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

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.

Investigation of fluorine adsorption on nitrogen doped MgAl_2O_4 surface by first-principles

International Nuclear Information System (INIS)

Lv, Xiaojun; Xu, Zhenming; Li, Jie; Chen, Jiangan; Liu, Qingsheng

2016-01-01

Graphical abstract: First-principles calculations indicate that MgAl_2O_4 surface is fluorine-loving, but hydrophobic. N doped MgAl_2O_4 (100) surface structure shows the highest fluorine adsorption performance and fluorine atom is more preferentially adsorbed on the Mg-Al bridge site. The fluorine adsorption intensity follow this order: N doped MgAl_2O_4 (100) > Al_2O_3 (0001) > MgAl_2O_4 (100) > MgO (100). N doped MgAl_2O_4 is a promising candidate for fluorine removal. - Highlights: • MgAl_2O_4 surface is fluorine-loving, not hydrophilic. • Fluorine preferentially adsorbs on the Mg-Al bridge site. • Adsorption intensity follow this order: N doped MgAl_2O_4 > Al_2O_3 > MgAl_2O_4 > MgO. • Excellent adsorption performance attributes to electron compensation of N atom. • Nitrogen doped MgAl_2O_4 is a promising candidate for fluorine removal. - Abstract: The nature of fluorine adsorption on pure and N doped MgAl_2O_4 surface has been investigated by first-principles calculations based on the density functional theory. Calculated results indicate that MgAl_2O_4 surface is fluorine-loving, not hydrophilic. Nitrogen doped MgAl_2O_4 (100) surface shows the highest fluorine adsorption performance and fluorine atom preferentially adsorbs on the Mg-Al bridge site. The fluorine adsorption intensity follow this order: Nitrogen doped MgAl_2O_4 (100) > Al_2O_3 (0001) > MgAl_2O_4 (100) > MgO (100). In-depth PDOS analysis suggested that 2p orbitals of F atom strongly hybridized with 3s- and 3p-orbitals of Al atom contribute to its high adsorption intensity. According to the analysis of Hirshfeld charge, the excellent fluorine adsorption performance of nitrogen doped MgAl_2O_4 attributes to the electron compensation effect of nitrogen atom and strong electrostatic interactions. All these evidences demonstrate a fact nitrogen doped MgAl_2O_4 is a promising candidate for fluorine removal.

TL and OSL studies of carbon doped magnesium aluminate (MgAl2O4:C)

Science.gov (United States)

Raj, Sanu S.; Mishra, D. R.; Soni, Anuj; Grover, V.; Polymeris, G. S.; Muthe, K. P.; Jha, S. K.; Tyagi, A. K.

2016-10-01

The MgAl2O4:C has been synthesized by using two different methods by electron gun and vacuum assisted melting of MgAl2O4 in presence of graphite. The MgAl2O4:C phosphor thus developed by these two different methods have similar types of the TL/OSL defects with multiple overlapping TL glow peaks from 100 °C to 400 °C. The Computerized Curve De-convolution Analysis (CCDA) has been used to measure TL parameters such as thermal trap depth, frequency factor and order of kinetic associated with charge transfer process in TL phenomenon. The investigated TL/OSL results show that these two methods of incorporating carbon in MgAl2O4 have generated closely resemble the defects of similar types in MgAl2O4:C lattice. However, the MgAl2O4:C synthesized by electron gun shows relatively larger concentration of the TL/OSL defects as compared to MgAl2O4:C synthesized using vacuum assisted melting method. The photo-ionization cross-section (PIC) associated with fastest OSL component of MgAl2O4: C is found to be ∼ 0.5 times than that of fastest OSL component of commercially available dosimetric grade α-Al2O3:C. The MgAl2O4:C thus developed shows good dynamic OSL dose linearity from few mGy to 1 Gy. This work reveals that MgAl2O4:C could be developed as potential tissue equivalent OSL / TL material.

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)

Heavy ion induced damage in MgAl sub 2 O sub 4 , an inert matrix candidate for the transmutation of minor actinides

CERN Document Server

Wiss, T

1999-01-01

Magnesium aluminum spinel (MgAl sub 2 O sub 4) is a material selected as a possible matrix for transmutation of minor actinides by neutron capture or fission in nuclear reactors. To study the radiation stability of this inert matrix, especially against fission product impact, irradiations with heavy energetic ions or clusters have been performed. The high electronic energy losses of the heavy ions in this material led to the formation of visible tracks as evidenced by transmission electron microscopy for 30 MeV C sub 6 sub 0 -Buckminster fullerenes and for ions of energy close to or higher than fission energy ( sup 2 sup 0 sup 9 Bi with 120 MeV and 2.38 GeV energy). The irradiations at high energies showed a pronounced degradation of the spinel. Additionally, MgAl sub 2 O sub 4 exhibited a large swelling for irradiation at high fluences with fission products of fission energy (here I-ions of 72 MeV) and at temperatures <= 500 deg. C. These observations are discussed from the technological point of view in ...

Extended defects in insulating MgAl2O4 ceramic materials studied by PALS methods

International Nuclear Information System (INIS)

Klym, H; Ingram, A; Shpotyuk, O; Filipecki, J; Hadzaman, I

2010-01-01

Extended positron-trapping defects in technological modified insulating nanoporous MgAl 2 O 4 ceramics are characterized by positron annihilation lifetime spectroscopy. The results are achieved using three-component fitting procedure with arbitrary lifetimes applied to treatment of measured spectra. Within this approach, the first component in the lifetime spectra reflects microstructure specificity of the spinel structure, the second component responsible to extended defects near intergranual boundaries and the third component correspond to ortho-positronium 'pick-off' decaying in nanopores of ceramics. It is shown that in ceramics of different technological modifications the same type of positron traps prevails.

A background subtraction routine for enhancing energy-filtered plasmon images of MgAl2O4 implanted with Al+ and Mg+ ions

International Nuclear Information System (INIS)

Evans, N.D.; Kenik, E.A.; Bentley, J.; Zinkle, S.J.

1995-01-01

MgAl 2 O 4 , a candidate fusion reactor material, was irradiated with Al + or Mg + ions; electron energy-loss spectra and energy-filtered plasmon images showed that metallic Al colloids are present in the ion-irradiated regions. This paper shows the subtraction of the spinel plasmon component in images using 15-eV-loss electrons in some detail

Linear thermal expansion coefficient of MgAl2O4(s)

International Nuclear Information System (INIS)

Dash, A.; Samui, P.; Naik, Y.P.; Chaudhary, Z.S.

2011-01-01

The coefficient of linear thermal expansion (α av ) of MgAl 2 O 4 (s) has been determined using a Netzsch 402 PC dilatometer with Al 2 O 3 (s) as the push-rod. The change in length per unit length was recorded as a function of temperature between room temperature to 1273 K at a heating rate of 8 K.min /1 , in argon flowing atmosphere. The average of three measurements was quoted as the α av for MgAl 2 O 4 (s). The linear thermal expansion was measured to an accuracy of ±3%. (author)

Anisotropic dislocation loop nucleation in ion-irradiated MgAl2O4

International Nuclear Information System (INIS)

Zinkle, S.J.

1992-01-01

This work is intended to investigate the effects of transmutation products and varying ionizing-to-displacive damage ratio on microstructural evolution in ceramics for fusion machine. Polycrystalline disks of stoichiometric magnesium aluminate spinel (MgAl 2 O 4 ) were irradiated with 2 MeV Al + ions at 650C and subsequently analyzed in cross section using transmission electron microscopy (TEM). Interstitial dislocation loops were observed on [110] and [111] 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 was 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 and may be associated with the structure of displacement cascades in ceramics

Mechanical Properties and Fabrication of Nanostructured Mg_2SiO_4-MgAl_2O_4 Composites by High-Frequency Induction Heated Combustion

International Nuclear Information System (INIS)

Shon, In-Jin; Kang, Hyun-Su; Hong, Kyung-Tae; Doh, Jung-Mann; Yoon, Jin-Kook

2011-01-01

Nanopowders of MgO, Al_2O_3 and SiO_2 were made by high energy ball milling. The rapid sintering of nanostructured MgAl_2O_4-Mg_2SiO_4 composites was investigated by a high-frequency induction heating sintering process. The advantage of this process is that it allows very quick densification to near theoretical density and inhibition of grain growth. Nanocrystalline materials have received much attention as advanced engineering materials with improved physical and mechanical properties. As nanomaterials possess high strength, high hardness, excellent ductility and toughness, undoubtedly, more attention has been paid for the application of nanomaterials. Highly dense nanostructured MgAl_2O_4-Mg_2SiO_4 composites were produced with simultaneous application of 80 MPa pressure and induced output current of total power capacity (15 kW) within 2 min. The sintering behavior, gain size and mechanical properties of MgAl_2O_4-Mg_2SiO_4 composites were investigated.

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

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

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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.

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)

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.

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.

Correlation between stoichiometry and surface structure of the polar MgAl2O4(100) surface as a function of annealing temperature

DEFF Research Database (Denmark)

Jensen, Thomas Nørregaard; Rasmussen, Morten Karstoft; Knudsen, Jan

2015-01-01

is found to significantly increase as the surface is sputtered and annealed in oxygen at intermediate temperatures ranging from 800-1000 [degree]C. The Al excess is explained by the observed surface structure, where the formation of nanometer sized pits and elongated patches with Al terminated step edges....... The excess of Al and high concentration of octahedral vacancies, very interestingly means, that the top few surface layers of the MgAl2O4(100) adopts a surface structure similar to that of a spinel-like transition Al2O3 film. However, after annealing at a high temperature of 1200 [degree]C, the Al/Mg ratio...... are filled by Mg from the bulk, due to the increased mobility at high annealing temperatures....

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.

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.

Synthesis and fabrication of MgAl2O4 ceramic foam via a simple, low-cost and eco-friendly method

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Shuvendu Tripathy

2016-06-01

Full Text Available The MgAl2O4 nanocrystalline powder was synthesized using naturally available egg white and inexpensive metal nitrate salts. During this process, the freshly extracted egg white was mixed with metal nitrate salt and subsequently heated at 350 °C in a pit furnace. The entire dehydration of the aqueous solution thus facilitates the low-density fluffy mass. From TGDTG results, it was observed that maximum decomposition of the precursors occurred below 600 °C. Therefore, the calcination temperature of as-synthesized powder was set at 600 °C. The MgAl2O4 bulk ceramic foam was fabricated by dispersing different loading of MgAl2O4 nanoparticles in the egg white, and then coating on polyurethane sponge prior to drying and sintering at a higher temperature. The ceramic suspensions exhibit a typical shear thinning behavior, and its viscosity was found to be significantly influenced by MgAl2O4 powder content. An optimum loading of 40 wt% MgAl2O4 nanoparticles in the egg white was found to show maximum porosity up to 90%. The obtained ceramic foam has potential applications in catalysis, absorption and sensor.

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

Effect of Grain Size on Mechanical Properties of Irradiated Mono- and Polycrystalline MgAl2O4

International Nuclear Information System (INIS)

Jagielski, J.; Piatkowska, A.; Wajler, A.; Boniecki, M.; Romaniec, M.; Jozwik, I.; Aubert, P.; Labdi, S.; Maciejak, O.; Thome, L.; Debelle, A.

2011-01-01

The influence of the size of crystalline regions on mechanical properties of irradiated oxides has been studied using a magnesium aluminate spinel MgAl 2 O 4 . The samples characterized by different dimensions of crystalline domains, varying from sintered ceramics with grains of few micrometers in size up to single crystals, were used in the experiments. The samples were irradiated at room temperature with 320 keV Ar 2+ ions up to fluences reaching 5x10 16 cm -2 . Nanomechanical properties (nanohardness and Young's modulus) were measured by using a nanoindentation technique and the resistance to crack formation by measurement of the total crack lengths made by the Vickers indenter. The results revealed several effects: correlation of nanohardness evolution with the level of accumulated damage, radiation-induced hardness increase in grain-boundary region and significant improvement of material resistance to crack formation. This last effect is especially surprising as the typical depth of cracks formed by Vickers indenter in unirradiated material exceeds several tens of micrometers, i.e. is more than hundred times larger than the thickness of the modified layer. (author)

Fabrication of Polycrystalline Transparent Co+2: MgAl2O4 by a Combination of Spark Plasma Sintering (SPS and Hot Isostatic Pressing (HIP Processes

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Sokol Maxim

2017-01-01

Full Text Available Transparent Co2+ doped MgAl2Ob4 spinel was fabricated by SPS consolidation followed by and HIP treatment. It was established that HIP treatment significantly improved transparency of the ceramic in a wide range of wavelengths, especially, in a range, which is relevant for Q-switching. Nonlinear absorption was demonstrated and the ground and excited state absorption cross sections were estimated. The positive effect of the HIP treatment on the optical properties is related to an elimination of extremely fine porosity and to the location of Co ions at Mg2+sites in the spinel ionic structure. The experimental results indicate that the fabricated specimens can be used as a passive laser Q-switching material.

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

Fabrication and Characterization of Porous MgAl2O4 Ceramics via a Novel Aqueous Gel-Casting Process

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Lei Yuan

2017-11-01

Full Text Available A novel and aqueous gel-casting process has been successfully developed to fabricate porous MgAl2O4 ceramics by using hydratable alumina and MgO powders as raw materials and deionized water as hydration agent. The effects of different amounts of deionized water on the hydration properties, apparent porosity, bulk density, microstructure, pore size distribution and compressive strength of the samples were investigated. The results indicated that the porosity and the microstructure of porous MgAl2O4 ceramics were governed by the amounts of deionized water added. The porous structure was formed by the liberation of physisorbed water and the decomposition of hydration products such as bayerite, brucite and boehmite. After determining the addition amounts of deionized water, the fabricated porous MgAl2O4 ceramics had a high apparent porosity (52.5–65.8%, a small average pore size structure (around 1–3 μm and a relatively high compressive strength (12–28 MPa. The novel aqueous gel-casting process with easy access is expected to be a promising candidate for the preparation of Al2O3-based porous ceramics.

A comparison of the doppler-broadened positron annihilation spectra of neutron irradiated Al 2O 3 and MgAl 2O 3

Science.gov (United States)

Jones, P. L.; Schaffer, J. P.; Cocks, F. H.; Clinard, F. W.; Hurley, G. F.

1985-01-01

Radiation damage studies of oxides and ceramics have become of increasing importance due to the projected use of these materials in thermonuclear fusion reactors as electronic insulators and first wall materials. In addition these materials are important in RAD waste disposal. As part of a study of the defect structure in radiation damaged ceramics Doppler-broadened positron annihilation spectra have been obtained for a series of single crystal sapphire (α-Al 2O 3) and polycrystal (1:1) and (1:2) magnesium aluminate spinel (MgO·Al 2O 3 and MgO-2Al 2O 3) samples. These samples were irradiated in EBR-II to a fluence of 3 × 10 25 n/m 2 (E > 0.1 MeV) at 740°C, and 2 × 10 26 n/m 2 (E > 0.1 MeV) at ~ 550°C respectively. Positron annihilation spectra lineshapes for the irradiated, annealed, and as-received samples of both materials were compared using S parameter analysis. These calculations were made on deconvoluted gamma ray spectra that were free of any instrumental broadening effects. In this way, absolute S parameter changes could be calculated. The observed changes in the S parameter are consistent with independent volume swelling measurements for both the α-A1 2O 3 and the (1:2) MgAl 2O 4 samples. However, the change in S parameter measured for the (1:1) spinel is contrary to the measured volume change. This apparent anomaly indicates a predominence of interstitial as opposed to vacancy type defects in this material.

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%

Mechanical properties of individual MgAl2O4 agglomerates and their effects on densification

International Nuclear Information System (INIS)

Rufner, Jorgen F.; Castro, Ricardo H.R.; Holland, Troy B.; Benthem, Klaus van

2014-01-01

The presence of agglomerates during nanopowder sintering can be problematic and can limit achievable final densities. Typically, the practical solution is to use high pressures to overcome agglomerate breakdown strengths to reach higher packing fractions. The strength of agglomerates is often difficult to determine and makes processing parameters challenging to optimize. In this work, we used in situ transmission electron microscopy nanoindentation experiments to assess the mechanical properties of individual MgAl 2 O 4 agglomerates under constant indenter head displacement rates. Electron microscopy revealed highly porous agglomerates with pores on both the micron and nanometric length scales. Individual agglomerate strength, at fracture, was calculated from compression tests with deformation behavior correlating well with previously reported modeling results. Macroscopic powder properties were also investigated using green-pressed pellets consolidated at pressures up to 910 MPa. The unexpectedly high strength is indicative of the role agglomerates play in MgAl 2 O 4 nanopowder densification

MgAl_2O_4 foams obtained by combustion synthesis

International Nuclear Information System (INIS)

Moraes, G.G.; Rosa, M.A.; Kronbauer, D.P.; Pozzobom, I.F.; Fernandes, C.P.; Oliveira, A.P. Novaes de

2014-01-01

This work aims to study magnesium aluminate (MgAl_2O_4) ceramic foams obtained by combustion synthesis in solution without the need of surfactants to stabilize bubbles. The precursors, Al(NO_3)_3_.9H_2O and Mg(NO_3)_2_.6H_2_O, dispersed in distilled water (20 wt%) were magnetically stirred under heating (70°C). At the beginning of the reaction, a fuel composed by a mixture of residual glycerins from the production of biodiesel was added. The foams were produced by controlling the stirring speed and temperature. The applied thermal cycle to consolidate the foams consisted of heating at 1°C/min to 600°C/120 min and subsequently raising the temperature at 10°C/min to 1600°C/120 min. The obtained materials were characterized by SEM,TEM and from tomographic images. The results showed that the obtained magnesium aluminate foams have a high porosity (97%), a high connectivity and pore sizes (diameters) between 30 and 1200 μm. (author)

Thermophysical properties of αAl2O3, MgAl2O4 and AlN at low tempertures

International Nuclear Information System (INIS)

Burghartz, S.

1995-12-01

A possibility for producing energy in future might be the nuclear fusion. The process of nuclear fusion is characterized by melting nuclei of hydrogen atoms (deuterium and tritium) which yield to the production of helium atom nuclei. For this process extremely high temperatures of the deuterium-tritium-gas plasma are necessary. The additional heating of the plasma by microwaves requires materials with low diaelectric losses and high thermal conductivity. The thermal conductivity can be increased by cooling the windows which lead to the plasma chambre. Experimental investigations with the aim to check the influence of liquid nitrogen (T=70 K) on the cooling of the windows were performed in the temperature region 70 K 2 O 3 , MgAl 2 O 4 and AlN were measured. The thermal conductivity can be calculated using the equation λ=αc p ρ λ=thermal conductivity α=thermal diffusivity c p =specific heat (at constant pressure) ρ=density. Furthermore a theoretical method to calculate the thermal conductivity at low temperatures is presented; this is done by using a model modification of heat transport in electric insulators. As result the influence of intrinsic parameters (crystal structure, interatomar binding, anharmonicity) and extrinsic parameters (point defects, dislocations, boundary areas) upon thermal conductivity of α-Al 2 O 3 , MgAl 2 O 4 and AlN are achieved. (orig.)

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.

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.

Ionizing radiation effects in MgAl2O4

International Nuclear Information System (INIS)

Ibarra Sanchez, A.

1990-01-01

The effect of ionizing radiation in MgAl2O4 has been studied, paying special interest to the influence of the high concentration of intrinsic dsefects of this material. Optical absorption, ESR, photoluminiscence, radioluminiscence, and thermoluminiscence are the main techniques used. The ionizing radiation induces to formation of V centres. During the work its characteristics (structure, thermal stability, absorption spectra, etc.) has been studied. The thermoluminiscence spectra allowed the discovery of several charge release processes between 85 and 650 K, all of them associated to electron release. The V-centres and several impurities (Cr, Mn,...) appear as recombination centres. The obtained data show that the kinetic of these charge release processes is regulated by the presence of a point defect with a very high concentration. This defect is an electron trap and its structure is an Al ion in a lattice site of tetraedral symmetry. (Author)

Color-tunable and highly thermal stable Sr_2MgAl_2_2O_3_6:Tb"3"+ phosphors

International Nuclear Information System (INIS)

Zhang, Haiming; Zhang, Haoran; Liu, Yingliang; Lei, Bingfu; Deng, Jiankun; Liu, Wei-Ren; Zeng, Yuan; Zheng, Lingling; Zhao, Minyi

2017-01-01

Tb"3"+ activated Sr_2MgAl_2_2O_3_6 phosphor was prepared by a high-temperature solid-state reaction route. The X-ray diffraction, scanning electron microscopy, and photoluminescence spectroscopy were used to characterize the as-prepared samples. The Sr_2MgAl_2_2O_3_6:Tb"3"+ phosphors show intense green light emission under UV excitation. The phosphor exhibit two groups of emission lines from about 370 to 700 nm, which originating from the characteristic "5D_3-"7F_J and "5D_4-"7F_J transitions of the Tb"3"+ ion, respectively. The cross-relaxation mechanism between the "5D_3 and "5D_4 emission was investigated and discussed. The emission colors of these phosphors can be tuned from bluish-green to green by adjusting the Tb"3"+ doping concentration. Furthermore, the thermal quenching temperature (T_1_/_2) is higher than 500 K. The excellent thermal stability and color-tunable luminescent properties suggest that the developed material is a promising green-emitting phosphor candidate for optical devices. - Highlights: • A Color-tunable emitting phosphor Sr_2MgAl_2_2O_3_6:Tb"3"+ was prepared successfully via high-temperature solid-state reaction. • The photoluminescence of Sr_2MgAl_2_2O_3_6:Tb"3"+ shows highly thermal stable. • The cross-relaxation mechanism between the "5D_3 and "5D_4 emission was investigated and discussed.

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)

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.

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.

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.

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....

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)

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).

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

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.

Effect of polymorphism of Al2O3 on the sintering and microstructure of transparent MgAl2O4 ceramics

Science.gov (United States)

Han, Dan; Zhang, Jian; Liu, Peng; Wang, Shiwei

2017-09-01

Transparent MgAl2O4 ceramics were fabricated by reactive sintering in air followed by hot isostatic press treatment using commercial Al2O3 powder (γ-Al2O3 or α-Al2O3) and MgO powder as raw materials. The densification rate, microstructure and optical properties of the ceramics were investigated. Densification temperature of the sample from γ-Al2O3/MgO was lower than that from α-Al2O3/MgO. However, in-line transmission (2 mm thick) of the sample from α-Al2O3/MgO at the wavelength of 600 nm and 1100 nm were respectively 77.7% and 84.3%, higher than those (66.7%, 81.4%) of the sample from γ-Al2O3/MgO. SEM observation revealed that the sample from α-Al2O3/MgO exhibited a homogeneous and pore-free microstructure, while, the sample from γ-Al2O3/MgO showed an apparent bimodal microstructure containing pores.

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)

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)

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....

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...

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.

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.

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

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.

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.

Perpendicular magnetic anisotropy in Ta|Co40Fe40B20|MgAl2O4 structures and perpendicular CoFeB|MgAl2O4|CoFeB magnetic tunnel junction

KAUST Repository

Tao, B. S.

2014-09-08

Magnetic properties of Co40Fe40B20(CoFeB) thin films sandwiched between Ta and MgAl2O4layers have been systematically studied. For as-grown state, Ta/CoFeB/MgAl2O4structures exhibit good perpendicular magnetic anisotropy (PMA) with interface anisotropy Ki=1.22erg/cm2, which further increases to 1.30erg/cm2after annealing, while MgAl2O4/CoFeB/Ta multilayer shows in-plane magnetic anisotropy and must be annealed in order to achieve PMA. For bottom CoFeB layer, the thickness window for PMA is from 0.6 to 1.0nm, while that for top CoFeB layer is between 0.8 and 1.4nm. Perpendicular magnetic tunnel junctions (p-MTJs) with a core structure of CoFeB/MgAl2O4/CoFeB have also been fabricated and tunneling magnetoresistance ratio of about 36% at room temperature and 63% at low temperature have been obtained. The intrinsic excitations in the p-MTJs have been identified by inelastic electron-tunneling spectroscopy.

Perpendicular magnetic anisotropy in Ta|Co40Fe40B20|MgAl2O4 structures and perpendicular CoFeB|MgAl2O4|CoFeB magnetic tunnel junction

KAUST Repository

Tao, B. S.; Li, D. L.; Yuan, Z. H.; Liu, H. F.; Ali, S. S.; Feng, J. F.; Wei, H. X.; Han, X. F.; Liu, Y.; Zhao, Y. G.; Zhang, Q.; Guo, Zaibing; Zhang, Xixiang

2014-01-01

Magnetic properties of Co40Fe40B20(CoFeB) thin films sandwiched between Ta and MgAl2O4layers have been systematically studied. For as-grown state, Ta/CoFeB/MgAl2O4structures exhibit good perpendicular magnetic anisotropy (PMA) with interface anisotropy Ki=1.22erg/cm2, which further increases to 1.30erg/cm2after annealing, while MgAl2O4/CoFeB/Ta multilayer shows in-plane magnetic anisotropy and must be annealed in order to achieve PMA. For bottom CoFeB layer, the thickness window for PMA is from 0.6 to 1.0nm, while that for top CoFeB layer is between 0.8 and 1.4nm. Perpendicular magnetic tunnel junctions (p-MTJs) with a core structure of CoFeB/MgAl2O4/CoFeB have also been fabricated and tunneling magnetoresistance ratio of about 36% at room temperature and 63% at low temperature have been obtained. The intrinsic excitations in the p-MTJs have been identified by inelastic electron-tunneling spectroscopy.

Spectroscopic properties of a novel near-infrared tunable laser material Ni:MgGa2O4

International Nuclear Information System (INIS)

Suzuki, Takenobu; Senthil Murugan, Ganapathy; Ohishi, Yasutake

2005-01-01

An intense emission band from Ni 2+ in MgGa 2 O 4 spinel in the range of 1.1-1.6μm was observed at room temperature. The emission band could be assigned to the downward d-d transition of T2g3->A2g3 of Ni 2+ ions in octahedral sites. The lifetime of the emission was more than 1.6ms from 5 to 300K. This material has potential as a near-infrared tunable-laser host

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.

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...

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.

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

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.

Depth-dependent and surface damages in MgAl sub 2 O sub 4 and MgO irradiated with energetic iodine ions

CERN Document Server

Aruga, T; Ohmichi, T; Okayasu, S; Kazumata, Y; Jitsukawa, S

2002-01-01

Samples of polycrystalline ceramics of MgAl sub 2 O sub 4 irradiated at the ambient temperature with 85 MeV I sup 7 sup + iodine ions to doses up to 1x10 sup 1 sup 9 m sup - sup 2 is observed to be amorphized up to depths around 6 mu m from the ion-incident surface for a dose of 1.2x10 sup 1 sup 9 m sup - sup 2 , through a cross-sectional transmission electron microscopy. A step height of 1 mu m is formed across the border between the masked and irradiated regions of the surface. The height of the step is observed to increase sharply from the irradiated area towards the edge at the border, forming a peak as tall as 1.5 mu m. A glossy, silver-gray film with a thickness less than 0.1 mu m is unexpectedly observed to have formed on the surface of samples of MgAl sub 2 O sub 4 and MgO, in about 3.5 years aging after the irradiation to 1.2x10 sup 1 sup 9 m sup - sup 2 , being left untouched in the air. The film is easily peeled off along grain boundaries and found to be amorphous from the electron diffraction patt...

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 .

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

Photoluminescence of the Mg2Al4Si5O18-Al2O3-MgAl2O4-SiO2 ceramic system containing Fe3+ and Cr3+ as impurity ions

Science.gov (United States)

Sosman, L. P.; López, A.; Pedro, S. S.; Papa, A. R. R.

2018-02-01

This work presents the results of photoluminescence, excitation and radiative decay time for a ceramic system containing Mg2Al4Si5O18-Al2O3-MgAl2O4-SiO2 with Fe3+ and Cr3+ as impurity ions. Emission data were obtained using several excitation wavelengths and the excitation data were acquired for the most intense emission bands. The optical results were analyzed according to the Tanabe-Sugano (TS) theory from which the crystalline field parameter Dq and Racah parameters B and C were obtained for the Fe3+ and Cr3+ sites. The results indicate that the Fe3+ and Cr3+ ions occupy tetrahedral and octahedral sites, respectively. The emission from Fe3+ and Cr3+ ions causes an intense and broad band ranging between 350 nm and 850 nm, showing that this material is a potential tunable radiation source at room temperature.

Tensile strain effect in ferroelectric perovskite oxide thin films on spinel magnesium aluminum oxide substrate

Science.gov (United States)

Zhou, Xiaolan

Ferroelectrics are used in FeRAM (Ferroelectric random-access memory). Currently (Pb,Zr)TiO3 is the most common ferroelectric material. To get lead-free and high performance ferroelectric material, we investigated perovskite ferroelectric oxides (Ba,Sr)TiO3 and BiFeO3 films with strain. Compressive strain has been investigated intensively, but the effects of tensile strain on the perovskite films have yet to be explored. We have deposited (Ba,Sr)TiO3, BiFeO3 and related films by pulsed laser deposition (PLD) and analyzed the films by X-ray diffractometry (XRD), atomic force microscopy (AFM), etc. To obtain inherently fully strained films, the selection of the appropriate substrates is crucial. MgAl2O4 matches best with good quality and size, yet the spinel structure has an intrinsic incompatibility to that of perovskite. We introduced a rock-salt structure material (Ni 1-xAlxO1+delta) as a buffer layer to mediate the structural mismatch for (Ba,Sr)TiO3 films. With buffer layer Ni1-xAlxO1+delta, we show that the BST films have high quality crystallization and are coherently epitaxial. AFM images show that the films have smoother surfaces when including the buffer layer, indicating an inherent compatibility between BST-NAO and NAO-MAO. In-plane Ferroelectricity measurement shows double hysteresis loops, indicating an antiferroelectric-like behavior: pinned ferroelectric domains with antiparallel alignments of polarization. The Curie temperatures of the coherent fully strained BST films are also measured. It is higher than 900°C, at least 800°C higher than that of bulk. The improved Curie temperature makes the use of BST as FeRAM feasible. We found that the special behaviors of ferroelectricity including hysteresis loop and Curie temperature are due to inherent fully tensile strain. This might be a clue of physics inside ferroelectric stain engineering. An out-of-plane ferroelectricity measurement would provide a full whole story of the tensile strain. However, a

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.

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.

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.

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

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.

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

Effects of γ-irradiation upon the optical behavior of spinel

International Nuclear Information System (INIS)

White, G.S.; Lee, K.H.; Crawford, J.H.Jr.

1977-01-01

The effect of 137 Cs gamma irradiation (0.67 MeV photons) upon the optical absorption and thermoluminescence of spinel (MgAl 2 O 4 ) is studied. Exposure to gamma radiation provides electrons which are captured at Fesup(3+) in octahedral sites, thereby producing Fesup(2+) and destroying the 4.8 and 6.4 eV absorption bands. Isochronal annealing curves of the 3.1 and 4.8 eV peaks are given. A reciprocal relationship between the recovery of the 4.8 eV band and the thermoluminescence immediately after irradiation and after sitting over night has been measured

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

Refractory castables Al2O3-MgO advanced boron-containing

International Nuclear Information System (INIS)

Morbioli, G.G.; Braulio, M.A.L.; Pandolfelli, V.C.

2011-01-01

Alumina-magnesia refractory castables present high corrosion resistance mainly due to the in situ spinel (MgAl 2 O 4 ) formation. For the steel industry, the earlier its generation the best would be the castable's working performance. Taking this aspect into account, alternatives to replace silica fume, which is the most traditional liquid former inducer in this system, were evaluated in this study, by adding boron-containing compounds. Faster spinel and calcium hexaaluminate (CA 6 ) formation was attained through a transient liquid, ensuring remarkable castable's creep resistance and hot modulus of rupture. In this context, a novel route to design in situ spinel forming castable is presented, with great potential to increase the performance of this class of refractory. (author)

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

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)

Coincident site lattice-matched InGaN on (111) spinel substrates

International Nuclear Information System (INIS)

Norman, A. G.; Dippo, P. C.; Moutinho, H. R.; Simon, J.; Ptak, A. J.

2012-01-01

Coincident site lattice-matched wurtzite (0001) In 0.31 Ga 0.69 N, emitting in the important green wavelength region, is demonstrated by molecular beam epitaxy on a cubic (111) MgAl 2 O 4 spinel substrate. The coincident site lattice matching condition involves a 30 deg. rotation between the lattice of the InGaN epitaxial layer and the lattice of the spinel. This work describes an alternative approach towards realizing more compositionally homogenous InGaN films with low dislocation density emitting in the ''green gap'' of low efficiency currently observed for semiconductor light emitting diodes (LEDs). This approach could lead to higher efficiency green LEDs presently of great interest for solid-state lighting applications.

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.

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.

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

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.

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...

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

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

Magnetic and optical properties of MgAl2O4-(Ni0.5Zn0.5Fe2O4 thin films prepared by pulsed laser deposition

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Takeshi Misu, Naonori Sakamoto, Kazuo Shinozaki, Nobuyasu Adachi, Hisao Suzuki and Naoki Wakiya

2011-01-01

Full Text Available Thin films composed of MgAl2O4 and (Ni0.5Zn0.5Fe2O4 ([MA(100-x-NZFx] films were grown on fused SiO2 substrates by pulsed laser deposition. X-ray diffraction measurements revealed that the films were polycrystalline, and that their lattice constant varied linearly with composition, indicating the formation of a solid solution. The film with x=60 was paramagnetic and those with x ≥ 70 were ferromagnetic. The films had a transparency above 75% in the visible range, but the transparency decreased with the x value. The optical band gaps were 2.95, 2.55, 2.30 and 1.89 eV for x=20, 40, 60, 80 and 100, respectively. The Faraday rotation angle increased with x in the visible range, and the film with x=70 exhibited a value of 2000 degrees cm-1 at 570 nm, which is comparable to the rotation angle of Y3Fe5O12. Owing to their high transparency, which extends into the visible range, the [MA(100-x-NZFx] films can be used in novel magneto-optical devices.

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

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.

Epitaxial growth of manganese oxide films on MgAl2O4 (001) substrates and the possible mechanism

Science.gov (United States)

Ren, Lizhu; Wu, Shuxiang; Zhou, Wenqi; Li, Shuwei

2014-03-01

Three types of manganese oxide films were grown on MgAl2O4 (001) substrates by plasma-assisted molecular beam epitaxy (PA-MBE) under different growth rates and substrate temperatures. The structural characteristics and chemical compositions of the films were investigated by using in-situ reflection high-energy electron diffraction (RHEED), ex-situ X-ray diffraction, Raman, and X-ray photoelectron spectra (XPS). At a lower substrate temperature (730 K), the epitaxial film tends to form mixed phases with a coexistence of Mn3O4 and Mn5O8 in order to relieve the mismatch-strain. However, at a higher substrate temperature (750 K), all of the films crystallize into Mn3O4; the critical thickness of the film grown under a lower growth rate (7 Å/min) is much larger than that under a high growth rate (10 Å/min). When the film reaches a certain critical thickness, the surface will become fairly rough, and another oriented phase Mn3O4 would crystallize on such a surface.

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

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...

Hardness and depth-dependent microstructure of ion-irradiated MgAl2O4

International Nuclear Information System (INIS)

Zinkle, S.J.

1988-01-01

Stoichiometric polycrystalline magnesium aluminate spinel has been irradiated at 25 and 650/degree/C with 2.4 MeV Mg/sup plus/ ions to a fluence of 1.4 /times/ 10 21 ions/m 2 (/approximately/35 dpa peak damage level). Microindentation hardness measurements and transmission electron microscopy combined with energy dispersive X-ray spectroscopy measurements were used to characterize the irradiation effects. The room-temperature hardness of spinel increased by about 5% after irradiation at both temperatures. There was no evidence for amorphization at either irradiation temperature. Interstitial-type dislocations loops lying on /l brace/110/r brace/ and /l brace/111/r brace/ planes with Burgers vectors were observed at intermediate depths (/approximately/1 μm) along the ion range. The /l brace/111/r brace/ loops are presumably formed from /l brace/111/r brace/ loops as a result of a shear on the anion sublattice. Only about 0.05% of the calculated displacements were visible in the form of loops, which indicates that spinel has a high resistance to aggregate damage accumulation. The peak damage region contained a high density of dislocations tangles. There was no evidence for the formation of voids or vacancy loops. The specimen irradiated at 650/degree/C was denuded of dislocation loops within /approximately/1 μm of the surface. 25 refs., 16 figs., 5 tabs

Evolution of an alumina-magnesia/self-forming spinel castable. Part I: Microstructural features Evolução de um refratário de espinélio auto-formado de alumina-magnésia. Parte I: Aspectos microestruturais

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D. Gutiérrez-Campos

1999-06-01

Full Text Available Refractories containing magnesium aluminate spinel (MgAl2O4 are materials for emerging technology in several applications like cement and steelmaking processes. In order to deep the understanding of these castables, this work presents the microstructural characteristics of an alumina-magnesia/self-forming spinel castable. Several variables such as MgO content, firing temperature and spinel formation are analyzed through XRD and SEM analysis. The results showed that the processes of spinel formation and nucleation are not strongly affected by the MgO content, but that the crystal growth is enhanced for samples with 6.0 wt% MgO. Hibonite (CA6 bonding in the castable matrix showed a needlelike structure that could increase hot properties of the material. MgO content in the castable seems to affect the hibonite development. The development of a self-forming spinel castable without any synthetic spinel grains appears to be promissory for optimum refractory linings.Refratários contendo espinélio de aluminato de magnésio (MgAl2O4 são materiais para tecnologia emergentes em várias aplicações tais como cimento e processos siderúrgicos. Com a finalidade de melhorar o entendimento destes refratários, este trabalho apresenta as características microestruturais de um refratário espinélio auto-formado de alumina-magnésia. Várias variáveis tais como teor de MgO, temperatura de queima e formação de espinélio são analisadas por meio de difração de raios X e microscopia eletrônica de varredura. Os resultados mostram que os processos de formação de espinélio e de nucleação não são fortemente influenciados pelo teor de MgO, mas que o crescimento de cristal é aumentado para amostras com 6.0% em peso de MgO. A ligação hibonita (CA6 na matriz do refratário mostrou uma estrutura tipo agulha que poderia melhorar as propriedades a quente do material. O teor de MgO no refratário parece influenciar o desenvolvimento da hibonita. O

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

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)

Síntese de MgAl2O4 por combustão assistida por micro-ondas: influência dos parâmetros de síntese na formação e na estrutura cristalina

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R. L. B. A. Medeiros

Full Text Available Resumo Nos últimos anos a técnica de combustão assistida por micro-ondas vem recebendo uma atenção especial, por ser uma técnica rápida, de baixo custo e de fácil manuseio, que permite obter materiais com boa homogeneidade química. O aluminato de magnésio (MgAl2O4 é um dos mais bem conhecidos materiais cerâmicos devido às suas excelentes propriedades, como alto ponto de fusão, elevada resistência mecânica em altas temperaturas, boa resistência ao choque térmico e resistência a ácidos e bases. O propósito deste trabalho é avaliar a influência da razão combustível/oxidante (Rco, temperatura de calcinação (Tcal e da potência do micro-ondas (Pmic na formação e na estrutura cristalina do MgAl2O4. Para realizar a reação de combustão foram utilizadas três potências (450, 675 e 900 W e três razões combustível/oxidante (0,8:1, 1:1 e 1,2:1. O material foi calcinado em três temperaturas (700, 800 e 900 ºC e foram realizadas análises de difração de raios X e microscopia eletrônica por varredura. Um planejamento fatorial 23 foi utilizado para avaliar a influência da Rco, Tcal e Pmic nos parâmetros como a cristalinidade e o tamanho de cristalito. Os resultados mostram que para os MgAl2O4 sintetizados com Rco maiores que 1:1 e Pmic menores que 675 W são obtidos tamanhos de cristalito entre 10 e 20 nm quando calcinados a 700 e 800 ºC. Com relação ao grau de cristalinidade, somente a Tcal exerce uma influência significativa.

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.

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.

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

Transparent magnesium aluminate spinel: a prospective biomaterial for esthetic orthodontic brackets.

Science.gov (United States)

Krishnan, Manu; Tiwari, Brijesh; Seema, Saraswathy; Kalra, Namitha; Biswas, Papiya; Rajeswari, Kotikalapudi; Suresh, Madireddy Buchi; Johnson, Roy; Gokhale, Nitin M; Iyer, Satish R; Londhe, Sanjay; Arora, Vimal; Tripathi, Rajendra P

2014-11-01

Adult orthodontics is recently gaining popularity due to its importance in esthetics, oral and general health. However, none of the currently available alumina or zirconia based ceramic orthodontic brackets meet the esthetic demands of adult patients. Inherent hexagonal lattice structure and associated birefringence limits the visible light transmission in polycrystalline alumina and make them appear white and non transparent. Hence focus of the present study was to assess the feasibility of using magnesium aluminate (MgAl2O4) spinel; a member of the transparent ceramic family for esthetic orthodontic brackets. Transparent spinel specimens were developed from commercially available white spinel powder through colloidal shaping followed by pressureless sintering and hot isostatic pressing at optimum conditions of temperature and pressure. Samples were characterized for chemical composition, phases, density, hardness, flexural strength, fracture toughness and optical transmission. Biocompatibility was evaluated with in-vitro cell line experiments for cytotoxicity, apoptosis and genotoxicity. Results showed that transparent spinel samples had requisite physico-chemical, mechanical, optical and excellent biocompatibility for fabricating orthodontic brackets. Transparent spinel developed through this method demonstrated its possibility as a prospective biomaterial for developing esthetic orthodontic brackets.

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-MnχCr2-χO4. 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.

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

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.

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.

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.

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.

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

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...

Environmental Benign Synthesis of Lithium Silicates and Mg-Al Layered Double Hydroxide from Vermiculite Mineral for CO2 Capture

Directory of Open Access Journals (Sweden)

Yu Zhang

2017-04-01

Full Text Available This research introduces a completely new environmental benign synthesis route for obtaining two kinds of inter-mediate and high temperature CO2 sorbents, Mg-Al layered double hydroxide (LDH and Li4SiO4, from vermiculite. The mineral vermiculite was leached with acid, from which the obtained SiO2 was used for the synthesis of Li4SiO4 and the leaching waste water was used for the synthesis of Mg-Al LDH. Therefore, no waste was produced during the whole process. Both Li4SiO4 and Mg-Al LDH sorbents were carefully characterized using XRD, SEM, and BET analyses. The CO2 capturing performance of these two sorbents was comprehensively evaluated. The influence of the Li/Si ratio, calcination temperature, calcination time, and sorption temperature on the CO2 sorption capacity of Li4SiO4, and the sorption temperature on the CO2 sorption capacity of LDH, were investigated. The optimal leaching acid concentration for vermiculite and the CO2 sorption/desorption cycling performance of both the Li4SiO4 and Mg-Al LDH sorbents were determined. In sum, this demonstrated a unique and environment-friendly scheme for obtaining two CO2 sorbents from cheap raw materials, and this idea is applicable to the efficient utilization of other minerals.

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.

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...

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

The far infrared radiation characteristics for Li2O.Al2O3.4SiO2(LAS) glass-ceramics and transition-metal oxide

International Nuclear Information System (INIS)

Huh, Nam Jung; Yang, Joong Sik

1991-01-01

The far infrared radiation characteristic for Li 2 O.Al 2 O 3 .4SiO 2 (LAS) glass, the LAS glass-ceramic and sintered transition metal oxides such as CuO, Fe 2 O 3 and Co 3 O 4 , were investigated. LAS glass and LAS glass-ceramic was higher than that of the LAS glass. Heat-treated CuO and Co 3 o 4 had radiation characteristic of high efficiency infrared radiant, and heat-treated Fe 2 O 3 had radiation characteristic that infrared emissivity decreased in higher was length above 15μm. (Author)

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.

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)

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)

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.

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.

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

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 .

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.

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.

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.

Impact of Nd{sup 3+} in CoFe{sub 2}O{sub 4} spinel 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.

Flame synthesis of nanoparticles - Applications in catalysis and product/process engineering

DEFF Research Database (Denmark)

Johannessen, Tue; Jensen, Joakim R.; Mosleh, Majid

2004-01-01

High-temperature flame processes for the production of nanoparticles can be applied in chemical product and process engineering. As an example one can produce well-defined spinel structures, e.g. zinc aluminate spinel (ZnAl2O4) and magnesium aluminate spinel (MgAl2O4) with high specific surface a...

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.

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.

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.

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

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.

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

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

Aqueous slip casting of MgAl2O4 spinel powder

Indian Academy of Sciences (India)

The reaction proceeds by counter diffusion of the cations through the product layer, .... tain powders, such as Ube E10 silicon nitride Starck, B10 silicon carbide .... 779 kg/mm2 for a nanocrystalline dense MAS consolidated by aqueous slip ...

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.

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

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.

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.

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

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)

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.

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

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.

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.

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 ...

Formation of a Spinel Coating on AZ31 Magnesium Alloy by Plasma Electrolytic Oxidation

Science.gov (United States)

Sieber, Maximilian; Simchen, Frank; Scharf, Ingolf; Lampke, Thomas

2016-03-01

Plasma electrolytic oxidation (PEO) is a common means for the surface modification of light metals. However, PEO of magnesium substrates in dilute electrolytes generally leads to the formation of coatings consisting of unfavorable MgO magnesium oxide. By incorporation of electrolyte components, the phase constitution of the oxide coatings can be modified. Coatings consisting exclusively of MgAl2O4 magnesium-aluminum spinel are produced by PEO in an electrolyte containing hydroxide, aluminate, and phosphate anions. The hardness of the coatings is 3.5 GPa on Martens scale on average. Compared to the bare substrate, the coatings reduce the corrosion current density in dilute sodium chloride solution by approx. one order of magnitude and slightly shift the corrosion potential toward more noble values.

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.

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.

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

Swelling of spinel after low-dose neutron irradiation

International Nuclear Information System (INIS)

Coghlan, W.A.; Clinard, F.W. Jr.; Itoh, N.; Greenwood, L.R.

1986-01-01

Swelling was determined in samples of single-crystal MgAl 2 O 4 spinel, irradiated to doses as high as 8 x 10 22 n/m 2 (E > 0.1 MeV) at approx. =50 0 C in the Omega West Reactor. Swelling effectively saturated at approx. =2 x 10 22 n/m 2 which corresponds to a damage level of only approx. =2 x 10 -3 dpa. In addition subsequent measurements after irradiation have revealed that the samples continued swelling for several weeks. These results imply that irradiation defects begin to interact by recombination and aggregation at low damage levels in this material at 50 0 C and perhaps continue to cluster at room temperature after irradiation. Rate equations have been employed to determine defect concentrations at saturation. Results to date show that the observed swelling is consistent with the number of surviving defects if swelling per Frenkel defect pair is taken to be one atomic volume

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.

Sintering behaviour of spinel–alumina composites

Indian Academy of Sciences (India)

% alumina dissolves in spinel (MgAl2O4) at 1600°C. Solid solubility of alumina in spinel decreases rapidly with decreasing temperature, which causes exsolution of alumina from spinel phase. Previous work of one of the authors revealed that ...

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

Activation of Mg-Al hydrotalcite catalysts for transesterification of rape oil

Energy Technology Data Exchange (ETDEWEB)

Hong-yan Zeng; Zhen Feng; Xin Deng; Yu-qin Li [University of Xiangtan, Hunan (China). Institute of Biotechnology

2008-10-15

Mg-Al hydrotalcites with different Mg/Al molar ratios were prepared and characterized by powder X-ray diffraction (XRD), Fourier-transform infrared spectra (FTIR), thermogravimetric apparatus and differential thermal analysis (TGA-DTA) and scanning electron micrograph (SEM). It was confirmed by XRD that the materials had hydrotalcite structure. The hydrotalcite catalyst calcined at 773 K with Mg/Al molar ratio of 3.0 exhibited the highest catalytic activity in the transesterification. In addition, a study for optimizing the transesterification reaction conditions such as molar ratio of the methanol to oil, the reaction temperature, the reaction time, the stirring speed and the amount of catalyst, was performed. The optimized parameters, 6:1 methanol/oil molar ratio with 1.5% catalyst (w/w of oil) reacted under stirring speed 300 rpm at 65{sup o}C for 4 h reaction, gave a maximum ester conversion of 90.5%. Moreover, the solid catalyst could be easily separated and possibly reused. 33 refs., 5 figs., 1 tab.

Nd: YAG laser irradiation effects on structural and magnetic properties of Ni1+xZrxFe2-2xO4 nanoparticles

Science.gov (United States)

Saraf, Tukaram S.; Kounsalye, Jitendra S.; Birajdar, Shankar D.; Shamkuwar, N. R.

2018-05-01

The effect of 112 mJ Nd: YAG laser irradiation on structural, morphological, infrared and magnetic properties of Ni1+xZrxFe2-2xO4 spinel ferrite nanoparticles has been systematically investigated in the present work. The sol-gel auto combustion synthesis method was successfully executed for the synthesis of the present system. All the samples were characterized by X-ray diffraction technique (XRD), scanning electron microscopy (SEM) and infrared spectroscopy (IR) technique. The magnetic properties of the present samples were measured by pulse field hysteresis loop technique. All the properties were measured for laser irradiated samples as well, to understand the effect of irradiation on the properties. The single-phase cubic spinel structure was confirmed by X-ray diffraction patterns of all samples and the disordered structure was observed for irradiated samples. The two principle absorption bands in IR spectra also confirm the formation of the spinel structure. Spherical and agglomerated morphology was observed for Zr4+ substituted nickel ferrite, whereas scratched morphology was observed for the irradiated samples. The grain size confirms the nanocrystalline nature, the crystallite size also evident the same. The magnetic parameters decreased after Zr4+ ion doping and strongly influenced by the irradiation.

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.

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.

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.

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)

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.

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.

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)

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.

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

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.

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

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).

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

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.

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.

A comparative investigation of SO2 oxidative transfer over CuO with a CeO2 surface

Science.gov (United States)

Liu, Yifeng; Shen, Benxian; Pi, Zhipeng; Chen, Hua; Zhao, Jigang

2017-04-01

To further improve the catalytic desulfurization function of the Mg-Al spinel sulfur transfer agent in a fluid catalytic cracking (FCC) unit, the reaction paths of SO2 oxidation by O2 over the metal oxide surface of CuO (111) and CeO2 (111) were investigated. In reference to the fact that SO2 reacting with O2 over CuO was a Mars-van Krevelen cycle, a similar reaction law for SO2 oxidation over CeO2 was also verified by characterization methods (e.g., IR, XPS). Meanwhile, the molecular simulation results indicated that the rate-control step of SO2 oxidation over CeO2 (111) and CuO (111) was a SO3 desorption step. The lower energy barrier in the rate-control step corresponded to better catalytic performance; hence, it could explain the reason that CeO2 had a better sulfur oxidization transfer performance than CuO.

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.

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...

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.

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.

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.

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 .

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.

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

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.

Characterization and evaluation of employment of nanostructured spinel MA on oxidation resistance of graffiti; Caracterizacao e avaliacao do emprego de espinelio MA nanoestruturado na resistencia a oxidacao de grafites

Energy Technology Data Exchange (ETDEWEB)

Vitor, P.A.M.; Guaglianoni, W.C.; Braganca, S.R.; Bergmann, C.P., E-mail: pedroaugusto89@hotmail.com [Universidade Federal do Rio Grande do Sul (LACER/UFRS), Porto Alegre, RS (Brazil). Laboratorio de Materiais Ceramicos

2016-07-01

This study aimed to investigate the obtaining of nanostructured powders of spinel MA (MgAl2O4) via synthesis of combustion in solution (SCS), and the influence of its incorporation in oxidation resistance in natural graphites. The crystalline phase only was obtained after a heat treatment at 900 ° C of the powder as-synthesized. The powders were characterized by differential thermal analysis (DTA) and thermogravimetric (ATG) and crystallographic analysis by X-ray diffraction (XRD) and Raman spectroscopy. The results, using thermogravimetric dynamic and isothermal analysis showed a relationship between embedded content of spinel (as-synthesized and calcined) and the raising of the temperature to start the oxidation process (onset temperature) of the samples. The rate of oxidation is reduced at temperatures from 700 ° C, retarding the oxidation of graphite with increasing level of spinel, but this effect ceases at temperatures above 1000 ° C. (author)

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.

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

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.

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

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.

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...

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...

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 ...

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.

Synthesis and optical properties of Mg-Al layered double hydroxides precursor powders

Directory of Open Access Journals (Sweden)

Chia-Hsuan Lin

2017-12-01

Full Text Available The synthesis and optical properties of Mg-Al layered double hydroxide (LDH precursor powders were investigated using X-ray diffraction (XRD, Fourier transform-infrared (FT-IR spectroscopy, transmission electron microscopy (TEM, selected area electron diffraction (SAED, high-resolution TEM (HRTEM, UV-transmission spectrometer, and fluorescence spectrophotometer. The FT-IR results show that the intense absorption at around 1363–1377 cm-1 can be assigned to the antisymmetric ν3 mode of interlayer carbonate anions because the LDH phase contains some CO32-. The XRD results show that all of the Mg-Al LDH precursor powders contain only a single phase of [Mg0.833Al0.167(OH2](CO30.083·(H2O0.75 but have broad and weak intensities of peaks. All of Mg-Al LDHs precursor powders before calcination have the same photoluminescence (PL spectra. Moreover, these spectra were excited at λex = 235 nm, and the broad emission band was in the range 325-650 nm. In the range, there were relatively strong intensity at around 360, 407 and 510 nm, respectively.

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

Newly synthesized MgAl2Ge2: A first-principles comparison with its silicide and carbide counterparts

Science.gov (United States)

Tanveer Karim, A. M. M.; Hadi, M. A.; Alam, M. A.; Parvin, F.; Naqib, S. H.; Islam, A. K. M. A.

2018-06-01

Using plane-wave pseudopotential density functional theory (DFT), the first-principle calculations are performed to investigate the structural aspects, mechanical behaviors and electronic features of the newly synthesized CaAl2Si2-prototype intermetallic compound, MgAl2Ge2 for the first time and the results are compared with those calculated for its silicide and carbide counterparts MgAl2Si2 and MgAl2C2. The calculated lattice constants agree fairly well with their corresponding experimental values. The estimated elastic tensors satisfy the mechanical stability conditions for MgAl2Ge2 along with MgAl2Si2 and MgAl2C2. The level of elastic anisotropy increases following the sequence of X-elements Ge → Si → C. MgAl2Ge2 and MgAl2Si2 are expected to be ductile and damage tolerant, while MgAl2C2 is a brittle one. MgAl2Ge2 and MgAl2Si2 should exhibit better thermal shock resistance and low thermal conductivity and accordingly these can be used as thermal barrier coating (TBC) materials. The Debye temperature of MgAl2Ge2 is lowest among three intermetallic compounds. MgAl2Ge2 and MgAl2Si2 should exhibit metallic conductivity; while the dual characters of weak-metals and semiconductors are expected for MgAl2C2. The values of theoretical Vickers hardness for MgAl2Ge2, MgAl2Si2, and MgAl2C2 are 3.3, 2.7, and 7.7 GPa, respectively, indicating that these three intermetallics are soft and easily machinable.

Quantum efficiencies of near-infrared emission from Ni2+-doped glass-ceramics

International Nuclear Information System (INIS)

Suzuki, Takenobu; Arai, Yusuke; Ohishi, Yasutake

2008-01-01

A systematic method to evaluate potentials of Ni 2+ -doped transparent glass-ceramics as a new broadband optical gain media is presented. At first, near-infrared emission of various ceramics were investigated to explore the suitable crystalline phase to be grown in the glass-ceramics. The quantum efficiency of Ni 2+ near-infrared emission estimated by the Struck-Fonger analysis was higher than 95% for spinel-type structure gallate crystals MgGa 2 O 4 and LiGa 5 O 8 at room temperature. Transparent glass-ceramics containing Ni 2+ :LiGa 5 O 8 could be prepared and the quantum efficiency for the glass-ceramics was measured to be about 10%. This value shows a potential of Ni-doped transparent glass-ceramics as a broadband gain media

Synthesis and characterization of reactions by nanoferrites Co2Fe2O4 combustion

International Nuclear Information System (INIS)

Santos, P.T.A.; Dantas, B.B.; Costa, A.C.F.M.; Araujo, P.M.A.G.

2012-01-01

In this work CoFe 2 O 4 of magnetic nanoparticles were synthesized by combustion reaction and the structural and morphological characteristics of the synthesized samples as well as the parameters of synthesis temperature and reaction time were investigated in order to assess the reproducibility of the synthesis. The maximum temperature and time of the combustion flame were obtained with pyrometer coupled to a computer with online measurement and a stopwatch. The resulting samples were characterized by X-ray diffraction (XRD), infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The maximum temperature achieved during synthesis for all reactions ranged from 623 deg C and 755 deg C. The combustion flame time varied between 18 and 23 seconds. The XRD showed the formation of only CoFe 2 O 4 inverse spinel phase, with crystallite size 28 nm and crystallinity 78%, with typical morphology of the formation of agglomerates of uniform size, brittle and comprising nanoparticles together by weak forces. (author)

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

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.

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.

Dislocation loops in spinel crystals irradiated successively with deep and shallow ion implants

International Nuclear Information System (INIS)

Ai, R.X.; Cooper, E.A.; Sickafus, K.E.; Nastasi, M.; Bordes, N.; Ewing, R.C.

1993-01-01

This study examines the influence of microstructural defects on irradiation damage accumulation in the oxide spinel. Single crystals of the compound MgAl 2 O 4 with surface normal [111] were irradiated under cryogenic temperature (100K) either with 50 keV Ne ions (fluence 5.0 x 10 12 /cm 2 ), 400 keV Ne ions (fluence 6.7 x 10 13 /cm 2 ) or successively with 400 keV Ne ions followed by 50 keV Ne ions. The projected range of 50 keV Ne ions in spinel is ∼50 mn (''shallow'') while the projected range of 400 keV Ne ions is ∼500 mn (''deep''). Transmission electron microscopy (TEM) was used to examine dislocation loops/defect clusters formed by the implantation process. Measurements of the dislocation loop size were made using weak-beam imaging technique on cross-sectional TEM ion-implanted specimens. Defect clusters were observed in both deep and shallow implanted specimens, while dislocation loops were observed in the shallow implanted sample that was previously irradiated by 400 keV Ne ions. Cluster size was seen to increase for shallow implants in crystals irradiated with a deep implant (size ∼8.5 nm) as compared to crystals treated only to a shallow implant (size ∼3.1 nm)

Mixed methanol/ethanol on transesterification of waste cooking oil using Mg/Al hydrotalcite catalyst

International Nuclear Information System (INIS)

Ma, Yingqun; Wang, Qunhui; Zheng, Lu; Gao, Zhen; Wang, Qiang; Ma, Yuhui

2016-01-01

Biodiesel production from waste cooking oil using calcined Mg/Al HT (hydrotalcite) as heterogeneous catalyst was investigated. This study describes the calcined Mg/Al HT prepared under optimal conditions to catalyse waste cooking oil for biodiesel preparation and proposes a plausible catalysis mechanism. The catalysts were characterised by Fourier Transform-Infrared, X-ray diffraction, Thermal Gravity Analysis-Differential thermal gravity and Brunner−Emmet−Teller measurements. Hydrotalcite with Mg/Al ratio of 3:1 showed a uniform mesoporous structure, excellent crystallinity, high surface area (270.5 m 2 /g) and good catalytic activity (at 500 °C calcination). The highest biodiesel yield obtained was 95.2% under optimised conditions of alcohol/oil molar ratio of 6:1, methanol/ethanol molar ratio of 4:2, catalyst content of 1.5%, reaction time of 2.5 h, reaction temperature of 80 °C. Mixed methanol/ethanol showed good synergistic effects as an ester exchange agent, and the catalyst was easily separated and recycled. Therefore, Mg/Al hydrotalcite can effectively catalyse waste cooking oil for biodiesel preparation with mixed methanol/ethanol. - Highlights: • Mg/Al hydrotalcite filtered and stirred with acetone has the better dispersion. • Mg/Al hydrotalcite used as catalyst to prepare biodiesel. • Catalytic mechanism of Mg/Al hydrotalcite was investigated. • Mixed Methanol/Ethanol used as transesterification agent to prepare biodiesel. • Regenerative catalyst was assessed to make catalyst reuse well.

Combustion synthesis of AlB2-Al2O3 composite powders with AlB2 nanowire structures

Science.gov (United States)

Yang, Pan; Xiao, Guoqing; Ding, Donghai; Ren, Yun; Yang, Shoulei; Lv, Lihua; Hou, Xing

2018-05-01

Using of Al and B2O3 powders as starting materials, and Mg-Al alloy as additives, AlB2-Al2O3 composite powders with AlB2 nanowire structures were successfully fabricated via combustion synthesis method in Ar atmosphere at a pressure of 1.5 MPa. The effect of different amount of Mg-Al alloy on the phase compositions and morphology of the combustion products was investigated. The results revealed that AlB2 and Al2O3 increased, whereas Al decreased with the content of Mg-Al alloy increasing. The impurities MgAl2O4 and AlB12 would exist in the sample with adding of 18 wt% Mg-Al alloy. Interestingly, FESEM/TEM/EDS results showed that AlB2 nanowires were observed in the products when the content of Mg-Al alloy is 6 wt% and 12 wt%. The more AlB2 nanowires can be found as the content of Mg-Al alloy increased. And the yield of AlB2 nanowires with the diameter of about 200 nanometers (nm) and the length up to several tens of micrometers (μm) in the combustion product is highest when the content of Mg-Al alloy is 12 wt%. The vapor, such as Mg-Al (g), B2O2 (g), AlO (g) and Al2O (g), produced during the process of combustion synthesis, reacted with each other to yield AlB2 nanowires by vapor-solid (VS) mechanism and the corresponding model was also proposed.

Nanosized spinel oxide catalysts for CO-oxidation prepared via CoMnMgAl quaternary hydrotalcite route

Energy Technology Data Exchange (ETDEWEB)

Mokhtar, M., E-mail: mmoustafa@kau.edu.s [Chemistry Department, Faculty of Science, King Abdulaziz University, 21589 Jeddah, P.O. Box 80203 (Saudi Arabia); Basahel, S.N.; Al-Angary, Y.O. [Chemistry Department, Faculty of Science, King Abdulaziz University, 21589 Jeddah, P.O. Box 80203 (Saudi Arabia)

2010-03-18

Catalytic activity of the Co-Mn-Mg-Al mixed oxide spinel catalysts was examined in CO oxidation by O{sub 2}. The prepared catalysts were characterized by chemical analysis (ICP), infrared spectroscopy (FTIR), thermal analysis (TG, DTG), powder X-ray diffraction (XRD), surface area measurements, and scanning electron microscopy (SEM).The calcined hydrotalcite-like precursor was composed of spinel-like Co-Mn-Mg-Al mixed oxide as the only XRD crystalline phases. The nanosized spinel oxide catalysts produced by calcination of hydrotalcites showed higher S{sub BET} than CoMn-hydrotalcite samples as calcination led to dehydroxylation and carbonate decomposition of anions in interlayer spaces. All the catalysts showed 100% CO conversion at high temperature even those calcined at 800 {sup o}C. A catalyst with Co/Mn = 4 and calcined at 500 {sup o}C showed 100% CO conversion at 160 {sup o}C. Moreover, this catalyst exhibited quite good durability without deactivation in 60 h stability test.

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

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.

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)

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.

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

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

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)

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)

Symmetry transition via tetravalent impurity and investigations on magnetic properties of Li0.5Fe2.5O4

Science.gov (United States)

Kounsalye, Jitendra S.; Kharat, Prashant B.; Chavan, Apparao R.; Humbe, Ashok V.; Borade, R. M.; Jadhav, K. M.

2018-04-01

The present study, deals with the phase symmetry transformation of lithium ferrite after introducing tetravalent (Ti4+) impurity. The sol-gel auto combustion technique was adopted for the synthesis of nanoparticle samples with generic chemical formula Li0.5Fe2.5O4 and Li0.55Ti0.10Fe2.35O4. The synthesized nanoparticles were characterized by X-ray diffraction (XRD) technique for structural analysis. The XRD patterns show the single phase cubic structure without any impurity phase but the P4332 to Fd-3m transformation was observed after introducing Ti4+ impurity. The Nano size of the synthesized particles was confirmed by crystallite size ( 20nm) calculated using Debye-Scherrer's formula. The Fourier transform infrared spectroscopy (FTIR) studies shows shifting of band frequencies which reflect the structural changes after tetravalent substitutional impurities. The magnetic properties were studied through pulse field hysteresis loop (M-H loop) technique at room temperature, the M-H loops showdecrease in magnetic properties afternonmagnetic Ti4+ ion substitution. This is attributed to transition of inverse spinel structure of lithium ferrite to random spinel structure.

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.

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.

Synthesis and characterization of reactions by nanoferrites Co{sub 2}Fe{sub 2}O{sub 4} combustion; Sintese por reacao de combustao e caracterizacao de nanoparticulas de Co{sub 2}Fe{sub 2}O{sub 4}

Energy Technology Data Exchange (ETDEWEB)

Santos, P.T.A.; Dantas, B.B.; Costa, A.C.F.M.; Araujo, P.M.A.G., E-mail: polyanaquimica@yahoo.com.br [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Departamento de Engenharia de Materiais

2012-07-01

In this work CoFe{sub 2}O{sub 4} of magnetic nanoparticles were synthesized by combustion reaction and the structural and morphological characteristics of the synthesized samples as well as the parameters of synthesis temperature and reaction time were investigated in order to assess the reproducibility of the synthesis. The maximum temperature and time of the combustion flame were obtained with pyrometer coupled to a computer with online measurement and a stopwatch. The resulting samples were characterized by X-ray diffraction (XRD), infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The maximum temperature achieved during synthesis for all reactions ranged from 623 deg C and 755 deg C. The combustion flame time varied between 18 and 23 seconds. The XRD showed the formation of only CoFe{sub 2}O{sub 4} inverse spinel phase, with crystallite size 28 nm and crystallinity 78%, with typical morphology of the formation of agglomerates of uniform size, brittle and comprising nanoparticles together by weak forces. (author)

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.

MZnFe{sub 2}O{sub 4} (M = Ni, Mn) cubic superparamagnetic nanoparticles obtained by hydrothermal synthesis

Energy Technology Data Exchange (ETDEWEB)

Freire, R. M. [Universidade Federal do Ceara-UFC, Grupo de Quimica de Materiais Avancados (GQMAT)- Departamento de Quimica Analitica e Fisico-Quimica (Brazil); Ribeiro, T. S.; Vasconcelos, I. F. [Universidade Federal do Ceara, Departamento de Engenharia Metalurgica e de Materiais (Brazil); Denardin, J. C. [Universidad de Santiago de Chile, USACH, Departamento de Fisica (Chile); Barros, E. B. [Universidade Federal do Ceara-UFC, Departamento de Fisica (Brazil); Mele, Giuseppe [Universita del Salento, Dipartimento di Ingegneria dell' Innovazione (Italy); Carbone, L. [IPCF-CNR, UOS Pisa (Italy); Mazzetto, S. E.; Fechine, P. B. A., E-mail: fechine@ufc.br [Universidade Federal do Ceara-UFC, Grupo de Quimica de Materiais Avancados (GQMAT)- Departamento de Quimica Analitica e Fisico-Quimica (Brazil)

2013-05-15

MZnFe{sub 2}O{sub 4} (M = Ni or Mn) cubic nanoparticles have been prepared by hydrothermal synthesis in mild conditions and short time without any procedure of calcinations. The structural and magnetic properties of the mixed ferrites were investigated by X-ray diffraction, Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, Moessbauer spectroscopy, vibrating sample magnetometer, and Transmission electron microscopy (TEM). X-ray analysis showed peaks characteristics of the spinel phase. The average diameter of the nanoparticles observed by TEM measurements was approximately between 4 and 10 nm. Spectroscopy study of the spinel structure was performed based on Group Theory. The predicted bands were observed in FTIR and Raman spectrum. The magnetic parameters and Moessbauer spectroscopy were measured at room temperature and superparamagnetic behavior was observed for mixed ferrites. This kind of nanoparticles can be used as precursor in drug delivery systems, magnetic hyperthermia, ferrofluids, or magnetic imaging contrast agents.

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.

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.

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

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.

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

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...

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.

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}.

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.

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)

High-pressure X-ray diffraction and Raman spectroscopy of CaFe2O4-type β-CaCr2O4

Science.gov (United States)

Zhai, Shuangmeng; Yin, Yuan; Shieh, Sean R.; Shan, Shuangming; Xue, Weihong; Wang, Ching-Pao; Yang, Ke; Higo, Yuji

2016-04-01

In situ high-pressure synchrotron X-ray diffraction and Raman spectroscopic studies of orthorhombic CaFe2O4-type β-CaCr2O4 chromite were carried out up to 16.2 and 32.0 GPa at room temperature using multi-anvil apparatus and diamond anvil cell, respectively. No phase transition was observed in this study. Fitting a third-order Birch-Murnaghan equation of state to the P-V data yields a zero-pressure volume of V 0 = 286.8(1) Å3, an isothermal bulk modulus of K 0 = 183(5) GPa and the first pressure derivative of isothermal bulk modulus K 0' = 4.1(8). Analyses of axial compressibilities show anisotropic elasticity for β-CaCr2O4 since the a-axis is more compressible than the b- and c-axis. Based on the obtained and previous results, the compressibility of several CaFe2O4-type phases was compared. The high-pressure Raman spectra of β-CaCr2O4 were analyzed to determine the pressure dependences and mode Grüneisen parameters of Raman-active bands. The thermal Grüneisen parameter of β-CaCr2O4 is determined to be 0.93(2), which is smaller than those of CaFe2O4-type CaAl2O4 and MgAl2O4.

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)

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.

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.

Nd:YAG laser irradiation effects on electrical properties of polycrystalline Li{sub 0.5}Fe{sub 2.5}O{sub 4}

Energy Technology Data Exchange (ETDEWEB)

Mane, Maheshkumar L., E-mail: mane.maheshkumar@hotmail.com [Department of physics, Dr. Babasaheb Ambedkar Marathwada University, Aurangabad (M.S.) 431 004 (India); Dhage, V.N.; Shirsath, Sagar E. [Department of physics, Dr. Babasaheb Ambedkar Marathwada University, Aurangabad (M.S.) 431 004 (India); Sundar, R.; Ranganathan, K.; Oak, S.M. [Solid State Laser Division, Raja Ramanna Centre for Advanced Technology, Indore (M.P.) (India); Jadhav, K.M. [Department of physics, Dr. Babasaheb Ambedkar Marathwada University, Aurangabad (M.S.) 431 004 (India)

2012-01-15

Highlights: > Standard double sintering ceramic method. > Infrared and electrical properties of spinel ferrite. > Laser irradiation study. > Conduction mechanism. > Temperature dependence dielectric properties. - Abstract: The polycrystalline spinel structured Li{sub 0.5}Fe{sub 2.5}O{sub 4} ferrite have been prepared by conventional double sintering ceramic method. The samples were palletized and irradiated by Nd:YAG laser with different laser fluencies and characterized by infrared spectroscopy and DC electrical resistivity in order to obtain phase, crystal structure and conduction mechanism in pristine and irradiated samples. The infrared spectroscopy is employed to study the local symmetry and conduction mechanism in crystalline solids before and after irradiation. The DC electrical resistivity measured by two-probe technique from room temperature to beyond Curie temperature with steps of 10 K increases after laser irradiation. Variation of dielectric properties like dielectric constant and dielectric loss tangent is also measured as a function of temperature. A significant reduction in the values of dielectric constant and dielectric loss tangent has been observed with the increase of laser dose.

Submillimeter H2O and H2O+emission in lensed ultra- and hyper-luminous infrared galaxies at z 2-4

NARCIS (Netherlands)

Yang, C.; Omont, A.; Beelen, A.; González-Alfonso, E.; Neri, R.; Gao, Y.; van der Werf, P.; Weiß, A.; Gavazzi, R.; Falstad, N.; Baker, A. J.; Bussmann, R. S.; Cooray, A.; Cox, P.; Dannerbauer, H.; Dye, S.; Guélin, M.; Ivison, R.; Krips, M.; Lehnert, M.; Michałowski, M. J.; Riechers, D. A.; Spaans, M.; Valiante, E.

2016-01-01

We report rest-frame submillimeter H2O emission line observations of 11 ultra- or hyper-luminous infrared galaxies (ULIRGs or HyLIRGs) at z 2-4 selected among the brightest lensed galaxies discovered in the Herschel-Astrophysical Terahertz Large Area Survey (H-ATLAS). Using the IRAM NOrthern

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.

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 .

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