latorre, and Ashley L. Ruth U.S...low toxicity, comparable capacity, and low cost. However, this spinel suffers from capacity fading due to fracturing of the cell structure...dopants of interest include compounds containing Group VIII Row 4 (Fe, Co, and Ni) elements, cobalt in particular. In addition to fabrication method

  20. Part II. Large scale applications of Ni{sub x}Mn{sub 0.8-x}Mg{sub 0.2}Fe{sub 2}O{sub 4}; 0.1 {<=} x {<=} 0.35 using laser irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Ahmed, M.A., E-mail: moala1947@yahoo.com [Materials Science. Lab (1), Physics Department, Faculty of Science, Cairo University, Giza (Egypt); Bishay, Samiha T. [Department of Physics, Faculty of Girls for Art, Science and Education, Ain Shams University, Cairo (Egypt); El-dek, S.I.; Omar, G. [Materials Science. Lab (1), Physics Department, Faculty of Science, Cairo University, Giza (Egypt)

    2011-07-28

    Highlights: >X-ray diffractograms of Ni{sub x}Mn{sub 0.8-x}Mg{sub 0.2}Fe{sub 2}O{sub 4} samples before and after laser irradiation are characteristic of cubic spinel structure with better crystallinity after irradiation. > The crystal size of the ferrite increases after laser irradiation. > The main conduction mechanism in the investigated system is the correlated barrier hopping and it is the same before and laser irradiation. > The conductivity decreases after laser irradiation. - Abstract: Ni{sub x}Mn{sub 0.8-x}Mg{sub 0.2}Fe{sub 2}O{sub 4}; 0.1 {<=} x {<=} 0.35 was prepared by standard ceramic technique at sintering temperature 1200 deg. C using heating / cooling rate 4 deg. C/min. The samples were irradiated by Nd YAG pulsed laser with energy of the pulse 250 mJ. X-ray diffractograms reveal cubic spinel structure for all the samples before and after laser irradiation. After laser irradiation, better crystallinity was obtained in a form of an increase in the calculated crystal size. This increase was discussed as due to the change in the valence of some ions like Fe{sup 3+}, Ni{sup 2+} and Mn{sup 2+}. The conductivity of all the investigated samples decreases after laser irradiation and becomes temperature independent for a wider range than that before irradiation. This was ascribed to electron rearrangement after laser irradiation. Accordingly, these ferrites are recommended to be useful in electronic devices.