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.

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.

Anisotropic dislocation loop nucleation in ion-irradiated MgAl2O4

International Nuclear Information System (INIS)

Zinkle, S.J.

1991-01-01

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

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)

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-04-01

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

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)

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

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.

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.

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.

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 ...

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 .

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.

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.

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.

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

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

Thermodynamics of CoAl2O4-CoGa2O4 solid solutions

International Nuclear Information System (INIS)

Lilova, Kristina I.; Navrotsky, Alexandra; Melot, Brent C.; Seshadri, Ram

2010-01-01

CoAl 2 O 4 , CoGa 2 O 4 , and their solid solution Co(Ga z Al 1-z ) 2 O 4 have been studied using high temperature oxide melt solution calorimetry in molten 2PbO.B 2 O 3 at 973 K. There is an approximately linear correlation between lattice parameters, enthalpy of formation from oxides, and the Ga content. The experimental enthalpy of mixing is zero within experimental error. The cation distribution parameters are calculated using the O'Neill and Navrotsky thermodynamic model. The enthalpies of mixing calculated from these parameters are small and consistent with the calorimetric data. The entropies of mixing are calculated from site occupancies and compared to those for a random mixture of Ga and Al ions on octahedral site with all Co tetrahedral and for a completely random mixture of all cations on both sites. Despite a zero heat of mixing, the solid solution is not ideal in that activities do not obey Raoult's Law because of the more complex entropy of mixing. - Graphical abstract: Measured enthalpies of mixing of CoAl 2 O 4 -CoGa 2 O 4 solid solutions are close to zero but entropies of mixing reflect the complex cation distribution, so the system is not an ideal solution.

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.

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)

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

Directory of Open Access Journals (Sweden)

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.

Solid solutions in the system Nd2(SeO4)3 - Sm2(SeO4)3 - H2O

International Nuclear Information System (INIS)

Serebrennikov, V.V.; Tsybukova, T.N.; Velikov, A.A.

1984-01-01

Using the method of isothermal solubility at 25 deg C the system Nd 2 (SeO 4 ) 3 -Sm 2 (SeO 4 ) 3 -H 2 O has been studied. Roentgenographic recording of solid ''residues'' is realized. For solid solutions energies of interchange and formation heats are calculated. Formation heats of solid solutions on the basis of samarium selenates are also found experimentally

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.

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

Directory of Open Access Journals (Sweden)

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.

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.

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.

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.)

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.

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)

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

Directory of Open Access Journals (Sweden)

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.

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

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

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)

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.

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...

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.

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.

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....

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

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.

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)

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...

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.

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.

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

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)

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....

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.

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.

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).

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.

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)

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.

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.

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.

Systems Li2B4O7 (Na2B4O7, K2B4O7)-N2H3H4OH-H2O at 25 deg C

International Nuclear Information System (INIS)

Skvortsov, V.G.; Sadetdinov, Sh.V.; Akimov, V.M.; Mitrasov, Yu.N.; Petrova, O.V.; Klopov, Yu.N.

1994-01-01

Phase equilibriums in the Li 2 B 4 O 7 (Na 2 B 4 O 7 , K 2 B 4 O 7 )-N 2 H 3 H 4 OH-H 2 O systems were investigated by methods of isothermal solubility, refractometry and PH-metry at 25 deg C for the first time. Lithium and sodium tetraborates was established to form phases of changed composition mM 2 B 4 O 7 ·nN 2 H 3 C 2 H 4 OH·XH 2 O, where M=Li, Na with hydrazine ethanol. K 2 B 4 O 7 ·4H 2 O precipitates in solid phase in the case of potassium salt. Formation of isomorphous mixtures was supported by X-ray diffraction and IR spectroscopy methods

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)

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.

Systems of OsO4-RuO4 and Re2O7-OsO4

International Nuclear Information System (INIS)

Nisel'son, L.A.; Sokolova, T.D.; Orlov, A.M.; Shorikov, Yu.S.

1981-01-01

The meltability diagrams of the systems OsO 4 -RuO 4 and Re 2 O 7 -OsO 4 are studied using the visual-polythermal method. The OsO 4 -RuO 4 system forms a continuous series of solid solutions with practically rectilinear line of the liquidus. The Re 2 O 7 -OsO 4 system of the eutectic type has the eutectics degenerated from the side of OsO 4 . For the system OsO 4 (basis)-RuO 4 (admixture) the equilibrium coefficient of distribution is determined using the method of directed crystallization [ru

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.

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

International Nuclear Information System (INIS)

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

2006-01-01

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

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

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...

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

Directory of Open Access Journals (Sweden)

Pošarac Milica

2009-01-01

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

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

LaCrO3/CuFe2O4 Composite-Coated Crofer 22 APU Stainless Steel Interconnect of Solid Oxide Fuel Cells

Science.gov (United States)

Hosseini, Seyedeh Narjes; Enayati, Mohammad Hossein; Karimzadeh, Fathallah; Dayaghi, Amir Masoud

2017-07-01

Rapidly rising contact resistance and cathode Cr poisoning are the major problems associated with unavoidable chromia scale growth on ferritic stainless steel (FSS) interconnects of solid oxide fuel cells. This work investigates the performance of the novel screen-printed composite coatings consisting of dispersed conductive LaCrO3 particles in a CuFe2O4 spinel matrix for Crofer 22 APU FSS, with emphasis on the oxidation behavior and electrical conductivity of these coatings. The results show that the presence of protective spinel coating, accompanied by the effective role of LaCrO3 particle incorporation, prevents the Cr2O3 subscale growth as well as chromium migration into the coating surface at the end of 400 hours of oxidation at 1073 K (800 °C) in air. In addition, the composite coatings decreased the area specific resistance (ASR) from 51.7 and 13.8 mΩ cm2 for uncoated and spinel-coated samples, respectively, to a maximum of 7.7 mΩ cm2 for composite-coated samples after 400 hours of oxidation.

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.

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

TL and OSL properties of Mn2+-doped MgGa2O4 phosphor

Science.gov (United States)

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

2018-04-01

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

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.

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

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.

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....

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

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

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...

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 equilibrium in Rb2MoO4-AMoO4-Zr(MOO4)2 systems (A - bivalent elements)

International Nuclear Information System (INIS)

Ivanova, M.N.; Tsyrenova, G.D.; Bazarova, Zh.G.

1993-01-01

The Rb 2 MoO 4 -AMoO 4 -Zr(MoO 4 ) 2 systems, where A - bivalent elements, were investigated by solid phase reactions, x-ray and differntial thermal analysis methods. Formation of new ternary molybdates was determined. Phase relationships in the Rb 2 MoO 4 -MnMoO 4 -Zr(MoO 4 ) 2 system in subsolidus range (550 deg C) were studied using x-ray analysis data

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

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%

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)

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

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.

Phase formation in the systems ZrO2-H2SO4-Na2SO4 (NaCl)-H2O

International Nuclear Information System (INIS)

Sozinova, Yu.P.; Motov, D.L.; Rys'kina, M.P.

1988-01-01

Formation of solid phases in the systems ZrO 2 - H 2 SO 4 - Na 2 SO 4 (NaCl) - H 2 O at 25 and 75 deg C is studied. Three basic Na 2 Zr(OH) 2 (SO 4 ) 2 x (0.2 - 0.4)H 2 O, NaZrOH(SO 4 ) 2 x H 2 O, NaZrO 0.5 (OH) 2 SO 4 x 2H 2 O and three normal sodium sulfatozirconates Na 2 Zr(SO 4 ) 3 x 3H 2 O, Na 4 Zr(SO 4 ) 4 x 3H 2 O, Na 6 Zr(SO 4 ) 5 x 4H 2 O have been isolated, their solubility and crystal optical properties are determined

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

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

Directory of Open Access Journals (Sweden)

Peltekov A.B.

2013-01-01

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

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.

High-Pressure Phase Relations and Crystal Structures of Postspinel Phases in MgV2O4, FeV2O4, and MnCr2O4: Crystal Chemistry of AB2O4 Postspinel Compounds.

Science.gov (United States)

Ishii, Takayuki; Sakai, Tsubasa; Kojitani, Hiroshi; Mori, Daisuke; Inaguma, Yoshiyuki; Matsushita, Yoshitaka; Yamaura, Kazunari; Akaogi, Masaki

2018-06-04

We have investigated high-pressure, high-temperature phase transitions of spinel (Sp)-type MgV 2 O 4 , FeV 2 O 4 , and MnCr 2 O 4 . At 1200-1800 °C, MgV 2 O 4 Sp decomposes at 4-7 GPa into a phase assemblage of MgO periclase + corundum (Cor)-type V 2 O 3 , and they react at 10-15 GPa to form a phase with a calcium titanite (CT)-type structure. FeV 2 O 4 Sp transforms to CT-type FeV 2 O 4 at 12 GPa via decomposition phases of FeO wüstite + Cor-type V 2 O 3 . MnCr 2 O 4 Sp directly transforms to the calcium ferrite (CF)-structured phase at 10 GPa and 1000-1400 °C. Rietveld refinements of CT-type MgV 2 O 4 and FeV 2 O 4 and CF-type MnCr 2 O 4 confirm that both the CT- and CF-type structures have frameworks formed by double chains of edge-shared B 3+ O 6 octahedra (B 3+ = V 3+ and Cr 3+ ) running parallel to one of orthorhombic cell axes. A relatively large A 2+ cation (A 2+ = Mg 2+ , Fe 2+ , and Mn 2+ ) occupies a tunnel-shaped space formed by corner-sharing of four double chains. Effective coordination numbers calculated from eight neighboring oxygen-A 2+ cation distances of CT-type MgV 2 O 4 and FeV 2 O 4 and CF-type MnCr 2 O 4 are 5.50, 5.16, and 7.52, respectively. This implies that the CT- and CF-type structures practically have trigonal prism (six-coordinated) and bicapped trigonal prism (eight-coordinated) sites for the A 2+ cations, respectively. A relationship between cation sizes of VIII A 2+ and VI B 3+ and crystal structures (CF- and CT-types) of A 2+ B 2 3+ O 4 is discussed using the above new data and available previous data of the postspinel phases. We found that CF-type A 2+ B 2 3+ O 4 crystallize in wide ionic radius ranges of 0.9-1.4 Å for VIII A 2+ and 0.55-1.1 Å for VI B 3+ , whereas CT-type phases crystallize in very narrow ionic radius ranges of ∼0.9 Å for VIII A 2+ and 0.6-0.65 Å for VI B 3+ . This would be attributed to the fact that the tunnel space of CT-type structure is geometrically less flexible due to the smaller coordination

Solid-state synthesis of Li_4Ti_5O_1_2 whiskers from TiO_2-B

International Nuclear Information System (INIS)

Yao, Wenjun; Zhuang, Wei; Ji, Xiaoyan; Chen, Jingjing; Lu, Xiaohua; Wang, Changsong

2016-01-01

Highlights: • The Li_4Ti_5O_1_2 whiskers were synthesized from TiO_2-B whiskers via a solid state reaction. • The TiO_2-B crystal structure for lithium diffusion is easier than anatase. • The separated diffusion and reaction process is crucial for the solid-state syntheses of Li_4Ti_5O_1_2 whiskers. - Abstract: In this work, Li_4Ti_5O_1_2 (LTO) was synthesized from the precursors of TiO_2-B and anatase whiskers, respectively. The synthesized LTO whiskers from TiO_2-B whiskers via a solid state reaction at 650 °C have a high degree of crystallinity with an average diameter of 300 nm. However, when anatase whiskers were used as the precursor, only particle morphology LTO was produced at 750 °C. The further analysis of the precursors, the intermediate products and the final products reveal that the crystal structure of the anatase hinders the diffusion of lithium, leading to a typical reaction–diffusion process. Under this condition, only particle morphology LTO can be produced. However, the crystal structure of the TiO_2-B is easy for lithium diffusion and the process is performed in two separated steps (i.e., diffusion and reaction), which makes it possible to decrease the solid-state reaction temperature down to 650 °C and then maintain the morphologies of whiskers.

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...

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.

Checkerboard deposition of lithium manganese oxide spinel (LiMn2O4) by RF magnetron sputtering on a stainless steel in all-solid-state thin film battery

Science.gov (United States)

Hsueh, T. H.; Yu, Y. Q.; Jan, D. J.; Su, C. H.; Chang, S. M.

2018-03-01

All-solid-state thin film lithium batteries (TFLBs) are the most competitive low-power sources to be applied in various kinds of micro-electro-mechanical systems and have been draw a lot of attention in academic research. In this paper, the checkerboard deposition of all-solid-state TFLB was composed of thin film lithium metal anode, lithium phosphorus oxynitride (LiPON) solid electrolyte, and checkerboard deposition of lithium manganese oxide spinel (LiMn2O4) cathode. The LiPON and LiMn2O4 were deposited by a radio frequency magnetron sputtering system, and the lithium metal was deposited by a thermal evaporation coater. The electrochemical characterization of this lithium battery showed the first discharge capacity of 107.8 μAh and the capacity retention was achieved 95.5% after 150 charge-discharge cycles between 4.3V and 3V at a current density of 11 μA/cm2 (0.5C). Obviously, the checkerboard of thin film increased the charge exchange rate; also this lithium battery exhibited high C-rate performance, with better capacity retention of 82% at 220 μA/cm2 (10C).

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.

Complexing in (NH4)2SeO4-UO2SeO4 H2O system

International Nuclear Information System (INIS)

Serezhkina, L.B.

1994-01-01

Isotherm of solubility in the (NH 4 ) 2 SeO 4 -UO 2 SeO 4 -H 2 O system has been constructed at 25 deg C. (NH 4 ) 2 (UO 2 ) 2 (SeO 4 ) 3 x6H 2 O formation is established for the first time and certain its physicochemical properties are determined. Regularities of complexing in the R 2 Se) 4 -UO 2 SeO 4 -H 2 O systems, where R-univalent cation are under discussion. 6 refs.; 3 tabs

Cu4Pr6(MoO4)11-Pr2(MoO4)3 system

International Nuclear Information System (INIS)

Arzumanyan, G.A.

1982-01-01

Existence boundaries and Dalton compositions (CuPr(MoO 4 ) 2 , CuPr 3 (MoO 4 ) 5 ) of solid solutions that in the mojority are of shcheelite dsitored structure have been determined in the Cu 4 Pr 6 (MoO 4 ) 11 -Pr 2 (MoO 4 ) 3 system. It has been revealed that regions of homogeneity near the CuPr(MoO 4 ) 2 composition have a horseshoeshaped profile

Conductivity And Thermal Stability of Solid Acid Composites CsH2PO4 /NaH2PO4/ SiO2

International Nuclear Information System (INIS)

Norsyahida Mohammad; Abu Bakar Mohamad; Abu Bakar Mohamad; Abdul Amir Hassan Kadhum

2016-01-01

Solid acid composites CsH 2 PO 4 / NaH 2 PO 4 / SiO 2 with different mole ratios of CsH 2 PO 4 and NaH 2 PO 4 to SiO 2 were synthesized and characterized. Preliminary infrared measurements of CsH 2 PO 4 and its composites indicated that hydrogen bonds breaking and formation were detected between 1710 to 2710 cm -1 , while the rotation of phosphate tetrahedral anions occurred between 900 and 1200 cm -1 . The superprotonic transition of CsH 2 PO 4 / NaH 2 PO 4 / SiO 2 composite was identified at superprotonic temperatures between 230 and 260 degree Celcius, under atmospheric pressure. This study reveals higher conductivity values for composites with higher CsH 2 PO 4 (CDP) content. Solid acid composite CDP 613 appeared as the composite with the highest conductivity that is 7.2x10 -3 S cm -1 at 230 degree Celcius. Thermal stability of the solid acid composites such as temperature of dehydration, melting and decomposition were investigated. The addition of NaH 2 PO 4 lowers the dehydration temperature of the solid acid composites. (author)

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.

Phase formation in the Li2MoO4–Rb2MoO4–Fe2(MoO4)3 system and crystal structure of a novel triple molybdate LiRb2Fe(MoO4)3

International Nuclear Information System (INIS)

Khal'baeva, Klara M.; Solodovnikov, Sergey F.; Khaikina, Elena G.; Kadyrova, Yuliya M.; Solodovnikova, Zoya A.; Basovich, Olga M.

2013-01-01

X-ray investigation of solid state interaction of the components in the Li 2 MoO 4 –Rb 2 MoO 4 –Fe 2 (MoO 4 ) 3 system was carried out, and a subsolidus phase diagram of the said system was constructed. The subsystem Rb 2 MoO 4 –LiRbMoO 4 –RbFe(MoO 4 ) 2 was shown to be non-quasiternary. Formation of a novel triple molybdate LiRb 2 Fe(MoO 4 ) 3 was established, conditions of solid state synthesis and crystallization of the compound were found. Its crystal structure (orthorhombic, space group Pnma, Z=4, a=24.3956(6), b=5.8306(1), c=8.4368(2) Å) represents a new structure type and includes infinite two-row ribbons ([Fe(MoO 4 ) 3 ] 3− ) ∞ parallel to the b axis and composed of FeO 6 octahedra, terminal Mo(3)O 4 tetrahedra, and bridge Mo(1)O 4 and Mo(2)O 4 tetrahedra connecting two or three FeO 6 octahedra. The ribbons are connected to form 3D framework via corner-sharing LiO 4 tetrahedra. Rubidium cations are 11- and 13-coordinated and located in cavities of this heterogeneous polyhedral framework. - Graphical abstract: Exploring the Li 2 MoO 4 –Rb 2 MoO 4 –Fe 2 (MoO 4 ) 3 system showed its partial non-quasiternarity and revealed a new compound LiRb 2 Fe(MoO 4 ) 3 which was structurally studied. - Highlights: • The Li 2 MoO 4 –Rb 2 MoO 4 –Fe 2 (MoO 4 ) 3 system study revealed a new compound LiRb 2 Fe(MoO 4 ) 3 . • Its structure of a new type includes ribbons of FeO 6 octahedra and MoO 4 tetrahedra. • The ribbons are connected into a 3D framework via corner-sharing LiO 4 tetrahedra

Three new d10 transition metal selenites containing PO4 tetrahedron: Cd7(HPO4)2(PO4)2(SeO3)2, Cd6(PO4)1.34(SeO3)4.66 and Zn3(HPO4)(SeO3)2(H2O)

Science.gov (United States)

Ma, Yun-Xiang; Gong, Ya-Ping; Hu, Chun-li; Mao, Jiang-Gao; Kong, Fang

2018-06-01

Three new d10 transition metal selenites containing PO4 tetrahedron, namely, Cd7(HPO4)2(PO4)2(SeO3)2 (1), Cd6(PO4)1.34(SeO3)4.66 (2) and Zn3(HPO4)(SeO3)2(H2O) (3), have been synthesized by hydrothermal reaction. They feature three different structural types. Compound 1 exhibits a novel 3D network composed of 3D cadmium selenite open framework with phosphate groups filled in the 1D helical tunnels. The structure of compound 2 displays a new 3D framework consisted of 2D cadmium oxide layers bridged by SeO3 and PO4 groups. Compound 3 is isostructural with the reported solids of Co3(SeO3)3-x(PO3OH)x(H2O) when x is equal to 1.0. Its structure could be viewed as a 3D zinc oxide open skeleton with SeO3 and HPO4 polyhedra attached on the wall of the tunnels. They represent the only examples in metal selenite phosphates in addition to the above cobalt compounds. Optical diffuse reflectance spectra revealed that these solids are insulators, which are consistent with the results of band structure computations based on DFT algorithm.

Nd(BrO3)3-Yb(BrO3)3-H2O and Nd2(SeO4)3-Yb2(SeO4)3-H2O systems at 25 deg C

International Nuclear Information System (INIS)

Serebrennikov, V.V.; Batyreva, V.A.; Tsybukova, T.N.

1981-01-01

Using the methods of isothermal solubility the Nd(BrO 3 ) 3 - Yb(BrO 3 ) 3 -H 2 O and Nd 2 (SeO 4 ) 3 -Yb 2 (SeO 4 ) 3 -H 2 O systems are studied at 25 deg C. The compositions of the solid phases are determined by the method of ''residues''. The formation of two series of solid solutions in both systems is established. Besides, there is a crystallization region of Nd 2 (SeO 4 ) 3 in the system of selenates. The solubility diagrams of the systems are presented [ru

Structural characterization and electrochemical behaviour of Li{sub (4−x)/3}Ti{sub (5−2x)/3}Mn{sub x}O{sub 4} solid solution with spinel-structure

Energy Technology Data Exchange (ETDEWEB)

Martín, P., E-mail: pmartinp@quim.ucm.es; López, M.L.; Pico, C.; Veiga, M.L.

2013-07-15

A series of new oxides Li{sub (4−x)/3}Ti{sub (5−2x)/3}Mn{sub x}O{sub 4} (0.1 ≤ x ≤ 0.9) have been synthesized by solid state reactions and characterized by thermal analysis and X-ray and neutron diffraction. In all phases, Li{sup +} cations mainly occupy tetrahedral sites and transition metals cations are located on the octahedral ones. These phases show a structural disorder–order transition associated to the proportion of manganese in the samples and to its oxidation state. All these factors have a marked influence on the electrochemical properties and the phase x = 0.1 shows the best characteristics to be used as anode in a solid state battery. - Highlights: • Lithium spinels anodes in batteries. • Influence of Ti/Mn ratio in the electrochemical behaviour. • Li{sub 1.3}Ti{sub 1.6}Mn{sub 0.1}O{sub 4}: a promising zero-strain material. • Influence of disorder–order transitions on the physical properties.

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

International Nuclear Information System (INIS)

Liu, Bao-Sheng; Wang, Zhen-Bo; Zhang, Yin; Yu, Fu-Da; Xue, Yuan; Ke, Ke; Li, Fang-Fei

2015-01-01

Graphical abstract: Spinal LiMn 2 O 4 particles synthesized at 800 °C for 12 h has the best crystallinity with a submicron size and smallest cation disorder, resulting in a superior capacity retention ratio of 90.4% after 200 cycles at 1 °C at room temperature, which possesses an initial capacity of 106.8 mA h/g. - Highlights: • High purity spinel LiMn 2 O 4 was synthesized from industrial grade raw materials. • LiMn 2 O 4 prepared by optimal conditions has the smallest cation mixing. • Optimized LiMn 2 O 4 has the highest initial capacity with 112.9 mA h/g. • Capacity retention of optimized LiMn 2 O 4 is 90.4% after 200 cycles at 1 °C. - Abstract: Spinel LiMn 2 O 4 has been synthesized by solid state reaction with industrial grade Mn 3 O 4 and Li 2 CO 3 as precursors without purification, and its electrochemical performance for lithium ion battery has been investigated by CR2025 coin cell. The results of X-ray diffraction (XRD) patterns and scanning electron microscope (SEM) images show that the size of LiMn 2 O 4 particles grow up with increasing temperature of calcination, and the sample synthesized at 800 °C for 12 h has the best crystallinity with a submicron size. It can deliver initial capacity of 112.9 mA h/g with capacity retention ratio of 89.1% after 200 cycles at charge/discharge rate of 1 C. The results of cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) also show that it has the highest electrochemical activity and lowest charge transfer impedance

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

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.

Topotactic synthesis of Co3O4 nanoboxes from Co(OH)2 nanoflakes

International Nuclear Information System (INIS)

Tian Li; Huang Kelong; Liu Younian; Liu Suqin

2011-01-01

Hollow nanocubes of spinel Co 3 O 4 with the dimension of 20 nm were successfully prepared via a facile and reproducible solvothermal route. The structure and morphology of Co 3 O 4 nanoboxes were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and high-resolution transmission electron microscope (HRTEM) techniques. And a possible growth mechanism of Co 3 O 4 nanoboxes were suggested that solid Co 3 O 4 nanocubes nucleate in-situ and grow epitaxially from hexagonal β-Co(OH) 2 precursors with the structural matching relationship of [0 0 1] β-Co(OH) 2 //[1 1 1] Co 3 O 4 , and then solid Co 3 O 4 nanocubes gradually hollow and convert to single-crystal nanoboxes owing to Ostwald ripening. - Graphical abstract: The formation mechanism of Co 3 O 4 nanoboxes can be expressed as epitaxial growth of Co 3 O 4 nanocubes from β-Co(OH) 2 nanoflakes due to a topotactic transformation and hollowing process owing to Ostwald ripening. Highlights: → Co 3 O 4 nanoboxes were prepared by a convenient, economical and controllable hydrothermal route. → Morphology and structure of Co 3 O 4 nanoboxes were characterized by XRD, SEM, and TEM techniques. → Co 3 O 4 nanoboxes grow epitaxially from Co(OH) 2 by topotactic transformation was suggested.

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

High-temperature x-ray diffraction study of HfTiO4-HfO2 solid solutions

International Nuclear Information System (INIS)

Carpenter, D.A.

1975-01-01

High-temperature x-ray diffraction techniques were used to determine the axial thermal expansion curves of HfTiO 4 -HfO 2 solid solutions as a function of composition. Data show increasing anisotropy with increasing HfO 2 content. An orthorhombic-to-monoclinic phase transformation was detected near room temperature for compositions near the high HfO 2 end of the orthorhombic phase field and for compositions within the two-phase region (HfTiO 4 solid solution plus HfO 2 solid solution). An orthorhombic-to-cubic phase transformation is indicated by data from oxygen-deficient materials at greater than 1873 0 K. (U.S.)

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.

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

Energy Technology Data Exchange (ETDEWEB)

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

2011-01-15

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

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.

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)

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.

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.

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...

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

Directory of Open Access Journals (Sweden)

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.

Tritium release in Li{sub 4}SiO{sub 4} and Li{sub 4.2}Si{sub 0.8}Al{sub 0.2}O{sub 4} ceramics

Energy Technology Data Exchange (ETDEWEB)

Zhao, Linjie, E-mail: zhaolinjie1989@163.com; Long, Xinggui, E-mail: xingguil@caep.cn; Peng, Shuming, E-mail: pengshuming@caep.cn; Chen, Xiaojun; Xiao, Chengjian; Ran, Guangming; Li, Jiamao

2016-12-15

Li{sub 4+x}Si{sub 1−x}Al{sub x}O{sub 4} solid solution materials, which were designed as the advanced tritium breeders, were obtained by indirect solid state reactions. The behaviors of tritium release from Li{sub 4}SiO{sub 4} and Li{sub 4.2}Si{sub 0.8}Al{sub 0.2}O{sub 4} powders were investigated by temperature programmed desorption. The tritium release curves show different characteristics for the Li{sub 4}SiO{sub 4} and Li{sub 4.2}Si{sub 0.8}Al{sub 0.2}O{sub 4} ceramics. The main tritium release peak in the Li{sub 4}SiO{sub 4} and Li{sub 4.2}Si{sub 0.8}Al{sub 0.2}O{sub 4} powders is at approximately 600 °C after a high dose irradiation. Moreover, the temperature of the tritium release from Li{sub 4.2}Si{sub 0.8}Al{sub 0.2}O{sub 4} was lower than that of the release from Li{sub 4}SiO{sub 4}. This suggests a possible advantage to using the solid solutions as the advanced tritium breeding materials.

Influence of the cation substitution on the magnetic properties of LiCo2O4 and Li(Me,Co2O4 spinels

Directory of Open Access Journals (Sweden)

Gautier, J. L.

2004-08-01

Full Text Available Lithium-based cells LiCo2O4 have been characterized by magnetic techniques, looking at the influence of the partial substitution of cobalt by 3d or 4d transition metal elements (Fe, Ni, Cu, Cr, Mo. The non-substituted compound LiCo2O4 behaves as an antiferromagnet, with a Néel temperature TN of 30 K, although antiferromagnetic interactions are much more important, as suggested by a Weiss parameter Θ of the order of ‑225 K. In the solid solution Li(NixCo2‑xO4 the Weiss parameter Θ changes with x(Ni, reaching large positive values (e.g., Θ ~ +230 K, for x = 0.5. This phenomenon suggests the existence of a canted‑antiferromagnetic or ferrimagnetic structures with large ferromagnetic components. Substitution of cobalt by other 3d or 4d transition metals in the LiMe0.5Co1.5O4 series shows dramatic effects with respect to the non-substituted LiCo2O4 compound : copper completely suppresses the magnetic order, while iron increases TN to almost room temperature. No modifications are observed when molybdenum substitutes cobalt, while chromium transforms the AF order in a ferromagnetic one, with Tc of about 90 K.Se ha caracterizado por técnicas magnéticas, el efecto de la sustitución parcial de Co por elementos de transición 3d o 4d (Fe, Ni, Cu, Cr, Mo en celdas LiCo2O4 a base de litio. El compuesto no sustituído LiCo2O4, se comporta como un antiferromagneto de temperatura de Néel TN de 30 K, aunque existen interacciones antiferromagnéticas mucho más importantes, como lo indica un parámetro de Weiss Θ del orden de -225K. En la solución sólida Li(NixCo2‑xO4, el parámetro de Weiss Θ cambia con x(Ni, alcanzando valores positivos altos (e.g., Θ ~ +230K, para x=0.5. Este fenómeno sugiere la existencia de una estructura antiferromagnética inclinada (“AF-canted” o de una estructura ferrimagnética, donde predominan componentes ferromagnéticas importantes. La sustitución del cobalto por otros elementos de transición 3d o 4d en

Synthetic, spectroscopic and structural studies on 4-aminobenzoate complexes of divalent alkaline earth metals: x-ray crystal structures of [[Mg(H2O)6] (4-aba)2].2H2O and [Ca(H2O)2(4-aba)2] (4-aba=4-aminobenzoate)

International Nuclear Information System (INIS)

Murugavel, Ramaswamy; Karambelkar, Vivek V.; Anantharaman, Ganapathi

2000-01-01

Reactions between MCl 2 .nH 2 O (M = Mg, Ca, Sr, and Ba) and 4-aminobenzoic acid (4-abaH) result in the formation of complexes [(Mg(H 2 O) 6 )(4-aba) 2 ) .2H 2 O (I), [Ca(4-aba) 2 (H2 O ) 2 ] (2), [Sr(4-aba) 2 (H2 O ) 2 ] (3), and [Ba(4-aba) 2 Cl] (4), respectively. The new compounds 1 and 2, as well as the previously reported 3 and 4 form an extended intra- and intermolecular hydrogen bonded network in the solid-state. The compounds have been characterized by elemental analysis, pH measurements, thermogravimetric studies, and IR, NMR, and UV-Vis spectroscopy. The solid state structures of the molecules 1 and 2 have been determined by single crystal x-ray diffraction studies. In the case of magnesium complex 1, the dipositively charged Mg cation is surrounded by six water molecules and the two 4-aminobenzoate ligands show no direct bonding to the metal ion. The calcium ion in 2 is octa-coordinated with direct coordination of the 4-aminobenzoate ligands to the metal ion. The Ca-Ca separation in the polymeric chain of 2 is 3.9047(5) A. (author)

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

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.

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

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)

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.

Systems Li[sub 2]B[sub 4]O[sub 7] (Na[sub 2]B[sub 4]O[sub 7], K[sub 2]B[sub 4]O[sub 7])-N[sub 2]H[sub 3]H[sub 4]OH-H[sub 2]O at 25 deg C. Sistemy Li[sub 2]B[sub 4]O[sub 7] (Na[sub 2]B[sub 4]O[sub 7], K[sub 2]B[sub 4]O[sub 7])-N[sub 2]H[sub 3]H[sub 4]OH-H[sub 2]O pri 25 grad S

Energy Technology Data Exchange (ETDEWEB)

Skvortsov, V G; Sadetdinov, Sh V; Akimov, V M; Mitrasov, Yu N; Petrova, O V; Klopov, Yu N [Chuvashskij Gosudarstvennyj Pedagogicheskij Inst., Cheboksary (Russian Federation) Universitet Druzhby Narodov, Moscow (Russian Federation)

1994-02-01

Phase equilibriums in the Li[sub 2]B[sub 4]O[sub 7] (Na[sub 2]B[sub 4]O[sub 7], K[sub 2]B[sub 4]O[sub 7])-N[sub 2]H[sub 3]H[sub 4]OH-H[sub 2]O systems were investigated by methods of isothermal solubility, refractometry and PH-metry at 25 deg C for the first time. Lithium and sodium tetraborates was established to form phases of changed composition mM[sub 2]B[sub 4]O[sub 7][center dot]nN[sub 2]H[sub 3]C[sub 2]H[sub 4]OH[center dot]XH[sub 2]O, where M=Li, Na with hydrazine ethanol. K[sub 2]B[sub 4]O[sub 7][center dot]4H[sub 2]O precipitates in solid phase in the case of potassium salt. Formation of isomorphous mixtures was supported by X-ray diffraction and IR spectroscopy methods.

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.

Study of ZrO2-H2SO4-(NH4)2SO4(NH4Cl)-H2O systems

International Nuclear Information System (INIS)

Motov, D.L.; Sozinova, Yu.P.; Rys'kina, M.P.

1988-01-01

Regions of formation, composition and solubility of ammonium sulfatozirconates (ASZ) in ZrO 2 -H 2 SO 4 -(NH 4 ) 2 SO 4 (NH 4 Cl)-H 2 O systems at 25 and 75 deg C are studied by the isothermal method. Five ASZ: (NH 4 ) 2 Zr(OH) 2 (SO 4 ) 2 , NH 4 ZrOH(SO 4 ) 2 xH 2 O, NH 4 ZrO 0.5 (OH) 2 SO 4 x1.5H 2 O, (NH 4 ) 2 Zr(SO 4 ) 3 x2H 2 O, (NH 4 ) 4 Zr(SO 4 ) 4 x4H 2 O are detected, their properties are investigated. Main sulfates are new compounds never described ealier

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

Directory of Open Access Journals (Sweden)

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.

Phase equilibria in the CdMoO4-Gd2(MoO4)3 system

International Nuclear Information System (INIS)

Tunik, T.A.; Fedorov, N.F.; Razumovskij, S.N.

1980-01-01

The constitutional diagram of the CdMoO 4 -Cd 2 (MoO 4 ) 3 system has been plotted using statistical and dynamic methods as well as a complex of instrumental analysis procedures. Three major phases have been found to occur in the systems, viz.: CdMoO 4 based solid solutions that crystallize in the range from 0 to 25 mol.percent of Cd 2 (MoO 4 ) 3 and pass in transit the two-phase narrow region becoming then solid solutions having a distorted scheelite structure and existing in concentrations from 40 to 65 mol.% of Cd 2 (MoO 4 ) 3 . The entire range, in which the Cd 2 (MoO 4 ) 3 solid solutions can exist, amounts to less than 5 mol.%. Certain crystallochemical constants of the phases that occur in the system have been determined [ru

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.

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

Surface Modification of LiMn2O4 for Lithium Batteries by Nanostructured LiFePO4 Phosphate

Directory of Open Access Journals (Sweden)

B. Sadeghi

2012-01-01

Full Text Available LiMn2O4 spinel cathode materials have been successfully synthesized by solid-state reaction. Surface of these particles was modified by nanostructured LiFePO4 via sol gel dip coating method. Synthesized products were characterized by thermally analyzed thermogravimetric and differential thermal analysis (TG/DTA, X-ray diffraction (XRD, scanning electron microscopy (SEM, transmission electron microscopy (TEM, and energy dispersive X-ray spectroscopy (EDX. The results of electrochemical tests showed that the charge/discharge capacities improved and charge retention of battery enhanced. This improved electrochemical performance is caused by LiFePO4 phosphate layer on surfaces of LiMn2O4 cathode particles.

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)

Disappearance of superconductivity in the solid solution between (Ca4Al2O6)(Fe2As2) and (Ca4Al2O6)(Fe2P2) superconductors.

Science.gov (United States)

Shirage, Parasharam M; Kihou, Kunihiro; Lee, Chul-Ho; Takeshita, Nao; Eisaki, Hiroshi; Iyo, Akira

2012-09-19

The effect of alloying the two perovskite-type iron-based superconductors (Ca(4)Al(2)O(6))(Fe(2)As(2)) and (Ca(4)Al(2)O(6))(Fe(2)P(2)) was examined. While the two stoichiometric compounds possess relatively high T(c)'s of 28 and 17 K, respectively, their solid solutions of the form (Ca(4)Al(2)O(6))(Fe(2)(As(1-x)P(x))(2)) do not show superconductivity over a wide range from x = 0.50 to 0.95. The resultant phase diagram is thus completely different from those of other typical iron-based superconductors such as BaFe(2)(As,P)(2) and LaFe(As,P)O, in which superconductivity shows up when P is substituted for As in the non-superconducting "parent" compounds. Notably, the solid solutions in the non-superconducting range exhibit resistivity anomalies at temperatures of 50-100 K. The behavior is reminiscent of the resistivity kink commonly observed in various non-superconducting parent compounds that signals the onset of antiferromagnetic/orthorhombic long-range order. The similarity suggests that the suppression of the superconductivity in the present case also has a magnetic and/or structural origin.

Phase formation in the Li2MoO4–K2MoO4–In2(MoO4)3 system and crystal structures of new compounds K3InMo4O15 and LiK2In(MoO4)3

International Nuclear Information System (INIS)

Khal’baeva, Klara M.; Solodovnikov, Sergey F.; Khaikina, Elena G.; Kadyrova, Yuliya M.; Solodovnikova, Zoya A.; Basovich, Olga M.

2012-01-01

XRD study of solid-phase interaction in the Li 2 MoO 4 –K 2 MoO 4 –In 2 (MoO 4 ) 3 system was performed. The boundary K 2 MoO 4 –In 2 (MoO 4 ) 3 system is an non-quasibinary join of the K 2 O–In 2 O 3 –MoO 3 system where a new polymolybdate K 3 InMo 4 O 15 isotypic to K 3 FeMo 4 O 15 was found. In the structure (a=33.2905(8), b=5.8610(1), c=15.8967(4) Å, β=90.725(1)°, sp. gr. C2/c, Z=8, R(F)=0.0407), InO 6 octahedra, Mo 2 O 7 diortho groups and MoO 4 tetrahedra form infinite ribbons {[In(MoO 4 ) 2 (Mo 2 O 7 )] 3− } ∞ along the b-axis. Between the chains, 8- to 10-coordinate potassium cations are located. A subsolidus phase diagram of the Li 2 MoO 4 –K 2 MoO 4 –In 2 (MoO 4 ) 3 system was constructed and a novel triple molybdate LiK 2 In(MoO 4 ) 3 was revealed. Its crystal structure (a=7.0087(2), b=9.2269(3), c=10.1289(3) Å, β=107.401(1)°, sp. gr. P2 1 , Z=2, R(F)=0.0280) contains an open framework of vertex-shared MoO 4 tetrahedra, InO 6 octahedra and LiO 5 tetragonal pyramids with nine- and seven-coordinate potassium ions in the framework channels. - Graphical abstract: Exploring the Li 2 MoO 4 –K 2 MoO 4 –In 2 (MoO 4 ) 3 system showed its partial non-quasibinarity and revealed new compounds K 3 InMo 4 O 15 (isotypic to K 3 FeMo 4 O 15 ) and LiK 2 In(MoO 4 ) 3 which were structurally studied. An open framework of the latter is formed by vertex-shared MoO 4 tetrahedra, InO 6 octahedra and LiO 5 tetragonal pyramids. Highlights: ► Subsolidus phase relations in the Li 2 MoO 4 –K 2 MoO 4 –In 2 (MoO 4 ) 3 system were explored. ► The K 2 MoO 4 –In 2 (MoO 4 ) 3 system is a non-quasibinary join of the K 2 O–In 2 O 3 –MoO 3 system. ► New compounds K 3 InMo 4 O 15 and LiK 2 In(MoO 4 ) 3 were obtained and structurally studied. ► K 3 InMo 4 O 15 is isotypic to K 3 FeMo 4 O 15 and carries bands of InO 6 , MoO 4 and Mo 2 O 7 units. ► An open framework of LiK 2 In(MoO 4 ) 3 is formed by polyhedra MoO 4 , InO 6 and LiO 5 .

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

International Nuclear Information System (INIS)

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

2008-01-01

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

Synthesis and electrochemical properties of LiNi0.4Mn1.5Cr0.1O4 and Li4Ti5O12

CSIR Research Space (South Africa)

Liu, GQ

2011-08-01

Full Text Available Spinel compound LiNi0.4Mn1.5Cr0.1O4 (LNMCO) and Li4Ti5O12 (LTO) were synthesized by the sol-gel method and the solid-state method, respectively. The particle sizes of the products LiNi0.4Mn1.5Cr0.1O4 and Li4Ti5O12 were 0.5 to 2 um and 0.5 to 0.8 um...

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 .

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

Science.gov (United States)

Gudfinnsson, Gudmundur H.; Presnall, Dean C.

1996-12-01

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

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

International Nuclear Information System (INIS)

Arumugam, D.; Kalaignan, G. Paruthimal

2010-01-01

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

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).

Solid-State Synthesis and Structure of the Enigmatic Ammonium Octaborate: (NH4)2[B7O9(OH)5]·3/4B(OH)3·5/4H2O.

Science.gov (United States)

Neiner, Doinita; Sevryugina, Yulia V; Schubert, David M

2016-09-06

The compound known since the 19th century as ammonium octaborate was structurally characterized revealing the ammonium salt of the ribbon isomer of the heptaborate anion, [B7O9(OH)5](2-), with boric acid and water molecules. Of composition (NH4)2B7.75O12.63·4.88H2O, it approximates the classical ammonium octaborate composition (NH4)2B8O13·6H2O and has the structural formula {(NH4)2[B7O9(OH)5]}4·3B(OH)3·5H2O. It spontaneously forms at room temperature in solid-state mixtures of ammonium tetraborate and ammonium pentaborate. It crystallizes in the monoclinic space group P21/c with a = 11.4137(2) Å, b = 11.8877(2) Å, c = 23.4459(3) Å, β = 90.092(1)°, V = 3181.19(8) Å(3), and Z = 2 and contains well-ordered ammonium cations and [B7O9(OH)5](2-) anions and disordered B(OH)3 and H2O molecules linked by extensive H bonding. Expeditious solid-state formation of the heptaborate anion under ambient conditions has important implications for development of practical syntheses of industrially useful borates.

Characterization of thin films of the solid electrolyte Li(x)Mg(1-2x)Al(2+x)O4 (x = 0, 0.05, 0.15, 0.25).

Science.gov (United States)

Put, Brecht; Vereecken, Philippe M; Mees, Maarten J; Rosciano, Fabio; Radu, Iuliana P; Stesmans, Andre

2015-11-21

RF-sputtered thin films of spinel Li(x)Mg(1-2x)Al(2+x)O4 were investigated for use as solid electrolyte. The usage of this material can enable the fabrication of a lattice matched battery stack, which is predicted to lead to superior battery performance. Spinel Li(x)Mg(1-2x)Al(2+x)O4 thin films, with stoichiometry (x) ranging between 0 and 0.25, were formed after a crystallization anneal as shown by X-ray diffraction and transmission electron microscopy. The stoichiometry of the films was evaluated by elastic recoil detection and Rutherford backscattering and found to be slightly aluminum rich. The excellent electronic insulation properties were confirmed by both current-voltage measurements as well as by copper plating tests. The electrochemical stability window of the material was probed using cyclic voltammetry. Lithium plating and stripping was observed together with the formation of a Li-Pt alloy, indicating that Li-ions passed through the film. This observation contradicted with impedance measurements at open circuit potential, which showed no apparent Li-ion conductivity of the film. Impedance spectroscopy as a function of potential showed the occurrence of Li-ion intercalation into the Li(x)Mg(1-2x)Al(2+x)O4 layers. When incorporating Li-ions in the material the ionic conductivity can be increased by 3 orders of magnitude. Therefore it is anticipated that the response of Li(x)Mg(1-2x)Al(2+x)O4 is more adequate for a buffer layer than as the solid electrolyte.

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.

Solid state reactions of MoO3 and Na2MoO4 with (U.85,Ce.15)O2x

International Nuclear Information System (INIS)

Dahale, N.D.; Keskar, Meera; Singh Mudher, K.D.; Chawla, K.L.

1999-01-01

(U .85 ,Ce .15 )MoO 6-x was prepared by the solid state reactions of (U .85 ,Ce .15 )O 2±x with MoO 3 in air at 600 deg C. Solid state reactions of Na 2 MoO 4 with (U .85 ,Ce .15 )MoO 6.x up to 550 deg C in air led to the formation of Na 2 (U .85 ,Ce .15 )Mo 2 O 10-x and Na 2 (U .85 , Ce .15 ) 2 Mo 3 O 16-x . These compounds were characterised by x-ray and thermal methods. The x-ray powder data of (U .85 , Ce .15 ) MoO 6-x were indexed on monoclinic system whereas, data of Na 2 (U .85 ,Ce .15 ) Mo 2 O 10-x and Na 2 (U .85 ,Ce .15 ) 2 Mo 3 O 16-x were indexed on orthorhombic and monoclinic system respectively. (author)

Determination and modeling for the solubility of Na_2WO_4·2H_2O and Na_2MoO_4·2H_2O in the (Na"+ + MoO_4"2"− + WO_4"2"− + SO_4"2"− + H_2O) system

International Nuclear Information System (INIS)

Ning, Pengge; Xu, Weifeng; Cao, Hongbin; Xu, Hongbin

2016-01-01

Highlights: • The solubility of Na_2MoO_4·2H_2O and Na_2WO_4·2H_2O in Na_2MoO_4–Na_2WO_4–Na_2SO_4–H_2O were performed. • The solubility of sodium tungstate dihydrate in Na_2WO_4–Na_2SO_4–H_2O was determined. • The new model was established via regressing the published and the determined data. • The Pitzer parameter and the solubility product constant of the salt in solution were calculated. • The model was used to estimate the solubility of the sodium molybdate and sodium tungstate. - Abstract: The solubility of sodium tungstate dihydrate and sodium molybdate dihydrate in the (Na_2MoO_4 + Na_2WO_4 + Na_2SO_4 + H_2O) system was studied using experimental and calculated methods. The osmotic coefficient of sodium tungstate was fitted to calculate the thermodynamics parameters of (Na_2WO_4 + H_2O) system. The solubility of sodium tungstate dihydrate was determined using the dynamic method in Na_2WO_4–Na_2SO_4–H_2O to establish the new model which can provide an estimate the solubility of sodium tungstate dihydrate in various conditions, combined with the data published, the solubility of sodium tungstate dihydrate and the sodium molybdate dihydrate in quaternary system of (Na_2MoO_4 + Na_2WO_4 + Na_2SO_4 + H_2O) was estimated using the parameters of the two ternary systems of (Na_2WO_4 + Na_2SO_4 + H_2O) and (Na_2MoO_4 + Na_2SO_4 + H_2O). The results show that the AARD is always small and the calculated value is basically consistent with the experimental values for the system studied.

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

Study of the Ni-NiAl{sub 2}O{sub 4}-YSZ cermet for its possible application as an anode in solid oxide fuel cells

Energy Technology Data Exchange (ETDEWEB)

Reyes-Rojas, A [Centro de Investigacion en Materiales Avanzados SC, Miguel de Cervantes 120, Complejo Industrial Chihuahua, Chihuahua (Mexico); Universidad Autonoma del Estado de Mexico, Facultad de Quimica, Toluca (Mexico); Esparza-Ponce, H E [Centro de Investigacion en Materiales Avanzados SC, Miguel de Cervantes 120, Complejo Industrial Chihuahua, Chihuahua (Mexico); Reyes-Gasga, J [Universidad Nacional Autonoma de Mexico, Instituto de Fisica, Mexico DF (Mexico)

2006-05-17

Nanocrystalline Ni-NiAl{sub 2}O{sub 4}-YSZ cermet with a possible application as anode in solid oxide fuel cells (SOFCs) has been developed. The powders were prepared by using an alternative solid-state method that includes the use of nickel acetylacetonate as an inorganic precursor to obtain a highly porous material after sintering at 1400 {sup o}C and oxide reduction (NiO -Al{sub 2}O{sub 3}-YSZ {yields} Ni-NiAl{sub 2}O{sub 4}-YSZ) at 800 {sup o}C for 8 h in a tubular reactor furnace using 10% H{sub 2}/N{sub 2}. Eight samples with 45% Ni and 55% Al{sub 2}O{sub 3}-YSZ in concentrations of Al{sub 2}O{sub 3} oxides from 10 to 80 wt% of were mixed to obtain the cermets. The obtained material was compressed using unidirectional axial pressing and calcinations from room temperature to 800 {sup o}C. Good results were registered using a heating rate of 1 {sup o}C min{sup -1} and a special ramp to avoid anode cracking. Thermal expansion, electrical conductivity, and structural characterization by thermo-mechanical analyser (TMA) techniques/methods, the four-point probe method for conductivity, scanning electron microscopy (SEM), x-ray energy dispersive spectroscopy (EDS), x-ray diffraction (XRD), and the Rietveld method were carried out. Cermets in the range 5.5 to 11% Al{sub 2}O{sub 3} present a crystal size around 200 nm. An inversion degree (I) in the NiAl{sub 2}O{sub 4} spinel structure of the cermets Ni-NiAl{sub 2}O{sub 4}-YSZ was found after the sintering and reduction processes. Good electrical conductivity and thermal expansion coefficient were obtained for the cermet with 12 wt% of spinel structure formation.

Neutron diffraction study of the reduction of NiAl2O4

International Nuclear Information System (INIS)

Ustundag, E.; Clausen, B.; Bourke, M. A. M.

2000-01-01

The reduction of a solid NiAl 2 O 4 cylinder to a metal-ceramic composite consisting of Ni particles in an Al 2 O 3 matrix was monitored in situ at 1220 degree sign C with neutron powder diffraction. The reaction kinetics was determined with a time resolution of 30 min. The reduction is associated with a volume shrinkage. A comparison of finite element calculations and the changes in the measured lattice parameters suggests that creep has relaxed the residual strains that would otherwise result from the volume shrinkage. The data also indicate that structural evolution in unreduced NiAl 2 O 4 via a change in the cationic sublattice towards inverse spinel occurred and that led to a variation in lattice parameters. (c) 2000 American Institute of Physics

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 .

Nanocrystalline spinel ferrites by solid state reaction route

Indian Academy of Sciences (India)

Wintec

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

Thermal expansion studies on Th(MoO4)2, Na2Th(MoO4)3 and Na4Th(MoO4)4

International Nuclear Information System (INIS)

Keskar, Meera; Krishnan, K.; Dahale, N.D.

2008-01-01

Thermal expansion behavior of Th(MoO 4 ) 2 , Na 2 Th(MoO 4 ) 3 and Na 4 Th(MoO 4 ) 4 was studied under vacuum in the temperature range of 298-1123 K by high temperature X-ray diffractometer. Th(MoO 4 ) 2 was synthesized by reacting ThO 2 with 2 mol of MoO 3 , at 1073 K in air and Na 2 Th(MoO 4 ) 3 and Na 4 Th(MoO 4 ) 4 were prepared by reacting Th(MoO 4 ) 2 with 1 and 2 mol of Na 2 MoO 4 , respectively at 873 K in air. The XRD data of Th(MoO 4 ) 2 was indexed on orthorhombic system where as XRD data of Na 2 Th(MoO 4 ) 3 and Na 4 Th(MoO 4 ) 4 were indexed on tetragonal system. The lattice parameters and cell volume of all the three compounds, fit into polynomial expression with respect to temperature, showed positive thermal expansion (PTE) up to 1123 K. The average value of thermal expansion coefficients for Th(MoO 4 ) 2 , Na 2 Th(MoO 4 ) 3 and Na 4 Th(MoO 4 ) 4 were determined from the high temperature data

Solid-solid interactions in Co3O4-MoO3/MgO system

International Nuclear Information System (INIS)

Radwan, Nagi R.E.; Ghozza, Ahmed M.; El-Shobaky, Gamil A.

2003-01-01

Cobalt/magnesium mixed oxide solids and cobalt-molybdenum/magnesium mixed oxide solids were prepared by thermal decomposition of basic magnesium carbonate pretreated with different proportions of cobalt nitrate and then with calculated amounts of ammonium molybdate. The proportions of cobalt expressed as Co 3 O 4 were 0.1, 0.2 and 0.3 mol while the concentrations of molybdenum expressed as mol% MoO 3 were 2.5 and 5.0. The prepared mixed solid specimens were calcined in air at 400-1000 deg. C. The solid-solid interactions in Co 3 O 4 -MoO 3 were investigated using DTA, TG and X-ray powder diffraction (XRD) techniques. The results obtained revealed that MgO dissolved cobalt oxide in its lattice forming CoO-MgO solid solution. The amount of cobalt dissolved increases by increasing the temperature in the range 800-1000 deg. C. This finding was confirmed by X-ray diffractograms in which all the diffraction lines of cobalt oxide disappeared at 1000 deg. C. MoO 3 present interacted readily with MgO and cobalt oxide by heat treatment at temperature starting from 400 deg. C producing MgMoO 4 and CoMoO 4 which remained stable by heating at 1000 deg. C. The impregnation of basic magnesium carbonate with cobalt nitrate much enhanced its thermal decomposition yielding MgO, which decomposed completely at 395.5 deg. C instead of 525 deg. C. The formation of magnesium cobaltite (MgCo 2 O 4 ) has been ruled out via XRD investigation at relatively high diffraction angles

Phase formation in the Li2MoO4-Rb2MoO4-Ln2(MoO4)3 systems and the properties of LiRbLn2(MoO4)4

International Nuclear Information System (INIS)

Basovich, O.M.; Khajkina, E.G.; Vasil'ev, E.V.; Frolov, A.M.

1995-01-01

Phase equilibria within subsolidus range of ternary salt systems Li 2 MoO 4 -Rb 2 MoO 4 -Ln 2 (MoO 4 ) 4 (Ln - Nd, Er) are analyzed. Formation of ternary molybdate LiRbNd 2 (MoO 4 ) 4 is proved along LiNd(MoO 4 ) 2 -RbNd(MoO 4 )-2 cross-section. Phase diagram of this cross-section is plotted. Similar compounds are synthesized for Ln = La-Eu. The parameters of their monoclinic elementary cells are determined. Luminescent properties of LiRbLa 2 (MoO 4 ) 4 -Nd 3+ are studied. 17 refs., 4 figs., 2 tabs

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...

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.

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.

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.

Topotactic Solid-State Metal Hydride Reductions of Sr2MnO4.

Science.gov (United States)

Hernden, Bradley C; Lussier, Joey A; Bieringer, Mario

2015-05-04

We report novel details regarding the reactivity and mechanism of the solid-state topotactic reduction of Sr2MnO4 using a series of solid-state metal hydrides. Comprehensive details describing the active reducing species are reported and comments on the reductive mechanism are provided, where it is shown that more than one electron is being donated by H(-). Commonly used solid-state hydrides LiH, NaH, and CaH2, were characterized in terms of reducing power. In addition the unexplored solid-state hydrides MgH2, SrH2, and BaH2 are evaluated as potential solid-state reductants and characterized in terms of their reductive reactivities. These 6 group I and II metal hydrides show the following trend in terms of reactivity: MgH2 < SrH2 < LiH ≈ CaH2 ≈ BaH2 < NaH. The order of the reductants are discussed in terms of metal electronegativity and bond strengths. NaH and the novel use of SrH2 allowed for targeted synthesis of reduced Sr2MnO(4-x) (0 ≤ x ≤ 0.37) phases. The enhanced control during synthesis demonstrated by this soft chemistry approach has allowed for a more comprehensive and systematic evaluation of Sr2MnO(4-x) phases than previously reported phases prepared by high temperature methods. Sr2MnO3.63(1) has for the first time been shown to be monoclinic by powder X-ray diffraction and the oxidative monoclinic to tetragonal transition occurs at 450 °C.

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

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.

Complexation in the system K2SeO4-UO2SeO4-H2O

International Nuclear Information System (INIS)

Serezhkina, L.B.; Kuchumova, N.V.; Serezhkin, V.N.

1994-01-01

Complexation in the system K 2 SeO 4 -UO 2 SeO 4 -H 2 O at 25 degrees C is studied by isothermal solubility. Congruently soluble K 2 UO 2 (SeO 4 ) 2 ·4H 2 O (I) and incongruently soluble K 2 (UO 2 ) 2 (SeO 4 ) 3 ·6H 2 O (II) are observed. The unit-cell constants of I and II are determined from an X-ray diffraction investigation. For I, a = 12,969, b = 11.588, c = 8.533 angstrom, Z = 4, space group Pmmb. For II, a = 23.36, b = 6.784, c = 13.699 angstrom, β = 104.42 degrees, Z = 4, space group P2/m, P2, or Pm. Complexes I and II are representatives of the crystal-chemical groups AB 2 2 M 1 and A 2 T 3 3 M 1 , respectively, of uranyl complexes

Phase relations in the M2MoO4 - Ag2MoO4 - Hf(MoO4)2 (M=Li, Na) systems

International Nuclear Information System (INIS)

Bazarova, Zh.G.; Bazarov, B.G.; Balsanova, L.V.

2002-01-01

The M 2 MoO 4 - Ag 2 MoO 4 - Hf(MoO 4 ) 2 (M=Li, Na) systems were studied by X-ray diffraction and differential thermal analyses in the subsolidus area (450 - 500 Deg C) for the first time. The formation of the binary compound with the variable composition Li 4-x Hf 1+0.2x (MoO 4 ) 4 (0 ≤ x ≤ 0.6) in the Li 2 MoO 4 - Hf(MoO 4 ) 2 system and the ternary molybdates Li 4 Ag 2 Hf(MoO 4 ) 5 (S 1 ) and Na 2 Ag 2 Hf(MoO 4 ) 4 (S 2 ) was established and the thermal characteristics of the prepared compounds were examined. The new binary molybdate Ag 2 Hf(MoO 4 ) 3 was prepared by the reaction between Ag 2 MoO 4 and Hf(MoO 4 ) 2 [ru

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

International Nuclear Information System (INIS)

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

2012-01-01

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

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.

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-07-15

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

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

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.

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

Neutron scattering study on cathode LiMn2O4 and solid electrolyte 5(Li2O)(P2O5)

International Nuclear Information System (INIS)

Kartini, E.; Putra, Teguh P.; Jahya, A. K.; Insani, A.; Adams, S.

2014-01-01

Neutron scattering is very important technique in order to investigate the energy storage materials such as lithium-ion battery. The unique advantages, neutron can see the light atoms such as Hydrogen, Lithium, and Oxygen, where those elements are negligible by other corresponding X-ray method. On the other hand, the energy storage materials, such as lithium ion battery is very important for the application in the electric vehicles, electronic devices or home appliances. The battery contains electrodes (anode and cathode), and the electrolyte materials. There are many challenging to improve the existing lithium ion battery materials, in order to increase their life time, cyclic ability and also its stability. One of the most scientific challenging is to investigate the crystal structure of both electrode and electrolyte, such as cathodes LiCoO 2 , LiMn 2 O 4 and LiFePO 4 , and solid electrolyte Li 3 PO 4 . Since all those battery materials contain Lithium ions and Oxygen, the used of neutron scattering techniques to study their structure and related properties are very important and indispensable. This article will review some works of investigating electrodes and electrolytes, LiMn 2 O 4 and 5(Li 2 O)(P 2 O 5 ), by using a high resolution powder diffraction (HRPD) at the multipurpose research reactor, RSG-Sywabessy of the National Nuclear Energy Agency (BATAN), Indonesia

Oxothiomolybdenum derivatives of the superlacunary crown heteropolyanion {P8W48}: structure of [K4{Mo4O4S4(H2O)3(OH)2}2(WO2)(P8W48O184)]30– and studies in solution.

Science.gov (United States)

Korenev, Vladimir S; Floquet, Sébastien; Marrot, Jérôme; Haouas, Mohamed; Mbomekallé, Israël-Martyr; Taulelle, Francis; Sokolov, Maxim N; Fedin, Vladimir P; Cadot, Emmanuel

2012-02-20

Reaction of the cyclic lacunary [H(7)P(8)W(48)O(184)](33-) anion (noted P(8)W(48)) with the [Mo(2)S(2)O(2)(H(2)O)(6)](2+) oxothiocation led to two compounds, namely, [K(4){Mo(4)O(4)S(4)(H(2)O)(3)(OH)(2)}(2)(WO(2))(P(8)W(48)O(184))](30-) (denoted 1) and [{Mo(4)O(4)S(4)(H(2)O)(3)(OH)(2)}(2)(P(8)W(48)O(184))](36-) (denoted 2), which were characterized in the solid state and solution. In the solid state, the structure of [K(4){Mo(4)O(4)S(4)(H(2)O)(3)(OH)(2)}(2)(WO(2))(P(8)W(48)O(184))](30-) reveals the presence of two disordered {Mo(4)O(4)S(4)(H(2)O)(3)(OH)(2)}(2+) "handles" connected on both sides of the P(8)W(48) ring. Such a disorder is consistent with the presence of two geometrical isomers where the relative disposition of the two {Mo(4)O(4)S(4)(H(2)O)(3)(OH)(2)}(2+) handles are arranged in a perpendicular or parallel mode. Such an interpretation is fully supported by (31)P and (183)W NMR solution studies. The relative stability of both geometrical isomers appears to be dependent upon the nature of the internal alkali cations, i.e., Na(+) vs K(+), and increased lability of the two {Mo(4)O(4)S(4)(H(2)O)(3)(OH)(2)}(2+) handles, compared to the oxo analogous, was clearly identified by significant broadening of the (31)P and (183)W NMR lines. Solution studies carried out by UV-vis spectroscopy showed that formation of the adduct [{Mo(4)O(4)S(4)(H(2)O)(3)(OH)(2)}(2)(P(8)W(48)O(184))](36-) occurs in the 1.5-4.7 pH range and corresponds to a fast and quantitative condensation process. Furthermore, (31)P NMR titrations in solution reveal formation of the "monohandle" derivative [{Mo(4)O(4)S(4)(H(2)O)(3)(OH)(2)}(P(8)W(48)O(184))](38-) as an intermediate prior to formation of the "bishandle" derivatives. Furthermore, the electrochemical behavior of [{Mo(4)O(4)S(4)(H(2)O)(3)(OH)(2)}(2)(P(8)W(48)O(184))](36-) was studied in aqueous medium and compared with the parent anion P(8)W(48).

NH4In(SeO4)2x4H2O crystal structure interpretation

International Nuclear Information System (INIS)

Soldatov, E.A.; Kuz'min, Eh.A.; Ilyukhin, V.V.

1979-01-01

The rhomb method has been applied to interpret the structure of monoclinic ammonium indium selenate NH 4 In(SeO 4 ) 2 x4H 2 O the elementary cell of which contains Z=4 formula units (a=10.728, b=9.434, c=11.086 A, γ=101.58). The space group is P2 1 /b. The structure foundation is composed of [In(SeO 4 ) 2 x2H 2 O] 1- mixed layers parallel to (100). ''Free'' H 2 O molecules and NH 4 + cations are situated between the layers

Thermal and x-ray studies on Tl2U(MoO4)3 and Tl4U(MoO4)4

International Nuclear Information System (INIS)

Dahale, N.D.; Keskar, Meera; Kulkarni, N.K.; Singh Mudher, K.D.

2006-01-01

In the quaternary Tl-U(IV)-Mo-O system, two new compounds namely Tl 2 U(MoO 4 ) 3 and Tl 4 U(MoO 4 ) 4 were prepared and characterized by powder X-ray diffraction and thermal methods. These compounds were prepared by solid state reactions of Tl 2 MoO 4 , UMoO 5 and MoO 3 in the required stoichiometric ratio at 500 deg C in evacuated sealed quartz ampoule. The XRD data of Tl 2 U(MoO 4 ) 3 and Tl 4 U(MoO 4 ) 4 were indexed on orthorhombic cell. TG curves of Tl 2 U(MoO 4 ) 3 and Tl 4 U(MoO 4 ) 4 did not show any weight change up to 700 deg C in an inert atmosphere. During heating in an inert atmosphere, Tl 2 U(MoO 4 ) 3 and Tl 4 U(MoO 4 ) 4 showed endothermic Dta peaks due to melting of the compounds at 519 and 565 deg C, respectively. (author)

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

Science.gov (United States)

Kurian, Jessyamma; Mathew, M. Jacob

2018-04-01

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

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 .

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.

Moessbauer spectroscopy study of the synthesis of SnFe2O4 by high energy ball milling (HEBM) of SnO and α-Fe2O3

International Nuclear Information System (INIS)

Uwakweh, Oswald N C; Perez Moyet, Richard; Mas, Rita; Morales, Carolyn; Vargas, Pedro; Silva, Josue; Rossa, Angel; Lopez, Neshma

2010-01-01

The formation of single phase nanoparticles of spinel structured ferrite, SnFe 2 O 4 , by mechanochemical syntheses using HEBM of stoichiometric amounts of solid SnO and α-Fe 2 O 3 with acetone as surfactant was achieved progressively as function of ball milling time. Single phase SnFe 2 O 4 formation commenced from five hours of continuous ball milling, and reached completion after 22 hours, thereby yielding a material with a lattice parameter of 8.543 A, and particle size of 10.91 nm. The coercivity was 4.44 mT, magnetic saturation value of 17.75 Am 2 /kg, and remanent magnetizations of 1.50 Am 2 /kg, correspondingly. The nanosized particles exhibited superparamagnetic behavior phenomenon based on Moessbauer spectroscopy measurements. The kinetic analyses based on the modified Kissinger method yielded four characteristic stages during the thermal evolution of the 22 hours milled state with activation energies of 0.23 kJ/mol, 2.52 kJ/mol, 0.024 kJ/mol, and 1.57 kJ/mol respectively.

Humidity sensitive electrical responce of K2CrO4 doped ZnCr2O4 ceramic sensors

International Nuclear Information System (INIS)

Kavasoglu, N.

2005-01-01

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

Ca{sub 2−x}Li{sub 2x}GeO{sub 4} solid solutions. Chemical composition range and flux crystal growth

Energy Technology Data Exchange (ETDEWEB)

Ivanov, V.A. [N.I. Lobachevsky State University of Nizhni Novgorod, Nizhni Novgorod, 603950 (Russian Federation); Marychev, M.O., E-mail: marychev@yandex.ru [N.I. Lobachevsky State University of Nizhni Novgorod, Nizhni Novgorod, 603950 (Russian Federation); Andreev, P.V.; Lykov, V.A.; Faddeev, M.A. [N.I. Lobachevsky State University of Nizhni Novgorod, Nizhni Novgorod, 603950 (Russian Federation); Koseva, I. [Bulgarian Academy of Science, Institute of General and Inorganic Chemistry, BU-1113 Sofia (Bulgaria); Nikolov, V. [N.I. Lobachevsky State University of Nizhni Novgorod, Nizhni Novgorod, 603950 (Russian Federation)

2015-11-01

A series of Ca{sub 2−x}Li{sub 2x}GeO{sub 4} specimens with 0 < 2x < 2, were synthesized by the classical solid state method. X-ray analysis revealed that for 0 < 2x < 0.6 only Ca{sub 2−x}Li{sub 2x}GeO{sub 4} solid solutions of Ca{sub 2}GeO{sub 4} structure crystallized. The cell parameters of these solid solutions linearly decreased upon increasing the lithium concentration, which means that the solutions are in accordance with the Vegard's law. For 2x > 0.6 the specimens contained two phases: (i) Ca{sub 2−x}Li{sub 2x}GeO{sub 4} solid solutions with maximum lithium concentration approximately equal to that for 2x = 0.6 and minimum values of the cell parameters and (ii) Li{sub 2}CaGeO{sub 4} phase. Li{sub 2}O·MoO{sub 3}–Ca{sub 2}GeO{sub 4} high-temperature solutions were used to grow Ca{sub 2−x}Li{sub 2x}GeO{sub 4} solid solutions and Li{sub 2}CaGeO{sub 4} single crystals by the high temperature solution (flux) method. Li{sub 2}CaGeO{sub 4} crystals were grown in the concentration range 8–26 wt. % Ca{sub 2}GeO{sub 4} in the temperature range 830–980 °C. Crystals with chemical compositions of the Ca{sub 2−x}Li{sub 2x}GeO{sub 4} solid solutions with different Li concentrations were grown in the concentration range 26–40 wt. % Ca{sub 2}GeO{sub 4} in the temperature range 980–1090 °C. - Highlights: • Ca{sub 2−x}Li{sub 2x}GeO{sub 4} solid solutions are established for the first time. • The Li concentration range into the solutions is between 0 and 0.6. • The solid solutions are in accordance to Vegard's law. • Suitable solutions are found out for Ca{sub 2−x}Li{sub 2x}GeO{sub 4} and Li{sub 2}CaGeO{sub 4} crystal growth.

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.

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.

Phase formation in Na2MoO4 - MgMoO4 - Cr2(MoO4)3 system

International Nuclear Information System (INIS)

Kotova, I.Yu.; Kozhevnikova, N.M.

1998-01-01

Interaction within Na 2 MoO 4 - MgMoO 4 - Cr 2 (MoO 4 ) 3 ternary system is studied by X ray phase and DTA methods. State diagram of NaCr(MoO 4 ) 2 - MgMoO 4 section is plotted. Production of ternary molybdates of Na 1-x Mg 1-x Cr 1+x (MoO 4 ) 3 , where 0 ≤ x ≤ 0.3, and NaMg 3 Cr(MoO 4 ) 5 composition is ascertained [ru

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.

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.

Examination of the magnetic hyperthermia and other magnetic properties of CoFe2O4@MgFe2O4 nanoparticles using external field Mössbauer spectroscopy

Science.gov (United States)

Park, Jeongho; Choi, Hyunkyung; Kim, Sam Jin; Kim, Chul Sung

2018-05-01

CoFe2O4@MgFe2O4 core/shell nanoparticles were synthesized by high temperature thermal decomposition with seed-mediated growth. The crystal structure and magnetic properties of the nanoparticles were investigated using X-ray diffractometry (XRD), vibrating sample magnetometry (VSM), and Mössbauer spectrometry. The magnetic hyperthermia properties were investigated using a MagneTherm device. Analysis of the XRD patterns showed that CoFe2O4@MgFe2O4 had a cubic spinel crystal structure with space group Fd-3m and a lattice constant (a0) of 8.3686 Å. The size and morphology of the CoFe2O4@MgFe2O4 nanoparticles were confirmed by HR-TEM. The VSM measurements showed that the saturation magnetization (MS) of CoFe2O4@MgFe2O4 was 77.9 emu/g. The self-heating temperature of CoFe2O4@MgFe2O4 was 37.8 °C at 112 kHz and 250 Oe. The CoFe2O4@MgFe2O4 core/shell nanoparticles showed the largest saturation magnetization value, while their magnetic hyperthermia properties were between those of the CoFe2O4 and MgFe2O4 nanoparticles. In order to investigate the hyperfine interactions of CoFe2O4, MgFe2O4, and CoFe2O4@MgFe2O4, we performed Mössbauer spectrometry at various temperatures. In addition, Mössbauer spectrometry of CoFe2O4@MgFe2O4 was performed at 4.2 K with applied fields of 0-4.5 T, and the results were analyzed with sextets for the tetrahedral A-site and sextets for the octahedral B-site.

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-07-15

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

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