Characterization of nano-crystalline ZrO{sub 2} synthesized via reactive plasma processing

Energy Technology Data Exchange (ETDEWEB)

Jayakumar, S., E-mail: sjayakumar.physics@gmail.com [Research and Development Centre, Bharathiar University, Coimbatore 641 014 (India); Ananthapadmanabhan, P.V. [Laser and Plasma Technology Division, BARC, Trombay, Mumbai 400 085 (India); Perumal, K. [Department of Physics, Sri Ramakrishna Mission Vidyalaya College of Arts and Science, Coimbatore 641 020 India (India); Thiyagarajan, T.K. [Laser and Plasma Technology Division, BARC, Trombay, Mumbai 400 085 (India); Mishra, S.C. [Department of Metallurgical and Materials Engg, National Institute of Technology, Rourkela 769 008 (India); Su, L.T.; Tok, A.I.Y.; Guo, J. [School of Materials Science and Engg, Nanyang Technological University, 50 Nanyang Avenue, Singapore 639 798 (Singapore)

2011-07-25

Highlights: > Direct conversion of micron-sized zirconium hydride powder to nanocrystalline ZrO{sub 2} powder. > The experimental approach uses reactive plasma processing technique. > The product has been characterized by various analytical tools to support the findings. - Abstract: Nano-crystalline ZrO{sub 2} powder has been synthesized via reactive plasma processing. The synthesized ZrO{sub 2} powders were characterized by X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy (TEM) and FTIR spectroscopy. The synthesized powder consists of a mixture of tetragonal and monoclinic phases of zirconia. Average crystallite size calculated from the XRD pattern shows that particles with crystallite size 20 nm or less than 20 nm are in tetragonal phase, whereas particles greater than 20 nm are in the monoclinic phase. TEM results show that particles have spherical morphology with maximum percentage of particles distributed in a narrow size from about 15 nm to 30 nm.

Crystal structure of superparamagnetic Mg{sub 0.2}Ca{sub 0.8}Fe{sub 2}O{sub 4} nanoparticles synthesized by sol–gel method

Energy Technology Data Exchange (ETDEWEB)

Escamilla-Pérez, A.M., E-mail: angel.mep@gmail.com [Cinvestav-Unidad Saltillo, Industria Metalúrgica No. 1062, Parque Industrial Saltillo-Ramos Arizpe, C.P. 25900, Ramos Arizpe, Coahuila (Mexico); Cortés-Hernández, D.A., E-mail: dora.cortes@cinvestav.edu.mx [Cinvestav-Unidad Saltillo, Industria Metalúrgica No. 1062, Parque Industrial Saltillo-Ramos Arizpe, C.P. 25900, Ramos Arizpe, Coahuila (Mexico); Almanza-Robles, J.M. [Cinvestav-Unidad Saltillo, Industria Metalúrgica No. 1062, Parque Industrial Saltillo-Ramos Arizpe, C.P. 25900, Ramos Arizpe, Coahuila (Mexico); Mantovani, D.; Chevallier, P. [Laboratory for Biomaterials and Bioengineering, Department of Materials Engineering and University Hospital Research Center, Laval University, Quebec City, QC (Canada)

2015-01-15

Powders of magnetic iron oxide nanoparticles (Mg{sub 0.2}Ca{sub 0.8}Fe{sub 2}O{sub 4}) were prepared by a sol–gel method using ethylene glycol and nitrates of Fe, Ca and Mg as starting materials. Those powders were heat treated at different temperatures (573, 673, 773 and 873 K). In order to evaluate the effect of the heat treatment temperature on the nanoferrites properties, X-ray diffraction (XRD), vibrating sample magnetometry (VSM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) techniques were used. It was found that the reaction products exhibit nanometric sizes and superparamagnetic behavior. It is also demonstrated that, as the heat treatment temperature increases, the particle size and the saturation magnetization of the nanoferrites are increased. - Highlights: • Mg{sub 0.2}Ca{sub 0.8}Fe{sub 2}O{sub 4} superparamagnetic nanoparticles were successfully synthesized. • Particle average sizes of Ca–Mg ferrites were within the range of 8–25 nm. • The nanoferrite treated at 873 K showed a stoichiometry close to Mg{sub 0.2}Ca{sub 0.8}Fe{sub 2}O{sub 4}. • The heat treatment temperature has a strong effect on the crystal structure. • These nanoparticles are potential materials for magnetic hyperthermia.

Characterization and densification studies on ThO{sub 2}-UO{sub 2} pellets derived from ThO{sub 2} and U{sub 3}O{sub 8} powders

Energy Technology Data Exchange (ETDEWEB)

Kutty, T.R.G. [Radiometallurgy Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400 085 (India)]. E-mail: tkutty@magnum.barc.ernet.in; Hegde, P.V. [Radiometallurgy Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400 085 (India); Khan, K.B. [Radiometallurgy Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400 085 (India); Jarvis, T. [Radiometallurgy Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400 085 (India); Sengupta, A.K. [Radiometallurgy Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400 085 (India); Majumdar, S. [Radiometallurgy Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400 085 (India); Kamath, H.S. [Nuclear Fuels Group, Bhabha Atomic Research Centre, Trombay, Mumbai 400 085 (India)

2004-12-01

ThO{sub 2} containing around 2-3% {sup 233}UO{sub 2} is the proposed fuel for the forthcoming Indian Advanced Heavy Water Reactor (AHWR). This fuel is prepared by powder metallurgy technique using ThO{sub 2} and U{sub 3}O{sub 8} powders as the starting material. The densification behaviour of the fuel was evaluated using a high temperature dilatometer in four different atmospheres Ar, Ar-8%H{sub 2}, CO{sub 2} and air. Air was found to be the best medium for sintering among them. For Ar and Ar-8%H{sub 2} atmospheres, the former gave a slightly higher densification. Thermogravimetric studies carried out on ThO{sub 2}-2%U{sub 3}O{sub 8} granules in air showed a continuous decrease in weight up to 1500 deg. C. The effectiveness of U{sub 3}O{sub 8} in enhancing the sintering of ThO{sub 2} has been established.

Synthesis of ceramic powders of La9,56 (SiO4)6O2,34 and La9,8Si5,7MgO,3O26,4 by modified sol-gel process

International Nuclear Information System (INIS)

Lira, Sabrina Lopes; Paiva, Mayara Rafaela Soares; Misso, Agatha Matos; Elias, Daniel Ricco; Yamagata, Chieko

2012-01-01

Lanthanum silicate oxyapatite materials are promising for application as electrolyte in solid oxide fuel cells because of high ionic conductivity at temperatures between 600 deg C and 800 deg C. In this work, oxyapatites with the composition La 9,56 (SiO 4 ) 6 O 2,34 , and La 9,8 Si 5,7 Mg 0,3 O 26,4 were synthesized by using the sol-gel method, followed by precipitation. Initially, the gel of silica was synthesized from sodium silicate solution, by acid catalysis using lanthanum and magnesium chloride solution. Then, the La and Mg hydroxides were precipitated with NaOH in the gel. The powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and measurements of specific surface area. The crystalline oxyapatite phase of La 9,56 (SiO 4 ) 6 O 2,34 , and was La 9,8 Si 5,7 Mg 0,3 O 26,4 obtained by calcination at 900 deg C for 2 and 1h respectively (author)

Granulometric analysis of metallic oxide in ceramic powder form synthesized by different methods

International Nuclear Information System (INIS)

Neiva, L.S.; Simoes, A.N.; Simoes, V.N.; Bispo, A.; Gama, L.

2012-01-01

The aim of this work is to synthesize ceramic powders based on CuO/CeO 2 by means two different synthesis methods, they are: the combustion reaction method and Pechini method. It's part of the aim of this work subject all samples to a synthesized qualitative and quantitative chemical analysis, using the technique EDX and then to a granulometric analysis. The samples of the ceramic powder based on CuO/CeO 2 synthesized in this work by means of the two above synthesis methods, contain various concentrations of CuO ranging between 0 and 0.5 mol. According to the results, only the Pechini method of synthesis exerted a significant and defined influence on the capacity of particle unit agglomeration in these powders (author)

Zirconium tungstate/epoxy nanocomposites: effect of nanoparticle morphology and negative thermal expansivity.

Science.gov (United States)

Wu, Hongchao; Rogalski, Mark; Kessler, Michael R

2013-10-09

The ability to tailor the coefficient of thermal expansion (CTE) of a polymer is essential for mitigating thermal residual stress and reducing microcracks caused by CTE mismatch of different components in electronic applications. This work studies the effect of morphology and thermal expansivity of zirconium tungstate nanoparticles on the rheological, thermo-mechanical, dynamic-mechanical, and dielectric properties of ZrW2O8/epoxy nanocomposites. Three types of ZrW2O8 nanoparticles were synthesized under different hydrothermal conditions and their distinct properties were characterized, including morphology, particle size, aspect ratio, surface area, and CTE. Nanoparticles with a smaller particle size and larger surface area led to a more significant reduction in gel-time and glass transition temperature of the epoxy nanocomposites, while a higher initial viscosity and significant shear thinning behavior was found in prepolymer suspensions containing ZrW2O8 with larger particle sizes and aspect ratios. The thermo- and dynamic-mechanical properties of epoxy-based nanocomposites improved with increasing loadings of the three types of ZrW2O8 nanoparticles. In addition, the introduced ZrW2O8 nanoparticles did not negatively affect the dielectric constant or the breakdown strength of the epoxy resin, suggesting potential applications of ZrW2O8/epoxy nanocomposites in the microelectronic insulation industry.

Effect of Sr substitution on superconductivity in Hg2(Ba1-ySry)2YCu2O8-d (part 1): a neutron powder diffraction study

OpenAIRE

Toulemonde, P.; Odier, P.; Bordet, P.; Floch, S. Le; Suard, E.

2002-01-01

The effect of Sr chemical pressure on superconductivity was investigated in Hg2(Ba1-ySry)2YCu2O8-d. The samples were synthesized at high pressure-high temperature from y = 0.0 to full substitution, y = 1.0. These Sr-substituted compounds are superconducting, without Ca doping on the Y site, and show an increasing Tc with Sr, reaching 42 K for y = 1.0. A detailed neutron powder diffraction study compares the structural changes induced by this chemical Sr/Ba substitution and the mechanical pres...

The effect of hydrothermal treatment on samaria and gadolinia doped ceria powders synthesized by coprecipitation

International Nuclear Information System (INIS)

Arakaki, Alexander Rodrigo; Yoshito, Walter Kenji; Ussui, Valter; Lazar, Dolores Ribeiro Ricci

2009-01-01

One of the main applications of ceria-based (CeO 2 ) ceramics is the manufacturing of Intermediate Temperature Solid Oxide Fuel Cells electrolytes. In order to improve ionic conductivity and densification of these materials various powder synthesis routes have been studied. In this work powders with composition Ce 0.8 (SmGd) 0.2 O 1.9h ave been synthesized by coprecipitation and hydrothermal treatment. A concentrate of rare earths containing 90wt% of CeO 2 and other containing 51% of Sm 2 O 3 and 30% of Gd 2 O 3 , both prepared from monazite processing, were used as precursor materials. The powders were characterized by X-ray diffraction, scanning and transmission electron microscopy, agglomerate size distribution by laser scattering and specific surface area by gas adsorption. Ceramic sinterability was evaluated by dilatometry and density measurements by Archimedes method. High specific surface area powders (~100m 2 /g) and cubic fluorite structure were obtained after hydrothermal treatment around 200 deg C. Ceramic densification was improved when compared to the one prepared from powders calcined at 800 deg C. (author)

Facile synthesis and electrical switching properties of V{sub 2}O{sub 3} powders

Energy Technology Data Exchange (ETDEWEB)

Ji, Haining; Liu, Dongqing, E-mail: dongqingliu@ymail.com; Cheng, Haifeng; Yang, Lixiang; Zhang, Chaoyang; Zheng, Wenwei

2017-03-15

Highlights: • Single crystal uniform V{sub 2}O{sub 3} powders have been synthesized without additional surfactant. • Powders were obtained in only 6 h. • Powders exhibit reversible phase transition properties. • Powders have excellent electrical switching properties with resistance changes as large as 10{sup 4}. - Abstract: V{sub 2}O{sub 3} powders were synthesized with mercaptoacetic acid (C{sub 2}H{sub 4}O{sub 2}S) as reducing agent and stabilizer via a facile hydrothermal approach. The crystalline structure, surface morphology, valence state of the derived V{sub 2}O{sub 3} powders were characterized via X-ray diffraction, scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy. It was found that the ratio and reaction time played a duel role in the formation and morphology of the V{sub 2}O{sub 3} powders. The metal-insulator transition properties of V{sub 2}O{sub 3} powders were studied by the differential scanning calorimetry curve and variable temperature Raman spectra. The change in electrical resistance due to the metal-insulator transition was measured from 80 to 240 K using physical property measurement system. The results showed V{sub 2}O{sub 3} samples had excellent electrical switching properties with resistance changes as large as 10{sup 4}. This simple and fast synthesis approach makes the V{sub 2}O{sub 3} powders easily accessible for exploring their fundamental properties and potential applications in novel electronic devices.

Sol-gel synthesis and structure of La2O3–CoO–SiO2 powders

Directory of Open Access Journals (Sweden)

Lachezar Radev

2008-12-01

Full Text Available LaCoO3 powders are studied because they exhibit interesting electrical, magnetic and catalytic properties. In this paper, new synthesized La2O3-CoO-SiO2 powders with different quantity of silica were prepared via solgel method in aqua media, starting from metal nitrates with different chelating agents. The relation between the reaction in solution, crystallization pathway and morphology were discussed. In LaCoO3-SiO2 powders, depending on the content of SiO2 and the treatment temperature (700–1100°C, different crystalline phases (LaCoO3, Co2SiO4 and La9.31(SiO46O2 were observed with the crystallite sizes ranging from 50 to 100 nm. It was proved that chemical composition and nature of used additives has influence on the phase formation and structure of obtained nanomaterials.

Crystallization kinetics and growth mechanism of 8 mol% yttria-stabilized zirconia (8YSZ) nano-powders prepared by a sol-gel process

International Nuclear Information System (INIS)

Kuo, C.-W.; Lee, Y.-H.; Hung, I-M.; Wang, M.-C.; Wen, S.-B.; Fung, K.-Z.; Shih, C.-J.

2008-01-01

Eight mol% yttria-stabilized zirconia (8YSZ) gel powders were synthesized at 348 K for 2 h using ZrOCl 2 .8H 2 O and Y(NO 3 ) 3 .6H 2 O as starting materials in an ethanol-water solution by a sol-gel process. The crystallization kinetics and growth mechanism of the 8YSZ gel powders have been investigated using differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). The XRD results and SAED pattern show that the 8YSZ gel powders calcined at 773 K for 2 h is a cubic ZrO 2 . The activation energy for the crystallization of the cubic ZrO 2 formation in the 8YSZ gel powders is determined as 231.76 kJ/mol by a non-isothermal DTA method. Both growth morphology parameter (n) and crystallization mechanism index (m) are close to 3.0, indicating that the bulk nucleation is dominant in the cubic ZrO 2 formation. The TEM examination shows that the cubic ZrO 2 has a spherical-like morphology with a size ranging from 10 to 20 nm

High power density cell using nanostructured Sr-doped SmCoO3 and Sm-doped CeO2 composite powder synthesized by spray pyrolysis

Science.gov (United States)

Shimada, Hiroyuki; Yamaguchi, Toshiaki; Suzuki, Toshio; Sumi, Hirofumi; Hamamoto, Koichi; Fujishiro, Yoshinobu

2016-01-01

High power density solid oxide electrochemical cells were developed using nanostructure-controlled composite powder consisting of Sr-doped SmCoO3 (SSC) and Sm-doped CeO2 (SDC) for electrode material. The SSC-SDC nano-composite powder, which was synthesized by spray pyrolysis, had a narrow particle size distribution (D10, D50, and D90 of 0.59, 0.71, and 0.94 μm, respectively), and individual particles were spherical, composing of nano-size SSC and SDC fragments (approximately 10-15 nm). The application of the powder to a cathode for an anode-supported solid oxide fuel cell (SOFC) realized extremely fine cathode microstructure and excellent cell performance. The anode-supported SOFC with the SSC-SDC cathode achieved maximum power density of 3.65, 2.44, 1.43, and 0.76 W cm-2 at 800, 750, 700, and 650 °C, respectively, using humidified H2 as fuel and air as oxidant. This result could be explained by the extended electrochemically active region in the cathode induced by controlling the structure of the starting powder at the nano-order level.

Preparation methods of U3O8 powder for MTR fuel elements

International Nuclear Information System (INIS)

Leal Neto, R.M.; Riella, H.G.

1990-01-01

Three preparation methods of U 3 O 8 powder have been studied with the aim of finding a simple and economic processing route: grinding of sintered U 3 O 8 pellets (Method-1); sintering of U 3 O 8 calcined granules (Method-2); and sintering of ammonium diuranate (ADU) granules (Method-3). Granulometric yield, powder characteristics and processing steps and difficulties have been taken into account for comparison purposes. Method-2 have been found to give the best results. Method-3 gives also good results, but there were some difficulties with ADU handling. (author) [pt

Characterization of Ce0.9Gd0.1O1.95 powders synthesized by spray drying

DEFF Research Database (Denmark)

Blennow Tullmar, Peter; Chen, Weiwu; Lundberg, Mats

2009-01-01

Ce0.9Gd0.1O1.95 powders were synthesized by spray drying and successive calcinations. The phase purity, BET surface area, and particle morphology of as-sprayed and calcined powders were characterized. After calcination above 300 °C, the powders were single phase and showed a BET surface area of 68...

Crystallization kinetics and growth mechanism of 8 mol% yttria-stabilized zirconia (8YSZ) nano-powders prepared by a sol-gel process

Energy Technology Data Exchange (ETDEWEB)

Kuo, C.-W. [Department of Resources Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Lee, Y.-H. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Hung, I-M. [Department of Chemical Engineering and Materials Science, Yuan Ze University, 135 Far-East Road, Chung-Li, Taoyuan, Taiwan (China); Wang, M.-C. [Faculty of Fragrance and Cosmetics, Kaohsiung Medical University, 100 Shi-Chuan 1st Road, Kaohsiung 807, Taiwan (China); Wen, S.-B. [Department of Resources Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Fung, K.-Z. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Shih, C.-J. [Faculty of Fragrance and Cosmetics, Kaohsiung Medical University, 100 Shi-Chuan 1st Road, Kaohsiung 807, Taiwan (China)], E-mail: cjshih@kmu.edu.tw

2008-04-03

Eight mol% yttria-stabilized zirconia (8YSZ) gel powders were synthesized at 348 K for 2 h using ZrOCl{sub 2}.8H{sub 2}O and Y(NO{sub 3}){sub 3}.6H{sub 2}O as starting materials in an ethanol-water solution by a sol-gel process. The crystallization kinetics and growth mechanism of the 8YSZ gel powders have been investigated using differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). The XRD results and SAED pattern show that the 8YSZ gel powders calcined at 773 K for 2 h is a cubic ZrO{sub 2}. The activation energy for the crystallization of the cubic ZrO{sub 2} formation in the 8YSZ gel powders is determined as 231.76 kJ/mol by a non-isothermal DTA method. Both growth morphology parameter (n) and crystallization mechanism index (m) are close to 3.0, indicating that the bulk nucleation is dominant in the cubic ZrO{sub 2} formation. The TEM examination shows that the cubic ZrO{sub 2} has a spherical-like morphology with a size ranging from 10 to 20 nm.

Plasma dynamic synthesis and obtaining ultrafine powders of iron oxides with high content of ε-Fe{sub 2}O{sub 3}

Energy Technology Data Exchange (ETDEWEB)

Sivkov, Alexander [Institute of Power Engineering, National Research Tomsk Polytechnic University, Lenin av., 30, Tomsk 634050 (Russian Federation); Naiden, Evgenii [Faculty of Radiophysics, National Research Tomsk State University, Lenin av., 36, Tomsk 634050 (Russian Federation); Ivashutenko, Alexander [Institute of Power Engineering, National Research Tomsk Polytechnic University, Lenin av., 30, Tomsk 634050 (Russian Federation); Shanenkov, Ivan, E-mail: Swordi@list.ru [Institute of Power Engineering, National Research Tomsk Polytechnic University, Lenin av., 30, Tomsk 634050 (Russian Federation)

2016-05-01

The ultrafine iron oxide powders were successfully synthesized using the plasma dynamic synthesis method, based on the use of a coaxial magnetoplasma accelerator with the iron electrode system. The synthesis was implemented in the high-speed iron-containing plasma jet, flowing into the space of the sealed chamber, filled with the gaseous mixture of oxygen and argon at different ratios. The XRD investigations showed that the synthesized products were heterophase and consisted of three main phases such as magnetite Fe{sub 3}O{sub 4}, hematite α-Fe{sub 2}O{sub 3} and ε-Fe{sub 2}O{sub 3}. The SEM data confirmed the presence of three particle types: the hollow spheroids with sizes about hundreds of micrometers (magnetite), the particles with sizes up to 100 μm from the porous material of sintered submicron particles (hematite), and nanoscale particles (ε-phase). We found that at the higher oxygen concentration the content of ε-Fe{sub 2}O{sub 3} is increased up to ~50% at the same time with decreasing the Fe{sub 3}O{sub 4} phase. The magnetic properties of the products are mainly determined by magnetite characteristics and are significantly reduced with decreasing its content in the powder. In order to investigate the synthesized ε-Fe{sub 2}O{sub 3} on the ability to absorb the electromagnetic radiation in the millimeter wavelength range, we separated the product with the higher ε-phase concentration. The fraction mainly, consisting of ε-Fe{sub 2}O{sub 3}, showed the occurrence of the natural resonance at frequencies of 8.3 GHz and 130 GHz. - Highlights: • We synthesized iron oxide powder with high content of ε-Fe{sub 2}O{sub 3}. • Synthesis is implemented using iron-containing plasma jet flowing into O{sub 2} atm. • Synthesized powders are heterophase and consist of ε-Fe{sub 2}O{sub 3,} α-Fe{sub 2}O{sub 3} and Fe{sub 3}O{sub 4}. • ε-Fe{sub 2}O{sub 3} content increases up to 50% with increasing the O{sub 2} volume concentration. • We found the

Ceramic grade (U,Pu)O2 powder fabrication

International Nuclear Information System (INIS)

Cristallini, O.A.; Villegas de Maroto, Marina; De Pino, J.I.; Osuna, H.A.

1980-01-01

Ceramic grade UO 2 powder was obtained by the homogeneous precipitation method. This procedure was afterwards applied to the fabrication of ceramic grade (U,Pu)O 2 powders, and mixed oxide powders with Pu content ranging from 0.7 to 16% were obtained. The obtainment of mixed ceramic oxides as well as the recuperation of fabrication scraps were developed in three steps: 1)study of the process of homogeneous precipitation of ammonium diuranate (ADU); 2) co-precipitation of ADU/PuO 2 .H 2 O for Pu concentrations of 0.6 and 6.8; 3) the thermal conditioning to mixed oxide (U,Pu)O 2 powders. The experimental procedure involves the following steps: preparation of the PuO 2 (NO 3 ) 4 solution; co-precipitation of the PuO 2 (NO 3 ) 2 solution with an UO 2 (NO 3 ) 2 solution; filtration and drying of the precipitate, thermal treatment and finally, mixing, pressing and sintering of the (U,Pu)O 2 and Nukem UO 2 powder with a 0. of zinc stearate. Different controls were made by means of physical, chemical and ceramographic tests. This method can be used for the fabrication of fast reactor fuels or, previous mechanical dispersion in UO 2 powder, for the fabrication of thermal reactors fuels. (M.E.L.) [es

Combined wet-chemical process to synthesize 65PMN-35PT nanosized powders

International Nuclear Information System (INIS)

Santos, Luis P.S.; Longo, Elson; Leite, Edson R.; Camargo, Emerson R.

2004-01-01

Columbite MgNb 2 O 6 precursors were synthesized by a wet-chemical method by means of the dissolution of Nb 2 O 5 .5H 2 O and magnesium carbonate in a solution of oxalic acid. Pure 65PMN-35PT powders could be obtained by the columbite method with the use of the partial oxalate and oxidant peroxo methods. Powders were characterized by X-ray diffraction and FT-Raman spectroscopy showing that pure 65PMN-35PT are obtained when the powders are calcined up to 800 deg. C, without any trace of Pb-Nb pyrochlore. Cubic Pb 1,86 Mg 0.24 Nb 1.76 O 6.5 pyrochlore phase is formed by lead loss in the powders calcined at 900 deg. C and higher temperatures as undoubtedly characterized by Raman spectroscopy

Extremely fine structured cathode for solid oxide fuel cells using Sr-doped LaMnO3 and Y2O3-stabilized ZrO2 nano-composite powder synthesized by spray pyrolysis

Science.gov (United States)

Shimada, Hiroyuki; Yamaguchi, Toshiaki; Sumi, Hirofumi; Nomura, Katsuhiro; Yamaguchi, Yuki; Fujishiro, Yoshinobu

2017-02-01

A solid oxide fuel cell (SOFC) for high power density operation was developed with a microstructure-controlled cathode using a nano-composite powder of Sr-doped LaMnO3 (LSM) and Y2O3-stabilized ZrO2 (YSZ) synthesized by spray pyrolysis. The individual LSM-YSZ nano-composite particles, formed by crystalline and amorphous nano-size LSM and YSZ particles, showed spherical morphology with uniform particle size. The use of this powder for cathode material led to an extremely fine microstructure, in which all the LSM and YSZ grains (approximately 100-200 nm) were highly dispersed and formed their own network structures. This microstructure was due to the two phase electrode structure control using the powder, namely, nano-order level in each particle and micro-order level between particles. An anode-supported SOFC with the LSM-YSZ cathode using humidified H2 as fuel and ambient air as oxidant exhibited high power densities, such as 1.29 W cm-2 under a voltage of 0.75 V and a maximum power density of 2.65 W cm-2 at 800 °C. Also, the SOFC could be stably operated for 250 h with no degradation, even at a high temperature of 800 °C.

New vanadium tellurites: Syntheses, structures, optical properties of noncentrosymmetric VTeO{sub 4}(OH), centrosymmetric Ba{sub 2}V{sub 4}O{sub 8}(Te{sub 3}O{sub 10})

Energy Technology Data Exchange (ETDEWEB)

Liang, Ming-Li [College of Chemistry, Fuzhou University, Fuzhou, Fujian 350108 (China); State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China); Marsh, Matthew [Department of Chemistry and Biochemistry, Florida State University, Tallahassee, FL 32306 (United States); Shang, Xian-Xing [College of Chemistry, Fuzhou University, Fuzhou, Fujian 350108 (China); State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China); Mao, Jiang-Gao [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China); Albrecht-Schmitt, Thomas E. [Department of Chemistry and Biochemistry, Florida State University, Tallahassee, FL 32306 (United States); Kong, Fang, E-mail: kongfang@fjirsm.ac.cn [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China); Department of Chemistry and Biochemistry, Florida State University, Tallahassee, FL 32306 (United States)

2017-05-15

Two new vanadium tellurites, VTeO{sub 4}(OH) (1) and Ba{sub 2}V{sub 4}O{sub 8}(Te{sub 3}O{sub 10}) (2), have been synthesized successfully with the use of hydrothermal reactions. The crystal structures of the two compounds were determined by single-crystal X-ray diffraction. Compound 1 crystallizes in the polar space group Pca2{sub 1} (No. 29) while compound 2 crystallizes in the centrosymmetric space group C2/c (No. 15). The topography of compound 1 reveals a two-dimensional, layered structure comprised of VO{sub 6} octahedral chains and TeO{sub 3}(OH) zig-zag chains. Compound 2, on the contrary, features a three-dimensional [V{sub 4}O{sub 8}(Te{sub 3}O{sub 10})]{sup 4-} anionic framework with Ba{sup 2+} ions filled into the 10-member ring helical tunnels. The [V{sub 4}O{sub 8}(Te{sub 3}O{sub 10})]{sup 4-} anionic network is the first 3D vanadium tellurite framework to be discovered in the alkaline-earth vanadium tellurite system. Powder second harmonic generation (SHG) measurements indicate that compound 1 shows a weak SHG response of about 0.3×KDP (KH{sub 2}PO{sub 4}) under 1064 nm laser radiation. Infrared spectroscopy, elemental analysis, thermal analysis, and dipole moment calculations have also been carried out. - Graphical abstract: VTeO{sub 4}(OH) (1) crystallizes in the noncentrosymmetric space group Pca2{sub 1} (No. 29) while Ba{sub 2}V{sub 4}O{sub 8}(Te{sub 3}O{sub 10}) (2) crystallizes in the centrosymmetric space group C2/c (No. 15). - Highlights: • VTeO{sub 4}(OH) (1) and Ba{sub 2}V{sub 4}O{sub 8}(Te{sub 3}O{sub 10}) (2) have been synthesized successfully with the use of hydrothermal reactions. • VTeO{sub 4}(OH) (1) crystallizes in the noncentrosymmetric space group Pca2{sub 1} and displays a weak SHG response. • VTeO{sub 4}(OH) (1) represents only the fourth SHG-active material found in vanadium tellurite systems. • Ba{sub 2}V{sub 4}O{sub 8}(Te{sub 3}O{sub 10}) (2) exhibits a novel three-dimensional [V{sub 4}O{sub 8}(Te{sub 3}O{sub 10

Synthesis of Nanocrystalline RuO2(60%)-SnO2(40%)Powders by Amorphous Citrate Route

Institute of Scientific and Technical Information of China (English)

无

2007-01-01

Nanometer RuO2-SnO2was synthesized by the citrate-gel method using RuCl3, SnCl4 as cation sources, citric acid as complexing agent and anhydrous ethanol as solvent. The structures of the derived powders were characterized by thermogravimetric and differential thermal analysis, X-ray diffraction, transmission electron microscope, and Brunauer-Emmett-Teller surface area measurement. The pure, fine and amorphous powders was obtained at 160℃. The materials calcined at above 400 ℃ were composed of rutile-type oxide phases having particle sizes of fairly narrow distribution and good thermal resistant properties. By adding SnO2 to RUO2, the Ru metallic phase can be effectively controlled under a traditional temperature of preparation for dimensional stable anode.

Thermal evolution of CaO-doped HfO{sub 2} films and powders

Energy Technology Data Exchange (ETDEWEB)

Barolin, S A; Sanctis, O A de [Lab. Materiales Ceramicos, FCEIyA, Universidad Nacional de Rosario, IFIR-CONICET (Argentina); Caracoche, M C; Martinez, J A; Taylor, M A; Pasquevich, A F [Departamento de Fisica, FCE, Universidad Nacional de La Plata, IFLP-CONICET (Argentina); Rivas, P C, E-mail: oski@fceia.unr.edu.a [Facultad de Ciencias Agronomicas y Forestales, Universidad Nacional de La Plata, IFLP (Argentina)

2009-05-01

Solid solutions of ZrO2 and HfO2 are potential electrolyte materials for intermediate-temperature SOFC because both are oxygen-ion conductors. The main challenge for these compounds is to reduce the relatively high value of the activation energies vacancies diffusion, which is influenced by several factors. In this work the thermal evolution of CaO-HfO{sub 2} materials have been investigated. (CaO)y-Hf(1-y)O(2-y) (y = 0.06, 0.14 y 0.2) coatings and powders were synthesized by chemical solution deposition (CSD). Films were deposited onto alumina substrates by Dip Coating technique, the burning of organic waste was carried out at 500 deg. C under normal atmosphere and then the films were thermally treated at intervals of temperature rising to a maximum temperature of 1250 deg. C. By means Glazing Incidence X-ray Diffraction (rho-2theta configuration) the phases were studied in the annealed films. On the other hand, the thermal evolution and crystallization process of powders were analyzed in-situ by HT-XRD. The phenomena crystallization occurred in films and powders were analyzed. The activation energies of diffusion of oxygen vacancies of HfO2-14 mole% CaO and HfO2-20 mole% CaO films were measured from the thermal evolution of the relaxation constant measured by Perturbed Angular Correlation Technique.

Effects of phosphorus-doping on energy band-gap, structural, surface, and photocatalytic characteristics of emulsion-based sol-gel derived TiO{sub 2} nano-powder

Energy Technology Data Exchange (ETDEWEB)

Ganesh, Ibram, E-mail: ibramganesh@arci.res.in

2017-08-31

Highlights: • Reported a novel route to synthesize high specific surface area P-doped TiO{sub 2} nano-powder photocatalysts. • Established methylene blue dye-sensitization mechanism of TiO{sub 2} photocatalyst. • Established the effects of methylene blue adsorption on the surface, structural and photocatalytic activity of P-doped TiO{sub 2}. • Established true quantum efficiency determination method for TiO{sub 2} photocatalysis. - Abstract: Different amounts of phosphorus (P)-doped TiO{sub 2} (PDT) nano-powders (P = 0–10 wt.%) were synthesized by following a new emulsion-based sol-gel (EBSG) route and calcined at 400 °C–800 °C for 6 h. These calcined PDT powders were then thoroughly characterized by means of XRD, XPS, SEM, FT-IR, FT-Raman, DRS, BET surface area, zeta-potential, cyclic-voltammetry and photocatalytic evaluation using methylene blue (MB) as a model-pollutant and established the effects of phosphorous doping on structural, surface, band-gap energy, and photocatalytic characteristics of TiO{sub 2} nano-powder formed in EBSG route. The characterization results suggest that the EBSG derived TiO{sub 2} nano-powder after calcination at 400 °C for 6 h is in the form of anatase phase when it was doped with <8 wt.% P, and it is in the amorphous state when doped with >8 wt.% P. Furthermore, these EBSG derived PDT powders own high negative zeta-potentials, high specific surface areas (up to >250 m{sup 2}/g), and suitable band-gap energies (<3.34 eV). Surprisingly, these PDT powders exhibit very high MB adsorption (up to 50%) from its aqueous 0.01 mM, 0.02 mM and 0.03 mM solutions during 30 min stirring in the dark, whereas, the commercial Degussa P-25 TiO{sub 2} nano-powder shows no adsorption. Among various photocatalysts investigated in this study, the 1 wt.% P-doped TiO{sub 2} nano-powder formed in EBSG route exhibited the highest photocatalytic activity for MB degradation reaction.

Photocatalytic behaviors and structural characterization of nanocrystalline Fe-doped TiO2 synthesized by mechanical alloying

International Nuclear Information System (INIS)

Kim, Dong Hyun; Hong, Hyun Seon; Kim, Sun Jae; Song, Jae Sung; Lee, Kyung Sub

2004-01-01

Nanocrystalline Fe-doped TiO 2 powders were synthesized by mechanical alloying (MA) with varying Fe contents from 0 up to 4.8 wt.% to shift the absorption threshold into the visible light region. The photocatalytic feasibility of the Fe-doped TiO 2 powder was evaluated by quantifying the visible light absorption capacity using ultraviolet and visible (UV-Vis) spectroscopy and photoluminescence spectroscopy. Effects of Fe additions on the crystal structures and the morphologies of the Fe-doped powders were also investigated as a function of the doping content using transmission electron microscopy-electron diffraction pattern (TEM-EDP), X-ray diffraction (XRD) and energy dispersive X-ray (EDAX) and X-ray photoelectron spectroscopy (XPS). The UV-Vis study showed that the UV absorption for the Fe-doped powder moved to a longer wavelength (red shift) and the photoefficiency was enhanced. Based on the analysis of the photoluminescence spectra, the red shift was believed to be induced by localizing the dopant level near the valence band of TiO 2 . The UV-Vis absorption depended on the Fe concentration. TEM-EDP and XRD investigations showed that the Fe-doped powder had a rutile phase in which the added Fe atoms were dissolved. The rutile phase was composed of spherical particles and chestnut bur shaped particles, resulting in a larger surface area than the spherical P-25 powder

Hydrothermal syntheses and characterization of two layered molybdenum selenites, Rb2(MoO3)3SeO3 and Tl2(MoO3)3SeO3

International Nuclear Information System (INIS)

Dussack, L.L.; Harrison, W.T.A.; Jacobson, A.J.

1996-01-01

The hydrothermal syntheses of Rb 2 (MoO 3 ) 3 SeO 3 , and Tl 2 (MoO 3 ) 3 SeO 3 are described. These compounds have structures built up from hexagonal-WO 3 -type sheets and are isostructural with the previously reported Cs 2 (MoO 3 ) 3 SeO 3 and (NH 4 ) 2 (MoO 3 ) 3 SeO 3 . Powder X-ray, thermogravimetric, and spectroscopic data are presented and discussed

TiO{sub 2} and TiO{sub 2}-SiO{sub 2} thin films and powders by one-step soft-solution method: Synthesis and characterizations

Energy Technology Data Exchange (ETDEWEB)

Ennaoui, A.; Sankapal, B.R.; Skryshevsky, V.; Lux-Steiner, M.Ch. [Division Solar Energy Research, Department Heterogeneous Material Systems, Hahn-Meitner-Institut, Glienicker Strasse 100, 14109 Berlin (Germany)

2006-06-15

Simple soft-solution method has been developed to synthesize films and powders of TiO{sub 2} and mixed TiO{sub 2}-SiO{sub 2} at relatively low temperatures. This method is simple and inexpensive. Furthermore, reactor can be designed for large-scale applications as well as to produce large quantities of composite powders in a single step. For the preparation of TiO{sub 2}, we used aqueous acidic medium containing TiOSO{sub 4} and H{sub 2}O{sub 2}, which results in a peroxo-titanium precursor while colloidal SiO{sub 2} has been added to the precursor for the formation of TiO{sub 2}-SiO{sub 2}. Post annealing at 500{sup o}C is necessary to have anatase structure. Resulting films and powders were characterized by different techniques. TiO{sub 2} (anatase) phase with (101) preferred orientation has been obtained. Also in TiO{sub 2}-SiO{sub 2} mixed films and powders, TiO{sub 2} (anatase) phase was found. Fourier transform infrared spectroscopy (FTIR) results for TiO{sub 2} and mixed TiO{sub 2}-SiO{sub 2} films have been presented and discussed. The method developed in this paper allowed obtaining compact and homogeneous TiO{sub 2} films. These compact films are highly photoactive when TiO{sub 2} is used as photo anode in an photoelectrochemical cell. Nanoporous morphology is obtained when SiO{sub 2} colloids are added into the solution. (author)

Nanosize stabilization of cubic and tetragonal phases in reactive plasma synthesized zirconia powders

Energy Technology Data Exchange (ETDEWEB)

Jayakumar, S., E-mail: sjayakumar.physics@gmail.com [Research and Development Centre, Bharathiar University, Coimbatore 641 014 (India); Department of Physics, Pollachi Institute of Engineering and Technology, Pollachi 642 205 (India); Ananthapadmanabhan, P.V.; Thiyagarajan, T.K. [Laser and Plasma Technology Division, BARC, Trombay, Mumbai 400 085 (India); Perumal, K. [Vision for Wisdom, Temple of Consciousness, Aliyar 642 101 (India); Mishra, S.C. [Department of Metallurgical and Materials Engg, National Institute of Technology, Rourkela 769 008 (India); Suresh, G. [Department of Physics, Park College of Engineering and Technology, Coimbatore 641 659 (India); Su, L.T.; Tok, A.I.Y. [School of Materials Science and Engg, Nanyang Technological University, 50 Nanyang Avenue, Singapore 639 798 (Singapore)

2013-06-15

Pure zirconium oxide powders with particle size 2–33 nm are synthesized by reactive plasma processing. Transmission electron microscopy investigation of these particles revealed size dependent behavior for their phase stabilization. The monoclinic phase is found to be stable when particle size is ≥20 nm; Tetragonal is found to be stabilized in the range of 7–20 nm and as the particle size decreases to 6 nm and less, the cubic phase is stabilized. - Highlights: ► Direct conversion of micron-sized zirconium hydride powder to single crystal ZrO{sub 2} nanopowder. ► Size dependent stabilization of cubic, tetragonal and monoclinic phases in the reactive plasma synthesized ZrO{sub 2} nanopowder. ► Transmission electron microscopic investigation to identify particles of different sizes and their corresponding phase structure.

Characterization of γ- Al2O3 nanopowders synthesized by Co-precipitation method

International Nuclear Information System (INIS)

Jbara, Ahmed S.; Othaman, Zulkafli; Ati, Ali A.; Saeed, M.A.

2017-01-01

Co-precipitation technique has been used to synthesize gamma-Al 2 O 3 (γ-Al 2 O 3 ) nanopowders under annealing temperature effect. The crystalline phase and purity for the prepared powder were characterized by different spectroscopy techniques. XRD analysis confirms the gamma phase of alumina nanopowders with particle diameter ranging from 6 to 24 nm, which confirms the quantum dots formation, which is also supported by the BET measurement. The surface area of the prepared nanopowders is in the range of 109–367 m 2 /g. Morphology analysis indicates that γ-Al 2 O 3 nanopowders are consisted of grains almost spherical in shape. Some agglomeration of nanoparticles occurs, which become more regular hexagonal shaped with the increasing annealing temperature. The small nanoparticles size and the high surface area from a simple procedure for preparing γ-Al 2 O 3 may make it more suitable for use as an adsorbent for malachite green. - Highlights: • Co-precipitation technique is used to synthesize gamma- Al 2 O 3 nanopowders. • Pure gamma- Al 2 O 3 phase was obtained having maximum nanoparticle size is 24 nm. • The quantum dots were formed inside powder. • High surface area of nanopowders at the low annealing temperature. • Increasing annealing temperature causes the hexagonal agglomeration shape.

Y2O3-MgO Nano-Composite Synthesized by Plasma Spraying and Thermal Decomposition of Solution Precursors

Science.gov (United States)

Muoto, Chigozie Kenechukwu

This research aims to identify the key feedstock characteristics and processing conditions to produce Y2O3-MgO composite coatings with high density and hardness using solution precursor plasma spray (SPPS) and suspension plasma spray (SPS) processes, and also, to explore the phenomena involved in the production of homogenized nano-composite powders of this material system by thermal decomposition of solution precursor mixtures. The material system would find potential application in the fabrication of components for optical applications such as transparent windows. It was shown that a lack of major endothermic events during precursor decomposition and the resultant formation of highly dense particles upon pyrolysis are critical precursor characteristics for the deposition of dense and hard Y2O3-MgO coatings by SPPS. Using these principles, a new Y2O3-MgO precursor solution was developed, which yielded a coating with Vickers hardness of 560 Hv. This was a considerable improvement over the hardness of the coatings obtained using conventional solution precursors, which was as low as 110 Hv. In the thermal decomposition synthesis process, binary solution precursor mixtures of: yttrium nitrate (Y[n]) or yttrium acetate (Y[a]), with magnesium nitrate (Mg[n]) or magnesium acetate (Mg[a]) were used in order to study the effects of precursor chemistry on the structural characteristics of the resultant Y2O3-MgO powders. The phase domains were coarse and distributed rather inhomogeneously in the materials obtained from the Y[n]Mg[n] and Y[a]Mg[a] mixtures; finer and more homogeneously-distributed phase domains were obtained for ceramics produced from the Y[a]Mg[n] and Y[n]Mg[a] mixtures. It was established that these phenomena were related to the thermal characteristics for the decomposition of the precursors and their effect on phase separation during oxide crystallization. Addition of ammonium acetate to the Y[n[Mg[n] mixture changed the endothermic process to exothermic

Crystallization behavior of ZrO{sub 2}−3Y{sub 2}O{sub 3}−xSrO precursor powders synthesized by a coprecipitation process

Energy Technology Data Exchange (ETDEWEB)

Chu, Hsueh-Liang [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta- Hsueh Road, Tainan 70101, Taiwan (China); Hwang, Weng-Sing [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta- Hsueh Road, Tainan 70101, Taiwan (China); Institute of Nanotechnology and Microsystems Engineering, National Cheng Kung University, 1 Ta- Hsueh Road, Tainan 70101, Taiwan (China); Du, Je-Kang [Department of Dentistry, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China); Department of Dentistry, Kaohsiung Medical University, Chung Ho Memorial Hospital, 100 Tzyou 1st Road, Kaohsiung 80708, Taiwan (China); Chen, Ker-Kong, E-mail: enamel@kmu.edu.tw [Department of Dentistry, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China); Department of Dentistry, Kaohsiung Medical University, Chung Ho Memorial Hospital, 100 Tzyou 1st Road, Kaohsiung 80708, Taiwan (China); Wang, Moo-Chin, E-mail: mcwang@kmu.edu.tw [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China)

2016-09-05

Crystallization behaviors of ZrO{sub 2}−3Y{sub 2}O{sub 3}−xSrO precursor powders were studied with zirconium nitrate (Zr(NO{sub 3}){sub 4}·xH{sub 2}O), yttrium nitrate (Y(NO{sub 3}){sub 3}·6H{sub 2}O) and strontium nitrate (Sr(NO{sub 3}){sub 2}) constituting the initial materials. Differential thermal analysis (DTA), X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), nano beam electron diffraction (NBED) and high-resolution TEM (HRTEM) were utilized to characterize the crystallization behavior of ZrO{sub 2}−3Y{sub 2}O{sub 3}−xSrO precursor powders. The activation energies of tetragonal ZrO{sub 2} (t-ZrO{sub 2}) crystallization were 389.1, 327.6, and 315.1 kJ/mol with SrO content for 1, 2, and 3 mol%, respectively, obtained with a non-isothermal method. The growth morphology parameter and growth mechanism index were close to 2.0 and 1.0, respectively, showing that t-ZrO{sub 2} had a plate-like morphology. - Highlights: • The single phase of tetragonal ZrO{sub 2} formed when calcined at 923 K for 2 h. • ZrO{sub 2}−3Y{sub 2}O{sub 3}−2SrO precursor powders crystallization is at 765.6 K. • The activation energy of t-ZrO{sub 2} crystallization was 389.1 kJ/mol with 1 mol% SrO. • The growth morphology and index of crystallization were close to 2.0 and 1.0.

Nano ZrO{sub 2} particles in nanocrystalline Fe–14Cr–1.5Zr alloy powders

Energy Technology Data Exchange (ETDEWEB)

Xu, W.Z.; Li, L.L.; Saber, M.; Koch, C.C.; Zhu, Y.T., E-mail: ytzhu@ncsu.edu; Scattergood, R.O.

2014-09-15

Here we report on the formation of nano ZrO{sub 2} particles in Fe–14Cr–1.5Zr alloy powders synthesized by mechanical alloying. The nano ZrO{sub 2} particles were found uniformly dispersed in the ferritic matrix powders with an average size of about 3.7 nm, which rendered the alloy powders so stable that it retained nanocrystalline structure after annealing at 900 °C for 1 h. The ZrO{sub 2} nanoparticles have a tetragonal crystal structure and the following orientation relationship with the matrix: (0 0 2){sub ZrO2}//(0 0 2){sub Matrix} and [0 1 0]{sub ZrO2}//[1 2 0]{sub Matrix}. The size and dispersion of the ZrO{sub 2} particles are comparable to those of Y–Ti–O enriched oxides reported in irradiation-resistant ODS alloys. This suggests a potential application of the new alloy powders for nuclear energy applications.

Synthesis and mechanical properties of stabilized zirconia ceramics: MgO-ZrO_2 and Y_2O_3-MgO- ZrO_2

International Nuclear Information System (INIS)

Yamagata, C.; Mello-Castanho, S.R.H.; Paschoal, J.O.A.

2014-01-01

Precursor MgO-ZrO_2 and Y_2O_3-MgO-ZrO_2 ceramic powders were synthesized by the method of co-precipitation and characterized by techniques such as laser diffraction, QELS (Quasi Elastic Light Scattering), XRD, BET, and SEM. Nanoscale powders with specific surface area higher than 60 m"2. g"-"1 was achieved. Sintered ceramic obtained from the synthesized powders, were characterized to mechanical tests using Vickers indentation technique. The addition of Y_2O_3 promoted an increase in hardness of the ceramics and total cubic crystalline phase stabilization. (author)

U3O8 powder from uranyl-loaded cation exchange resin

International Nuclear Information System (INIS)

Mosley, W.C.

1985-01-01

Large batches of U 3 O 8 , suitable for powder metallurgy fabrication of Al-U 3 O 8 cores for reactor fuel tubes, have been produced by deep-bed calcination of granular uranyl-loaded macroporous sulfonate cation exchange resin at 900 to 950 0 C in air. Deep-bed calcination is the backup process for the reference process of rotary calcination and sintering. These processes are to be used for recycling uranium, and to produce U 3 O 8 in the Fuel Production Facility to be built at the Savannah River Plant. 2 refs., 6 figs

Synthesis and characterization of high volume fraction Al-Al2O3 nanocomposite powders by high-energy milling

International Nuclear Information System (INIS)

Prabhu, B.; Suryanarayana, C.; An, L.; Vaidyanathan, R.

2006-01-01

Al-Al 2 O 3 metal matrix composite (MMC) powders with volume fractions of 20, 30, and 50% Al 2 O 3 were synthesized by high-energy milling of the blended component powders. The particle sizes of Al 2 O 3 studied were 50 nm, 150 nm, and 5 μm. A uniform distribution of the Al 2 O 3 reinforcement in the Al matrix was successfully obtained after milling the powders for a period of 20 h at a ball-to-powder ratio of 10:1 in a SPEX mill. The uniform distribution of Al 2 O 3 in the Al matrix was confirmed by characterizing these nanocomposite powders by scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), X-ray mapping, and X-ray diffraction (XRD) techniques

Synthesis of ceramic powders of La{sub 9,56} (SiO{sub 4}){sub 6}O{sub 2,34} and La{sub 9,8}Si{sub 5,7}Mg{sub O,3}O{sub 26,}4 by modified sol-gel process; Sintese de pos ceramicos de La{sub 9,56} (SiO{sub 4}){sub 6}O{sub 2,34} e La{sub 9,8}Si{sub 5,7}Mg{sub O,3}O{sub 26,}4 por processo sol-gel modificado

Energy Technology Data Exchange (ETDEWEB)

Lira, Sabrina Lopes; Paiva, Mayara Rafaela Soares; Misso, Agatha Matos; Elias, Daniel Ricco; Yamagata, Chieko, E-mail: yamagata@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (CCTM/IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Ciencia e Tecnologia de Materiais

2012-07-01

Lanthanum silicate oxyapatite materials are promising for application as electrolyte in solid oxide fuel cells because of high ionic conductivity at temperatures between 600 deg C and 800 deg C. In this work, oxyapatites with the composition La{sub 9,56}(SiO{sub 4}){sub 6}O{sub 2,34}, and La{sub 9,8}Si{sub 5,7}Mg{sub 0,3}O{sub 26,4} were synthesized by using the sol-gel method, followed by precipitation. Initially, the gel of silica was synthesized from sodium silicate solution, by acid catalysis using lanthanum and magnesium chloride solution. Then, the La and Mg hydroxides were precipitated with NaOH in the gel. The powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and measurements of specific surface area. The crystalline oxyapatite phase of La{sub 9,56}(SiO{sub 4}){sub 6}O{sub 2,34}, and was La{sub 9,8}Si{sub 5,7}Mg{sub 0,3}O{sub 26,4} obtained by calcination at 900 deg C for 2 and 1h respectively (author)

and α-Fe 2 O 3 nano powders synthesized by emulsion precipitation

African Journals Online (AJOL)

Nano crystals of γ-Fe2O3 (maghemite) were synthesized by emulsion precipitation method using kerosene as oil phase, SPAN- 80 (sorbitane monooleate) as the surfactant and sodium hydroxide as the precipitating agent. The characterization of the samples by FTIR (Fourier transform infra-red) and XRD (X-ray diffraction) ...

Sonochemically synthesized MnO2 nanoparticles as electrode material for supercapacitors.

Science.gov (United States)

Gnana Sundara Raj, Balasubramaniam; Asiri, Abdullah M; Qusti, Abdullah H; Wu, Jerry J; Anandan, Sambandam

2014-11-01

In this study, manganese oxide (MnO2) nanoparticles were synthesized by sonochemical reduction of KMnO4 using polyethylene glycol (PEG) as a reducing agent as well as structure directing agent under room temperature in short duration of time and characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Scanning electron microscope (SEM), Transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) analysis. A supercapacitor device constructed using the ultrasonically-synthesized MnO2 nanoparticles showed maximum specific capacitance (SC) of 282Fg(-1) in the presence of 1M Ca(NO3)2 as an electrolyte at a current density of 0.5mAcm(-2) in the potential range from 0.0 to 1.0V and about 78% of specific capacitance was retained even after 1000 cycles indicating its high electrochemical stability. Copyright © 2013 Elsevier B.V. All rights reserved.

Combustion synthesis of nanocrystalline ceria (CeO2) powders by a dry route

International Nuclear Information System (INIS)

Hwang, C.-C.; Huang, T.-H.; Tsai, J.-S.; Lin, C.-S.; Peng, C.-H.

2006-01-01

In this study, ceria (CeO 2 ) powders were synthesized with 50 g per batch via a combustion technique using two kinds of starting materials-urea [(NH 2 ) 2 CO] (as a fuel) and ceric ammonium nitrate [Ce(NH 4 ) 2 (NO 3 ) 6 ] (acting as both the source of cerium ion and an oxidizer). The starting materials were mixed thoroughly without adding water, and then ignited in the air at room temperature. It underwent a self-combustion process with a large amount of smoke, a voluminous loose product. The as-synthesized powders were characterized by X-ray diffraction (XRD) analysis, transmission electron microscope (TEM), scanning electron microscope (SEM), CHN elemental analyzer, surface area measurements, and sinterability. Experimental results revealed that the nanocrystalline CeO 2 powders with low impurity content ( 2 /g and ∼25 nm, respectively, through the stoichiometric fuel/oxidizer ratio reaction. The powder, when cold pressed and sintered in the air at 1250 deg. C for 1 h, was measured to attain the sintered density ∼92% of theoretical density having submicron grain size. In addition, the thermal decomposition and combustion process of the reactant mixture were investigated using thermogravimetry (TG), differential scanning calorimetry (DSC), and mass spectrometry (MS) techniques simultaneously. Based on the results of thermal analysis, a possible mechanism concerning the combustion reaction is proposed

High performance Sm{sub 0.5}Sr{sub 0.5}CoO{sub 3}-La{sub 0.8}Sr{sub 0.2}Ga{sub 0.8}Mg{sub 0.15}Co{sub 0.05}O{sub 3} composite cathodes

Energy Technology Data Exchange (ETDEWEB)

Wang, Shizhong; Zou, Yuman [College of Chemistry and Chemical Engineering, Department of Chemistry, Xiamen University, Xiamen 361005, Fujian (China)

2006-06-15

High performance Sm{sub 0.5}Sr{sub 0.5}CoO{sub 3}(SSC)-La{sub 0.8}Sr{sub 0.2}Ga{sub 0.8}Mg{sub 0.15}Co{sub 0.05}O{sub 3} (LSGMC5) composite cathodes for intermediate temperature solid oxide fuel cells (ITSOFC) were prepared and characterized. The SSC powders were synthesized using the glycine-nitrate method and La{sub 0.8}Sr{sub 0.2}Ga{sub 0.8}Mg{sub 0.15}Co{sub 0.05}O{sub 3}(LSGMC5) powders were synthesized using the citrate method. The calcining temperature for the SSC and LSGMC5 powders had strong effect on the microstructure of the composite electrode and electrode/electrolyte interface, which affected the performance of the SSC-LSGMC5 electrode strongly. The electrode based on SSC calcined at 1223K and LSGMC5 calcined at 1273K exhibited the highest performance among the electrodes studied. The electrode resistance was about 0.07{omega}cm{sup 2}, and the overpotential under 1Acm{sup -2} current density was as low as 0.077V at 973K in oxygen, which could be an ideal cathode for ITSOFC based on lanthanum gallate electrolytes. (author)

Comment on 'Pressure-induced changes in transport properties of layered La1.2Ca1.8Mn2O7'

International Nuclear Information System (INIS)

Ganguly, R.; Siruguri, V.; Gopalakrishnan, I.K.; Yakhmi, J.V.

2000-01-01

We show that the compound La 1.2 Ca 1.8 Mn 2 O 7 does not form with layered Sr 3 Ti 2 O 7 -type structure as reported by Kamenev et al. [Phys. Rev. B 56, R12 688 (1997)]. Detailed analysis of the powder x-ray diffraction pattern of this compound (synthesized by using the solid-state method) by Rietveld method shows that it forms a multiphase mixture comprising hole-doped perovskite manganates (La 1-x Ca x MnO 3 ) as the majority phases and CaO as the minority phase

Bioactivity and cell proliferation in radiopaque gel-derived CaO-P2O5-SiO2-ZrO2 glass and glass-ceramic powders.

Science.gov (United States)

Montazerian, Maziar; Yekta, Bijan Eftekhari; Marghussian, Vahak Kaspari; Bellani, Caroline Faria; Siqueira, Renato Luiz; Zanotto, Edgar Dutra

2015-10-01

In this study, 10 mol% ZrO2 was added to a 27CaO-5P2O5-68SiO2 (mol%) base composition synthesized via a simple sol-gel method. This composition is similar to that of a frequently investigated bioactive gel-glass. The effects of ZrO2 on the in vitro bioactivity and MG-63 cell proliferation of the glass and its derivative polycrystalline (glass-ceramic) powder were investigated. The samples were characterized using thermo-gravimetric and differential thermal analysis (TG/DTA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM) coupled to energy dispersive X-ray spectroscopy (EDS). Release of Si, Ca, P and Zr into simulated body fluid (SBF) was determined by inductively coupled plasma (ICP). Upon heat treatment at 1000 °C, the glass powder crystallized into an apatite-wollastonite-zirconia glass-ceramic powder. Hydroxycarbonate apatite (HCA) formation on the surface of the glass and glass-ceramic particles containing ZrO2 was confirmed by FTIR and SEM. Addition of ZrO2 to the base glass composition decreased the rate of HCA formation in vitro from one day to three days, and hence, ZrO2 could be employed to control the rate of apatite formation. However, the rate of HCA formation on the glass-ceramic powder containing ZrO2 crystal was equal to that in the base glassy powder. Tests with a cultured human osteoblast-like MG-63 cells revealed that the glass and glass-ceramic materials stimulated cell proliferation, indicating that they are biocompatible and are not cytotoxic in vitro. Moreover, zirconia clearly increased osteoblast proliferation over that of the Zr-free samples. This increase is likely associated with the lower solubility of these samples and, consequently, a smaller variation in the media pH. Despite the low solubility of these materials, bioactivity was maintained, indicating that these glassy and polycrystalline powders are potential candidates for bone graft substitutes and bone cements with

Structural and morphological characterization of TiO2-ZrO2 powders obtained by the polymeric precursors method

International Nuclear Information System (INIS)

Ribeiro, M.A.; Gama, L.; Bispo, A.; Neiva, L.S.; Bernardi, M.I.B.; Kiminami, R.H.G.A.

2010-01-01

This work aims to characterize the structure and morphology of TiO 2 -ZrO 2 powders obtained by polymeric precursor method. For this we studied the following compositions: 0.25, 0.5 and 0.75 moles of Zr and calcined at 800 deg C for one hour. The powders obtained were characterized by XRD, SEM and nitrogen adsorption (BET). The analysis of X-ray diffraction showed that the powders had a phase of TiO 2 in the anatase form and a tetragonal phase of ZrO 2 . The crystallite size was between 8, 13 and 11 nm respectively. The analysis of scanning electron microscopy showed the growth of ZrO 2 nanoparticles and that these comprise spherical agglomerates of less than 100 nm. Particle size determined by the BET ranging 28.1-29.5 nm, showing thereby the character of nanosized powders. (author)

Preparation of U3O8 powder for MTR type fuel from ammonium uranyl carbonate

International Nuclear Information System (INIS)

Marcondes, G.H.; Riella, H.G.

1990-08-01

In this paper it is described the research done at IPEN-CNEN/SP on the preparation of U 3 O 8 powder from calcination of the AUC, with appropriate characteristics to be used as dispersoid for MTR type fuel. The calcination in air of the AUC leads a U 3 O 8 powder that is further processed to obtain a powder with density and particle size as especifications. The important process parameters are here discussed with the variation AUC calcination temperature and sintering time of the U 3 O 8 powder. (author) [pt

Morphology control and negative thermal expansion in cubic ZrWMoO8 powders

International Nuclear Information System (INIS)

Liu, Qinqin; Yang, Juan; Sun, Xiujuan; Cheng, Xiaonong

2008-01-01

Cubic ZrWMoO 8 powders with rod-like aggregate and thin fasciculus-like and flower-like rod cluster morphologies have been successfully fabricated with different amounts of (NH 4 ) 2 HPO 4 as surfactant using a hydrothermal method. X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy and differential scanning calorimetry were utilized to investigate the influence of the addition of (NH 4 ) 2 HPO 4 on the crystallization process and crystal morphology of the resulting products. The results show that the purity and the thermal expansion property of the resulting products are not influenced by the addition of (NH 4 ) 2 HPO 4 . The cubic ZrWMoO 8 powders with both rod-like aggregate and flower-like rod cluster morphologies show a positive thermal expansion property in the temperature range from room temperature to 120 C, while they show a negative thermal expansion property in the temperature range from 120 C to 700 C. The abnormal thermal expansion property of cubic ZrWMoO 8 below 120 C is caused by the presence of water molecules. Investigations also show that the essence of the different morphologies of the ZrWMoO 8 particles obtained is the result of the different aggregation modes of the nanorods, which act as nuclei, and the corresponding aggregation process is dominated by the addition of (NH 4 ) 2 HPO 4 and its amount. (copyright 2008 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Plasma dynamic synthesis and obtaining ultrafine powders of iron oxides with high content of ε-Fe2O3

Science.gov (United States)

Sivkov, Alexander; Naiden, Evgenii; Ivashutenko, Alexander; Shanenkov, Ivan

2016-05-01

The ultrafine iron oxide powders were successfully synthesized using the plasma dynamic synthesis method, based on the use of a coaxial magnetoplasma accelerator with the iron electrode system. The synthesis was implemented in the high-speed iron-containing plasma jet, flowing into the space of the sealed chamber, filled with the gaseous mixture of oxygen and argon at different ratios. The XRD investigations showed that the synthesized products were heterophase and consisted of three main phases such as magnetite Fe3O4, hematite α-Fe2O3 and ε-Fe2O3. The SEM data confirmed the presence of three particle types: the hollow spheroids with sizes about hundreds of micrometers (magnetite), the particles with sizes up to 100 μm from the porous material of sintered submicron particles (hematite), and nanoscale particles (ε-phase). We found that at the higher oxygen concentration the content of ε-Fe2O3 is increased up to 50% at the same time with decreasing the Fe3O4 phase. The magnetic properties of the products are mainly determined by magnetite characteristics and are significantly reduced with decreasing its content in the powder. In order to investigate the synthesized ε-Fe2O3 on the ability to absorb the electromagnetic radiation in the millimeter wavelength range, we separated the product with the higher ε-phase concentration. The fraction mainly, consisting of ε-Fe2O3, showed the occurrence of the natural resonance at frequencies of 8.3 GHz and 130 GHz.

Synthesis of Sc{sub 2}O{sub 3} powders for preparation of transparent ceramics; Synthese de poudres de Sc{sub 2}O{sub 3} destinees a l'elaboration d'une ceramique transparente

Energy Technology Data Exchange (ETDEWEB)

Bravo, A.C.; Longuet, L.; Autissier, D. [CEA Centre d' Etudes du Ripault, 37 - Tours (France); Baumard, J.F. [Laboratoire Science des Procedes Ceramiques et de Traitements de Surfaces, SPCTS, UMR CNRS 6638, 87 - Limoges (France)

2007-07-01

Different precursors have been prepared by precipitation from scandium nitrates salts using ammonium hydrogeno-carbonate as precipitating agent. The influence of the precipitation technique, of the preparation temperature and of the 'precipitating agent/Sc{sup 3+}' molar ratio on the characteristics (nature, grain size...) of the synthesized precursors has been observed. A heat treatment at 700 C of these precursors has allowed to obtain thin and homogeneous Sc{sub 2}O{sub 3} powders well adapted for transparent ceramics preparation. (O.M.)

Nanoparticles of La0.8Ca0.2Fe0.8Ni0.2O3-δ perovskite for solid oxide fuel cell application

International Nuclear Information System (INIS)

Ortiz-Vitoriano, N.; Ruiz de Larramendi, I.; Gil de Muro, I.; Ruiz de Larramendi, J.I.; Rojo, T.

2010-01-01

Polycrystalline samples of La 0.8 Ca 0.2 Fe 0.8 Ni 0.2 O 3-δ (LCFN) with perovskite type structure have been prepared by combustion, freeze drying, citrate-gel process and liquid mix method. The analysis of X-ray powder diffraction indicated that the samples were single phase and crystallized in an orthorhombic (space group, Pnma no. 62) structure. Transmission electron microscopy (TEM) analysis on the synthesized powder at 600 o C by liquid mix method showed clusters of 150 nm formed by nanoparticles of 20 nm. Electrochemical performance of LCFN cathodes, which are used for intermediate temperature solid oxide fuel cells, were investigated. The polarization resistance was studied using two different electrolytes: Y-doped zirconia (YSZ) and Sm-doped ceria (SDC). The dc four-probe measurement exhibits a total electrical conductivity, over 100 S cm -1 at T ≥ 600 o C, pointing out that strontium can be substituted for the cheaper calcium cation without destroying the electrochemical properties. Experimental results indicate that nanoparticles have more advantages in terms of smaller particle size and better electrochemical performance.

Selective Oxidation Using Flame Aerosol Synthesized Iron and Vanadium-Doped Nano-TiO2

Directory of Open Access Journals (Sweden)

Zhong-Min Wang

2011-01-01

Full Text Available Selective photocatalytic oxidation of 1-phenyl ethanol to acetophenone using titanium dioxide (TiO2 raw and doped with Fe or V, prepared by flame aerosol deposition method, was investigated. The effects of metal doping on crystal phase and morphology of the synthesized nanostructured TiO2 were analyzed using XRD, TEM, Raman spectroscopy, and BET nitrogen adsorbed surface area measurement. The increase in the concentration of V and Fe reduced the crystalline structure and the anatase-to-rutile ratios of the synthesized TiO2. Synthesized TiO2 became fine amorphous powder as the Fe and V concentrations were increased to 3 and 5%, respectively. Doping V and Fe to TiO2 synthesized by the flame aerosol increased photocatalytic activity by 6 folds and 2.5 folds, respectively, compared to that of pure TiO2. It was found that an optimal doping concentration for Fe and V were 0.5% and 3%, respectively. The type and concentration of the metal dopants and the method used to add the dopant to the TiO2 are critical parameters for enhancing the activity of the resulting photocatalyst. The effects of solvents on the photocatalytic reaction were also investigated by using both water and acetonitrile as the reaction medium.

White LED based on CaAl2Si2O8:Eu2+ Mn2+ phosphor and CdS/ZnS quantum dots

Science.gov (United States)

Shen, Changyu; Zhong, Chuan; Hou, Qianglong; Li, Ke

2011-02-01

Core/shell CdS/ZnS quantum dots (QDs) with the emission wavelength of 610nm, was synthesized by thermal deposition using cadmium oxide and selenium as precursors in a hot lauric acid and hexadecylamine trioctylphosphine oxide hybrid. CaAl2Si2O8:Eu2+ Mn2+ phosphor was synthesized by high-temperature solid state reaction at 1290 °C for 2 hours under the H2 reducing atmosphere, and X-ray powder diffraction analysis confirmed the formation of it. It has two emission bands peaking at 420 nm and 580nm originated from the transition 5d to 4f of Eu2+ and 4T1-6A1 of Mn2+, respectively. Blends of CaAl2Si2O8:Eu2+,Mn2+ phosphor and CdS/ZnS QDs exhibited the prominent spectral evolution with an increasing content of QDs. A hybrid white LED, which combines a blue LED with the blend of CaAl2Si2O8:Eu2+ Mn2+ phosphor and QDs with a weight ratio of 2:1, with the CIE coordinate of (0.3183, 0.3036) and CRI of 85 was obtained.

Effect of silver addition on the properties of combustion synthesized nanocrystalline LiCoO2

International Nuclear Information System (INIS)

Ghosh, Paromita; Mahanty, S.; Basu, R.N.

2008-01-01

Nanocrystalline (∼50 nm) LiCoO 2 powders containing 0-10 mol% of Ag have been prepared by combustion synthesis using citrate-nitrate combustion route. Thermal analyses show a sharp decomposition of the gel at ∼177 deg. C for pristine LiCoO 2 . With addition of silver, the decomposition becomes sluggish and it completes only above 430 deg. C. X-ray powder diffraction analyses show an increase in lattice parameter, c, with increasing Ag content suggesting the occupation of Ag within LiCoO 2 interlayer spacings. Transmission electron microscopy indicates diffusion of Ag into LiCoO 2 grains. It has been observed that adding 1.0 mol% silver increases the room temperature electrical conductivity by more than two orders of magnitude (1.5 x 10 -3 S cm -1 ). Galvanostatic charge-discharge profiles of coin cells fabricated with the synthesized powders show a two-fold enhancement in the discharge capacity for 1.0 mol% Ag-added LiCoO 2 cathode (140 mAh g -1 ) compared to that for pristine LiCoO 2 (70 mAh g -1 )

Characterization of γ- Al{sub 2}O{sub 3} nanopowders synthesized by Co-precipitation method

Energy Technology Data Exchange (ETDEWEB)

Jbara, Ahmed S., E-mail: ahmedsbhe@yahoo.com [Center for Sustainable Nanomaterials, Universiti Teknologi Malaysia, Skudai - 81310, Johor Bahru (Malaysia); Physics Department, Science College, Al-Muthanna University, Samawah - 66001 (Iraq); Department of Physics, Faculty of Science, Universiti Teknologi Malaysia, Skudai - 81310, Johor Bahru (Malaysia); Othaman, Zulkafli [Center for Sustainable Nanomaterials, Universiti Teknologi Malaysia, Skudai - 81310, Johor Bahru (Malaysia); Department of Physics, Faculty of Science, Universiti Teknologi Malaysia, Skudai - 81310, Johor Bahru (Malaysia); Ati, Ali A. [Department of Physics, Faculty of Science, Universiti Teknologi Malaysia, Skudai - 81310, Johor Bahru (Malaysia); Saeed, M.A., E-mail: moalsd@gmail.com [Department of Physics, Faculty of Science, Universiti Teknologi Malaysia, Skudai - 81310, Johor Bahru (Malaysia); Division of Science and Technology, University of Education, Township, Lahore - 54770 (Pakistan)

2017-02-15

Co-precipitation technique has been used to synthesize gamma-Al{sub 2}O{sub 3} (γ-Al{sub 2}O{sub 3}) nanopowders under annealing temperature effect. The crystalline phase and purity for the prepared powder were characterized by different spectroscopy techniques. XRD analysis confirms the gamma phase of alumina nanopowders with particle diameter ranging from 6 to 24 nm, which confirms the quantum dots formation, which is also supported by the BET measurement. The surface area of the prepared nanopowders is in the range of 109–367 m{sup 2}/g. Morphology analysis indicates that γ-Al{sub 2}O{sub 3} nanopowders are consisted of grains almost spherical in shape. Some agglomeration of nanoparticles occurs, which become more regular hexagonal shaped with the increasing annealing temperature. The small nanoparticles size and the high surface area from a simple procedure for preparing γ-Al{sub 2}O{sub 3} may make it more suitable for use as an adsorbent for malachite green. - Highlights: • Co-precipitation technique is used to synthesize gamma- Al{sub 2}O{sub 3} nanopowders. • Pure gamma- Al{sub 2}O{sub 3} phase was obtained having maximum nanoparticle size is 24 nm. • The quantum dots were formed inside powder. • High surface area of nanopowders at the low annealing temperature. • Increasing annealing temperature causes the hexagonal agglomeration shape.

Preparation of TiO2 Nanocrystallite Powders Coated with 9 mol% ZnO for Cosmetic Applications in Sunscreens

Directory of Open Access Journals (Sweden)

Moo-Chin Wang

2012-02-01

Full Text Available The preparation of TiO2 nanocrystallite powders coated with and without 9 mol% ZnO has been studied for cosmetic applications in sunscreens by a co-precipitation process using TiCl4 and Zn(NO32·6H2O as starting materials. XRD results show that the phases of anatase TiO2 and rutile TiO2 coexist for precursor powders without added ZnO (T-0Z and calcined at 523 to 973 K for 2 h. When the T-0Z precursor powders are calcined at 1273 K for 2 h, only the rutile TiO2 appears. In addition, when the TiO2 precursor powders contain 9 mol% ZnO (T-9Z are calcined at 873 to 973 K for 2 h, the crystallized samples are composed of the major phase of rutile TiO2 and the minor phases of anatase TiO2 and Zn2Ti3O8. The analyses of UV/VIS/NIR spectra reveal that the absorption of the T-9Z precursor powders after being calcined has a red-shift effect in the UV range with increasing calcination temperature. Therefore, the TiO2 nanocrystallite powders coated with 9 mol% ZnO can be used as the attenuate agent in the UV-A region for cosmetic applications in sunscreens.

Magnetic, hyperthermic and structural properties of zn substituted CaFe2O4 powders

Science.gov (United States)

Kheradmand, Abbas; Vahidi, Omid; Masoudpanah, S. M.

2018-03-01

In the present study, we have synthesized single phase Ca1 - x Zn x Fe2O4 powders by hydrothermal method. The cation distribution between the tetrahedral and octahedral sites in the spinel structure and the magnetic properties as a function of the zinc substitution have been investigated by X-ray diffraction (XRD), infrared spectroscopy and vibrating sample magnetometer methods. The obtained XRD pattern indicated that the synthesized particles had single phase cubic spinel structure with no impurity. The magnetic measurements showed that the saturation magnetization increased from 83 to 98 emu/g with the addition of zinc due to the decrease of inversity. The particle size observed by electron microscopy decreased from 1.38 to 0.97 µm with the increase of zinc addition. The Ca0.7Zn0.3Fe2O4 powders exhibited appropriate heating capability for hyperthermia applications with the maximum AC heating temperature of 20 °C and specific loss power of 9.29 W/g.

Electrochemical reduction behavior of U3O8 powder in a LiCl molten salt

International Nuclear Information System (INIS)

Jeong, Sang Mun; Shin, Ho-Sup; Hong, Sun-Seok; Hur, Jin-Mok; Do, Jae Bum; Lee, Han Soo

2010-01-01

The reduction path of the U 3 O 8 powder vol-oxidized at 1200 deg. C has been determined by a series of electrochemical experiments in a 1 wt.% Li 2 O/LiCl molten salt. Various reaction intermediates are observed by during electrolysis of U 3 O 8 . The formation of the metallic uranium is caused from two different reduction paths, a direct reduction of uranium oxide and an electro-lithiothermic reduction. As the uranium oxide is converted to the metallic uranium, the lithium metal is more actively formed in the cathode basket. The reducibility of the rare earth oxides with the U 3 O 8 powder has been tested by constant voltage electrolysis. The results suggest the advanced vol-oxidation could lead to the enhancement in the reducibility of the rare earth fission products.

New quaternary oxides with both families of second-order Jahn–Teller (SOJT) distortive cations: Solid-state synthesis, structure determination, and characterization of YNbTe{sub 2}O{sub 8} and YNbSe{sub 2}O{sub 8}

Energy Technology Data Exchange (ETDEWEB)

Kim, Yeong Hun [Department of Chemistry, Chung-Ang University, 84 Heukseok-ro, Dongjak-gu, Seoul 156-756 (Korea, Republic of); Jeon, Beom-Yong; You, Tae-Soo [Department of Chemistry, Chungbuk National University, Cheongju, Chungbuk 361-763 (Korea, Republic of); Ok, Kang Min, E-mail: kmok@cau.ac.kr [Department of Chemistry, Chung-Ang University, 84 Heukseok-ro, Dongjak-gu, Seoul 156-756 (Korea, Republic of)

2015-07-15

Graphical abstract: Ball-and-stick representation of YNbTe{sub 2}O{sub 8} composed of polyhedra of SOJT distortive cations, i.e., NbO{sub 6} and TeO{sub 3}, in the ac-plane. - Highlights: • Two novel tellurite and selenite (YNbQ{sub 2}O{sub 8}; Q = Te and Se) are synthesized. • YNbQ{sub 2}O{sub 8} possess both families of second-order Jahn–Teller distortive cations. • The distortive environments and bonding nature are supported by electronic structure calculations. - Abstract: Two novel quaternary mixed metal tellurite and selenite, YNbTe{sub 2}O{sub 8} and YNbSe{sub 2}O{sub 8}, respectively, have been synthesized through standard solid-state reactions using Y{sub 2}O{sub 3}, Nb{sub 2}O{sub 5}, TeO{sub 2} or SeO{sub 2} as reagents. Single crystal X-ray and powder neutron diffraction analyses have been utilized to determine the structures of the reported materials. YNbTe{sub 2}O{sub 8} and YNbSe{sub 2}O{sub 8} are isostructural to each other and crystallize in the monoclinic centrosymmetric space group, C2/m (No. 12). Due to the two families of constituent second-order Jahn–Teller (SOJT) distortive cations, i.e., Nb{sup 5+} and Te{sup 4+}/Se{sup 4+}, local asymmetric environments occur from the three-dimensional frameworks. Intra-octahedral distortions along the local C{sub 4} direction and asymmetric trigonal pyramidal coordination moieties generated by stereoactive lone pairs are observed from the NbO{sub 6} octahedra and TeO{sub 3} (or SeO{sub 3}) polyhedra, respectively. Thermogravimetric analysis, infrared and UV–vis diffuse reflectance spectroscopies, elemental analysis, out-of-center distortions, dipole moment calculations, and electronic structure calculations for the reported materials are presented.

Some peculiarities of zirconium tungstate synthesis by thermal decomposition of hydrothermal precursors

International Nuclear Information System (INIS)

Gubanov, Alexander I.; Dedova, Elena S.; Plyusnin, Pavel E.; Filatov, Eugeny Y.; Kardash, Tatyana Y.; Korenev, Sergey V.; Kulkov, Sergey N.

2014-01-01

Highlights: • Synthesis of ZrW 2 O 8 using hydrothermal method. • On hydrothermal synthesis optimal conc. of HCl in the reaction mixture is 2.3 M. • Thermal decomposition of ZrW 2 O 7 ((OH) 1.5 ,Cl 0.5 )·2H 2 O begins are 200 °S. • Amorphous intermediate crystallizes into cubic single-phase ZrW 2 O 8 above 550 °S. • ZrW 2 O 8 destructed at temperatures above 700 °S. - Abstract: This article discusses some peculiarities of the synthesis of ZrW 2 O 8 (1) using thermal decomposition of the precursor ZrW 2 O 7 ((OH) 1.5 ,Cl 0.5 )·2H 2 O (2) prepared by hydrothermal method. On hydrothermal synthesis of 2 the optimal concentration of hydrochloric acid in the reaction mixture is about 2.3 M. TG approach to determine the chemical composition of the precursor was suggested. It has been found that the precursor for the synthesis of zirconium tungstate has chemical formula 2. Thermal decomposition of the precursor 2 begins at 200 °S and affords an amorphous intermediate, which crystallizes as a cubic phase 1 above 550 °S with an exoeffect. The temperature of the beginning of the transition from amorphous to the crystalline state is 350 ± 25 °S

Black TiO2 synthesized via magnesiothermic reduction for enhanced photocatalytic activity

Science.gov (United States)

Wang, Xiangdong; Fu, Rong; Yin, Qianqian; Wu, Han; Guo, Xiaoling; Xu, Ruohan; Zhong, Qianyun

2018-04-01

Utilizing solar energy for hydrogen evolution is a great challenge for its insufficient visible-light power conversion. In this paper, we report a facile magnesiothermic reduction of commercial TiO2 nanoparticles under Ar atmosphere and at 550 °C followed by acid treatment to synthesize reduced black TiO2 powders, which possesses a unique crystalline core-amorphous shell structure composed of disordered surface and oxygen vacancies and shows significantly improved optical absorption in the visible region. The unique core-shell structure and high absorption enable the reduced black TiO2 powders to exhibit enhanced photocatalytic activity, including splitting of water in the presence of Pt as a cocatalyst and degradation of methyl blue (MB) under visible light irradiation. Photocatalytic evaluations indicate that the oxygen vacancies play key roles in the catalytic process. The maximum hydrogen production rates are 16.1 and 163 μmol h-1 g-1 under the full solar wavelength range of light and visible light, respectively. This facile and versatile method could be potentially used for large scale production of colored TiO2 with remarkable enhancement in the visible light absorption and solar-driven hydrogen production.

Thermoluminescence in HfO_2:Eu"3"+ powders irradiated in UV

International Nuclear Information System (INIS)

Ceron R, P. V.; Montes R, E.; Rivera M, T.; Diaz G, J. A. I.; Guzman M, J.

2016-10-01

Various inorganic compounds synthesized for photo luminescent applications have also presented a thermoluminescent (Tl) response, for example the metal oxides doped with rare earths. This property extends the use of these materials to the radiation dosimetry. For this reason, in this work the Tl response is presented in HfO_2:Eu"3"+ powders synthesized by the hydrothermal path, exposed to ultraviolet (UV) radiation of 254 nm. The kinetic parameters of its brightness curve were also calculated using the Chen expressions and the analysis method based on the shape of the curve. For the powders irradiated for 10 min the highest Tl response corresponds to the sample with 5% of the impurity, which is 6.5 times higher than the signal corresponding to the intrinsic sample. Its bright curve shows a main peak with a maximum in 148 degrees Celsius and a second order kinetics. Another test with the same material shows the Tl response against the exposure time, with a maximum in the 3 minutes. These calculations and tests constitute a first approach for the study of these powders as Tl dosimeter for UV radiation. (Author)

Photocatalytic and Escherichia antibacterial activities of Ag-TiO2-SiO2 nanocomposite powder under simulated solar light irradiation

Science.gov (United States)

Van Dang, Han; Le, Vien Minh; Hoang, Hoang Anh

2017-09-01

The photocatalytic nanocomposite powder TiO2, TiO2-SiO2 and Ag-TiO2-SiO2 (ATS) were synthesized by sol-gel method assisted with hydrothermal treatment and characterized by X-ray diffraction (XRD), Raman spectroscopy (RAMAN), Fourier transformed infrared spectroscopy (FT-IR), Energy dispersive X-ray (EDX), Transmission electron microscope (TEM), Brunauer-Emmett-Teller (BET) surface area and UV-Vis absorption spectra analysis. The Escherichia coli (E. coli) antibacterial activity of synthesized photo-catalysts under simulated solar light have been also investigated. The heterogeneous A4TS10 with the 4 wt.% Ag and 10 wt.% SiO2 had anatase and rutile phase, spherical in shape with the particle size about 20 - 30 nm, specific surface area (SSA) of 218.4 m2/g, the band gap of 3.06 eV. The E. coli antibacterial activities of the synthesized samples under simulated solar light were also investigated under simulated solar light with 25 W of light intensity. The E. coli antibacterial ability of A4TS10 performed the highest photo-activity. E. coli bacteria was entirely killed after 30-minute irradiation and no bacterial regrowth was observed after 24 hours. The research results demonstrated that the photocatalytic A4TS10 is a promising green material to treatment wastewater infected bacteria application.

Structural study of Sr{sub 2}CuO{sub 3+delta} by neutron powder diffraction

Energy Technology Data Exchange (ETDEWEB)

Shimakawa, Y. [NEC Corp., Tsukuba (Japan). Fundamental Research Labs.; Jorgensen, J.D.; Mitchell, J.F.; Hunter, B.A. [Argonne National Lab., IL (United States); Shaked, S. [Israel Atomic Energy Commission, Beersheba (Israel). Nuclear Research Center-Negev][Ben-Gurion Univ. of the Negev, Beersheba (Israel). Dept. of Physics; Hinks, D.G.; Hitterman, R.L. [Argonne National Lab., IL (United States); Hiroi, Z.; Takano, M. [Kyoto Univ., Uji (Japan). Inst. for Chemical Research

1996-11-01

Average crystal structures of superconducting Sr{sub 2}CuO{sub 3+{delta}} synthesized at ambient pressure from a hydroxometallate precursor were refined from neutron powder diffraction data. A simplified model was used to fit the modulated superstructures. Both compounds have an oxygen deficient La{sub 2}CuO{sub 4}-type tetragonal T structure with O vacancies located in the CuO{sub 2} planes, not in the Sr{sub 2}O{sub 2} layers. This raises important questions about the superconductivity in Sr{sub 2}CuO{sub 3+{delta}} reported to be a 70 K superconductor.

Synchrotron WAXS and XANES studies of silica (SiO2) powders synthesized from Indonesian natural sands

International Nuclear Information System (INIS)

Muchlis, Khairanissa; Fauziyah, Nur Aini; Pratapa, Suminar; Soontaranon, Siriwat; Limpirat, Wanwisa

2017-01-01

In this study, we have investigated polymorphic silica (SiO 2 ) powders using, Wide Angle X-ray Scattering (WAXS) and X-Ray Absorption Near Edge Spectroscopy (XANES), laboratory X-Ray Diffraction (XRD) instruments. The WAXS and XANES spectra were collected using synchrotron radiation at Synchrotron Light Research Institute (SLRI), Nakhon Ratchasima, Thailand. The silica powders were obtained by processing silica sand from Tanah Laut, South Kalimantan, Indonesia. Purification process of silica sand was done by magnetic separation and immersion with HCl. The purification step was needed to reduce impurity or undesirable non Si elements. Three polymorphs of silica were produced, i.e. amorphous phase (A), quartz (B), and cristobalite (C). WAXS profile for each phase was presented in terms of intensity vs. 2θ prior to analyses. Both XRD (λ CuKα =1.54056 Å) and WAXS (λ=1.09 Å) patttern show that (1) A sample contains no crystallites, (2) B sample is monophasic, contains only quartz, and (3) C sample contains cristobalite and trydimite. XRD quantitative analysis using Rietica gave 98,8 wt% cristobalite, while the associated WAXS data provided 98.7 wt% cristobalite. Si K-edge XANES spectra were measured at energy range 1840 to 1920 eV. Qualitatively, the pre-edge and edge features for all phases are similar, but their main peaks in the post-edge region are different. (paper)

CO Sensing Properties of Nanostructured La0.8Sr0.2CoO3 Sensors Synthesized by EDTA-Glycol Method

Directory of Open Access Journals (Sweden)

G. N. Chaudhari

2008-11-01

Full Text Available We report a simple method for the preparation of pure LaCoO3 and La1-xSrxCoO3 (x = 0.1, 0.2 and 0.25 nanostructures by the EDTA-Glycol method. The final powders obtained by this method have been investigated by X-ray diffraction (XRD and scanning electron microscopy (SEM measurements. The gas sensitivity of pure and Sr doped LaCoO3 samples were investigated for CO, NH3, H2 and LPG. La0.8Sr0.2CoO3 powders (sample GIII calcined at 6500C, exhibited a good sensor response towards CO gas at 2500C. On impregnation of 1 wt.% Pd over sample GIII, the operation temperature reduced to 2000C with a significant rise in sensitivity. The response time also decreases from about 3.5 min for sample GIII to less than 2.5 min for the Pd loaded element. The electronic interaction between Pd and metal oxide semiconductor is proposed to account for the sensitization effect.

Preparation and melting of uranium from U3O8

International Nuclear Information System (INIS)

Hur, Jin-Mok; Choi, In-Kyu; Cho, Soo-Haeng; Jeong, Sang-Mun; Seo, Chung-Seok

2008-01-01

In this paper, we report on the preparation and melting of uranium in association with a spent nuclear fuel conditioning process. U 3 O 8 powder was electrochemically reduced in a mixture of molten LiCl-Li 2 O (∼3 wt.% of Li 2 O in LiCl) at 650 deg. C resulting in the formation of uranium and Li 2 O with a yield of >99%. When the powder of uranium with a residual LiCl-Li 2 O salt was heated in order to melt the metal, the uranium oxidation to UO 2 due to the reaction with Li 2 O was observed. We were able to synthesize FeU 6 by using a Fe based cathode during the U 3 O 8 reduction procedure. FeU 6 could be melted to below the temperatures where the oxidation of uranium by Li 2 O occurred. The idea of compound formation and melting is applicable to the melting and casting of a spent nuclear fuel which contains oxidative residual salts due to its conditioning in a molten salt

Microstructural, structural and optical properties of nanoparticles of PbO-CrO3 pigment synthesized by a soft route

Directory of Open Access Journals (Sweden)

V. D. Araújo

2015-03-01

Full Text Available PbCrO4 and Pb2CrO5 particles were synthesized by the polymeric precursor method. Structural and microstructural properties of the particles were characterized by scanning electron microscopy with field emission gun, X-ray diffraction, and Raman spectroscopy techniques. The diffuse reflectance technique was employed to study the optical properties in the 400-700 nm range. The optical bandgap of the samples was obtained indirectly. Colorimetric coordinates L*, a*, b* were calculated for the pigment powders as a function of the heat treatment (400-700 ºC. The powders displayed colors ranging from green to red. X-ray diffraction patterns showed the presence of monoclinic PbCrO4 phase in green samples, while red powders had a monoclinic Pb2CrO5 phase structure. The Raman spectra of the PbCrO4 and Pb2CrO5 powders were in good agreement with those reported in the literature. The synthesized compounds can be used as green and red pigments with high thermal stability.

Influence of Ultrafine 2CaO·SiO2 Powder on Hydration Properties of Reactive Powder Concrete

Directory of Open Access Journals (Sweden)

Hongfang Sun

2015-09-01

Full Text Available In this research, we assessed the influence of an ultrafine 2CaO·SiO2 powder on the hydration properties of a reactive powder concrete system. The ultrafine powder was manufactured through chemical combustion method. The morphology of ultrafine powder and the development of hydration products in the cement paste prepared with ultrafine powder were investigated by scanning electron microscopy (SEM, mineralogical composition were determined by X-ray diffraction, while the heat release characteristics up to the age of 3 days were investigated by calorimetry. Moreover, the properties of cementitious system in fresh and hardened state (setting time, drying shrinkage, and compressive strength with 5% ordinary Portland cement replaced by ultrafine powder were evaluated. From SEM micrographs, the particle size of ultrafine powder was found to be up to several hundred nanometers. The hydration product started formulating at the age of 3 days due to slow reacting nature of belitic 2CaO·SiO2. The initial and final setting times were prolonged and no significant difference in drying shrinkage was observed when 5% ordinary Portland cement was replaced by ultrafine powder. Moreover, in comparison to control reactive powder concrete, the reactive powder concrete containing ultrafine powder showed improvement in compressive strength at and above 7 days of testing. Based on above, it can be concluded that the manufactured ultrafine 2CaO·SiO2 powder has the potential to improve the performance of a reactive powder cementitious system.

Study of fluorine doped (Nb,Ir)O_2 solid solution electro-catalyst powders for proton exchange membrane based oxygen evolution reaction

International Nuclear Information System (INIS)

Kadakia, Karan Sandeep; Jampani, Prashanth H.; Velikokhatnyi, Oleg I.; Datta, Moni Kanchan; Patel, Prasad; Chung, Sung Jae; Park, Sung Kyoo; Poston, James A.; Manivannan, Ayyakkannu; Kumta, Prashant N.

2016-01-01

Graphical abstract: High surface area (∼300 m"2/g) nanostructured powders of nominal composition (Nb_1_−_xIr_x)O_2 and (Nb_1_−_xIr_x)O_2:10F have been synthesized and tested as oxygen evolution electro-catalysts for PEM based water electrolysis using a simple two-step chemical synthesis procedure. Superior electrochemical activity was demonstrated by fluorine doped compositions of (Nb_1_−_xIr_x)O_2 with an optimal composition (Nb_0_._7_5Ir_0_._2_5)O_2:10F (x = 0.25) demonstrating on-par performance with commercial hydrated IrO_2 and nanostructured in-house chemically synthesized IrO_2. Using first principles calculations, the electronic structure modification resulting in ∼75 at.% reduction (experimentally observed) in noble metal content without loss in catalytic performance and stability has been established. - Highlights: • (Nb_1_−_xIr_x)O_2:10F nanopowder electrocatalysts have been wet chemically synthesized. • (Nb_0_._7_5Ir_0_._2_5)O_2:10F exhibits superior electrochemical activity than pure IrO_2. • Stability of the (Nb,Ir)O_2:10F nanomaterials is comparable to pure (Nb,Ir)O_2. • High surface area F doped (Nb,Ir)O_2 are promising OER anode electro-catalysts. - Abstract: High surface area (∼300 m"2/g) nanostructured powders of (Nb_1_−_xIr_x)O_2 and (Nb_1_−_xIr_x)O_2:10F (∼100 m"2/g) have been examined as promising oxygen evolution reaction (OER) electro-catalysts for proton exchange membrane (PEM) based water electrolysis. Nb_2O_5 and 10 wt.% F doped Nb_2O_5 powders were prepared by a low temperature sol-gel process which were then converted to solid solution (Nb,Ir)O_2 and 10 wt.% F doped (Nb,Ir)O_2 [(NbIr)O_2:10F] electro-catalysts by soaking in IrCl_4 followed by heat treatment in air. Electro-catalyst powders of optimal composition (Nb_0_._7_5Ir_0_._2_5)O_2:10F with ∼75 at.% reduction in noble metal content exhibited comparable OER activity to commercial hydrated IrO_2 and nanostructured in-house chemically synthesized IrO_2

Morphologic and structural characterization of the CoFe2O4 synthesized by combustion reaction

International Nuclear Information System (INIS)

Lima, M.S.; Sousa, J.-P.L.M.L.; Vieira, D.A.; Lira, H.L.; Costa, A.C.F.M.; Sasaki, J.M.

2009-01-01

CoFe 2 O 4 powders were synthesized by combustion reaction using glycine as fuel, aiming obtaining nanosized and monophase powders. Thus, different conditions of external heating during the synthesis were investigated. The powders were prepared according to the propellants and explosives theory, using glycine as fuel in the stoichiometric proportion (Φe = 1). During the synthesis the flame temperature and time were measured. The resulting powders were characterized by X-rays diffraction and scanning electronic microscopy (SEM). The results show that the condition in which the synthesis was realized it influences in the combustion flame temperature and time and contributes for the obtainment of powders with majority phase without secondary phases. Crystallite size varied of 33 to 50 nm. All powders presented morphology constituted by soft agglomerated formed by nanoparticles. (author). (author)

Morphology, structure and optical properties of hydrothermally synthesized CeO2/CdS nanocomposites

Science.gov (United States)

Mohanty, Biswajyoti; Nayak, J.

2018-04-01

CeO2/CdS nanocomposites were synthesized using a two-step hydrothermal technique. The effects of precursor concentration on the optical and structural properties of the CeO2/CdS nanoparticles were systematically studied. The morphology, composition and the structure of the CeO2/CdS nanocomposite powder were studied by scanning electron microscopy (SEM), energy dispersive X-ray spectrum analysis (EDXA) and X-ray diffraction (XRD), respectively. The optical properties of CeO2/CdS nanocomposites were studied by UV-vis absorption and photoluminescence (PL) spectroscopy. The optical band gaps of the CeO2/CdS nanopowders ranged from 2.34 eV to 2.39 eV as estimated from the UV-vis absorption. In the room temperature photoluminescence spectrum of CeO2/CdS nanopowder, a strong blue emission band was observed at 400 nm. Since the powder shows strong visible luminescence, it may be used as a blue phosphor in future. The original article published with this DOI was submitted in error. The correct article was inadvertently left out of the original submission. This has been rectified and the correct article was published online on 16 April 2018.

THERMAL EXPANSION BEHAVIOR OF THE Ba0.2Sr0.8Co0.8Fe0.2O3−δ (BSCF WITH Sm0.2Ce0.8O1.9

Directory of Open Access Journals (Sweden)

M. AHMADREZAEI

2014-03-01

Full Text Available Nanostructured perovskite oxides of Ba0.2Sr0.8Co0.8Fe0.2O3−δ (BSCF were synthesized through the co-precipitation method. The thermal decomposition, phase formation and thermal expansion behavior of BSCF were characterized by thermogravimetric analysis, X-ray diffraction (XRD, and dilatometry, respectively. XRD peaks were indexed to a cubic perovskite structure with a Pm3m (221 space group. All the combined oxides produced the desired perovskite-phase BSCF. The microstructures were characterized by scanning electron microscopy (SEM and transmission electron microscopy (TEM. The TEM analysis showed that BSCF powders had uniform nanoparticle sizes and high homogeneity. The cross-sectional SEM micrograph of BSCF exhibited a continuous and no delaminated layer from the electrolyte-supported cell. The thermal expansion coefficient (TEC of BSCF was 16.2×10-6 K-1 at a temperature range of 600°C to 800°C. Additional experiments showed that the TEC of BSCF is comparable to that of Sm0.2Ce0.8O1.9 (SDC within the same temperature range. The results demonstrate that BSFC is a promising cathode material for intermediate-temperature solid-oxide fuel cells.

Adsorption of methyl orange by synthesized and functionalized-CNTs with 3-aminopropyltriethoxysilane loaded TiO2 nanocomposites.

Science.gov (United States)

Ahmad, Amirah; Razali, Mohd Hasmizam; Mamat, Mazidah; Mehamod, Faizatul Shimal Binti; Anuar Mat Amin, Khairul

2017-02-01

This study aims to develop a highly efficient adsorbent material. CNTs are prepared using a chemical vapor deposition method with acetylene and synthesized mesoporous Ni-MCM41 as the carbon source and catalyst, respectively, and are then functionalized using 3-aminopropyltriethoxysilane (APTES) through the co-condensation method and loaded with commercial TiO 2 . Results of X-ray powder diffraction (XRD), Raman spectra, and Fourier transform infrared spectroscopy (FTIR) confirm that the synthesized CNTs grown are multi-walled carbon nanotubes (MWNTs). Transmission electron microscopy shows good dispersion of TiO 2 nanoparticles onto functionalized-CNTs loaded TiO 2 , with the diameter of a hair-like structure measuring between 3 and 8 nm. The functionalized-CNTs loaded TiO 2 are tested as an adsorbent for removal of methyl orange (MO) in aqueous solution, and results show that 94% of MO is removed after 10 min of reaction, and 100% after 30 min. The adsorption kinetic model of functionalized-CNTs loaded TiO 2 follows a pseudo-second order with a maximum adsorption capacity of 42.85 mg/g. This study shows that functionalized-CNTs loaded TiO 2 has considerable potential as an adsorbent material due to the short adsorption time required to achieve equilibrium. Copyright © 2016 Elsevier Ltd. All rights reserved.

Tailoring of K0.8Al0.7Fe0.15Si2.25O6 Leucite Based Dental Ceramic Material

Directory of Open Access Journals (Sweden)

Aleksandar Kremenović

2016-06-01

Full Text Available Potassium based ceramic materials composed from leucite in which 5 % of Al is exchanged with Fe and 4 % of hematite was synthesized by mechanochemical homogenization and annealing of K2O-SiO2-Al2O3-Fe2O3 mixtures. Synthesized material was characterized by X-ray Powder Diffraction (XRPD and Scanning Electron Microscopy coupled with Energy Dispersive X-ray spectroscopy (SEM/EDX. The two methods are in good agreement in regard to the specimen chemical composition suggesting that a leucite chemical formula is K0.8Al0.7Fe0.15Si2.25O6. Rietveld structure refinement results reveal that about 20 % of vacancies exist in the position of K atoms. This work is licensed under a Creative Commons Attribution 4.0 International License.

Improved electrochemical performance of Li1.2Mn0.54Ni0.13Co0.13O2 cathode material synthesized by citric acid assisted sol-gel method for lithium ion batteries

Science.gov (United States)

Li, Shiyou; Liang, Youwei; Lei, Dan; Xie, Yingchun; Ai, Ling; Xie, Jing

2018-03-01

A citric acid assisted sol-gel method is employed for synthesizing Li1.2Mn0.54Ni0.13Co0.13O2 used as a cathode material in lithium-ion batteries. Powder X-ray diffraction (XRD) and scanning electron microscopy (SEM) characterizations prove that materials have a typical a-NaFeO2 structure with primary nano-sized particles. Electrochemical performances have been investigated by charge-discharge test and results show that the synthesized product exhibits excellent electrochemical performance with a high initial discharge capacity of 253.5 mAh g-1 at 0.1 C and a preferable capacity retention of 84.8% after 50 cycles.

Electrical and optical properties of thermally-evaporated thin films from A2[TiO(C2O4)2] (A = K, PPh4) and 1,8-dihydroxyanthraquinone

International Nuclear Information System (INIS)

Carbia-Ruelas, E.; Sanchez-Vergara, M.E.; Garcia-Montalvo, V.; Morales-Saavedra, O.G.; Alvarez-Bada, J.R.

2011-01-01

In this work, the synthesis of molecular materials formed from A 2 [TiO(C 2 O 4 ) 2 ] (A = K, PPh4) and 1,8 dihydroxyanthraquinone is reported. The synthesized materials were characterized by atomic force microscopy (AFM), infrared (IR) and ultraviolet-visible (UV-vis) spectroscopy. IR spectroscopy showed that the molecular-material thin-films, deposited by vacuum thermal evaporation, exhibit the same intra-molecular vibration modes as the starting powders, which suggests that the thermal evaporation process does not alter the initial chemical structures. Electrical transport properties were studied by dc conductivity measurements. The electrical activation energies of the complexes, which were in the range of 0.003-1.16 eV, were calculated from Arrhenius plots. Optical absorption studies in the wavelength range of 190-1090 nm at room temperature showed that the optical band gaps of the thin films were around 1.9-2.3 eV for direct transitions Eg d . The cubic NLO effects were substantially enhanced for materials synthesized from K 2 [TiO(C 2 O 4 ) 2 ], where χ (3) (-3ω; ω, ω, ω) values in the promising range of 10 -12 esu have been evaluated.

Long lasting behavior of Gd2O2S:Eu3+ phosphor synthesized by hydrothermal routine

International Nuclear Information System (INIS)

Hang Tao; Liu Qun; Mao Dali; Chang Chengkang

2008-01-01

This paper reports the detailed preparation process and afterglow properties of Eu 3+ activated long lasting Gd 2 O 2 S phosphor by hydrothermal routine. Rod-like Gd(OH) 3 were firstly synthesized by hydrothermal method to serve as the precursor. Long lasting Gd 2 O 2 S:Eu 3+ ,Ti 4+ ,Mg 2+ phosphor was obtained by calcinating the precursor with co-activators and S powder. It was found from the results that the hydrothermally prepared Gd(OH) 3 revealed a rod-like morphology, while the calcinated Gd 2 O 2 S:Eu 3+ ,Ti 4+ ,Mg 2+ phosphor showed a round granular shape. The morphological change can be explained by the etching effect of the melt that was formed by the carbonate and S powder during the high temperature calcination. The obtained Gd 2 O 2 S:Eu 3+ ,Ti 4+ ,Mg 2+ phosphor produced a red emission upon 243 nm UV excitation, which is a typical emission of Eu 3+ from 5 D j to 7 F j states. Long lasting behavior was observed after the UV source was switched off, due to the formation of electron traps with suitable trap depth within the matrix by the codoped Ti 4+ and Mg 2+ ions

Solid-state reactions to synthesize nanostructured lead selenide semiconductor powders by high-energy milling

Energy Technology Data Exchange (ETDEWEB)

Rojas-Chavez, H., E-mail: uu_gg_oo@yahoo.com.mx [Centro de Investigacion e Innovacion Tecnologica - IPN, Cerrada de CECATI s/n, Col. Santa Catarina, Del. Azcapotzalco (Mexico) and Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada - IPN, Legaria 694, Col. Irrigacion, Del. Miguel Hidalgo (Mexico); Reyes-Carmona, F. [Facultad de Quimica - UNAM, Circuito de la Investigacion Cientifica s/n, C.U. Del. Coyoacan (Mexico); Jaramillo-Vigueras, D. [Centro de Investigacion e Innovacion Tecnologica - IPN, Cerrada de CECATI s/n, Col. Santa Catarina, Del. Azcapotzalco (Mexico)

2011-10-15

Highlights: {yields} PbSe synthesized from PbO instead of Pb powder do not require an inert atmosphere. {yields} During high-energy milling oxygen has to be chemically reduced from the lead oxide. {yields} Solid-state and solid-gas chemical reactions promote both solid and gaseous products. -- Abstract: Both solid-solid and gas-solid reactions have been traced during high-energy milling of Se and PbO powders under vial (P, T) conditions in order to synthesize the PbSe phase. Chemical and thermodynamic arguments are postulated to discern the high-energy milling mechanism to transform PbO-Se micropowders onto PbSe-nanocrystals. A set of reactions were evaluated at around room temperature. Therefore an experimental campaign was designed to test the nature of reactions in the PbO-Se system during high-energy milling.

Solid-state reactions to synthesize nanostructured lead selenide semiconductor powders by high-energy milling

International Nuclear Information System (INIS)

Rojas-Chavez, H.; Reyes-Carmona, F.; Jaramillo-Vigueras, D.

2011-01-01

Highlights: → PbSe synthesized from PbO instead of Pb powder do not require an inert atmosphere. → During high-energy milling oxygen has to be chemically reduced from the lead oxide. → Solid-state and solid-gas chemical reactions promote both solid and gaseous products. -- Abstract: Both solid-solid and gas-solid reactions have been traced during high-energy milling of Se and PbO powders under vial (P, T) conditions in order to synthesize the PbSe phase. Chemical and thermodynamic arguments are postulated to discern the high-energy milling mechanism to transform PbO-Se micropowders onto PbSe-nanocrystals. A set of reactions were evaluated at around room temperature. Therefore an experimental campaign was designed to test the nature of reactions in the PbO-Se system during high-energy milling.

Ce O2-Zr O2 powder synthesis by alcohol dehydration of aqueous salt solutions

International Nuclear Information System (INIS)

Andrade Nono, M.C. de

1993-01-01

A method for the precipitation of Ce O 2 -Zr O 2 powder is reported. It involves the powder synthesis by precipitation from an aqueous of Y and Zr sulphates in ethanol and isopropanol followed by calcination. The powder characteristics and their relations with the green compaction and densification by sintering are shown and discussed. It is observed that the ethanol gives powders with the best compaction and sintering behavior. (author)

Effect of Co2+ and Y3+ ions insertion on the microstructure development and magnetic properties of Ni0.5Zn0.5Fe2O4 powders synthesized using Co-precipitation method

Science.gov (United States)

Rashad, M. M.; Rayan, D. A.; Turky, A. O.; Hessien, M. M.

2015-01-01

Nanocrystalline Ni0.5Zn0.5-xCoxFe2-zYzO4 powders (x=0-0.3 and z from 0 to 0.3) have been synthesized via a facile co-precipitation technique. X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM) are utilized in order to study the effect of variation of cobalt and yttrium substitutions and its impact on crystalline size, lattice parameter, X-ray density, microstructure and magnetic properties of the formed powders. X-ray diffraction data indicated that, after doping, all samples consisted of the main spinel phase for the formed precursors precipitated at pH 10 annealed at 1000 oC for 2 h. The lattice parameter and the unit cell were decreased linearly with increasing Co content whereas they were increased with increasing the Y incorporation. Additionally, the porosity was increased with increasing Co concentration while it was decreased with increasing the Y insertion. The mean ionic radii and hopping and bond lengths was decreased with the value of Co2+ and they were increased with the value of Y3+ ion as well as both of Y3+ and Co2+ ions. The microstructures of the produced powders were found to be cubic like structure. The addition of Y3+ ion suppressed the grain size whereas addition of Co2+ ion enhanced the grain growth availably. An examination of the magnetic properties revealed an increase in saturation magnetization with increasing Co and Y concentrations incorporation up to x=0.3. Meanwhile, the formed powders exhibited superparamagnetic characteristics. A high saturation magnetization (77.0 emu/g) was achieved for Ni0.5Zn0.2Co0.3Fe2O4 sample annealed at 1000 oC for 2 h.

A study of stability of MgH{sub 2} in Mg-8at%Al alloy powder

Energy Technology Data Exchange (ETDEWEB)

Tanniru, Mahesh; Ebrahimi, Fereshteh [Materials Science and Engineering Department, University of Florida, Gainesville, FL 32611 (United States); Slattery, Darlene K. [Florida Solar Energy Center (FSEC), Cocoa, FL (United States)

2010-04-15

To investigate the effect of Al addition on the stability of magnesium hydride, the hydrogenation characteristics of a Mg-8at%Al alloy powder synthesized using the electrodeposition technique were evaluated. The characterization of the hydrogenation behavior within the 180 C-280 C temperature range and the subsequent microstructural analysis elucidated that the amount of Al present in the hydride decreased with increasing temperature. This observation suggests that Al has very low solubility in magnesium hydride but Al can be accommodated in MgH{sub 2} by processing under non-equilibrium conditions. Pressure-composition isotherms were developed at different temperatures for the Mg-Al powder as well as pure Mg powder. The results indicate that the enthalpy of formation was slightly lower for the Mg-8at%Al powder while the enthalpy of dissociation did not change. The absence of noticeable influence of Al addition on the stability of magnesium hydride is attributed to its lack of solubility. (author)

Study of processes for the preparation of U3O8 powder for MTR fuel elements

International Nuclear Information System (INIS)

Neto, R.M.L.

1989-01-01

Three preparation methods of high-density U 3 O 8 powder have been studied: grinding of sintered U 3 O 8 pellets, sintering of calcined U 3 O 8 granules; and sintering of ammonium diuranate (ADU) granules. Experiments have been carried out varying ADU calcination time and temperature as well as sintering time, yielding ten U 3 O 8 batches. Powder characteristics, granulometric yield, and number of process steps have been taken into account for comparison purposes. Impurity content, specific surface area, stoichiometry, morphology, density, porosity distribution and phase identification have been considered as parameters for powder characterization. The main conclusions show that the second method (following a 600 0 C/3h ADU calcination) gives the best results. Moreover, the third method gives also good results, but there were some difficulties with ADU handling. (author) [pt

Synthesis of high-performance Li2FeSiO4/C composite powder by spray-freezing/freeze-drying a solution with two carbon sources

Science.gov (United States)

Fujita, Yukiko; Iwase, Hiroaki; Shida, Kenji; Liao, Jinsun; Fukui, Takehisa; Matsuda, Motohide

2017-09-01

Li2FeSiO4 is a promising cathode active material for lithium-ion batteries due to its high theoretical capacity. Spray-freezing/freeze-drying, a practical process reported for the synthesis of various ceramic powders, is applied to the synthesis of Li2FeSiO4/C composite powders and high-performance Li2FeSiO4/C composite powders are successfully synthesized by using starting solutions containing both Indian ink and glucose as carbon sources followed by heating. The synthesized composite powders have a unique structure, composed of Li2FeSiO4 nanoparticles coated with a thin carbon layer formed by the carbonization of glucose and carbon nanoparticles from Indian ink. The carbon layer enhances the electrochemical reactivity of the Li2FeSiO4, and the carbon nanoparticles play a role in the formation of electron-conducting paths in the cathode. The composite powders deliver an initial discharge capacity of 195 and 137 mAh g-1 at 0.1 C and 1 C, respectively, without further addition of conductive additive. The discharge capacity at 1 C is 72 mAh g-1 after the 100th cycle, corresponding to approximately 75% of the capacity at the 2nd cycle.

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

International Nuclear Information System (INIS)

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

2013-01-01

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

(La, Pr)0.8Sr0.2FeO3-δ-Sm 0.2Ce0.8O2-δ composite cathode for proton-conducting solid oxide fuel cells

KAUST Repository

Chen, Yonghong

2014-08-01

Mixed rare-earth (La, Pr)0.8Sr0.2FeO 3-δ-Sm0.2Ce0.8O2-δ (LPSF-SDC) composite cathode was investigated for proton-conducting solid oxide fuel cells based on protonic BaZr0.1Ce0.7Y 0.2O3-δ (BZCY) electrolyte. The powders of La 0.8-xPrxSr0.2FeO3-δ (x = 0, 0.2, 0.4, 0.6), Sm0.2Ce0.8O2-δ (SDC) and BaZr0.1Ce0.7Y0.2O3-δ (BZCY) were synthesized by a citric acid-nitrates self-propagating combustion method. The XRD results indicate that La0.8-xPrxSr 0.2FeO3-δ samples calcined at 950 °C exhibit perovskite structure and there are no interactions between LPSF0.2 and SDC at 1100 °C. The average thermal expansion coefficient (TEC) of LPSF0.2-SDC, BZCY and NiO-BZCY is 12.50 × 10-6 K-1, 13.51 × 10-6 K-1 and 13.47 × 10-6 K -1, respectively, which can provide good thermal compatibility between electrodes and electrolyte. An anode-supported single cell of NiO-BZCY|BZCY|LPSF0.2-SDC was successfully fabricated and operated from 700 °C to 550 °C with humidified hydrogen (∼3% H2O) as fuel and the static air as oxidant. A high maximum power density of 488 mW cm -2, an open-circuit potential of 0.95 V, and a low electrode polarization resistance of 0.071 Ω cm2 were achieved at 700 °C. Preliminary results demonstrate that LPSF0.2-SDC composite is a promising cathode material for proton-conducting solid oxide fuel cells. © 2014, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.

Syntheses, structures, and characterizations of a new second-order nonlinear optical material: Pb2(SeO3)(NO3)2

International Nuclear Information System (INIS)

Meng, Chang-Yu; Geng, Lei; Chen, Wen-Ting; Wei, Ming-Fang; Dai, Kai; Lu, Hong-Yan; Cheng, Wen-Dan

2015-01-01

Highlights: • The new polar compound Pb 2 (SeO 3 )(NO 3 ) 2 was synthesized by the conventional hydrothermal method. • The compound was characterized structurally and optically, showing SHG efficiency about 2 times that of KDP. • The electronic band structures and density of states are investigated theoretically. - Abstract: A new polar compound Pb 2 (SeO 3 )(NO 3 ) 2 was synthesized by the conventional facile hydrothermal method at middle temperature 200 °C and characterized by X-ray single crystal diffraction, powder diffraction, UV–vis−NIR optical absorption spectrum and infrared spectrum. It crystallizes in the orthorhombic system, space group Pmn2 1 with a = 5.4669(3) Å, b = 10.3277(6) Å, c = 7.2610(4) Å, V = 409.96(4) Å 3 . The compound features a 2D [Pb 2 (SeO 3 )] 2 ∞ architectures composed of SeO 3 and PbO 2 /PbO 3 units. Two unequivalent N(1)O 3 and N(2)O 3 units is inserted between adjacent [Pb 2 (SeO 3 )] 2 ∞ layers to stabilize the whole crystal structure. Second-harmonic generation (SHG) efficiency has been evaluated for powder Pb 2 (SeO 3 )(NO 3 ) 2 samples, showing about 2 times that of KDP reference. Moreover, the compound can achieve I-type phase-matching according to measurements by the Kurtz–Perry method. Theoretical investigations based on the first-principle DFT method were also performed to gain further insights into the crystal structure and optical properties relationship. The calculated band gap value of 3.38 eV is consistent with the optical reflectance measurements value of 3.76 eV

Magnetic properties of Sn-substituted Ni-Zn ferrites synthesized from nano-sized powders of NiO, ZnO, Fe2O3, and SnO2

Science.gov (United States)

Ali, MA; Uddin, MM; Khan, MNI; Chowdhury, FUZ; Hoque, SM; Liba, SI

2017-06-01

A series of Ni0.6-x/2Zn0.4-x/2Sn x Fe2O4 (x = 0.0, 0.05, 0.1, 0.15, 0.2, and 0.3) (NZSFO) ferrite composities have been synthesized from nano powders using a standard solid state reaction technique. The spinel cubic structure of the investigated samples has been confirmed by x-ray diffraction (XRD). The magnetic properties such as saturation magnetization ({M}{{s}}), remanent magnetization ({M}{{r}}), coercive field ({H}{{c}}), and Bohr magneton (μ) are calculated from the hysteresis loops. The value of {M}{{s}} is found to decrease with increasing Sn content in the samples. This change is successfully explained by the variation of A-B interaction strength due to Sn substitution in different sites. The compositional stability and quality of the prepared ferrite composites have also been endorsed by the fairly constant initial permeability ({μ }^{\\prime }) over a wide range of frequency. The decreasing trend of {μ }^{\\prime } with increasing Sn content has been observed. Curie temperature {T}{{C}} has been found to increase with the increase in Sn content. A wide spread frequency utility zone indicates that the NZSFO can be considered as a good candidate for use in broadband pulse transformers and wide band read-write heads for video recording. The composition of x = 0.05 shows unusual results and the possible reason is also mentioned with the established formalism.

Structure and magnetic properties of Mg0.35Cu0.2Zn0.45Fe2O4 ferrite synthesized by co-precipitation method

Directory of Open Access Journals (Sweden)

Bo Yang

2017-05-01

Full Text Available Mg0.35Cu0.2Zn0.45Fe2O4 nanosize particles have been synthesized by chemical co-precipitation method and characterized by X-ray diffraction (XRD and vibrating sample magnetometry (VSM. The XRD patterns confirmed the single phase spinel structure of the synthesized powder. The average crystallite size of the powder varied from 14 to 55 nm by changing annealing temperature. The activation energy for crystal growth was estimated as about 18.61KJ/mol. With the annealing temperature increasing, saturation magnetization (MS was successively increased while the coercivity (HC was first increased, passed through a maximum and then declined. The sintering temperature has significant influence on bulk density, initial permeability and Curie temperature of Mg0.35Cu0.2Zn0.45Fe2O4 ferrite.

Optical properties and visible-light-driven photocatalytic activity of Bi8V2O17 nanoparticles

International Nuclear Information System (INIS)

Pu, Yinfu; Liu, Ting; Huang, Yanlin; Chen, Cuili; Kim, Sun Il; Seo, Hyo Jin

2015-01-01

Bi 8 V 2 O 17 (4Bi 2 O 3 ·V 2 O 5 ) nanoparticles with the uniform size of about 50 nm were fabricated through the Pechini method. The crystal structure was investigated by X-ray powder diffraction and the structural refinement. The surface of the as-synthesized samples was characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy (EDX), transmission electron microscopy, and X-ray photoelectron spectroscopy. The optical properties, band structure, and the degradation mechanisms were discussed. The experimental results demonstrate that Bi 8 V 2 O 17 nanoparticles have an efficient visible-light absorption with band-gap energy of 1.85 eV and a direct allowed electronic transition. The photocatalytic activity was evaluated by the photodegradation of the methylene blue (MB) under visible-light irradiation (λ > 420 nm) as a function of time. These results indicate that Bi 8 V 2 O 17 could be a potential photocatalyst driven by visible light. The effective photocatalytic activity was discussed on the base of the crystal structure characteristic

Determination of Uranium In UO2 And U3O8 Powder Using UV-VIS Spectrophotometry

International Nuclear Information System (INIS)

Natalia Adventini; Diah Dwiana Lestiani; Muhayatun; Endah Damastuti

2009-01-01

Lab. TAR PTNBR BATAN - Bandung has been accredited by National Accreditation Committee on May 2 nd , 2006 as a test laboratory with number LP-311-ID, has to maintain its laboratory performance by participating in a proficiency test. In this activity, the determination of uranium in 2 samples of UO 2 with A1 and A2 codes and other 2 samples of U 3 O 8 with B1 and B2 codes using UV-Vis spectrophotometry was carried out. Colouring method was used by reacting thiocyanate ion with the uranyl ion in acidic solution to develop a stable yellow colour of uranyl thiocyanate complex solution and measured at wavelength of 380 nm. The result gave that concentration of uranium in A1, A2, B1 and B2 samples were 77.95; 75.29; 64.58 and 63.69% respectively. The Z-score value for A samples was - 1.99, meanwhile for B samples the Z score value of between laboratory was −1.29 with intra laboratory was -1,09. It meant that Z-score values for both samples were in good category. From this result, it showed that UV-Vis spectrophotometry is one of the several methods that can be used to determine uranium in UO 2 and U 3 O 8 powder. The Lab. TAR’s proficiency test for determination of uranium in UO 2 and U 3 O 8 gave a good result and it was hoped to support BATAN's program in the nuclear fuel field. (author)

Oxygen isotope effect in YBa2Cu3O7 prepared by burning YBa2Cu3 in 16O and 18O

Science.gov (United States)

Yvon, Pascal J.; Schwarz, R. B.; Pierce, C. B.; Bernardez, L.; Conners, A.; Meisenheimer, R.

1989-04-01

We prepared YBa2Cu3 powder by ball milling a 2:1 molar mixture of the intermetallics BaCu and CuY. We synthesized YBa2Cu3(16O)7-x and YBa2Cu3(18O)7-x by oxidizing the YBa2Cu3 powder in 16O and 18O. The 16O/18O ratios were determined by laser-ionization and sputtering-ionization mass spectroscopy. The YBa2Cu3(160)7-x sample had 99.8 at. %16O, and the YBa2Cu3(18O)7-x sample had 96.5 at. %18O. Susceptibility measurements of the superconducting transition temperature (Tc=91.7 K for 16O; half-point transition at 84 K show an isotope effect of 0.4+/-0.1 K.

Syntheses and crystal structure determination by X-ray powder diffraction of new compounds of Benzovesamicol

International Nuclear Information System (INIS)

Rukiah, M.; Assaad, Th.

2012-06-01

The compound 2,2,2-Trifluoro-N-(1a,2,7,7 a-tetra-hydronaphtho[2,3-b]oxiren-3-yl)- acetamide, C 1 2H 1 0F 3 NO 2 , an important precursor in the preparation of benzovesamicol analogues for the diagnosis of Alzheimers disease, was prepared by the epoxidation of 5,8-dihydronaphthalene-1-amine using 3-chloroperoxybenzoic acid. The structure was determined by X-ray powder diffraction, multinuclear NMR spectroscopy and FT-IR spectroscopy. A pair of molecules form intermolecular N- H...O hydrogen bonds, involving the amino and oxirene groups, to produce a dimer.The two racemic compounds (2RS,3RS)-5-amino-3-(4-phenylpiperazin-1-yl)-1,2,3,4 tetrahydronaphthalene-2-ol, C 2 0H 2 5N 3 O, (I) and (2RS,3RS)-5-amino-3-[4-(3- methoxyphenyl)piperazin-1-yl]-1,2,3,4-tetrahydronaphthalene-2-ol, C 2 1H 2 7N 3 O 2 , (II) important benzovesamicol analogues for the diagnosis of Alzheimer's disease, have been synthesized and characterized by FT-IR, and 1 H and 13 C NMR spectroscopic analyses. The crystal structures were analyses using powder diffraction as no suitable single crystal were obtained. The two compounds are racemic mixtures of enantiomers which crystallize in the monoclinic system in a centrosymmetric space group (P21/c). Crystallography, in particular powder X-ray diffraction, was pivotal in revealing that the enantio-resolution did not succeed. In two compounds, the piperazine ring has a chair conformation, while the cyclohexene ring assumes a half-chair conformation. In (I) the crystal packing is mediated by weak contacts, principally by complementary intermolecular N--H...O hydrogen bonds that connect successive molecules into a chain. Further stabilization is provided by weak C--H...N contacts and by a weak intermolecular C--H...π interaction. While in (II), the crystal packing is dominated by intermolecular O--H...N hydrogen bonding which links molecules along the c direction. (authors)

Rietveld refinement of the orthorhombic Pbca structures of Rb2CdSi5O12, Cs2MnSiO5O12, Cs2CoSi5O12 and Cs2NiSi5O12 leucites by synchrotron X-ray powder diffraction

International Nuclear Information System (INIS)

Bell, A.M.T.; Henderson, C.M.B.

1996-01-01

Analysis of high-resolution synchrotron X-ray powder diffraction patterns for hydrothermally synthesized Rb 2 CdSi 5 O 12 and Cs 2 MnSi 5 O 12 leucite analogues, and dry-synthesized Cs 2 CoSi 5 O 12 and Cs 2 NiSi 5 O 12 leucite analogues showed that they have an orthorhombic Pbca structure. The structures have been refined by the Rietveld method, showing that the tetrahedrally coordinated atoms (Si, Cd, Mn, Co and Ni) are ordered on separate sites. The Cs 2 MnSi 5 O 12 , Cs 2 CoSi 5 O 12 and Cs 2 NiSi 5 O 12 leucite samples are unusual in containing SiO 4 tetrahedra which are more distorted, on average, than the larger MnO 4 , CoO 4 and NiO 4 tetrahedra. The JCPDS file numbers for Rb 2 CdSi 5 O 12 , Cs 2 MnSi 5 O 12 and Cs 2 CoSi 5 O 12 are 46-1491, 46-1492 and 46-1493, respectively. (orig.)

Structural, optical, and magnetic properties of Fe doped In{sub 2}O{sub 3} powders

Energy Technology Data Exchange (ETDEWEB)

Krishna, N. Sai [Thin Films Laboratory, School of Advanced Sciences, VIT University, Vellore 632 014, Tamilnadu (India); Kaleemulla, S., E-mail: skaleemulla@gmail.com [Thin Films Laboratory, School of Advanced Sciences, VIT University, Vellore 632 014, Tamilnadu (India); Amarendra, G. [Materials Science Group, Indira Gandhi Centre for Atomic Research, Kalpakkam 603 102, Tamilnadu (India); UGC-DAE-CSR, Kalpakkam Node, Kokilamedu 603 104, Tamilnadu (India); Rao, N. Madhusudhana; Krishnamoorthi, C.; Kuppan, M.; Begam, M. Rigana [Thin Films Laboratory, School of Advanced Sciences, VIT University, Vellore 632 014, Tamilnadu (India); Reddy, D. Sreekantha [Department of Physics and Sungkyunkwan Advanced Institute of Nanotechnology (SAINT), Sungkyunkwan University, Suwon 440-746 (Korea, Republic of); Omkaram, I. [Department of Electronics and Radio Engineering, Kyung Hee University, Yongin-si, Gyeonggi-do 446-701 (Korea, Republic of)

2015-01-15

Highlights: • Synthesis of Fe doped In{sub 2}O{sub 3} powders using a solid state reaction. • Characterization of the samples using XRD, UV–vis-NIR, FT-IR, and VSM. • All Fe doped In{sub 2}O{sub 3} powders exhibited the cubic structure of In{sub 2}O{sub 3}. • All the Fe doped In{sub 2}O{sub 3} samples exhibited room temperature ferromagnetism. - Abstract: Iron doped indium oxide dilute magnetic semiconductor (In{sub 1−x}Fe{sub x}){sub 2}O{sub 3} (x = 0.00, 0.03, 0.05, and 0.07) powders were synthesized by standard solid state reaction method followed by vacuum annealing. The effect of Fe concentration on structural, optical, and magnetic properties of the (In{sub 1−x}Fe{sub x}){sub 2}O{sub 3} powders have been systematically studied. X-ray diffraction patterns confirmed the polycrystalline cubic structure of all the samples. An optical band gap increases from 3.12 eV to 3.16 eV while Fe concentration varying from 0.03 to 0.07. Magnetic studies reveal that virgin/undoped In{sub 2}O{sub 3} is diamagnetic. However, all the Fe-doped In{sub 2}O{sub 3} samples are ferromagnetic. The saturation magnetization (M{sub s}) of ferromagnetic (In{sub 1−x}Fe{sub x}){sub 2}O{sub 3} (x = 0.03, 0.05, and 0.07) samples increases from 11.56 memu/g to 148.64 memu/g with x = 0.03–0.07. The observed ferromagnetism in these samples was attributed to magnetic nature of the dopant (Fe) as well as defects created in the samples during vacuum annealing.

Synthesis and characterization of Li{sub 4}SiO{sub 4} nano-powders by a water-based sol-gel process

Energy Technology Data Exchange (ETDEWEB)

Wu Xiangwei [Shanghai Institute of Ceramics, Chinese Academy of Sciences, 1295 Dingxi Road, Shanghai 200050 (China); Wen Zhaoyin, E-mail: zywen@mail.sic.ac.c [Shanghai Institute of Ceramics, Chinese Academy of Sciences, 1295 Dingxi Road, Shanghai 200050 (China); Xu Xiaogang; Wang Xiuyan; Lin Jiu [Shanghai Institute of Ceramics, Chinese Academy of Sciences, 1295 Dingxi Road, Shanghai 200050 (China)

2009-08-01

The water-based sol-gel process for the synthesis of Li{sub 4}SiO{sub 4} nano-powders was reported for the first time. LiOH.H{sub 2}O and aerosil SiO{sub 2} were used as the starting materials with citric acid (C{sub 6}H{sub 8}O{sub 7}.H{sub 2}O) as the chelating agent. Li{sub 4}SiO{sub 4} powders with particle size as small as 100 nm were successfully synthesized at the temperature as low as 675 deg. C. Phase analysis, morphology, sintering behavior of the powders and ionic conductivity of the sintered bodies were investigated systematically. The experimental results showed that the powders obtained by the water-based sol-gel process (SG) possessed excellent sinterability, exhibiting a linear shrinkage of 5.2% while sintered to 900 deg. C, more than 3 times that of the powders obtained by solid state reaction (SSR). The bulk conductivity of the SG sintered bodies was much higher than that of the SSR samples at the same testing temperature.

Synthesis, characterization, and analysis of enhanced photocatalytic activity of Zr-doped TiO2 nanostructured powders under UV light

Science.gov (United States)

Sekhar, M. Chandra; Purusottam Reddy, B.; Mallikarjuna, K.; Shanmugam, Gnanendra; Ahn, Chang-Hoi; Park, Si-Hyun

2018-01-01

Zr-doped and pure TiO2 nanoparticles (NPs) were synthesized using a simple inexpensive sol-gel method. X-ray powder diffractometry and Fourier transform infrared spectrometry revealed the presence of anatase-phase TiO2 NPs. Scanning electron microscopy and transmission electron microscopy revealed that the average nanocrystalline size of approximately 15 nm. The photocatalytic activities of these materials were evaluated using Rhodamine B (Rh B) as an organic contaminant. The photocatalytic activity of pure and Zr-doped TiO2 NPs (with at% 4, 8, 12 and 16) was measured in terms of the degradation of Rh B under UV light. The antibacterial activities of pure and Zr-doped (with 8 at%) TiO2 NPs were evaluated against Bacillus subtillis, Escherichia coli, and Pseudomonas aeruginosa. A maximum inhibition zone (19 mm) was observed for pure TiO2 NPs, against Bacillus subtillis and Pseudomonas aeruginosa, while Zr-doped TiO2 (8 at%) exhibited a lesser inhibition zone (18 mm) against the same Bacillus subtillis and Pseudomonas aeruginosa (18 mm). However, Zr-doped TiO2 (8 at%) NPs exhibited a greater inhibition zone against Escherichia coli (17 mm), while the activity of pure TiO2 NPs against Escherichia coli (15 mm) was retarded. Thus, pure TiO2 NPs and Zr-doped TiO2 (8 at%) NPs have competent activities and can be used as antibacterial agents against different bacteria.

Synthesis of Bi{sub 1.8}Pb{sub 0.4}Sr{sub 2}Ca{sub 2}Cu{sub 3}O{sub x} superconductor

Science.gov (United States)

Smith, M.G.

1996-10-29

Two-powder processes for the synthesis of superconducting (Bi, Pb)-2223/Ag-clad wires by the oxide-powder-in-the-robe are provided. The first precursor powder, of nominal stoichiometry CaCuO{sub x}, is a solution-synthesized mixture of Ca{sub 0.45}Cu{sub 0.55}O{sub 2} and CaO. Using these oxide precursor mixtures, superconducting tapes with well-aligned grains and reproducible critical current densities J{sub c} in the range of 20,000 to 26,000 A/cm{sup 2} at 75 K in self-field after annealing less than 200 hours were obtained. 2 figs.

ELECTRON MICROSCOPIC INVESTIGATION OF YTTRIUM ALUMINUM GARNET POWDERS Y3AL5O12, SYNTHESIZED BY SOL–GEL METHOD

Directory of Open Access Journals (Sweden)

A. E. Baranchikov

2015-09-01

Full Text Available Subject of Study. The paper presents results of characterization for neodymium doped yttrium aluminum garnet nanopowders - YAG:Nd3+ by the method of scanning electronic microscopy. Method. Synthesis of YAG:Nd3+ was carried out by sol-gel method from nitrate or acetate - nitrate solutions with addition of some organic compounds and ammonia as well. Such substances were used as the source ones: oxides of neodymium and yttrium with the content of the basic substance equal to 99.999 %; organic compounds: citric acid with the content of the basic substance not less than 99.0 %; ethylene glycol (99.5%; the ammonium lauryl sulfate (99.0 %; urea (99.0 % of Alfa Aesar, Fluka, Aldrich companies. Oxides of yttrium and neodymium (5 at. % were dissolved in 50% acetic acid, nitrate aluminum was added with a view to the resulting product Y2,85Nd0,15Al5,0O12, the solution was stirred and heated to 60С before reaching its transparency and uniformity. The weight of the portion corresponding to the stoichiometry YAG was 2.0 g. 50 % aqueous solutions of organic substances or 5% NH4OH in a weight ratio of 1:1 to the weight of the garnet were added in aqueous solutions, placed into glass cups. The solutions were thoroughly mixed first using a conventional stirrer, then on ultrasonic installation with simultaneous 60 С heating for 2 hours. Drying of solutions to the consistency of a powder or a thick gel was carried out at 110 С. Then the samples were placed into platinum cups and annealed in a tube furnace at 950 - 1050 С for the period from 0.5 to 2 hours. Additional annealing of the powders in the air at 950 - 1060С were carried out for the purpose of powders clarifying for residual amorphous carbon removal. Main Results. The synthesized powder precursors and powders after annealing were examined using a polarizing microscope to identify anisotropic crystalline phases. X-ray analysis of the synthesized samples was carried out on a DRON - 4 and UDR - 63

Study of fluorine doped (Nb,Ir)O{sub 2} solid solution electro-catalyst powders for proton exchange membrane based oxygen evolution reaction

Energy Technology Data Exchange (ETDEWEB)

Kadakia, Karan Sandeep [Chemical and Petroleum Engineering, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); Jampani, Prashanth H., E-mail: pjampani@pitt.edu [Bioengineering, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); Velikokhatnyi, Oleg I.; Datta, Moni Kanchan [Bioengineering, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); Center for Complex Engineered Multifunctional Materials, University of Pittsburgh, PA 15261 (United States); Patel, Prasad [Chemical and Petroleum Engineering, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); Chung, Sung Jae [Mechanical Engineering and Materials Science, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); Park, Sung Kyoo [Bioengineering, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); Poston, James A.; Manivannan, Ayyakkannu [US Department of Energy, National Energy Technology Laboratory, Morgantown, WV 26507 (United States); Kumta, Prashant N. [Chemical and Petroleum Engineering, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); Bioengineering, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); Center for Complex Engineered Multifunctional Materials, University of Pittsburgh, PA 15261 (United States); Mechanical Engineering and Materials Science, Swanson School of Engineering, University of Pittsburgh, PA 15261 (United States); Department of Oral Biology, School of Dental Medicine, University of Pittsburgh, PA 15217 (United States)

2016-10-15

Graphical abstract: High surface area (∼300 m{sup 2}/g) nanostructured powders of nominal composition (Nb{sub 1−x}Ir{sub x})O{sub 2} and (Nb{sub 1−x}Ir{sub x})O{sub 2}:10F have been synthesized and tested as oxygen evolution electro-catalysts for PEM based water electrolysis using a simple two-step chemical synthesis procedure. Superior electrochemical activity was demonstrated by fluorine doped compositions of (Nb{sub 1−x}Ir{sub x})O{sub 2} with an optimal composition (Nb{sub 0.75}Ir{sub 0.25})O{sub 2}:10F (x = 0.25) demonstrating on-par performance with commercial hydrated IrO{sub 2} and nanostructured in-house chemically synthesized IrO{sub 2}. Using first principles calculations, the electronic structure modification resulting in ∼75 at.% reduction (experimentally observed) in noble metal content without loss in catalytic performance and stability has been established. - Highlights: • (Nb{sub 1−x}Ir{sub x})O{sub 2}:10F nanopowder electrocatalysts have been wet chemically synthesized. • (Nb{sub 0.75}Ir{sub 0.25})O{sub 2}:10F exhibits superior electrochemical activity than pure IrO{sub 2}. • Stability of the (Nb,Ir)O{sub 2}:10F nanomaterials is comparable to pure (Nb,Ir)O{sub 2}. • High surface area F doped (Nb,Ir)O{sub 2} are promising OER anode electro-catalysts. - Abstract: High surface area (∼300 m{sup 2}/g) nanostructured powders of (Nb{sub 1−x}Ir{sub x})O{sub 2} and (Nb{sub 1−x}Ir{sub x})O{sub 2}:10F (∼100 m{sup 2}/g) have been examined as promising oxygen evolution reaction (OER) electro-catalysts for proton exchange membrane (PEM) based water electrolysis. Nb{sub 2}O{sub 5} and 10 wt.% F doped Nb{sub 2}O{sub 5} powders were prepared by a low temperature sol-gel process which were then converted to solid solution (Nb,Ir)O{sub 2} and 10 wt.% F doped (Nb,Ir)O{sub 2} [(NbIr)O{sub 2}:10F] electro-catalysts by soaking in IrCl{sub 4} followed by heat treatment in air. Electro-catalyst powders of optimal composition (Nb{sub 0.75}Ir

Molten salt synthesis of ZnNb2O6 powder

International Nuclear Information System (INIS)

Guo Liangzhai; Dai Jinhui; Tian Jintao; Zhu Zhibin; He Tian

2007-01-01

Pure ZnNb 2 O 6 powder was successfully prepared by the molten salt synthesis method using Nb 2 O 5 and ZnO as raw materials and a mixture of NaCl and KCl as the solvent. The phase form and morphology of the prepared powder were characterized by X-ray diffraction and scanning electron microscopy. The effect of reacting temperature on phase formation was investigated. The results indicated that the single phase ZnNb 2 O 6 powder can be obtained by the molten salt synthesis method at 600 deg. C, and the SEM photographs show that the grains of the powder are rod-like particles

Synthesis of Nano-Structured La0.6Sr0.4Co0.2Fe0.8O3 Perovskite by Co-Precipitation Method

Directory of Open Access Journals (Sweden)

Ebrahim Mostafavi

2015-06-01

Full Text Available Nano-structured lanthanum strontium cobalt ferrite, La0.6Sr0.4Co0.2Fe0.8O3 (LSCF, was successfully synthesized via co-precipitation method using metal nitrates as starting materials. Effects of precipitating agent and calcination temperature on the phase composition and morphology of synthesized powders were systematically studied using X-ray diffraction (XRD and field emission scanning electron microscopy (FESEM, respectively. XRD analysis revealed that a single phase La0.6Sr0.4Co0.2Fe0.8O3 perovskite was obtained in the processed sample using ammonium carbonate as precipitating agent with a NH4+/NO3-molar ratio of 2 after calcination at 1000C for 1 h. The phase composition of products was also affected by changing pH values. Moreover, using sodium hydroxide as a precipitant resulted in a mixture of La0.6Sr0.4Co0.2Fe0.8O3 and cobalt ferrite (CoFe2O4 phases. Careless washing of the precursors can also led to the formation of mixed phase after calcination of final powders. Mean crystallite size of the obtained powders was not noticeably affected by varying calcination temperature from 900 to 1050C and remained almost the same at 10 nm, however increasing calcination temperature to 1100C resulted in sharp structural coarsening. FESEM studies demonstrate that relatively uniform particles with mean particle size of 90 nm were obtained in the sample processed with a NH4+/NO3- molar ratio of 2 after calcination at 1000C for 1 h.

Influence of Ce-precursor and fuel on structure and catalytic activity of combustion synthesized Ni/CeO2 catalysts for biogas oxidative steam reforming

International Nuclear Information System (INIS)

Vita, Antonio; Italiano, Cristina; Fabiano, Concetto; Laganà, Massimo; Pino, Lidia

2015-01-01

A series of nanosized Ni/CeO 2 catalysts were prepared by Solution Combustion Synthesis (SCS) varying the fuel (oxalyldihydrazide, urea, carbohydrazide and glycerol), the cerium precursor (cerium nitrate and cerium ammonium nitrate) and the nickel loading (ranging between 3.1 and 15.6 wt%). The obtained powders were characterized by X-ray Diffraction (XRD), N 2 -physisorption, CO-chemisorption, Temperature Programmed Reduction (H 2 -TPR) and Scanning Electron Microscopy (SEM). The catalytic activity towards the Oxy Steam Reforming (OSR) of biogas was assessed. The selected operating variables have a strong influence on the nature of combustion and, in turn, on the morphological and structural properties of the synthesized catalysts. Particularly, the use of urea allows to improve nickel dispersion, surface area, particle size and reducibility of the catalysts, affecting positively the biogas OSR performances. - Highlights: • Synthesis of Ni/CeO 2 nanopowders by quick and easy solution combustion synthesis. • The fuel and precursor drive the structural and morphological properties of the catalysts. • The use of urea as fuel allows to improve nickel dispersion, surface area and particle size. • Ni/CeO 2 (7.8 wt% of Ni loading) powders synthesized by urea route exhibits high performances for the biogas OSR process

Effects of milling method and calcination condition on phase and morphology characteristics of Mg4Nb2O9 powders

International Nuclear Information System (INIS)

Wongmaneerung, R.; Sarakonsri, T.; Yimnirun, R.; Ananta, S.

2006-01-01

Magnesium niobate, Mg 4 Nb 2 O 9 , powders has been synthesized by a solid-state reaction. Both conventional ball- and rapid vibro-milling have been investigated as milling methods, with the formation of the Mg 4 Nb 2 O 9 phase investigated as a function of calcination conditions by DTA and XRD. The particle size distribution of the calcined powders was determined by laser diffraction technique, while morphology, crystal structure and phase composition were determined via a combination of SEM, TEM and EDX techniques. The type of milling method together with the designed calcination condition was found to show a considerable effect on the phase and morphology evolution of the calcined Mg 4 Nb 2 O 9 powders. It is seen that optimization of calcination conditions can lead to a single-phase Mg 4 Nb 2 O 9 in both milling methods. However, the formation temperature and dwell time for single-phase Mg 4 Nb 2 O 9 powders were lower with the rapid vibro-milling technique

Preparation and Crystal Structures of Some AIVB2IIO4 Compounds: Powder X-Ray Diffraction and Rietveld Analysis

Directory of Open Access Journals (Sweden)

K. Jeyadheepan

2014-01-01

Full Text Available The AIVB2IIO4 compounds such as cadmium tin oxide (Cd2SnO4 or CTO and zinc tin oxide (Zn2SnO4 or ZTO are synthesized by solid state reaction of the subsequent binary oxides. The synthesized powders were analyzed through the powder X-ray diffraction (PXRD. Cell search done on the PXRD patterns shows that the Cd2SnO4 crystallizes in orthorhombic structure with space group Pbam and the cell parameters as a=5.568(2 Å, b=9.894(3 Å, and c=3.193(1 Å and the Zn2SnO4 crystallizes as cubic with the space group Fd3 -m and with the cell parameter a=8.660(2 Å. Rietveld refinement was done on the PXRD patterns to get the crystal structure of the Cd2SnO4 and Zn2SnO4 and to define the site deficiency of atoms which causes the electrical properties of the materials.

Powder neutron diffraction study on Pb2Sr2YCu3O8+δ(δ = 0.0 and 1.67)

International Nuclear Information System (INIS)

Fujishita, Hideshi; Sato, Masatoshi; Morii, Yukio; Funahashi, Satoru.

1993-01-01

Powder neutron diffraction patterns of Pb 2 Sr 2 YCu 3 O 8+δ (δ = 0.0 and 1.67) were analyzed by Rietveld method. For δ = 0, it had been indicated, by powder X-ray diffraction, that the structure was a monoclinic one. The R factors of the present analysis for the monoclinic structure were about 3/4 of those for the previous orthorhombic ones. The structure was almost the same as the previous X-ray result except z (02). For the annealed phase, the tetragonal and the orthorhombic structures had been presented by X-ray diffraction and by neutron diffraction, respectively. The R factors of the present analysis for the orthorhombic structure were about 5/6 of those for the tetragonal structure. The distance between the Pb plane and the oxygen deficient Cu plane was found to become larger in proportion to δ, though there occurs a phase separation in low δ region. (author)

Structure and electrochemical properties of Mg2SnO4 nanoparticles synthesized by a facile co-precipitation method

International Nuclear Information System (INIS)

Tang, Hao; Cheng, Cuixia; Yu, Gaige; Liu, Haowen; Chen, Weiqing

2015-01-01

Nanosized Mg 2 SnO 4 has been synthesized by a facile co-precipitation method. The structure and morphology of the as-prepared samples are characterized by X-ray diffraction (XRD), X-ray photoelectron spectrometer (XPS), fourier Transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). It is found that Mg 2 SnO 4 sample is very sensitive to the aging time of the precursor. The single phase Mg 2 SnO 4 nanoparticles with ∼23 nm can be obtained at 900 °C using the aging 35 min percusor as source. The electrochemical properties of the powder obtained at 900 °C are investigated by galvanostatic discharge-charge tests and cyclic voltammograms (CVs). The initial specific discharge capacity reaches as high as 927.7 mAh g −1 at 0.2 mA cm −2 in 0.05–3.0 V, which indicates that Mg 2 SnO 4 nanoparticles could be a promising candidate of anode material for Li-ion batteries. - Highlights: • Nanosized Mg 2 SnO 4 has been synthesized by a facile co-precipitation method. • We find that Mg 2 SnO 4 sample is very sensitive to the ageing time of the precursor. • The single phase Mg 2 SnO 4 nanoparticles with about 23 nm can be obtained by calcining the ageing 35 min percusor at 900 °C. • The obtained powders show a better electrochemical performance

α-ScVSe2O8, β-ScVSe2O8, and ScVTe2O8: new quaternary mixed metal oxides composed of only second-order Jahn-Teller distortive cations.

Science.gov (United States)

Kim, Yeong Hun; Lee, Dong Woo; Ok, Kang Min

2013-10-07

Three new quaternary scandium vanadium selenium/tellurium oxides, α-ScVSe2O8, β-ScVSe2O8, and ScVTe2O8 have been synthesized through hydrothermal and standard solid-state reactions. Although all three reported materials are stoichiometrically similar, they exhibit different crystal structures: α-ScVSe2O8 has a three-dimensional framework structure consisting of ScO6, VO6, and SeO3 groups. β-ScVSe2O8 reveals another three-dimensional framework composed of ScO7, VO5, and SeO3 polyhedra. ScVTe2O8 shows a layered structure with ScO6, VO4, and TeO4 polyhedra. Interestingly, the constituent cations, that is, Sc(3+), V(5+), Se(4+), and Te(4+) are all in a distorted coordination environment attributable to second-order Jahn-Teller (SOJT) effects. Complete characterizations including infrared spectroscopy, elemental analyses, thermal analyses, dipole moment calculation, and the magnitudes of out-of-center distortions for the compounds are reported. Transformation reactions suggest that α-ScVSe2O8 may change to β-ScVSe2O8, and then to Sc2(SeO3)3·H2O under hydrothermal conditions.

Crystal structure and optical property of complex perovskite oxynitrides ALi0.2Nb0.8O2.8N0.2, ANa0.2Nb0.8O2.8N0.2, and AMg0.2Nb0.8O2.6N0.4 (A = Sr, Ba)

Science.gov (United States)

Moon, Keon Ho; Avdeev, Maxim; Kim, Young-Il

2017-10-01

Oxynitride type complex perovskites AM0.2Nb0.8O3-xNx (A = Sr, Ba; M = Li, Na, Mg) were newly synthesized by the solid state diffusion of Li+, Na+, or Mg2+ into the layered oxide, A5Nb4O15, with concurrent O/N substitution. Neutron and synchrotron X-ray Rietveld refinement showed that SrLi0.2Nb0.8O2.8N0.2, SrNa0.2Nb0.8O2.8N0.2, and SrMg0.2Nb0.8O2.6N0.4 had body-centered tetragonal symmetry (I4/mcm), while those with A = Ba had simple cubic symmetry (Pm 3 ̅ m). In the tetragonal Sr-compounds, the nitrogen atoms were localized on the c-axial 4a site. However, the octahedral cations, M/Nb (M = Li, Na, Mg) were distributed randomly in all six compounds. The lattice volume of AM0.2Nb0.8O3-xNx was dependent on various factors including the type of A and the electronegativity of M. Compared to the simple perovskites, ANbO2N (A = Sr, Ba), AM0.2Nb0.8O3-xNx had wider band gaps (1.76-2.15 eV for A = Sr and 1.65-2.10 eV for A = Ba), but significantly lower sub-gap absorption.

Electrochemical behaviors of wax-coated Li powder/Li 4Ti 5O 12 cells

Science.gov (United States)

Park, Han Eol; Seong, Il Won; Yoon, Woo Young

The wax-coated Li powder specimen was effectively synthesized using the drop emulsion technique (DET). The wax layer on the powder was verified by SEM, Focused Ion Beam (FIB), EDX and XPS. The porosity of a sintered wax-coated Li electrode was measured by linear sweep voltammetry (LSV) and compared with that of a bare, i.e., un-coated Li electrode. The electrochemical behavior of the wax-coated Li powder anode cell was examined by the impedance analysis and cyclic testing methods. The cyclic behavior of the wax-coated Li powder anode with the Li 4Ti 5O 12 (LTO) cathode cell was examined at a constant current density of 0.35 mA cm -2 with the cut-off voltages of 1.2-2.0 V at 25 °C. Over 90% of the initial capacity of the cell remained even after the 300th cycle. The wax-coated Li powder was confirmed to be a stable anode material.

Thermoluminescence properties of Li2B4O7:Cu, B phosphor synthesized using solution combustion technique

Science.gov (United States)

Ozdemir, A.; Altunal, V.; Kurt, K.; Depci, T.; Yu, Y.; Lawrence, Y.; Nur, N.; Guckan, V.; Yegingil, Z.

2017-12-01

To determine the effects of various concentrations of the activators copper (Cu) and boron (B) on the thermoluminescence (TL) properties of lithium tetraborate, the phosphor was first synthesized and doped with five different concentrations of copper (0.1-0.005 wt%) using solution combustion method. 0.01 wt% Cu was the concentration which showed the most significant increase in the sensitivity of the phosphor. The second sort of Li2B4O7:Cu material was prepared by adding B (0.001-0.03 wt%) to it. The newly developed copper-boron activated lithium tetraborate (Li2B4O7:Cu, B) material with 0.01 wt% Cu and 0.001 wt% B impurity concentrations was shown to have promise as a TL phosphor. The material formation was examined using powder x-Ray Diffraction (XRD) analysis and Scanning Electron Microscope (SEM) imaging. Fourier Transform Infrared (FT-IR) spectrum of the synthesized polycrystalline powder sample was also recorded. The TL glow curves were analyzed to determine various dosimetric characteristics of the synthesized luminophosphors. The dose response increased in a ;linear; way with the beta-ray exposure between 0.1-20 Gy, a dose range being interested in medical dosimetry. The response with changing photon and electron energy was studied. The rate of decay of the TL signal was investigated both for dark storage and under direct sunlight. Li2B4O7:Cu, B showed no individual variation of response in 9 recycling measurements. The fluorescence spectrum was determined. The kinetic parameters were estimated by different methods and the results discussed. The studied properties of synthesized Li2B4O7:Cu, B were found all favorable for dosimetric purposes.

Characteristics and properties of a novel in situ method of synthesizing mesoporous TiO2 nanopowders by a simple coprecipitation process without adding surfactant

International Nuclear Information System (INIS)

Yeh, Shang-Wei; Ko, Horng-Huey; Chiang, Hsiu-Mei; Chen, Yen-Ling; Lee, Jian-Hong; Wen, Chiu-Ming; Wang, Moo-Chin

2014-01-01

Highlights: • The TiO 2 precursor powder contained anatase and 19.5% NH 4 Cl. • Mesoporous anatase TiO 2 nanopowders were successfully synthesized. • Uncalcined precursor powder contained the phases of type I NH 4 Cl and anatase TiO 2 . • Anatase size increases from 3.3 to 14.3 nm when calcined at 473–773 K for 2 h. • The average pore size between 3.80 and 14.0 nm when calcined between 473 and 773 K. - Abstract: In situ synthesis of mesoporous TiO 2 nanopowders using titanium tetrachloride (TiCl 4 ) and NH 4 OH as initial materials has been successfully fabricated by a coprecipitation process without the addition of surfactant. Characteristics and properties of the mesoporous TiO 2 nanopowders were investigated using differential scanning calorimetry/thermogravimetry (DSC/TG), X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET) and Barrent–Joyner–Halenda (BJH) analyses, transmission electron microscopy (TEM), selected area electron diffraction (SAED) and high resolution TEM (HRTEM). The results of TG and XRD showed that the NH 4 Cl decomposed between 513 and 673 K. XRD results showed that the anatase TiO 2 only contained a single phase when the calcination temperature of the precursor powder was less than 673 K. Whereas phases of anatase and rutile TiO 2 coexist after calcining at 773 K for 2 h. The crystalline size of the anatase and rutile TiO 2 was 14.3 and 26.6 nm, respectively, when the precursor powder was calcined at 773 K for 2 h. The BET and BJH results showed a significant increase in surface area and pore volumes when the NH 4 Cl was completely decomposed. The maximum values of BET specific surface area and volume were 172.8 m 2 /g and 0.392 cm 3 /g, respectively. The average pore sizes when calcination was at 473 and 773 K for 2 h were 3.8 and 14.0 nm, respectively

Influence of Ce-precursor and fuel on structure and catalytic activity of combustion synthesized Ni/CeO{sub 2} catalysts for biogas oxidative steam reforming

Energy Technology Data Exchange (ETDEWEB)

Vita, Antonio, E-mail: antonio.vita@itae.cnr.it; Italiano, Cristina; Fabiano, Concetto; Laganà, Massimo; Pino, Lidia

2015-08-01

A series of nanosized Ni/CeO{sub 2} catalysts were prepared by Solution Combustion Synthesis (SCS) varying the fuel (oxalyldihydrazide, urea, carbohydrazide and glycerol), the cerium precursor (cerium nitrate and cerium ammonium nitrate) and the nickel loading (ranging between 3.1 and 15.6 wt%). The obtained powders were characterized by X-ray Diffraction (XRD), N{sub 2}-physisorption, CO-chemisorption, Temperature Programmed Reduction (H{sub 2}-TPR) and Scanning Electron Microscopy (SEM). The catalytic activity towards the Oxy Steam Reforming (OSR) of biogas was assessed. The selected operating variables have a strong influence on the nature of combustion and, in turn, on the morphological and structural properties of the synthesized catalysts. Particularly, the use of urea allows to improve nickel dispersion, surface area, particle size and reducibility of the catalysts, affecting positively the biogas OSR performances. - Highlights: • Synthesis of Ni/CeO{sub 2} nanopowders by quick and easy solution combustion synthesis. • The fuel and precursor drive the structural and morphological properties of the catalysts. • The use of urea as fuel allows to improve nickel dispersion, surface area and particle size. • Ni/CeO{sub 2} (7.8 wt% of Ni loading) powders synthesized by urea route exhibits high performances for the biogas OSR process.

Effect of Co{sup 2+} and Y{sup 3+} ions insertion on the microstructure development and magnetic properties of Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} powders synthesized using Co-precipitation method

Energy Technology Data Exchange (ETDEWEB)

Rashad, M.M., E-mail: rashad133@yahoo.com [Central Metallurgical Research and Development Institute (CMRDI), P.O. Box 87, Helwan 11421, Cairo (Egypt); Rayan, D.A.; Turky, A.O. [Central Metallurgical Research and Development Institute (CMRDI), P.O. Box 87, Helwan 11421, Cairo (Egypt); Hessien, M.M. [Central Metallurgical Research and Development Institute (CMRDI), P.O. Box 87, Helwan 11421, Cairo (Egypt); Chemistry Department, Taif University (Saudi Arabia)

2015-01-15

Nanocrystalline Ni{sub 0.5}Zn{sub 0.5−x}Co{sub x}Fe{sub 2−z}Y{sub z}O{sub 4} powders (x=0–0.3 and z from 0 to 0.3) have been synthesized via a facile co-precipitation technique. X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM) are utilized in order to study the effect of variation of cobalt and yttrium substitutions and its impact on crystalline size, lattice parameter, X-ray density, microstructure and magnetic properties of the formed powders. X-ray diffraction data indicated that, after doping, all samples consisted of the main spinel phase for the formed precursors precipitated at pH 10 annealed at 1000 {sup o}C for 2 h. The lattice parameter and the unit cell were decreased linearly with increasing Co content whereas they were increased with increasing the Y incorporation. Additionally, the porosity was increased with increasing Co concentration while it was decreased with increasing the Y insertion. The mean ionic radii and hopping and bond lengths was decreased with the value of Co{sup 2+} and they were increased with the value of Y{sup 3+} ion as well as both of Y{sup 3+} and Co{sup 2+} ions. The microstructures of the produced powders were found to be cubic like structure. The addition of Y{sup 3+} ion suppressed the grain size whereas addition of Co{sup 2+} ion enhanced the grain growth availably. An examination of the magnetic properties revealed an increase in saturation magnetization with increasing Co and Y concentrations incorporation up to x=0.3. Meanwhile, the formed powders exhibited superparamagnetic characteristics. A high saturation magnetization (77.0 emu/g) was achieved for Ni{sub 0.5}Zn{sub 0.2}Co{sub 0.3}Fe{sub 2}O{sub 4} sample annealed at 1000 {sup o}C for 2 h. - Highlights: • Ni{sub 0.5}Zn{sub 0.5−x}Co{sub x}Fe{sub 2−z}Y{sub z}O{sub 4} powders were synthesized. • The porosity decreases with Y{sup 3+} and increases with Co{sup 2+}. • The bond lengths decrease with Co{sup 2

Magnetic measurements and neutron diffraction study of the layered hybrid compounds Mn(C8H4O4)(H2O)2 and Mn2(OH)2(C8H4O4)

International Nuclear Information System (INIS)

Sibille, Romain; Mesbah, Adel; Mazet, Thomas; Malaman, Bernard; Capelli, Silvia; François, Michel

2012-01-01

Mn(C 8 H 4 O 4 )(H 2 O) 2 and Mn 2 (OH) 2 (C 8 H 4 O 4 ) layered organic–inorganic compounds based on manganese(II) and terephthalate molecules (C 8 H 4 O 4 2− ) have been studied by DC and AC magnetic measurements and powder neutron diffraction. The dihydrated compound behaves as a 3D antiferromagnet below 6.5 K. The temperature dependence of its χT product is typical of a 2D Heisenberg system and allows determining the in-plane exchange constant J≈−7.4 K through the carboxylate bridges. The magnetic structure confirms the in-plane nearest neighbor antiferromagnetic interactions and the 3D ordering. The hydroxide based compound also orders as a 3D antiferromagnet with a higher Néel temperature (38.5 K). Its magnetic structure is described from two antiferromagnetically coupled ferromagnetic sublattices, in relation with the two independent metallic sites. The isothermal magnetization data at 2 K are consistent with the antiferromagnetic ground-state of these compounds. However, in both cases, a slope change points to field-induced modification of the magnetic structure. - Graphical abstract: The macroscopic magnetic properties and magnetic structures of two metal-organic frameworks based on manganese (II) and terephthalate molecules are presented. Highlights: ► Magnetic study of Mn(C 8 H 4 O 4 )(H 2 O) 2 and Mn 2 (OH) 2 (C 8 H 4 O 4 ). ► Two compounds with common features (interlayer linker/distance, S=5/2 spin). ► Magnetic measurements quantitatively analyzed to deduce exchange constants. ► Magnetic structures determined from neutron powder diffraction experiments.

Structural and morphological characterization of TiO{sub 2}-ZrO{sub 2} powders obtained by the polymeric precursors method; Caracterizacao estrutural e morfologica de pos de TiO{sub 2}-ZrO{sub 2} obtidos pelo metodo dos precursores polimericos

Energy Technology Data Exchange (ETDEWEB)

Ribeiro, M.A.; Gama, L.; Bispo, A.; Neiva, L.S., E-mail: m_aparecidaribeiro@yahoo.com.b [Universidade Federal de Campina Grande (DEMa/UFCG), PB (Brazil). Dept. de Engenharia de Materiais; Bernardi, M.I.B. [Universidade de Sao Paulo (IFSC/USP), Sao Carlos, SP (Brazil). Inst. de Fisica; Kiminami, R.H.G.A. [Universidade Federal de Sao Carlos (DEMa/UFSCar), SP (Brazil). Dept. de Engenharia de Materiais

2010-07-01

This work aims to characterize the structure and morphology of TiO{sub 2}-ZrO{sub 2} powders obtained by polymeric precursor method. For this we studied the following compositions: 0.25, 0.5 and 0.75 moles of Zr and calcined at 800 deg C for one hour. The powders obtained were characterized by XRD, SEM and nitrogen adsorption (BET). The analysis of X-ray diffraction showed that the powders had a phase of TiO{sub 2} in the anatase form and a tetragonal phase of ZrO{sub 2}. The crystallite size was between 8, 13 and 11 nm respectively. The analysis of scanning electron microscopy showed the growth of ZrO{sub 2} nanoparticles and that these comprise spherical agglomerates of less than 100 nm. Particle size determined by the BET ranging 28.1-29.5 nm, showing thereby the character of nanosized powders. (author)

Syntheses, characterization and nonlinear optical properties of sodium-scandium carbonate Na5Sc(CO3)4·2H2O

Science.gov (United States)

Chen, Jie; Luo, Min; Ye, Ning

2014-10-01

A novel nonlinear optical (NLO) material Na5Sc(CO3)4·2H2O has been synthesized under a subcritical hydrothermal condition. The structure is determined by single-crystal X-ray diffraction and further characterized by TG analyses and UV-vis-NIR diffuse reflectance spectrum. It crystallizes in the tetragonal space group P-421c, with a = b = 7.4622(6) Å, C = 11.5928(15) Å. The Second-harmonic generation (SHG) on polycrystalline samples was measured using the Kurtz and Perry technique, which indicated that Na5Sc(CO3)4·2H2O was a phase-matchable material, and its measured SHG coefficient was about 1.8 times as large as that of d36 (KDP). The results from the UV-vis diffuse reflectance spectroscopy study of the powder samples indicated that the short-wavelength absorption edges of Na5Sc(CO3)4·2H2O is about 220 nm, suggesting that this crystal is a promising UV nonlinear optical (NLO) materials.

Blue to Yellow Photoluminescence Emission and Photocatalytic Activity of Nitrogen Doping in TiO2 Powders

Directory of Open Access Journals (Sweden)

Gabriela Byzynski

2015-01-01

Full Text Available The defects caused by doping are important for understanding the increased photocatalytic activities of TiO2:N in organic reactions and in the evaluation of OH radical production after doping. TiO2:N was therefore synthesized using a modified polymeric method and N doping was performed by calcination with urea. The resulting powders were characterized using field emission scanning electron microscopy, X-ray diffraction, diffuse reflectance spectroscopy, Raman spectroscopy, Fourier transformation infrared spectroscopy, and photoluminescence emission spectroscopy (PL. N doping did not alter the morphology of the nanoparticles, and the anatase phase predominated, with the retention of the rutile phase. The band gap values, superficial areas, and crystallite sizes of the powders decreased after doping. The PL results showed an additional energy level in the TiO2:N band gap structure as a result of TiO2 lattice defects caused by doping. At low N contents, the powders showed continuous emissions from the blue region to the yellow region and a high N content shifted the PL emissions to the red region. These results suggest that the use of these powders could increase the efficiencies of solar cells and water-splitting processes. The photocatalytic activity of the powders under UVC illumination was confirmed for different organic dye molecules. The OH radical production did not change extensively after doping, as shown by experiments with terephthalic acid, and higher photocatalytic efficiencies in Rhodamine-B degradation under UVC illumination were achieved using the doped samples.

Thermoluminescence properties of Li2B4O7:Cu, B phosphor synthesized using solution combustion technique

International Nuclear Information System (INIS)

Ozdemir, A.; Altunal, V.; Kurt, K.; Depci, T.; Yu, Y.; Lawrence, Y.; Nur, N.; Guckan, V.; Yegingil, Z.

2017-01-01

To determine the effects of various concentrations of the activators copper (Cu) and boron (B) on the thermoluminescence (TL) properties of lithium tetraborate, the phosphor was first synthesized and doped with five different concentrations of copper (0.1–0.005 wt%) using solution combustion method. 0.01 wt% Cu was the concentration which showed the most significant increase in the sensitivity of the phosphor. The second sort of Li 2 B 4 O 7 :Cu material was prepared by adding B (0.001–0.03 wt%) to it. The newly developed copper-boron activated lithium tetraborate (Li 2 B 4 O 7 :Cu, B) material with 0.01 wt% Cu and 0.001 wt% B impurity concentrations was shown to have promise as a TL phosphor. The material formation was examined using powder x-Ray Diffraction (XRD) analysis and Scanning Electron Microscope (SEM) imaging. Fourier Transform Infrared (FT-IR) spectrum of the synthesized polycrystalline powder sample was also recorded. The TL glow curves were analyzed to determine various dosimetric characteristics of the synthesized luminophosphors. The dose response increased in a “linear” way with the beta-ray exposure between 0.1–20 Gy, a dose range being interested in medical dosimetry. The response with changing photon and electron energy was studied. The rate of decay of the TL signal was investigated both for dark storage and under direct sunlight. Li 2 B 4 O 7 :Cu, B showed no individual variation of response in 9 recycling measurements. The fluorescence spectrum was determined. The kinetic parameters were estimated by different methods and the results discussed. The studied properties of synthesized Li 2 B 4 O 7 :Cu, B were found all favorable for dosimetric purposes. - Highlights: • Li 2 B 4 O 7 :Cu, B synthesis using solution combustion method with various concentrations. • Structure analysis of Li 2 B 4 O 7 :Cu, B using XRD, SEM and FTIR methods. • Investigation of thermoluminescent properties of Li 2 B 4 O 7 :Cu, B. • Relatively good

Structural and magnetic properties of Ni0.8M0.2Fe2O4 (M = Cu, Co) nano-crystalline ferrites

Science.gov (United States)

Vijaya Babu, K.; Satyanarayana, G.; Sailaja, B.; Santosh Kumar, G. V.; Jalaiah, K.; Ravi, M.

2018-06-01

Nano-crystalline nickel ferrites are interesting materials due to their large physical and magnetic properties. In the present work, two kinds of spinel ferrites Ni0.8M0.2Fe2O4 (M = Cu, Co) are synthesized by using sol-gel auto-combustion method and the results are compared with NiFe2O4. The structural properties of synthesized ferrites are determined by using X-ray powder diffraction; scanning electron microscope and Fourier transform infrared spectroscopy. The cation distribution obtained from X-ray diffraction show that cobalt/copper occupies only tetrahedral site in spinel lattice. The lattice constant increases with the substitution of cobalt/copper. The structural parameters like bond lengths, tetrahedral and octahedral edges have been varied with the substitution. The microstructural study is carried out by using SEM technique and the average grain size is increased with nickel ferrite. The initial permeability (μi) is improving with the substitution. The observed g-value from ESR is approximately equal to standard value.

Ag doped (Bi1.6Pb0.4Sr2CaCu2O8+δ textured rods

Directory of Open Access Journals (Sweden)

Díez, J. C.

2008-06-01

Full Text Available In this work, superconducting samples of (Bi1.6Pb0.4Sr2CaCu2O8+δ with Ag additions have been studied. (Bi1.6Pb0.4Sr2CaCu2O8+δ + x wt.% Ag (with x = 0, 1 and 3 powders were synthesized using a sol-gel method. The obtained powders were used as precursors to fabricate long textured cylindrical bars through a floating zone melting method. A drastic change on the microstructure has been found when comparing with undoped Bi2Sr2CaCu2O8+δ samples. The results showed that electrical resistivity at room temperature, critical current as well as flexural strength are improved when Ag is added to these Pb doped samples, while critical temperature does not change. On the other hand, it has been found that samples with composition (Bi1.6Pb0.4Sr2CaCu2O8+δ + Ag shown E-I curves with very high sharpness values on the zone of the superconducting to normal transition, reaching n-values (E∼In as high as 45 at 65K.Se han preparado polvos cerámicos de composición (Bi1.6Pb0.4Sr2CaCu2O8+δ + x % Ag en peso (con x = 0, 1 y 3 mediante un proceso sol-gel. Estos polvos se han utilizado para fabricar precursores que se texturaron por medio del método de fusión zonal flotante. Se ha encontrado un gran cambio en la microestructura cuando se compara con muestras de composición pura Bi2Sr2CaCu2O8+δ. Tanto la resistividad eléctrica a temperatura ambiente, como la corriente crítica, así como la resistencia a flexión se mejoran cuando la Ag se adiciona a estas muestras dopadas con Pb, mientras que no se observa cambio en la temperatura crítica. Por otra parte, se ha encontrado que las muestras de composición (Bi1.6Pb0.4Sr2CaCu2O8+δ + Ag presentan una gran pendiente de la curva E-I en la zona de transición entre el estado superconductor y el estado normal. Con estas composiciones, se han encontrado valores de n (E∼In de hasta 45 a 65K.

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

Synthesis and Characterization of 8-Yttrium(III-Containing 81-Tungsto-8-Arsenate(III, [Y8(CH3COO(H2O18(As2W19O684(W2O62(WO4]43−

Directory of Open Access Journals (Sweden)

Masooma Ibrahim

2015-06-01

Full Text Available The 8-yttrium(III-containing 81-tungsto-8-arsenate(III [Y8(CH3COO(H2O18(As2W19O684(W2O62(WO4]43− (1 has been synthesized in a one-pot reaction of yttrium(III ions with [B-α-AsW9O33]9− in 1 M NaOAc/HOAc buffer at pH 4.8. Polyanion 1 is composed of four {As2W19O68} units, two {W2O10} fragments, one {WO6} group, and eight YIII ions. The hydrated cesium-sodium salt of 1 (CsNa-1 was characterized in the solid-state by single-crystal XRD, FT-IR spectroscopy, thermogravimetric and elemental analyses.

Bioactivity of gel-glass powders in the CaO-SiO2 system: a comparison with ternary (CaO-P2O5-SiO2) and quaternary glasses (SiO2-CaO-P2O5-Na2O).

Science.gov (United States)

Saravanapavan, Priya; Jones, Julian R; Pryce, Russell S; Hench, Larry L

2003-07-01

Bioactive glasses react chemically with body fluids in a manner that is compatible with the repair processes of the tissues. This results in the formation of an interfacial bond between the glasses and living tissue. Bioactive glasses also stimulate bone-cell proliferation. This behavior is dependent on the chemical composition as well as the surface texture of the glasses. It has been recently reported that gel-derived monolith specimens in the binary SiO2 - CaO are bioactive over a similar molar range of SiO2 content as the previously studied ternary CaO-P2O5-SiO2 system. In this report, the preparation and bioactivity of the binary gel-glass powder with 70 mol % SiO2 is discussed and its bioactivity is compared with the melt-derived 45S5 (quaternary) Bioglass and sol-gel-derived 58S (ternary) bioactive gel-glass compositions. Dissolution kinetic parameters K(1) and K(2) were also computed based on the silicon release for all glass powders. It was shown that the simple two-component SiO2-CaO gel-glass powder is bioactive with comparable dissolution rates as the clinically used melt-derived 45S5 Bioglass powder and extensively studied sol-gel-derived 58S gel-glass powder. Copyright 2003 Wiley Periodicals, Inc.

High rate performances of the cathode material LiNi1/3Co1/3Mn1/3O2 synthesized using low temperature hydroxide precipitation

International Nuclear Information System (INIS)

Cheng, Cuixia; Tan, Long; Liu, Haowen; Huang, Xintang

2011-01-01

Graphical abstract: A low-temperature reaction route is introduced based on hydroxide precipitation method to synthesize a cathode material LiNi 1/3 Co 1/3 Mn 1/3 O 2 . The charge-discharge tests were performed at 1000 mA g -1 between 2.5 and 4.5 V and the discharge capacity is about 160 mAh g -1 . The discharge capacity of the material is strongly impacted by the reaction temperature. The powders sintered at 850 o C show the best electrochemical performance. Highlights: → A low-temperature reaction route is introduced based on hydroxide precipitation method to synthesize a novel cathode material LiNi 1/3 Co 1/3 Mn 1/3 O 2 . → The charge-discharge tests were performed at higher current as 5 C between 2.5 and 4.5 V. → The discharge capacity of the material is strongly impacted by the reaction temperature. The powders sintered at 850 o C show the best electrochemical performance. -- Abstract: A low-temperature reaction route is introduced based on hydroxide precipitation method to synthesize the cathode material LiNi 1/3 Co 1/3 Mn 1/3 O 2 . The crystal structure and morphology of the prepared powder have been characterized by X-ray diffraction and Scan electron microscope, respectively. The charge-discharge tests were performed between 2.5 and 4.5 V. The discharge capacity of the material is strongly impacted by the reaction temperature. The powders sintered at 850 o C show the best electrochemical performance and the initial discharge capacity is about 160 mAh g -1 at 5 C. Powder X-ray diffraction and Scan electron microscope results reveal that the excellent electrochemical performances should be ascribed to the lower precursor reaction temperature, the lower degree of cation mixing and analogous spherical small particles, which can improve the transfer of Li ions and electrons. All these results indicate that this material has potential application in lithium-ion batteries.

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-02-15

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

Electrochemical behavior of Li/LiV3O8 secondary cells

Science.gov (United States)

Bak, Hyo Rim; Lee, Jae Ha; Kim, Bok Ki; Yoon, Woo Young

2013-03-01

Li/LiV3O8 secondary cells with Li-foil and Li-powder anodes were fabricated, and their electrical properties were compared. Using the powder anode, a cell with an initial discharge capacity of 260 mAh g-1 that could be operated for over 100 cycles was obtained. The porous Li-powder electrode was safely synthesized by pressing an emulsion droplet onto an SUS mesh. A threefold increase in the electrical conductivity of the LiV3O8 cathode was achieved by the addition of carbon using a vibration pot mill. Using the powder anode resulted in 80% capacity retention at the 100th cycle, while that using the foil electrode was 46%; the 1.0 Crate/ 0.1 C-rate capacity ratio also increased from 44% to 60%. A cell employing the LiV3O8-carbon composite cathode showed better electrical performance, a capacity retention of 90% after 50 cycles, and an increase in rate capacity ratio. The crystal structure and morphology of the LiV3O8-C composite were investigated by x-ray diffraction and scanning electron microscopy.

Superparamagnetic behavior of nanosized Co{sub 0.2}Zn{sub 0.8}Fe{sub 2}O{sub 4} synthesized by a flow rate controlled chemical coprecipitation method

Energy Technology Data Exchange (ETDEWEB)

Dey, S. [Department of Physics, Jadavpur University, Kolkata 700032 (India); Dey, S.K. [Department of Physics, Jadavpur University, Kolkata 700032 (India); Department of Physics, NITMAS, 24 Pargana(s) 743368 (India); Majumder, S. [Department of Physics, Jadavpur University, Kolkata 700032 (India); Saha Institute of Nuclear Physics, 1/AF Bidhannagar, Kolkata 700064 (India); Poddar, A.; Dasgupta, P.; Banerjee, S. [Saha Institute of Nuclear Physics, 1/AF Bidhannagar, Kolkata 700064 (India); Kumar, S., E-mail: kumars@phys.jdvu.ac.in [Department of Physics, Jadavpur University, Kolkata 700032 (India)

2014-09-01

We have studied the structural, microstructural and magnetic properties of nanosized (∼20 nm) Co{sub 0.2}Zn{sub 0.8}Fe{sub 2}O{sub 4} synthesized by a flow rate controlled coprecipitation method. The phase purity and crystallinity of the sample have been confirmed by powder X-ray diffraction and high resolution transmission electron microscopic studies. According to the results of dc magnetic measurements the sample exhibits superparamagnetic behavior above 70 K due to its nanometric size. This has been corroborated by Mössbauer spectroscopic study at 300 K. The infield Mössbauer spectroscopic study indicates that the sample behaves ferrimagnetically at 10 K and it possesses equilibrium cation distribution. The saturation magnetization of the sample (M{sub SAT}∼32 emu g{sup −1} at 300 K) is substantially lower than its bulk counterpart (M{sub SAT}=80 emu g{sup −1}) but higher than those having same composition synthesized by the conventional coprecipitation method. This has been attributed to finite size and spin canting effects as well as good crystalline character and bulk like equilibrium cation distribution of the sample. We have shown that the flow rate controlled coprecipitation method can produce nanosized ferrites with very good crystalline order and equilibrium cation distribution but they exhibit reduction of magnetization, magnetic order and ordering temperature compared to their bulk counterparts due to spin canting effect and finite size effect.

Room-temperature ferromagnetism in pure and Co doped CeO2 powders

International Nuclear Information System (INIS)

Wen Qiye; Zhang Huaiwu; Song Yuanqiang; Yang Qinghui; Zhu Hao; Xiao, John Q

2007-01-01

We report the room-temperature (RT) ferromagnetism (FM) observed in pure and Co doped CeO 2 powder. An insulating nonmagnetic CeO 2 single crystal, after grinding into fine powder, shows an RT-FM with a small magnetization of 0.0045 emu g -1 . However, the CeO 2 powder became paramagnetic after oxygen annealing, which strongly suggests an oxygen vacancy meditated FM ordering. Furthermore, by doping Co into CeO 2 powder the FM can significantly enhance through a F-centre exchange (FCE) coupling mechanism, in which both oxygen vacancies and magnetic ions are involved. As the Co content increases, the FM of Co doped CeO 2 initially increases to a maximum 0.47 emu g -1 , and then degrades very quickly. The complex correlation between the Co content and saturation magnetization was well interpreted by supposing the coexistence of three subsets of Co ions in CeO 2 . Our results reveal that the large RT-FM observed in Co doped CeO 2 powder originates from a combination effect of oxygen vacancies and transition metal doping

CH3 NH3 PbI3 and HC(NH2 )2 PbI3 Powders Synthesized from Low-Grade PbI2 : Single Precursor for High-Efficiency Perovskite Solar Cells.

Science.gov (United States)

Zhang, Yong; Kim, Seul-Gi; Lee, Do-Kyoung; Park, Nam-Gyu

2018-05-09

High-efficiency perovskite solar cells are generally fabricated by using highly pure (>99.99 %) PbI 2 mixed with an organic iodide in polar aprotic solvents. However, the use of such an expensive chemical may impede progress toward large-scale industrial applications. Here, we report on the synthesis of perovskite powders by using inexpensive low-grade (99 %) PbI 2 and on the photovoltaic performance of perovskite solar cells prepared from a powder-based single precursor. Pure APbI 3 [A=methylammonium (MA) or formamidinium (FA)] perovskite powders were synthesized by treating low-grade PbI 2 with MAI or FAI in acetonitrile at ambient temperature. The structural phase purity was confirmed by X-ray diffraction. The solar cell with a MAPbI 3 film prepared from the synthesized perovskite powder demonstrated a power conversion efficiency (PCE) of 17.14 %, which is higher than the PCE of MAPbI 3 films prepared by using both MAI and PbI 2 as precursors (PCE=13.09 % for 99 % pure PbI 2 and PCE=16.39 % for 99.9985 % pure PbI 2 ). The synthesized powder showed better absorption and photoluminescence, which were responsible for the better photovoltaic performance. For the FAPbI 3 powder, a solution with a yellow non-perovskite δ-FAPbI 3 powder synthesized at room temperature was found to lead to a black perovskite film, whereas a solution with the black perovskite α-FAPbI 3 powder synthesized at 150 °C was not transformed into a black perovskite film. The α↔δ transition between the powder and film was assumed to correlate with the difference in the iodoplumbates in the powder-dissolved solution. An average PCE of 17.21 % along with a smaller hysteresis [ΔPCE=PCE reverse -PCE forward )=1.53 %] was demonstrated from the perovskite solar cell prepared by using δ-FAPbI 3 powder; this PCE is higher than the average PCE of 17.05 % with a larger hysteresis (ΔPCE=2.71 %) for a device based on a conventional precursor solution dissolving MAI with high

Synthesis of LiNi0.8Co0.1Mn0.1O2 cathode material by chloride co-precipitation method

Institute of Scientific and Technical Information of China (English)

李灵均; 李新海; 王志兴; 伍凌; 郑俊超; 李金辉

2010-01-01

LiNi0.8Co0.1Mn0.1O2 was prepared by a chloride co-precipitation method and characterized by thermogravimetric analysis, X-ray diffractometry with Rietveld refinement,electron scanning microscopy and electrochemical measurements.Effects of lithium ion content and sintering temperature on physical and electrochemical performance of LiNi0.8Co0.1Mn0.1O2 were also investigated. The results show that the sample synthesized at 750℃with 105%lithium content has fine particle sizes around 200 nm and homogenous sizes distribution.The initial discharge capacity for the powder is 184 mA·h/g between 2.7 and 4.3 V at 0.1C and room temperature.

Carbothermal preparation of Si2N2O powder

NARCIS (Netherlands)

Bolech, M.; Metselaar, R.; van Dijen, F.K.; Blömer, F.; With, de G.; Ramaekers, P.P.J.; Vincenzini, P.

1987-01-01

At temperatures 1400 - 1450 °C silicon oxynitride powder can be produced from silica/carbon mixtures with a molar ratio 2/3 under a nitrogen flow. The conversion rate is considerably exhanced by the presence of oxide additions like CaO, BaO and SrO, which form a liquid phase with silica at the

Preparation of high-purity ZrSiO4 powder using sol-gel processing and mechanical properties of the sintered body

International Nuclear Information System (INIS)

Mori, T.; Yamamura, H.; Kobayashi, H.; Mitamura, T.

1992-01-01

This paper reports that effects of the concentration of ZrOCl 2 , calcination temperature, heating rate, and the size of secondary particles after hydrolysis on the preparation of high-purity ZrSiO 4 fine powders from ZrOCl 2 :8H 2 O (0.2M to 1.7M) and equimolar colloidal SiO 2 using Sol--gel processing have been studied. Mechanical properties of the sintered ZrSiO 4 from the high-purity ZrSiO 4 powders have been also investigated. Single-phase ZrSiO 4 fine powders were synthesized at 1300 degrees C by forming ZrSiO 4 precursors having a Zr---O---Si bond, which was found in all the hydrolysis solutions, and by controlling a secondary particle size after hydrolysis. The conversion rate of ZrSiO 4 precursor gels to ZrSiO 4 powders from concentrations other than 0.4M ZrOCl 2 ·8H 2 O increased when the heating rate was high, whereupon the crystallization of unreacted ZrO 2 and SiO 2 was depressed and the propagation and increase of ZrSiO 4 nuclei in the gels were accelerated. The density of the ZrSiO 4 sintered bodies, manufactured by firing the ZrSiO 4 compacts at 1600 degrees to 1700 degrees C, was more than 95% of the theoretical density, and the grain size ranged around 2 to 4 μm. The mechanical strength was 320 MPa (room temperature to 1400 degrees C), and the thermal shock resistance was superior to that of mullite and alumina, with fairly high stability at higher temperatures

Sol-gel auto-combustion synthesis and properties of Co2Z-type hexagonal ferrite ultrafine powders

Science.gov (United States)

Liu, Junliang; Yang, Min; Wang, Shengyun; Lv, Jingqing; Li, Yuqing; Zhang, Ming

2018-05-01

Z-type hexagonal ferrite ultrafine powders with chemical formulations of (BaxSr1-x)3Co2Fe24O41 (x varied from 0.0 to 1.0) have been synthesized by a sol-gel auto-combustion technique. The average particle sizes of the synthesized powders ranged from 2 to 5 μm. The partial substitution of Ba2+ by Sr2+ led to the shrinkage of the crystal lattices and resulted in changes in the magnetic sub-lattices, which tailored the static and dynamic magnetic properties of the as-synthesized powders. As the substitution ratio of Ba2+ by Sr2+, the saturation magnetization of the synthesized powders almost consistently increased from 43.3 to 56.1 emu/g, while the real part of permeability approached to a relatively high value about 2.2 owing to the balance of the saturation magnetization and magnetic anisotropy field.

EFFECT OF CUP AND BALL TYPES ON MECHANO-CHEMICAL SYNTHES IS OF Al2O3–TiC NANOCOMPOSITE POWDER

Directory of Open Access Journals (Sweden)

M. Zakeri

2012-07-01

Full Text Available Al2O3–TiC nanocomposite powder was successfully synthesized by ball milling TiO2, Al and graphite powders. Effects of cup and ball type, milling time and annealing were investigated. XRD was used to characterize milled and annealed powders. The morphological and microstructural evolutions were studied by SEM and TEM. Results showed that the formation of this composite begins after 20 h and completes after 35 h of milling with stainless steel cup and balls. In contrast, there is no reaction during milling (up to 80 h with ZrO2 cup and balls. Fe and ZrO2 were the major impurities introduced during milling with stainless steel and ZrO2 cups, respectively. The Fe impurity was removed by leaching in 3HCl·HNO3 solution for 4 days. Mean grain size less than 7 nm was achieved at the end of milling. In spite of grain growth, this composite maintained its nanocrystalline nature after annealing at 1000°C.

NiTiO3 powders obtained by polymeric precursor method: Synthesis and characterization

International Nuclear Information System (INIS)

Lopes, K.P.; Cavalcante, L.S.; Simoes, A.Z.; Varela, J.A.; Longo, E.; Leite, E.R.

2009-01-01

Nickel titanate (NiTiO 3 ) powders were synthesized by the polymeric precursor method after thermal treatment at different temperatures for 2 h in air atmosphere. The decomposition of the precursors was monitored by differential scanning calorimetry and thermogravimetric analysis. The NiTiO 3 powders presented a reduction in the specific surface area and increase of the average particle size with the evolution of the temperature. The structural evolution of NiTiO 3 phase was accompanied by X-ray diffraction and Fourier transform Raman spectroscopy. By scanning electron microscopy was revealed the agglomerated nature of very fine particles of NiTiO 3 powders annealed from 600 to 1000 deg. C

Fabrication and properties of La2-xGdxHf2O7 transparent ceramics

International Nuclear Information System (INIS)

Wang, Zhengjuan; Zhou, Guohong; Zhang, Fang; Qin, Xianpeng; Ai, Jianping; Wang, Shiwei

2016-01-01

La 2-x Gd x Hf 2 O 7 (x=0–2.0) transparent ceramics were fabricated through vacuum sintering from nano-powders synthesized by a simple combustion method. The phase composition of the powders and final ceramics, the in-line transmittance, microstructures and density of the ceramics were investigated. With the increasing of Gd content, the ceramics maintained the cubic pyrochlore structure, and the lattice parameters decreased, whilst the densities increased linearly. All the ceramics were transparent. The highest in-line transmittance was 76.1% at 800 nm (x=1.2). With high density (7.91–8.88 g/cm 3 ) and effective atomic number, some of the La 2-x Gd x Hf 2 O 7 (x=0–2.0) transparent ceramics are promising candidates for scintillator hosts. - Highlights: • A new series of La 2-x Gd x Hf 2 O 7 transparent ceramics were fabricated by vacuum sintering using combustion-synthesized powders. • All the ceramics are transparent and the in-line transmittance can reach to 76.1% at 800 nm when x=1.2. • The Gd content has effects on the crystal structure, in-line transmittance, microstructures and densities of the ceramics. • With high density (7.91~8.88 g/cm3) and effective atomic number, some of the La2-xGdxHf2O7 transparent ceramics are promising candidates for scintillator hosts.

In situ preparation of (TiB + TiC + Nd2O3)/Ti composites by powder metallurgy

International Nuclear Information System (INIS)

Lu Junqiang; Qin Jining; Lu Weijie; Liu Yang; Gu Jiajun; Zhang Di

2009-01-01

Titanium matrix composites reinforced with multiple ceramic particulates TiB, TiC and Nd 2 O 3 were prepared by powder metallurgy utilizing the chemical reactions among Ti, B 4 C, NdB 6 and oxygen in Ti powder. The thermodynamic feasibility of the in situ reaction has been calculated. The phases were identified by X-ray diffraction (XRD). The result shows that multiple ceramic phases TiB, TiC and Nd 2 O 3 particulates have been synthesized. The microstructures were examined by means of optical microscopy (OM), scanning electron microscopy (SEM), backscattered electron microscopy and transmission electron microscope (TEM). The results show that the reinforcements are distributed uniformly in the matrix alloy and grow in different shapes. TiB grows in needle shape; TiC and Nd 2 O 3 grow in equiaxed or near-equiaxed shapes. The addition of NdB 6 is beneficial to grain refinement, grain-boundary purification and porosity reduction

Hydrothermal synthesis and enhanced photocatalytic activity of mixed-phase TiO2 powders with controllable anatase/rutile ratio

Science.gov (United States)

Wang, Qi; Qiao, Zhi; Jiang, Peng; Kuang, Jianlei; Liu, Wenxiu; Cao, Wenbin

2018-03-01

In this study, mixed-phase TiO2 powders were novelly synthesized via a facile and mild hydrothermal method without any post-heat treatment. TiOSO4 and peroxide titanic acid (PTA) were used as inorganic titanium sources, while no special solvent or additive were introduced. The XRD and TEM results showed the mixed-phase TiO2 powders were composed of anatase and rutile phases, and the PTA sol played an important role on forming the rutile nucleus. The proportion of rutile in the mixed-phase TiO2 could be easily controlled in the range of 0%-70.5% by changing the amount of PTA sol used in the synthesis process. The UV-Visible absorption spectra indicated the prepared mixed-phase TiO2 showed enhanced visible light absorption with the increase of rutile ratio. The photodegradation experiments revealed the mixed-phase TiO2 exhibited the best photocatalytic activity at the rutile ratio of 41.5%, while a higher or lower rutile ratio both resulted in the decrease of photocatalytic activity.

Electrical and optical properties of thermally-evaporated thin films from A{sub 2}[TiO(C{sub 2}O{sub 4}){sub 2}] (A = K, PPh{sub 4}) and 1,8-dihydroxyanthraquinone

Energy Technology Data Exchange (ETDEWEB)

Carbia-Ruelas, E. [Coordinacion de Ingenieria Mecatronica. Facultad de Ingenieria, Universidad Anahuac Mexico Norte. Avenida Universidad Anahuac 46, Col. Lomas Anahuac, 52786, Huixquilucan (Mexico); Sanchez-Vergara, M.E., E-mail: elena.sanchez@anahuac.mx [Coordinacion de Ingenieria Mecatronica. Facultad de Ingenieria, Universidad Anahuac Mexico Norte. Avenida Universidad Anahuac 46, Col. Lomas Anahuac, 52786, Huixquilucan (Mexico); Garcia-Montalvo, V. [Instituto de Quimica, Universidad Nacional Autonoma de Mexico. Circuito Exterior, Ciudad Universitaria, 04510, Mexico, D. F (Mexico); Morales-Saavedra, O.G. [Centro de Ciencias Aplicadas y Desarrollo Tecnologico, Universidad Nacional Autonoma de Mexico, CCADET-UNAM. A. P. 70-186, Coyoacan, 04510, Mexico, D. F (Mexico); Alvarez-Bada, J.R. [Coordinacion de Ingenieria Mecatronica. Facultad de Ingenieria, Universidad Anahuac Mexico Norte. Avenida Universidad Anahuac 46, Col. Lomas Anahuac, 52786, Huixquilucan (Mexico)

2011-02-01

In this work, the synthesis of molecular materials formed from A{sub 2}[TiO(C{sub 2}O{sub 4}){sub 2}] (A = K, PPh4) and 1,8 dihydroxyanthraquinone is reported. The synthesized materials were characterized by atomic force microscopy (AFM), infrared (IR) and ultraviolet-visible (UV-vis) spectroscopy. IR spectroscopy showed that the molecular-material thin-films, deposited by vacuum thermal evaporation, exhibit the same intra-molecular vibration modes as the starting powders, which suggests that the thermal evaporation process does not alter the initial chemical structures. Electrical transport properties were studied by dc conductivity measurements. The electrical activation energies of the complexes, which were in the range of 0.003-1.16 eV, were calculated from Arrhenius plots. Optical absorption studies in the wavelength range of 190-1090 nm at room temperature showed that the optical band gaps of the thin films were around 1.9-2.3 eV for direct transitions Eg{sub d}. The cubic NLO effects were substantially enhanced for materials synthesized from K{sub 2}[TiO(C{sub 2}O{sub 4}){sub 2}], where {chi}{sup (3)} (-3{omega}; {omega}, {omega}, {omega}) values in the promising range of 10{sup -12} esu have been evaluated.

Sintering behaviour of CeO2-Gd2O3 powders prepared by the oxalate coprecipitation method

International Nuclear Information System (INIS)

Duran, P.; Jurado, J.R.; Moure, C.

1993-01-01

The powder and compact characteristics as well as the sintering behaviour of two CeO 2 -Gd 2 O 3 compositions prepared by the oxalate coprecipitation method are studied as a function of the powder particle size and the pore-size distribution in the powder compacts. Shrinkage was measured at a constant heating rate and the results are compared with those obtained by isothermal sintering experiments. Grain growth and microstructural development on sintered samples were studied. (orig.)

In situ synthesis of Ti{sub 2}AlC–Al{sub 2}O{sub 3}/TiAl composite by vacuum sintering mechanically alloyed TiAl powder coated with CNTs

Energy Technology Data Exchange (ETDEWEB)

Wang, Jian [Department of Materials Science and Engineering of Tianjin University, Tianjin Key Laboratory of Composite and Functional Materials, Tianjin 300072 (China); Zhao, Naiqin, E-mail: nqzhao@tju.edu.cn [State Key Laboratory of Hydraulic Engineering Simulation and Safety, Tianjin (China); Department of Materials Science and Engineering of Tianjin University, Tianjin Key Laboratory of Composite and Functional Materials, Tianjin 300072 (China); Nash, Philip [Thermal Processing Technology Center, Illinois Institute of Technology, IL (United States); Liu, Enzuo; He, Chunnian; Shi, Chunsheng; Li, Jiajun [Department of Materials Science and Engineering of Tianjin University, Tianjin Key Laboratory of Composite and Functional Materials, Tianjin 300072 (China)

2013-11-25

Highlights: •Using zwitterionic surfactant to enhance the dispersion of the CNTs on the powder surface. •CNTs as carbon source decreased the formation temperature of Ti{sub 2}AlC. •Al{sub 2}O{sub 3} was generated in situ from the oxygen atoms introduced in the drying procedure. •Nanosized Ti{sub 3}Al was precipitated at 1250 °C and distribute in the TiAl matrix homogeneously. •Ti{sub 2}AlC–Al{sub 2}O{sub 3}/TiAl composite was synthesized in situ by sintering pre-alloy Ti–Al coated with CNTs. -- Abstract: Bulk Ti{sub 2}AlC–Al{sub 2}O{sub 3}/TiAl composites were in situ synthesized by vacuum sintering mechanically alloyed Ti–50 at.% Al powders coated with carbon nanotubes (CNTs). The pre-alloyed Ti–50 at.% Al powder was obtained by ball milling Ti and Al powders. The multi-walled carbon nanotubes as the carbon resource were covered on the surface of the pre-alloyed powders by immersing them into a water solution containing the CNTs. A zwitterionic surfactant was used to enhance the dispersion of the CNTs on the powder surface. The samples were cold pressed and sintered in vacuum at temperatures from 950 to 1250 °C, respectively. The results show that the reaction of forming Ti{sub 2}AlC can be achieved below 950 °C, which is 150 °C lower than in the Ti–Al–TiC system and 250 °C lower than for the Ti–Al–C system due to the addition of CNTs. Additionally, the reinforcement of Al{sub 2}O{sub 3} particles was introduced in situ in Ti{sub 2}AlC/TiAl by the drying process and subsequent sintering of the composite powders. Dense Ti{sub 2}AlC–Al{sub 2}O{sub 3}/TiAl composites were obtained by sintering at 1250 °C and exhibited a homogeneous distribution of Ti{sub 2}AlC, Al{sub 2}O{sub 3} and precipitated Ti{sub 3}Al particles and a resulting high hardness.

A-Site Deficient (Pr0.6Sr0.4)(1-s)Fe0.8Co0.2O3-delta Perovskites as Solid Oxide Fuel Cell Cathodes

DEFF Research Database (Denmark)

Kammer Hansen, Kent

2009-01-01

Five A-site deficient (Pr0.6Sr0.4)1−sFe0.8Co0.2O3− perovskites (s=0.01, 0.05, 0.10, 0.15, and 0.20) were synthesized using the glycine-nitrate process. The perovskites were characterized with powder X-ray diffraction (XRD), dilatometry, four-point dc conductivity measurements, and electrochemical...... resistance more than 3 times lower than the weakly A-site deficient (Pr0.6Sr0.4)0.99Fe0.8Co0.2O3− perovskite. ©2009 The Electrochemical Society...

Synthesis of MSnO{sub 3} (M = Ba, Sr) nanoparticles by reverse micelle method and particle size distribution analysis by whole powder pattern modeling

Energy Technology Data Exchange (ETDEWEB)

Ahmed, Jahangeer; Blakely, Colin K.; Bruno, Shaun R. [Department of Chemistry, Michigan State University, East Lansing, MI 48824 (United States); Poltavets, Viktor V., E-mail: poltavets@chemistry.msu.edu [Department of Chemistry, Michigan State University, East Lansing, MI 48824 (United States)

2012-09-15

Highlights: ► BaSnO{sub 3} and SrSnO{sub 3} nanoparticles synthesized using the reverse micelle method. ► Particle size and size distribution studied by whole powder pattern modeling. ► Nanoparticles are of optimal size for investigation in dye-sensitized solar cells. -- Abstract: Light-to-electricity conversion efficiency in dye-sensitized solar cells critically depends not only on the dye molecule, semiconducting material and redox shuttle selection but also on the particle size and particle size distribution of the semiconducting photoanode. In this study, nanocrystalline BaSnO{sub 3} and SrSnO{sub 3} particles have been synthesized using the microemulsion method. Particle size distribution was studied by whole powder pattern modeling which confirmed narrow particle size distribution with an average size of 18.4 ± 8.3 nm for SrSnO{sub 3} and 15.8 ± 4.2 nm for BaSnO{sub 3}. These values are in close agreement with results of transmission electron microscopy. The prepared materials have optimal microstructure for successive investigation in dye-sensitized solar cells.

Synthesis and investigation of uranyl molybdate UO2MoO4

International Nuclear Information System (INIS)

Nagai, Takayuki; Sato, Nobuaki; Kitawaki, Shin-ichi; Uehara, Akihiro; Fujii, Toshiyuki; Yamana, Hajimu; Myochin, Munetaka

2013-01-01

In order to examine easily synthetic conditions of uranyl molybdate, UO 2 MoO 4 , used for the reprocessing process study of spent nuclear oxide fuels in alkaline molybdate melts, the uranium molybdate compounds were produced from U 3 O 8 powder and anhydrous MoO 3 reagent. The results of having investigated them in solid state by using X-ray diffractometry and Raman spectrometry, it was confirmed that UO 2 MoO 4 could be synthesized by heating mixed powder of U 3 O 8 and MoO 3 with stoichiometric mole ratio at 770 °C for 4 h under air atmosphere. Moreover, adding this UO 2 MoO 4 into Li 2 MoO 4 -Na 2 MoO 4 eutectic melt, most of the dissolved uranium species in the melt were observed as hexa–valent uranyl ions by absorption spectrophotometry

Characteristics and properties of a novel in situ method of synthesizing mesoporous TiO{sub 2} nanopowders by a simple coprecipitation process without adding surfactant

Energy Technology Data Exchange (ETDEWEB)

Yeh, Shang-Wei [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80782, Taiwan (China); Department of Life Science, National University of Kaohsiung, 700 Kaohsiung University Road, Kaohsiung 811, Taiwan (China); Ko, Horng-Huey [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80782, Taiwan (China); Chiang, Hsiu-Mei [Department of Cosmeceutics, China Medical University, 91 Hsueh-Shih Road, Taichung 40402, Taiwan (China); Chen, Yen-Ling, E-mail: yelichen@kmu.edu.tw [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80782, Taiwan (China); Lee, Jian-Hong [Clean Energy and Eco-Technology Center, Industrial Technology Research Institute, 8 Gongyan Road, Tainan 734, Taiwan (China); Wen, Chiu-Ming [Department of Life Science, National University of Kaohsiung, 700 Kaohsiung University Road, Kaohsiung 811, Taiwan (China); Wang, Moo-Chin, E-mail: mcwang@kmu.edu.tw [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80782, Taiwan (China)

2014-11-15

Highlights: • The TiO{sub 2} precursor powder contained anatase and 19.5% NH{sub 4}Cl. • Mesoporous anatase TiO{sub 2} nanopowders were successfully synthesized. • Uncalcined precursor powder contained the phases of type I NH{sub 4}Cl and anatase TiO{sub 2}. • Anatase size increases from 3.3 to 14.3 nm when calcined at 473–773 K for 2 h. • The average pore size between 3.80 and 14.0 nm when calcined between 473 and 773 K. - Abstract: In situ synthesis of mesoporous TiO{sub 2} nanopowders using titanium tetrachloride (TiCl{sub 4}) and NH{sub 4}OH as initial materials has been successfully fabricated by a coprecipitation process without the addition of surfactant. Characteristics and properties of the mesoporous TiO{sub 2} nanopowders were investigated using differential scanning calorimetry/thermogravimetry (DSC/TG), X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET) and Barrent–Joyner–Halenda (BJH) analyses, transmission electron microscopy (TEM), selected area electron diffraction (SAED) and high resolution TEM (HRTEM). The results of TG and XRD showed that the NH{sub 4}Cl decomposed between 513 and 673 K. XRD results showed that the anatase TiO{sub 2} only contained a single phase when the calcination temperature of the precursor powder was less than 673 K. Whereas phases of anatase and rutile TiO{sub 2} coexist after calcining at 773 K for 2 h. The crystalline size of the anatase and rutile TiO{sub 2} was 14.3 and 26.6 nm, respectively, when the precursor powder was calcined at 773 K for 2 h. The BET and BJH results showed a significant increase in surface area and pore volumes when the NH{sub 4}Cl was completely decomposed. The maximum values of BET specific surface area and volume were 172.8 m{sup 2}/g and 0.392 cm{sup 3}/g, respectively. The average pore sizes when calcination was at 473 and 773 K for 2 h were 3.8 and 14.0 nm, respectively.

Determination of U{sub 3}O{sub 8} in UO{sub 2} by infrared spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Silva, Liliane Aparecida; Lameiras, Fernando Soares; Santos, Ana Maria Matildes dos; Ferraz, Wilmar Barbosa; Barbosa, Joao Batista Santos, E-mail: lasfisica@gmail.com, E-mail: sl@cdtn.br, E-mail: amms@cdtn.br, E-mail: ferrazw@cdtn.br, E-mail: jbsb@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN), Belo Horizonte, MG (Brazil)

2017-01-15

The oxygen-uranium (O-U) system has various oxides, such as UO{sub 2}, U{sub 4}O{sub 9}, U{sub 3}O{sub 8}, and UO{sub 3}. Uranium dioxide is the most important one because it is used as nuclear fuel in nuclear power plants. UO{sub 2} can have a wide stoichiometric variation due to excess or deficiency of oxygen in its crystal lattice, which can cause significant modifications of its proprieties. O/U relation determination by gravimetry cannot differentiate a stoichiometric deviation from contents of other uranium oxides in UO{sub 2}. The presence of other oxides in the manufacturing of UO{sub 2} powder or sintered pellets is a critical factor. Fourier Transform Infrared Spectroscopy (FTIR) was used to identify U{sub 3}O{sub 8} in samples of UO{sub 2} powder. UO{sub 2} can be identified by bands at 340 cm{sup -1} and 470 cm{sup -1}, and U{sub 3}O{sub 8} and UO{sub 3} by bands at 735 cm{sup -1}, 910 cm{sup -1}, respectively. The methodology for sample preparation for FTIR spectra acquisition is presented, as well as the calibration for quantitative measurement of U{sub 3}O{sub 8} in UO{sub 2}. The content of U{sub 3}O{sub 8} in partially calcined samples of UO{sub 2} powder was measured by FTIR with good agreement with X-rays diffractometry (XRD). (author)

Kinetics of CO Oxidation over Unloaded and Pd-Loaded α-Fe2O3 Spherical Submicron Powder Catalysts: Photoacoustic Investigations at Low Pressure

Directory of Open Access Journals (Sweden)

Joong-Seok Roh

2018-02-01

Full Text Available In this study, α-Fe2O3 spherical particles with an average diameter of approximately 200 nm were synthesized by a solvothermal method for use as both a catalyst and medium for a Pd catalyst. The kinetics of CO oxidation over powders of α-Fe2O3 spherical particles and 14 wt % Pd/α-Fe2O3 spherical particles were measured in a static reactor by using a CO2 laser-based photoacoustic technique. The total pressure was fixed at 40 Torr for the CO/O2/N2 mixture for temperatures in the range of 225–350 °C. The variation in the CO2 photoacoustic signal with the CO2 concentration during CO oxidation was recorded as a function of time, and the CO2 photoacoustic data at the early reaction stage was used to estimate the rates of CO2 formation. Based on plots of ln(rate vs. 1/T, apparent activation energies were calculated as 13.4 kcal/mol for the α-Fe2O3 submicron powder and 13.2 kcal/mol for the 14 wt % Pd/α-Fe2O3 submicron powder. Reaction orders with respect to CO and O2 were determined from the rates measured at various partial pressures of CO and O2 at 350 °C. The zero-order of the reaction with respect to Po2 was observed for CO oxidation over α-Fe2O3 submicron powder, while 0.48 order to Po2 was observed for CO oxidation over Pd/α-Fe2O3 submicron powder. The partial orders with respect to PCO were determined as 0.58 and 0.54 for the α-Fe2O3, and the Pd/α-Fe2O3 submicron powders, respectively. The kinetic results obtained from both catalysts were compared with those for the α-Fe2O3 fine powder catalysts and were used to understand the reaction mechanism.

Optical properties and visible-light-driven photocatalytic activity of Bi{sub 8}V{sub 2}O{sub 17} nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Pu, Yinfu; Liu, Ting; Huang, Yanlin [Soochow University, College of Chemistry, Chemical Engineering and Materials Science (China); Chen, Cuili; Kim, Sun Il; Seo, Hyo Jin, E-mail: hjseo@pknu.ac.kr [Pukyong National University, Department of Physics and Interdisciplinary Program of Biomedical, Mechanical & Electrical Engineering (Korea, Republic of)

2015-05-15

Bi{sub 8}V{sub 2}O{sub 17} (4Bi{sub 2}O{sub 3}·V{sub 2}O{sub 5}) nanoparticles with the uniform size of about 50 nm were fabricated through the Pechini method. The crystal structure was investigated by X-ray powder diffraction and the structural refinement. The surface of the as-synthesized samples was characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy (EDX), transmission electron microscopy, and X-ray photoelectron spectroscopy. The optical properties, band structure, and the degradation mechanisms were discussed. The experimental results demonstrate that Bi{sub 8}V{sub 2}O{sub 17} nanoparticles have an efficient visible-light absorption with band-gap energy of 1.85 eV and a direct allowed electronic transition. The photocatalytic activity was evaluated by the photodegradation of the methylene blue (MB) under visible-light irradiation (λ > 420 nm) as a function of time. These results indicate that Bi{sub 8}V{sub 2}O{sub 17} could be a potential photocatalyst driven by visible light. The effective photocatalytic activity was discussed on the base of the crystal structure characteristic.

High-Pressure Synthesis and Characterization of the Ammonium Yttrium Borate (NH4)YB8O14.

Science.gov (United States)

Schmitt, Martin K; Podewitz, Maren; Liedl, Klaus R; Huppertz, Hubert

2017-11-20

The first high-pressure yttrium borate (NH 4 )YB 8 O 14 was synthesized at 12.8 GPa/1300 °C using a Walker-type multianvil module. The compound crystallizes in the orthorhombic space group Pnma (no. 62) with the lattice parameters a = 17.6375(9), b = 10.7160(5), and c = 4.2191(2) Å. (NH 4 )YB 8 O 14 constitutes a novel structure type but exhibits similarities to the crystal structure of β-BaB 4 O 7 . X-ray single-crystal and powder diffraction, EDX, vibrational spectroscopy as well as quantum chemical calculations were used to characterize (NH 4 )YB 8 O 14 .

A novel method for stoichiometric reduction of (U{sub 3}O{sub 8},PuO{sub 2}) and its controlled oxidation using microwave

Energy Technology Data Exchange (ETDEWEB)

Singh, G., E-mail: gitendars@barctara.gov.in [Advanced Fuel Fabrication Facility (AFFF), Bhabha Atomic Research Centre, Tarapur, 401 502 (India); Kumar, Pradeep [Integrated Fuel Fabrication Facility, Bhabha Atomic Research Centre, Mumbai, 400 085 (India); Aher, S.; Purohit, P.; Khot, P.M. [Advanced Fuel Fabrication Facility (AFFF), Bhabha Atomic Research Centre, Tarapur, 401 502 (India); Prakash, Amrit [Radio-Metallurgy Division, Bhabha Atomic Research Centre, Mumbai, 400 085 (India); Das, D.K.; Behere, P.G.; Afzal, Mohd [Advanced Fuel Fabrication Facility (AFFF), Bhabha Atomic Research Centre, Tarapur, 401 502 (India)

2016-10-15

We report a process for stoichiometric reduction of U{sub 3}O{sub 8} and (U{sub 3}O{sub 8},PuO{sub 2}) mixed oxide powders using an indigenously developed 2.4 GHz microwave processing system. The process parameters were optimized by interpreting reduction kinetic curves at a temperature which is 150 °C lower than the conventional reduction. The process improved the sinterability of the powder which was evaluated in terms of average particle size, BET specific surface area and bulk density. A quick method for controlled oxidation of the reduced powder to incorporate a controlled amount of hyper-stoichiometry was demonstrated by modifying the same reduction process. The percent reduction was measured experimentally using O:(U + Pu) ratio. The X-ray diffraction analysis confirmed the various phases present. The process is novel considering shorter processing cycle, lower temperature processing, improved powder properties, energy efficiency and cost effectiveness. - Highlights: • A process for stoichiometric reduction of (U{sub 3}O{sub 8},PuO{sub 2}) was demonstrated using 2.4 GHz microwave. • A simple and quick method for obtaining controlled hyper-stoichiometry in the reduced powder was successfully demonstrated. • The process is novel relative to conventional methods in terms of time and energy economy and sinter-activity.

Cathodoluminescence study of SnO{sub 2} powders aimed for gas sensor applications

Energy Technology Data Exchange (ETDEWEB)

Korotcenkov, G. [Technical University of Moldova, Chisinau (Moldova, Republic of)]. E-mail: ghkoro@yahoo.com; Nazarov, M. [Technical University of Moldova, Chisinau (Moldova, Republic of); Zamoryanskaya, M.V. [A.F. Ioffe Physical Technical Institute, RAS, St. Petersburg, Russia (Russian Federation); Ivanov, M. [Technical University of Moldova, Chisinau (Moldova, Republic of); Cirera, A. [EME/CERMAE. Dep. Elect., University of Barcelona, Barcelona (Spain); Shimanoe, K. [Kyushu University, Kasuga-shi, Fukuoka (Japan)

2006-06-15

In this paper we report on cathodoluminescence (CL) spectra of SnO{sub 2} powders, synthesized using the wet chemical route. The analysis of influence of the modes of calcination (T {sub an}-450-800 deg. C), and doping by both Pd and Pt (0.01-10.0 wt.%) on CL spectra was made. It was found that the measurement of CL spectra could be an effective research method of nanostructured metal oxides, aimed for gas sensor applications. It was established that in nanocrystalline SnO{sub 2} the same system of energy levels, associated with radiative recombination, as in single crystalline and polycrystalline SnO{sub 2}, is retained. It was found that doping by both Pd and Pt modifies the structural properties of SnO{sub 2} grains. Also, there is an optimum doping; near 0.1-0.2 wt.%, at which a maximum intensity of cathodoluminescence is reached. It was concluded that for low concentrations of both Pd and Pt additives in SnO{sub 2} an improvement of the material's crystal structure is promoted, and is associated with a decrease in the non-radiating recombination rate.

Enhanced microwave absorption properties of MnO{sub 2} hollow microspheres consisted of MnO{sub 2} nanoribbons synthesized by a facile hydrothermal method

Energy Technology Data Exchange (ETDEWEB)

Wang, Yan; Han, Bingqian; Chen, Nan; Deng, Dongyang; Guan, Hongtao [Department of Materials Science and Engineering, Yunnan University, 650091, Kunming (China); Wang, Yude, E-mail: ydwang@ynu.edu.cn [Department of Materials Science and Engineering, Yunnan University, 650091, Kunming (China); Yunnan Province Key Lab of Micro-Nano Materials and Technology, Yunnan University, 650091, Kunming (China)

2016-08-15

MnO{sub 2} hollow microspheres consisted of nanoribbons were successfully fabricated via a facile hydrothermal method with SiO{sub 2} sphere templates. The crystal structure, morphology and microwave absorption properties in X and Ku band of the as-synthesized samples were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and a vector network analyzer. The results show that the three-dimensional (3D) hollow microspheres are assembled by ultra thin and narrow one-dimensional (1D) nanoribbons. A rational process for the formation of hollow microspheres is proposed. The 3D MnO{sub 2} hollow microspheres possess improved dielectric and magnetic properties than the 1D nanoribbons prepared by the same procedures with the absence of SiO{sub 2} hard templates, which are closely related to their special nanostructures. The MnO{sub 2} microspheres also show much better microwave absorption properties in X (8–12 GHz) and Ku (12–18 GHz) microwave band compared with 1D MnO{sub 2} nanoribbons. The minimum reflection loss of −40 dB for hollow microsphere can be observed at 14.2 GHz and reflection loss below −10 dB is 3.5 GHz with a thickness of only 4 mm. The possible mechanism for the enhanced microwave absorption properties is also discussed. - Graphical abstract: MnO{sub 2} hollow microspheres composed of nanoribbons show the excellent microwave absorption properties in X and Ku band. - Highlights: • MnO{sub 2} hollow microspheres consisted of MnO{sub 2} nanoribbons were successfully prepared. • MnO{sub 2} hollow microspheres possess good microwave absorption performances. • The excellent microwave absorption properties are in X and Ku microwave band. • Electromagnetic impedance matching is great contribution to absorption properties.

Structural and optical studies of Mg doped nanoparticles of chromium oxide (Cr2O3) synthesized by co-precipitation method

Science.gov (United States)

Singh, Jarnail; Verma, Vikram; Kumar, Ravi

2018-04-01

We present here the synthesization, structural and optical studies of Mg doped nanoparticles of Chromium oxide (Cr2O3) prepared using co-precipitation method. These samples were characterized using powder X-ray diffraction (XRD), Field emission scanning electron microscopy (FESEM), Raman spectroscopy and UV-Vis spectroscopy techniques. We have demonstrated that there is negligible change in optical band gap with the Mg doping. The prepared Cr2O3 nanoparticles are spherical in shape, but they are transformed into platelets when doped with Mg. The XRD studies reveal that the Mg doping in Cr2O3 doesn't affect the structure of Chromium oxide (Cr2O3).

Characterization of mechano-thermally synthesized Curie temperature-adjusted La0.8Sr0.2MnO3 nanoparticles coated with (3-aminopropyl) triethoxysilane

International Nuclear Information System (INIS)

Salili, S.M.; Ataie, A.; Barati, M.R.; Sadighi, Z.

2015-01-01

This research aimed to synthesize nanostructured strontium-doped lanthanum manganite, La 0.8 Sr 0.2 MnO 3 (LSMO), with its Curie temperature (T c ) adjusted to the therapeutic range, through a mechanothermal route. In order to investigate the effect of heat treatment temperature and duration on the resulting crystallite size, morphology, magnetic behavior and Curie temperature, the starting powder mixture was milled in a planetary ball mill before being subsequently heat treated at distinct temperatures for different time lengths. The composition, morphology, and magnetic behavior were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED) and vibrating sample magnetometer (VSM). In addition, magnetic properties were further investigated using an alternating current (AC) susceptometer and thermo-magnetic analyzer. 20 h of milling produced a crystallite size reduction leading to a decrease in the heat treatment temperature of LSMO synthesis to 800 °C. Moreover, SEM analysis has shown the morphology of a strong agglomeration of fine nanoparticles. HRTEM showed clear lattice fringes of high crystallinity. The mean crystallite and particle size of 20-hour milled sample heat treated at 1100 °C for 10 h are relatively 69 and 100 nm, respectively. The VSM data at room temperature, indicated a paramagnetic behavior for samples heat treated at 800 °C. However, by increasing heat treatment temperature to 1100 °C, LSMO indicates a ferromagnetic behavior with well-adjusted Curie temperature of 320 K, suitable for hyperthermia applications. Also, reentrant spin glass (RSG) behavior has been found in heat treated samples. The particles are coated with (3-aminopropyl) triethoxysilane (APTES) for biocompatibility purposes; Fourier transform infrared spectroscopy (FTIR) and thermo-gravimetric analysis (TGA) are

Determination of the hydrogen positions in the novel barium boroarsenate Ba[B{sub 2}As{sub 2}O{sub 8}(OH){sub 2}] by combined single crystal X-ray and powder neutron investigations

Energy Technology Data Exchange (ETDEWEB)

Lieb, Alexandra [School of Chemistry, University of Southampton (United Kingdom); Fakultaet fuer Verfahrens- und Systemtechnik, Lehrstuhl fuer Technische Chemie, Otto-von-Guericke-Universitaet, Magdeburg (Germany); Weller, Mark T. [School of Chemistry, University of Southampton (United Kingdom); Department of Chemistry, University of Bath (United Kingdom)

2017-11-17

The boroarsenate Ba[B{sub 2}As{sub 2}O{sub 8}(OH){sub 2}] was obtained by the reaction of NH{sub 4}H{sub 2}AsO{sub 4}, B(OH){sub 3} and BaBr{sub 2}.2H{sub 2}O in the melt. Ba[B{sub 2}As{sub 2}O{sub 8}(OH){sub 2}] was obtained as thin colorless needles, together with spherical crystals of BAsO{sub 4} as by-product, grown on a pellet of Ba[BAsO{sub 5}]. The products could be separated mechanically. For neutron scattering experiments a sample was prepared with {sup 11}B(OH){sub 3} as a starting material. The crystal structure of Ba[B{sub 2}As{sub 2}O{sub 8}(OH){sub 2}] was determined by single-crystal X-ray diffraction and exhibits a layer structure with an unprecedented layer topology. The exact positions of the hydrogen atoms were determined using combined single-crystal X-ray and powder neutron diffraction investigations. Ba[B{sub 2}As{sub 2}O{sub 8}(OH){sub 2}] was further characterized by IR spectroscopy and EDX analysis. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

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

Syntheses, crystal structures, and characterization of two new Tl{sup +}-Cu{sup 2+}-Te{sup 6+} oxides: Tl{sub 4}CuTeO{sub 6} and Tl{sub 6}CuTe{sub 2}O{sub 10}

Energy Technology Data Exchange (ETDEWEB)

Yeon, Jeongho; Kim, Sang-Hwan [Department of Chemistry, University of Houston, 136 Fleming Building, Houston, TX 77204-5003 (United States); Green, Mark A. [Department of Materials Science and Engineering, University of Maryland, College Park, MD, 20742-2115 and NIST Center for Neutron Research, National Institute of Standard and Technology, 100 Bureau Drive, Gaithersburg, MD 20899-6103 (United States); Bhatti, Kanwal Preet; Leighton, C. [Department of Chemical Engineering and Materials Science, University of Minnesota, Minneapolis, MN 55455-0132 (United States); Shiv Halasyamani, P., E-mail: psh@uh.edu [Department of Chemistry, University of Houston, 136 Fleming Building, Houston, TX 77204-5003 (United States)

2012-12-15

Crystals and polycrystalline powders of two new oxide materials, Tl{sub 4}CuTeO{sub 6} and Tl{sub 6}CuTe{sub 2}O{sub 10}, have been synthesized by hydrothermal and solid-state methods. The materials were structurally characterized by single-crystal X-ray diffraction. Tl{sub 4}CuTeO{sub 6} and Tl{sub 6}CuTe{sub 2}O{sub 10} exhibit one dimensional anionic slabs of [CuTeO{sub 6}]{sup 4-} and [CuTe{sub 2}O{sub 10}]{sup 6-}, respectively. Common to both slabs is the occurrence of Cu{sup 2+}O{sub 4} distorted squares and Te{sup 6+}O{sub 6} octahedra. The slabs are separated by Tl{sup +} cations. For Tl{sub 4}CuTeO{sub 6}, magnetic measurements indicate a maximum at {approx}8 K in the temperature dependence of the susceptibility. Low temperature neutron diffraction data confirm no long-range magnetic ordering occurs and the susceptibility was adequately accounted for by fits to a Heisenberg alternating chain model. For Tl{sub 6}CuTe{sub 2}O{sub 10} on the other hand, magnetic measurements revealed paramagnetism with no evidence of long-range magnetic ordering. Infrared, UV-vis spectra, thermogravimetric, and differential thermal analyses are also reported. Crystal data: Tl{sub 4}CuTeO{sub 6}, Triclinic, space group P-1 (No. 2), a=5.8629(8) A, b=8.7848(11) A, c=9.2572(12) A, {alpha}=66.0460(10), {beta}=74.2010(10), {gamma}=79.254(2), V=417.70(9) A{sup 3}, and Z=2; Tl{sub 6}CuTe{sub 2}O{sub 10}, orthorhombic, space group Pnma (No. 62), a=10.8628(6) A, b=11.4962(7) A, c=10.7238(6) A, V=1339.20(13) A{sup 3}, and Z=4. - Graphical Abstract: Two new oxide materials, Tl{sub 4}CuTeO{sub 6} and Tl{sub 6}CuTe{sub 2}O{sub 10}, have been synthesized and characterized. The materials exhibit one dimensional crystal structures consisting of CuO{sub 4} and TeO{sub 6} polyhedra. Highlights: Black-Right-Pointing-Pointer Two New Tl-Te-Cu-oxides have been synthesized and structurally characterized. Black-Right-Pointing-Pointer For Tl{sub 4}CuTeO{sub 6}, magnetic measurements indicate a

Thermal behavior and phase transformation of ZrO2–10%SiO2 precursor powder prepared by a co-precipitation route without adding stability agent

International Nuclear Information System (INIS)

Chu, Hsueh-Liang; Hwang, Weng-Sing; Wang, Cheng-Li; Wang, Moo-Chin; Lee, Kuen-Chan; Huang, Hong-Hsin; Lee, Huey-Er

2014-01-01

Highlights: • The precursor powders contained about 68.3 wt% ZrO 2 , which corresponds to ZrO 2 ·1/8 H 2 O. • The exothermic peak temperature of tetragonal ZrO 2 formation occurred at 1014 K. • The activation energy of ZrO 2 –10%SiO 2 precursors crystallization is 993.7 kJ/mol. • Only the tetragonal ZrO 2 formed when the precursor calcined at 1173–1373 K for 2 h. • As calcined at 1473 K for 2 h, tetragonal ZrO 2 fully converted to monoclinic ZrO 2 . - Abstract: Thermal behavior and phase transformation of ZrO 2 –10%SiO 2 precursor powder prepared by a co-precipitation route without adding stability agent has been studied using different thermal analysis/thermogravimetry (DTA/TG), X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), nano beam electron diffraction (NBED), high-resolution TEM (HRTEM) and energy-dispersive X-ray spectrometer (EDS). The TG results show that four weight loss regions were from 298 to 443 K, 443 to 743 K, 743 to 793 K and 793 to 1400 K. The DTA result shows that the ZrO 2 freeze-dried precursor powders crystallization at 1014 K. The activation energy of 993.7 kJ/mol was obtained for tetragonal ZrO 2 crystallization using a non-isothermal process. The XRD result shows that only a single phase of tetragonal ZrO 2 appears when the freeze-dried precursor powders after calcination between 1173 and 1373 K for 2 h. Moreover, when calcined at 1473 K for 2 h, the phase transformation from tetragonal ZrO 2 fully converted to monoclinic ZrO 2 occurred

Growth Oscillatory Zoning in Erythrite, Ideally Co3(AsO4)2·8H2O: Structural Variations in Vivianite-Group Minerals

Energy Technology Data Exchange (ETDEWEB)

Antao, Sytle M.; Dhaliwal, Inayat

2017-08-01

The crystal structure of an oscillatory zoned erythrite sample from Aghbar mine, Bou Azzer, Morocco, was refined using synchrotron high-resolution powder X-ray diffraction (HRPXRD) data, Rietveld refinement, space group C2/m, and Z = 2. The crystal contains two sets of oscillatory zones that appear to have developed during epitaxial growth. The unit-cell parameters obtained are a = 10.24799(3) Å, b = 13.42490(7) Å, c = 4.755885(8) Å, β = 105.1116(3)°, and V = 631.680(4) Å3. The empirical formula for erythrite, obtained with electron-probe micro-analysis (EPMA), is [Co2.78Zn0.11Ni0.07Fe0.04]Σ3.00(AsO4)2·8H2O. Erythrite belongs to the vivianite-type structure that contains M1O2(H2O)4 octahedra and M22O6(H2O)4 octahedral dimers that are linked by TO4 (T5+ = As or P) tetrahedra to form complex layers parallel to the (010) plane. These layers are connected by hydrogen bonds. The average O>[6] = 2.122(1) Å and average 2–O>[6] = 2.088(1) Å. With space group C2/m, there are two solid solutions: M3(AsO4)2·8H2O and M3(PO4)2·8H2O where M2+ = Mg, Fe, Co, Ni, or Zn. In these As- and P-series, using data from this study and from the literature, we find that their structural parameters evolve linearly with V and in a nearly parallel manner despite of the large difference in size between P5+ (0.170 Å) and As5+ (0.355 Å) cations. Average O>[4], O>[6], and 2–O>[6] distances increase linearly with V. The average O> distance is affected by M atoms, whereas the average O> distance is unaffected because it contains shorter and stronger P–O bonds. Although As- and P-series occur naturally, there is no structural reason why similar V-series vivianite-group minerals do not occur naturally or cannot be synthesized.

Characterization of Bi2/3Cu3Ti4O12 ceramics synthesized by semi-wet route

Directory of Open Access Journals (Sweden)

Pooja Gautam

2016-12-01

Full Text Available Bi2/3Cu3Ti4O12 (BCTO ceramic was synthesized by the semi-wet route using metal nitrate solutions and solid TiO2 powder in a stoichiometric ratio. Fourier transform infrared (FTIR study of BCTO precursor powder and calcined ceramic showed the presence of alcoholic functional groups and the stretching band of Ti-O and Cu-O respectively. X-ray diffraction (XRD, scanning electron microscope (SEM and energy dispersive x-ray spectroscopy (EDX were employed to characterize the structure, surface morphology and purity of the sintered BCTO ceramic respectively. X-ray diffraction study confirmed the single phase formation of BCTO ceramic at 1073 K. The average dimension of grains calculated by SEM and AFM was found to be in the range of 0.73±0.2 µm with clear grain boundaries. Magnetic property was investigated over a wide temperature range 2–300 K at a magnetic field of 7 tesla. The Curie temperature was calculated by zero field cooled (MZFC and field cooled (MFC magnetization at 100 Oe applied field which was found to be 125 K. The sintered BCTO ceramic shows high dielectric constant (ε'=2.9×104 at 323 K and 100 Hz.

Structural and magnetic properties of turmeric functionalized CoFe2O4 nanocomposite powder

International Nuclear Information System (INIS)

Mehran, E; Farjami Shayesteh, S; Sheykhan, M

2016-01-01

The structural and magnetic properties of the synthesized pure and functionalized CoFe 2 O 4 magnetic nanoparticles (NPs) are studied by analyzing the results from the x-ray diffraction (XRD), transmission electron microscopy (TEM), FT–IR spectroscopy, thermogravimetry (TG), and vibrating sample magnetometer (VSM). To extract the structure and lattice parameters from the XRD analysis results, we first apply the pseudo-Voigt model function to the experimental data obtained from XRD analysis and then the Rietveld algorithm is used in order to optimize the model function to estimate the true intensity values. Our simulated intensities are in good agreement with the experimental peaks, therefore, all structural parameters such as crystallite size and lattice constant are achieved through this simulation. Magnetic analysis reveals that the synthesized functionalized NPs have a saturation magnetization almost equal to that of pure nanoparticles (PNPs). It is also found that the presence of the turmeric causes a small reduction in coercivity of the functionalized NPs in comparison with PNP. Our TGA and FTIR results show that the turmeric is bonded very well to the surface of the NPs. So it can be inferred that a nancomposite (NC) powder of turmeric and nanoparticles is produced. As an application, the anti-arsenic characteristic of turmeric makes the synthesized functionalized NPs or NC powder a good candidate for arsenic removal from polluted industrial waste water. (paper)

Effect of Milling Time on the Microstructure, Physical and Mechanical Properties of Al-Al2O3 Nanocomposite Synthesized by Ball Milling and Powder Metallurgy

Science.gov (United States)

Matori, Khamirul Amin; Ostovan, Farhad; Abdul Aziz, Sidek; Mamat, Md Shuhazlly

2017-01-01

The effect of milling time on the morphology, microstructure, physical and mechanical properties of pure Al-5 wt % Al2O3 (Al-5Al2O3) has been investigated. Al-5Al2O3 nanocomposites were fabricated using ball milling in a powder metallurgy route. The increase in the milling time resulted in the homogenous dispersion of 5 wt % Al2O3 nanoparticles, the reduction of particle clustering, and the reduction of distances between the composite particles. The significant grain refining during milling was revealed which showed as a reduction of particle size resulting from longer milling time. X-Ray diffraction (XRD) analysis of the nanocomposite powders also showed that designated ball milling contributes to the crystalline refining and accumulation of internal stress due to induced severe plastic deformation of the particles. It can be argued that these morphological and microstructural variations of nanocomposite powders induced by designated ball milling time was found to contribute to an improvement in the density, densification, micro-hardness (HV), nano-hardness (HN), and Young’s modulus (E) of Al-5Al2O3 nanocomposites. HV, HN, and E values of nanocomposites were increased by ~48%, 46%, and 40%, after 12 h of milling, respectively. PMID:29072632

Effect of Milling Time on the Microstructure, Physical and Mechanical Properties of Al-Al2O3 Nanocomposite Synthesized by Ball Milling and Powder Metallurgy

Directory of Open Access Journals (Sweden)

Meysam Toozandehjani

2017-10-01

Full Text Available The effect of milling time on the morphology, microstructure, physical and mechanical properties of pure Al-5 wt % Al2O3 (Al-5Al2O3 has been investigated. Al-5Al2O3 nanocomposites were fabricated using ball milling in a powder metallurgy route. The increase in the milling time resulted in the homogenous dispersion of 5 wt % Al2O3 nanoparticles, the reduction of particle clustering, and the reduction of distances between the composite particles. The significant grain refining during milling was revealed which showed as a reduction of particle size resulting from longer milling time. X-Ray diffraction (XRD analysis of the nanocomposite powders also showed that designated ball milling contributes to the crystalline refining and accumulation of internal stress due to induced severe plastic deformation of the particles. It can be argued that these morphological and microstructural variations of nanocomposite powders induced by designated ball milling time was found to contribute to an improvement in the density, densification, micro-hardness (HV, nano-hardness (HN, and Young’s modulus (E of Al-5Al2O3 nanocomposites. HV, HN, and E values of nanocomposites were increased by ~48%, 46%, and 40%, after 12 h of milling, respectively.

Characterization of TiO2–MnO2 composite electrodes synthesized using spark plasma sintering technique

CSIR Research Space (South Africa)

Tshephe, TS

2015-03-01

Full Text Available and electrochemical stability of the resulting materials were investigated. Relative densities of 99.33% and 98.49% were obtained for 90TiO2–10MnO2 and 80TiO2–10MnO2 when ball was incorporated. The 90TiO2–10MnO2 powder mixed with balls had its Vickers hardness value...

Synthesis of alumina powder with seeds by Pechini Method using O2 as calcination atmosphere

International Nuclear Information System (INIS)

Salem, R.E.P.; Guilherme, K.A.; Chinelatto, A.S.A.; Chinelatto, A. L.

2012-01-01

Alumina is a very investigated material due to its excellent refractory characteristics and mechanical properties. Its alpha phase, the most stable one, has a formation temperature of about 1200 ° C. Due to its high temperature of formation, many researches have been trying to reduce it through addition of seeds of alpha phase in chemical processes of synthesis. This work aims to synthesize ultrafine powders of alpha-alumina by the Pechini method with seeding, and using an O 2 atmosphere in the pre-calcination (500 ° C) and calcination (1000 ° C and 1100° C) steps. The resulting powders were characterized through X-ray diffractometry, infrared spectroscopy and scanning electron microscopy. The results were compared with samples calcined on ai. It was verified that the presence of oxygen in the calcination atmosphere favored the elimination of residual carbon from the precursor powders, forthcoming from the great amount of organic material used on the synthesis, modifying its morphology and favoring reduction of particle size. (author)

White light emission from Er2O3 nano-powder excited by infrared radiation

Science.gov (United States)

Tabanli, Sevcan; Eryurek, Gonul; Di Bartolo, Baldassare

2017-07-01

Phosphors of Er2O3 nano-crystalline powders were synthesized by the thermal decomposition method. The structural properties of the nano-powders were investigated with XRD and HRTEM measurements. The cubic phase with a = 10.540 Å was the only phase observed. The average crystalline sizes and the widths of the grain size distribution curves were determined to be 27.2, 18.7 and 9.7 nm, respectively. The spectroscopic properties of the Er2O3 nano-powder were studied by measuring the luminescence, decay and rise patterns under 808 and 975 nm diode laser excitations. A peculiar effect of the pressure was observed since an optically active ion (Er) is part of the complex and not a dopant. A broad band of the white light emission combined with blue, green and red up-conversion emission bands of Er3+ ions were observed at 0.03 mbar pressure under both excitation wavelengths. Only, an intense broad band white light emission was observed from these nanocrystals at atmospheric pressure. Rising patterns show that the white light intensity reaches its maximum value more rapidly under 975 nm excitation although it decays slower than that of 808 nm excitation. The color quality parameters such as the color coordinate (CRI), correlated color temperature and the color rendering index were found to vary with both the excitation wavelength and the ambient pressure indicating that these nanocrystals could be considered good white light emitting source under the infrared excitations.

Synthesis and Characterization of TiO2(B Nanotubes Prepared by Hydrothermal Method Using [Ti8O12(H2O24]Cl8.HCl.7H2O as Precursor

Directory of Open Access Journals (Sweden)

Hari Sutrisno

2010-04-01

Full Text Available Low-dimension TiO2-related material has been synthesized by hydrothermal treatment of [Ti8O12(H2O24]Cl8.HCl.7H2O crystal as precursor in a 10 M NaOh aqueous solution at 150 C for 24 h. Characterization of the obtained product was carried out by a range of techniques including X-ray diffraction (XRD, high resolution scanning electron microscopy (HRSEM, high resolution transmission electron microscopy (HRTEM, Raman spectroscopy and nitrogen adsorption-desorption isotherm (Brunauer-Emmett-Teller (BET-Barret-Joyner-Halender (BJH. From HRTEM, XRD and Raman spectra showed that the obtained product has a TiO2(B structure. According to HRTEM observations, it was found that TiO2(B has nanotubular structure with approximately 5-8 nm in outer and 3-6 nm in inner diameter. The BET surface area of TiO2(B nanotubes is quiet large, values of 418.3163 m2/g being obtained. Pore structure analyisis by the BJH method showed that the average pore diameter of TiO2(B nanotubes has 5.5781 nm.

Influence of Feedstock Powder Modification by Heat Treatments on the Properties of APS-Sprayed Al2O3-40% TiO2 Coatings

Science.gov (United States)

Berger, Lutz-Michael; Sempf, Kerstin; Sohn, Yoo Jung; Vaßen, Robert

2018-04-01

The formation and decomposition of aluminum titanate (Al2TiO5, tialite) in feedstock powders and coatings of the binary Al2O3-TiO2 system are so far poorly understood. A commercial fused and crushed Al2O3-40%TiO2 powder was selected as the feedstock for the experimental series presented in this paper, as the composition is close to that of Al2TiO5. Part of that powder was heat-treated in air at 1150 and 1500 °C in order to modify the phase composition, while not influencing the particle size distribution and processability. The powders were analyzed by thermal analysis, XRD and FESEM including EDS of metallographically prepared cross sections. Only a maximum content of about 45 wt.% Al2TiO5 was possible to obtain with the heat treatment at 1500 °C due to inhomogeneous distribution of Al and Ti in the original powder. Coatings were prepared by plasma spraying using a TriplexPro-210 (Oerlikon Metco) with Ar-H2 and Ar-He plasma gas mixtures at plasma power levels of 41 and 48 kW. Coatings were studied by XRD, SEM including EDS linescans of metallographically prepared cross sections, and microhardness HV1. With the exception of the powder heat-treated at 1500 °C an Al2TiO5-Ti3O5 (tialite-anosovite) solid solution Al2- x Ti1+ x O5 instead of Al2TiO5 existed in the initial powder and the coatings.

The dimeric [V2O2F8]4− anion: Structural characterization of a magnetic basic-building-unit

International Nuclear Information System (INIS)

Lu, Hongcheng; Gautier, Romain; Li, Zuo-Xi; Jie, Wanqi; Liu, Zhengtang; Poeppelmeier, Kenneth R.

2013-01-01

New materials built from the [V 2 O 2 F 8 ] 4− anionic basic-building-unit (BBU) exhibit interesting magnetic properties owing to the proximity of the two d 1 V(IV) cations and the orbital interactions of fluoride and oxide ligands. In our search to target such materials, the vanadium oxide–fluoride compound [dpaH 2 ] 2 [V 2 O 2 F 8 ] in which a dimeric anion [V 2 O 2 F 8 ] 4− is isolated in a hydrogen bond network was hydrothermally synthesized (dpa=2,2′-dipyridylamine). This hydrogen bond network is able to stabilize the highly ionic species [V 2 O 2 F 8 ] 4− as demonstrated with bond valence calculations. The coordination of the O 2− /F − ordered ligands was investigated and antiferromagnetic coupling of the isolated BBU was measured. - The new hybrid compound [dpaH 2 ] 2 [V 2 O 2 F 8 ] built from the interesting [V 2 O 2 F 8 ] 4− magnetic basic-building-unit (BBU) was synthesized by the hydrothermal method. The coordination of the O 2− /F − ordered ligands was investigated by BVS calculations and antiferromagnetic coupling was measured. Highlights: ► A new vanadium oxyfluoride was synthesized by hydrothermal method. ► The Dimeric [V 2 O 2 F 8 ] 4− basic building unit is isolated in the hydrogen bond networks. ► The coordination of [V 2 O 2 F 8 ] 4− units to the extended structure is investigated. ► Isolated [V 2 O 2 F 8 ] 4− units exhibit antiferromagnetic coupling

A novel hydrothermal approach for synthesizing α-Fe2O3, γ-Fe2O3 and Fe3O4 mesoporous magnetic nanoparticles

International Nuclear Information System (INIS)

Jayanthi, S. Amala; Nathan, D. Muthu Gnana Theresa; Jayashainy, J.; Sagayaraj, P.

2015-01-01

A novel method to synthesize the three phases of iron oxide nanoparticles (hematite, maghemite and magnetite) using the same non-toxic inorganic precursors via a water–organic interface under the low temperature hydrothermal conditions is reported. The synthesized particles are characterized by Powder X-ray Diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM) and Transmission Electron Microscopy (TEM). The Brunauer–Emmett–Teller (BET) results reveal the mesoporous nature of the particles. The magnetic properties of the nanoparticles are studied by Vibrating Sample Magnetometer (VSM) at various low temperatures and also at room temperature. The XRD peaks corresponding to each sample clearly depict the presence of the respective phase of the as-prepared magnetic nanoparticles. The nanoparticles of maghemite and magnetite have saturation magnetization of 58.56 and 40.30 emu/g respectively at room temperature, whereas the particles of hematite possess very low saturation magnetization value of 1.89 emu/g. Further, the magnetization is studied at four different temperatures and the zero field cooled (ZFC) and field cooled (FC) magnetization are reported. - Graphical abstract: Display Omitted - Highlights: • Hematite, maghemite and magnetite are obtained under hydrothermal synthesis. • α-Fe 2 O 3 , γ-Fe 2 O 3 and Fe 3 O 4 prepared are mesoporous and nearly monodisperse. • Near superparamagnetism is observed at room temperature for maghemite and magnetite

Structural and optical properties of Er{sup 3+} doped SiO{sub 2}–Al{sub 2}O{sub 3}–GeO{sub 2} compounds prepared by a simple route

Energy Technology Data Exchange (ETDEWEB)

Filho, Fausto M. Faria [Instituto de Física, Universidade Federal de Goiás-UFG, Campus II, Caixa Postal 131, CEP 74001-970 Goiânia, GO (Brazil); Gonçalves, Rogéria R. [Departamento de Química, Faculdade de Filosofia, Ciências e Letras de Ribeirão Preto, Universidade de São Paulo-USP, Av. Bandeirantes, 3900, CEP 14040-901 Ribeirão Preto, SP (Brazil); Ribeiro, Sidney J.L. [Institute of Chemistry, São Paulo State University-UNESP, Rua Professor Francisco Degni, 55, CEP 14801-970 Araraquara, SP (Brazil); Maia, Lauro J.Q., E-mail: lauro@ufg.br [Instituto de Física, Universidade Federal de Goiás-UFG, Campus II, Caixa Postal 131, CEP 74001-970 Goiânia, GO (Brazil)

2015-04-15

Highlights: • We developed a simple route to obtain gels and powders using GeO{sub 2}, TEOS and TMAH solution. • Al{sub 6}Ge{sub 2}O{sub 13} crystalline nanoparticles embedded in amorphous matrix were obtained. • The Al{sub 2}O{sub 3} enhance Er{sup 3+} dispersion in GeO{sub 2}–SiO{sub 2} increasing its emission and the full width at half maximum from 41 to 56 nm. • The {sup 4}I{sub 13/2} Er{sup 3+} level lifetime varies between 4.8 and 5.6 ms (1533 nm emission). - Abstract: Samples of (1 − x)[0.70SiO{sub 2} + 0.30Al{sub 2}O{sub 3}] + xGeO{sub 2} compositions, containing x = 0.05, 0.10, 0.20, 0.30, 0.40 and 0.50, and doped with 1 mol% of Er{sup 3+}, were prepared by a mixed route (sol–gel process and Pechini method). Transparent gels were synthesized and homogeneous powders were obtained by heat treatments from 800 °C to 1050 °C. The final powders were characterized by X-ray diffraction, Fourier transform infrared spectroscopy and high-resolution transmission electron microscopy. The optical properties were studied by photoluminescence measurements in the infrared region, and the average lifetime of the metastable state {sup 4}I{sub 13/2} of Er{sup 3+} ions and the full-width at half maximum (FWHM) were determined. A silica-rich amorphous phase and nanocrystallites with orthorhombic structure of Al{sub 6}Ge{sub 2}O{sub 13} phase were obtained. The samples present a broad emission centered at around 1532 nm under excitation at 977 nm, with a FWHM of 53 nm and a lifetime of 5.6 ms. The synthesized compounds by an easy chemical procedure are potentially applicable in integrated optical systems.

Bacteria-assisted preparation of nano α-Fe2O3 red pigment powders from waste ferrous sulfate

International Nuclear Information System (INIS)

Li, Xiang; Wang, Chuankai; Zeng, Yu; Li, Panyu; Xie, Tonghui; Zhang, Yongkui

2016-01-01

Highlights: • A route to prepare nano α-Fe 2 O 3 red pigment from waste ferrous sulfate is proposed. • Acidithiobacillus ferrooxidans is introduced for accelerating iron oxidation. • The particle size of synthetic α-Fe 2 O 3 is ranged from 22 nm to 86 nm. • The prepared nano α-Fe 2 O 3 red pigment fulfills ISO 1248-2006. - Abstract: Massive ferrous sulfate with excess sulfuric acid is produced in titanium dioxide industry each year, ending up stockpiled or in landfills as solid waste, which is hazardous to environment and in urgent demand to be recycled. In this study, waste ferrous sulfate was used as a second raw material to synthesize nano α-Fe 2 O 3 red pigment powders with a bacteria-assisted oxidation process by Acidithiobacillus ferrooxidans. The synthesis route, mainly consisting of bio-oxidation, precipitation and calcination, was investigated by means of titration, thermogravimetric analysis (TGA), X-ray diffraction (XRD), scanning electron microscope (SEM) and X-ray fluorescence (XRF) to obtain optimum conditions. Under the optimum conditions, nano α-Fe 2 O 3 red pigment powders contained 98.24 wt.% of Fe 2 O 3 were successfully prepared, with a morphology of spheroidal and particle size ranged from 22 nm to 86 nm and averaged at 45 nm. Moreover, the resulting product fulfilled ISO 1248-2006, the standards of iron oxide pigments.

The Synthesis of BaAl2O4 Powder with High Surface Area%高比表面积BaAl2O4粉体合成研究

Institute of Scientific and Technical Information of China (English)

乔彦辉; 顾士甲; 王明辉; 田元; 李欢; 江莞

2017-01-01

BaAl2O4是优良的NOx存储催化剂材料,同时也是一种理想的荧光基体材料,受到了研究人员的广泛关注.但是一般的BaAl2O4粉体由于比表面积相对较小,使用受到了限制.虽然纳米颗粒有大的比表面积,但其团聚的缺陷严重限制了其应用.本文采用了一种简单的软模板法合成了BaAl2O4粉体.该粉体经过XRD表征表明为BaAl2O4,经BET表征具有较大比表面积.BaAl2O4粉体不仅化学稳定性好,而且具有相对较大的比表面积.其合成方法节省能源、生产效率高,在特定场合极有可能替代普通粉体做实际应用.%BaAl2O4 is an excellent NOx storage catalyst material. At the same time, it is also an ideal fluorescent matrix material and draws extensive attention. However, the general BaAl2O4 powder is limited by the relatively small surface area. Although the nanoparticles have larger surface area, the defect of their aggregation severely limits their applications. In this study, BaAl2O4 powder was synthesized by a simple soft template method, which not only had a good chemical stability, but also had a relatively large surface area. After characterizing by XRD, BET and TEM, the powder proved exactly the BaAl2O4 with a larger surface area. The synthesis method in this paper has high production efficiency and energy efficiency, and the powder is likely to replace the commonly-used powder on particular occasions.

Liquid phase surface melting of AA8011 aluminum alloy by addition of Al/Al{sub 2}O{sub 3} nano-composite powders synthesized by high-energy milling

Energy Technology Data Exchange (ETDEWEB)

Sohi, M. Heydarzadeh [School of Metallurgy and Materials Engineering, College of Engineering, University of Tehran, Tehran (Iran, Islamic Republic of); Hojjatzadeh, S.M.H., E-mail: Hojatzadeh@yahoo.com [Department of Welding, Science and Research Branch, Azad University, Tehran (Iran, Islamic Republic of); Moosavifar, Sh. S.; Heshmati-Manesh, S. [School of Metallurgy and Materials Engineering, College of Engineering, University of Tehran, Tehran (Iran, Islamic Republic of)

2014-09-15

Highlights: • Aluminum matrix composite layers reinforced with alumina particles were fabricated. • Non milled powders caused porosity in the microstructures because of poor wettability. • The ball milling of powders was significantly improved the wettability of nano ceramic particles. • The micro hardness of the layers was approximately 3 times greater than that of the base metal. - Abstract: Poor wettability of particles is an obstacle in formation of sound composite layer via surface melting. Pre-coating of particles with metallic material by different techniques, such as ball milling may enhance the wettability of the particles with molten metal. In this study, composite surface layers containing Al{sub 2}O{sub 3} particles were fabricated on the surface of AA8011 aluminum substrates by tungsten inert gas (TIG) surface melting using preplaced layers of Al/Al{sub 2}O{sub 3} powder mixtures in two different forms: (1) a mixture of 40 wt% Al and 60 wt% of 50 nm Al{sub 2}O{sub 3} powders and (2) a mixture obtained by mechanical alloying of 40 wt% Al and 60 wt% of 60 μm Al{sub 2}O{sub 3} powders. Morphology evolution of powders during ball milling and the microstructure of the fabricated composite layers were studied through conventional characterization techniques, such as optical microscopy, scanning electron microscopy (SEM), and X-ray diffraction (XRD). Microhardness measurements were also performed across the alloyed zone. The results indicated that the layer fabricated by the second route showed a defect free structure with a more uniform distribution of Al{sub 2}O{sub 3} particles in comparison with the layer obtained by the first route. It was also noticed that the uniform dispersion of Al{sub 2}O{sub 3} particles in the fabricated layer increased the hardness to 133 HV which was over 3 times of that of the base metal.

Air Plasma-Sprayed La2Zr2O7-SrZrO3 Composite Thermal Barrier Coating Subjected to CaO-MgO-Al2O3-SiO2 (CMAS)

Science.gov (United States)

Cai, Lili; Ma, Wen; Ma, Bole; Guo, Feng; Chen, Weidong; Dong, Hongying; Shuang, Yingchai

2017-08-01

La2Zr2O7-SrZrO3 composite thermal barrier coatings (TBCs) were prepared by air plasma spray (APS). The La2Zr2O7-SrZrO3 composite TBCs covered with calcium-magnesium-aluminum-silicate (CMAS) powder, as well as the powder mixture of CMAS and spray-dried La2Zr2O7-SrZrO3 composite powder, were heat-treated at 1250 °C in air for 1, 4, 8, and 12 h. The phase constituents and microstructures of the reaction products were characterized by x-ray diffraction, scanning electron microscopy, and energy-dispersive spectroscopy. Experimental results showed that the La2Zr2O7-SrZrO3 composite TBCs had higher CMAS resistance than 8YSZ coating. A dense new layer developed between CMAS and La2Zr2O7-SrZrO3 composite TBCs during interaction, and this new layer consisted mostly of apatite (Ca2La8(SiO4)6O2) and c-ZrO2. The newly developed layer effectively protected the La2Zr2O7-SrZrO3 composite TBCs from further CMAS attack.

Phase behaviour, thermal expansion and compressibility of SnMo 2 O 8

Energy Technology Data Exchange (ETDEWEB)

Araujo, Luiza R.; Gallington, Leighanne C.; Wilkinson, Angus P.; Evans, John S.O. (Durham); (GIT)

2018-02-01

The phase behaviour and thermoelastic properties of SnMo2O8, derived from variable temperature and pressure synchrotron powder diffraction data, are reported. SnMo2O8 is a member of the AM2O8 family of negative thermal expansion (NTE) materials, but unexpectedly, has positive thermal expansion. Over the P-T space explored (298–513 K, ambient to 310 MPa) four different forms of SnMo2O8 are observed: α, β, γ and γ'. The γ to β transition is temperature-, pressure-, and time-dependent. SnMo2O8 is a much softer material (α and γ form have BT = 29 and 26 GPa at 298 K) than other members of the AM2O8 family. Counter-intuitively, its high temperature β phase becomes stiffer with increasing temperature (BT ~36 GPa at 490 K). The pressure dependence of the thermal expansion for each phase is reported.

Studies on powder processing and sintering behaviour of ZrO2-9.0 mol% Y2O3 ceramics

International Nuclear Information System (INIS)

Ghosh, A.; Gonal, M.R.; Upadhyaya, D.D.; Ram Prasad

1998-01-01

In the present investigation the synthesis and densification behaviour of ZrO 2 -9.0 mol% Y 2 O 3 ceramics has been described. Powder preparation was based on the co-precipitation method. It was found that variation in the precipitation conditions and washing steps of the precipitated gels resulted in powder of different agglomerate sizes. The effect of different precipitations and washing conditions on the crystallite size of the 600 deg C calcined powders were examined by x-ray diffraction. The powders produced were essentially of the cubic fluorite phase. The ball-milled powders were analyzed for particle size distribution. Densification behaviour of the bodies made by slip casting has also been studied. (author)

Synthesis and characterization of Zn3Ta2O8 nanomaterials by hydrothermal method

International Nuclear Information System (INIS)

Bîrdeanu, M.; Bîrdeanu, A.-V.; Gruia, A.S.; Fagadar-Cosma, E.; Avram, C.N.

2013-01-01

Graphical abstract: The results of an experimental program that was focused on obtaining the Zn 3 Ta 2 O 8 nanocrystalline synthesized by hydrothermal method using tantalum (V) oxide and zinc nitrate, the results of the nanomaterial’s structure characterization and the optical spectral properties of such nanomaterials that were thoroughly investigated. Also, the experimental results are compared with ab initio calculations of electronic properties of Zn 3 Ta 2 O 8 . Highlights: •Zn 3 Ta 2 O 8 nanomaterials were synthesized by hydrothermal method and characterized. •The obtained nanomaterials has excellent phosphor, optical and morphological properties. •The material can be used in designing high performance optoelectronical devices. -- Abstract: Zn 3 Ta 2 O 8 has been synthesized by hydrothermal method using tantalum (V) oxide and zinc nitrate. The crystal structure and microstructure, phase composition and the absorption of Zn 3 Ta 2 O 8 nanomaterials were characterized by X-ray diffraction, FT/IR measurements, UV–VIS measurements, PL measurements, SEM and AFM techniques and BET analysis. XRD results show the single phase of Zn 3 Ta 2 O 8 and the average particle size that is 52 nm. This narrow nanometer size was also confirmed by AFM measurements. BET analysis revealed that the nanomaterials are mesoporous. The PL spectra show the blue luminescence of Ta 2 Zn 3 O 8 . Besides, in the present work we report ab initio calculations regarding electronic properties of Zn 3 Ta 2 O 8 ; the theoretical results are compared with the experimental ones

Investigations on the crystal-structure and non-ambient behaviour of K2Ca2Si8O19 - a new potassium calcium silicate

Science.gov (United States)

Schmidmair, Daniela; Kahlenberg, Volker; Praxmarer, Alessandra; Perfler, Lukas; Mair, Philipp

2017-09-01

Within the context of a systematic re-investigation of phase relationships between compounds of the ternary system K2O-CaO-SiO2 a new potassium calcium silicate with the chemical formula K2Ca2Si8O19 was synthesized via solid state reactions as well as the flux method using KCl as a solvent. Its crystal structure was determined from single-crystal X-ray diffraction data by applying direct methods. The new compound crystallizes in the triclinic space group P 1 bar . Unit cell dimensions are a = 7.4231(7) Å, b = 10.7649(10) Å, c = 12.1252(10) Å, α = 70.193(8)°, β = 83.914(7)° and γ = 88.683(7)°. K2Ca2Si8O19 is built up of corner-connected, slightly distorted [SiO4]-tetrahedra forming double-sheets, which are linked by double-chains of edge-sharing [CaO6]-octahedra. Electroneutrality of the material is provided by additional potassium atoms that are located within the voids of the silicate layers and between adjacent [Ca2O6]-double-chains. Further characterization of the compound was performed by Raman spectroscopy and differential thermal analysis. The behaviour of K2Ca2Si8O19 under high-temperature and high-pressure was investigated by in-situ high-temperature powder X-ray diffraction up to a maximum temperature of 1125 °C and a piston cylinder experiment at 1.5 GPa and 1100 °C. Additionally an overview of known double-layer silicates is given as well as a comparison of K2Ca2Si8O19 to closely related structures.

Synthesis and X-ray Powder Structure of a New Pillared Layered Cadmium Phosphonate, Giving Evidence that the Intercalation of Alkylamines into Cd(O(3)PR).H(2)O Is Topotactic.

Science.gov (United States)

Fredoueil, Florence; Massiot, Dominique; Janvier, Pascal; Gingl, Franz; Bujoli-Doeuff, Martine; Evain, Michel; Clearfield, Abraham; Bujoli, Bruno

1999-04-19

A new pillared layered phosphonate, cadmium 2-aminoethylphosphonate, Cd(O(3)PC(2)H(4)NH(2)) (1), has been synthesized, and its structure was solved ab initio from X-ray powder diffraction data and refined by Rietveld methods. Compound 1 is orthorhombic: space group Pna2(1), a = 15.4643(2) Å, b = 5.16512(7) Å, c = 6.27650(8) Å, and Z = 4. Its layer arrangement is similar to that in Cd(O(3)PR).H(2)O, except that the water molecule coordinated to cadmium in Cd(O(3)PR).H(2)O is replaced by the nitrogen atom from the amino ends of the ethyl chains borne by phosphorus of the upper and lower layers. The strong similarity of the IR, (31)P, and (113)Cd NMR data for Cd(O(3)PC(2)H(4)NH(2)) and Cd(O(3)PCH(3)).n-NH(2)C(4)H(9) clearly shows the topotactic character of the intercalation of n-alkylamines in the dehydrated form of Cd(O(3)PR).H(2)O to yield Cd(O(3)PR).n-NH(2)R'.

Muonium in Al2O3 powder at low temperature

International Nuclear Information System (INIS)

Kiefl, R.F.; Warren, J.B.; Oram, C.J; Brewer, J.H.; Harshman, D.R.

1982-04-01

Measurements of muonium (μ + e - ) spin relaxation in a finely powdered sample of γ-Al 2 O 3 in a He (or Ne) atmosphere indicate that the muonium atoms escape the powder grains with a high efficiency at low temperatures (T < 30 K). The muonium spin relaxation rate is proportional to the fraction of the powder surface area not covered by adsorbed He (Ne)

Direct synthesis of La9.33Si6O26 ultrafine powder via sol-gel self-combustion method

International Nuclear Information System (INIS)

Tian Changan; Liu Junliang; Cai Jun; Zeng Yanwei

2008-01-01

Single phase La 9.33 Si 6 O 26 ultrafine powder, as a kind of highly activated precursor to prepare medium-to-low temperature electrolyte for solid oxide fuel cells (SOFCs), has been successfully synthesized via a non-aqueous sol-gel and self-combustion approach from the starting materials: lanthanum nitrate (La(NO 3 ) 3 .6H 2 O), citric acid, ethylene glycol (EG), tetraethyl orthosilicate (TEOS) and ammonium nitrate. The details of gel's self-combustion were investigated by DTA-TG and the structural characterization of as-synthesized powder from self-combustion was performed by XRD and SEM. The results show that La 9.33 Si 6 O 26 single phase of apatite-type crystal structure can be directly synthesized by sol-gel self-combustion method without further calcinations on the condition that the molar ratio (R) of NO 3 - to citric acid and ethylene glycol being 6:1. Such powders composed of well-dispersed particles with an average size of 200 nm and a specific surface area of 5.54 m 2 /g. It can be sintered to 90% of its theoretical density at 1500 deg. C for 10 h, about 200 deg. C lower than the sintering temperature for the powder derived from traditional solid reactions. The sintered material has a thermal expansion coefficient of 9.2 x 10 -6 K -1 between room temperature and 800 deg. C

Mullite and Mullite/ZrO2-7wt.%Y2O3 Powders for Thermal Spraying of Environmental Barrier Coatings

Science.gov (United States)

Garcia, E.; Mesquita-Guimarães, J.; Miranzo, P.; Osendi, M. I.; Wang, Y.; Lima, R. S.; Moreau, C.

2010-01-01

Mullite and mullite/ZrO2-7wt.%Y2O3 coatings could be thought among the main protective layers for environment barrier coatings (EBCs) to protect Si-based substrates in future gas turbine engines. Considering that feedstock of the compound powder is not commercially available, two powder processing routes Spray Drying (SD) and Flame Spheroidization (FS) were implemented for both types of powders. For each method the particle size, the morphology, and microstructure of the powder particles was determined. In addition, the effect of the heat treatment on the powder crystallinity and microstructure of FS powders was also investigated. To evaluate their suitability as feedstock materials, the powders were plasma sprayed and their in-flight particle characteristics monitored for coatings production. The powder morphology was correlated to the in-flight particle characteristics and splat morphology to gain insight about into the influence of powder characteristics on the coating formation.

Mixture of fuels for solution combustion synthesis of porous Fe3O4 powders

Science.gov (United States)

Parnianfar, H.; Masoudpanah, S. M.; Alamolhoda, S.; Fathi, H.

2017-06-01

The solution combustion synthesis of porous magnetite (Fe3O4) powders by a mixture of glycine and urea fuels was investigated concerning the thermodynamic aspects and powder characteristics. The adiabatic combustion temperature and combusted species were thermodynamically calculated as a function of the fuel to oxidant molar ratio (ϕ). The combustion behavior, phase evolution, porous structure and magnetic properties were characterized by thermal analysis, X-ray diffractometry, N2 adsorption-desorption, electron microscopy and vibrating sample magnetometry techniques. Nearly single phase Fe3O4 powders were synthesized by the mixture of fuels at ϕ values of 0.75 and 1. The as-combusted Fe3O4 powders at ϕ = 1 exhibited porous structure with the specific surface area of 83.4 m2/g. The highest saturation magnetization of 75.5 emu/g and the lowest coercivity of 84 Oe were achieved at ϕ = 1, due to the high purity and large crystallite size, inducing from the highest adiabatic combustion temperature.

Nanocrystals-based Macroporous Materials Synthesized by Freeze-drying Combustion

International Nuclear Information System (INIS)

Yan, Ruiqiang; Chen, Yu; Lin, Ye; Chen, Fanglin

2016-01-01

We present a novel freeze-drying combustion method for synthesis of macroporous powders with nano-network, using Sm 0.2 Ce 0.8 O 1.9 (SDC) as an example. The metal nitrate salt solution mixed with glycine is frozen to form homogeneous nitrate/glycine mixture and then freeze-dried through sublimation of ice crystals. Upon combustion of the freeze-dried mixture, SDC powders with macroporous microstructure consisting of 10–20 nm nanocrystals, high surface area and excellent sinterability are achieved. High resolution transmission electron microscopy (HRTEM) analysis indicates that nanodomains due to aggregation/segregation of dopants in the SDC powders obtained from freeze-drying combustion are much smaller than those in the SDC powders synthesized by the conventional nitrate solution combustion approach, demonstrating better elemental homogeneity and improved conductivity. Using low cost precursors and simple processing conditions, freeze-drying combustion can be a versatile method to synthesize nanocrystalline powders with excellent composition homogeneity for broad applications.

Interactions of a La{sub O.9}Sr{sub O.1}Ga{sub O.8}Mg{sub O.2}O{sub 3-{delta}} electrolyte with Fe{sub 2}O{sub 3}, Co{sub 2}O{sub 3} and NiO anode materials

Energy Technology Data Exchange (ETDEWEB)

Zhang, X.; Ohara, S.; Okawa, H.; Maric, R.; Fukui, T. [Japan Fine Ceramics Center, 2-4-1 Mutsuo, Atsuta-ku, 456-8587 Nagoya (Japan)

2001-01-02

In this study, the interactions of a Sr- and Mg-doped lanthanum gallate (LSGM with composition La{sub O.9}Sr{sub O.1}Ga{sub O.8}Mg{sub O.2}O{sub 3-{delta}}) electrolyte with Fe{sub 2}O{sub 3}, Co{sub 2}O{sub 3} and NiO as the anode starting materials were investigated. It was found that the order of reactivity of the LSGM with the three oxides was Co{sub 2}O{sub 3}>NiO>Fe{sub 2}O{sub 3}, and La-containing oxides were detected in these binary powder mixtures after firing. The anode performance was greatly influenced by the interaction. The Fe{sub 2}O{sub 3}-LSGM anode, mixed with 40 vol.% LSGM powder and sintered at 1150C, exhibited the highest initial performance in comparison with NiO-LSGM and Co{sub 2}O{sub 3}-LSGM anodes. It seems that Fe{sub 2}O{sub 3} is a possible anode starting material for a LSGM-based solid oxide fuel cell.

Microwave, sonochemical and combustion synthesized CuO nanostructures and their electrical and bactericidal properties

International Nuclear Information System (INIS)

Karunakaran, C.; Manikandan, G.; Gomathisankar, P.

2013-01-01

Highlights: •CuO nanoleaves synthesized by CTAB-assisted hydrothermal method. •CuO nanodiscs synthesized by CTAB-assisted sonochemical method. •Combustion synthesized CuO is highly porous. •Synthetic method and morphology influence CuO bactericidal activity. -- Abstract: Cetyltrimethylammonium bromide (CTAB)-assisted microwave synthesis of CuO provides nanoleaves and in the absence of CTAB the shape of CuO is irregular. Sonochemical synthesis of CuO using CTAB gives nanodiscs whereas irregularly shaped flake-like structure is obtained without CTAB. Combustion synthesized CuO is highly porous with innumerable large holes. CTAB does not provide any structure in combustion synthesis. Transmission electron micrographs (TEM) display the constituent nanoparticles of microwave and sonochemically synthesized CuO. The powder X-ray diffractogram (XRD) shows the sample obtained by sonochemical method in the absence of CTAB as a mixture of monoclinic CuO, cubic Cu 2 O, and orthorhombic Cu(OH) 2 . But the rest of the samples are pure CuO in monoclinic phase. The selected area electron diffractograms (SAED) of the microwave and sonochemically synthesized samples, in the presence as well as in the absence of CTAB, confirm the monoclinic phase of CuO and indicates the presence of amorphous CuO in traces. All the samples are characteristic of Fourier Transform infrared (FT-IR) Cu–O stretching frequencies. The method of synthesis and also the morphology influence the electrical properties as well as the bactericidal activity of CuO

Preparation and Characterization of Nano-structured Ceramic Powders Synthesized by Emulsion Combustion Method

International Nuclear Information System (INIS)

Takatori, Kazumasa; Tani, Takao; Watanabe, Naoyoshi; Kamiya, Nobuo

1999-01-01

The emulsion combustion method (ECM), a novel powder production process, was originally developed to synthesize nano-structured metal-oxide powders. Metal ions in the aqueous droplets were rapidly oxidized by the combustion of the surrounding flammable liquid. The ECM achieved a small reaction field and a short reaction period to fabricate the submicron-sized hollow ceramic particles with extremely thin wall and chemically homogeneous ceramic powder. Alumina, zirconia, zirconia-ceria solid solutions and barium titanate were synthesized by the ECM process. Alumina and zirconia powders were characterized to be metastable in crystalline phase and hollow structure. The wall thickness of alumina was about 10 nm. The zirconia-ceria powders were found to be single-phase solid solutions for a wide composition range. These powders were characterized as equiaxed-shape, submicron-sized chemically homogeneous materials. The powder formation mechanism was investigated through the synthesis of barium titanate powder with different metal sources

Structural and magnetic properties of turmeric functionalized CoFe2O4 nanocomposite powder

Science.gov (United States)

Mehran, E.; Farjami Shayesteh, S.; Sheykhan, M.

2016-10-01

The structural and magnetic properties of the synthesized pure and functionalized CoFe2O4 magnetic nanoparticles (NPs) are studied by analyzing the results from the x-ray diffraction (XRD), transmission electron microscopy (TEM), FT-IR spectroscopy, thermogravimetry (TG), and vibrating sample magnetometer (VSM). To extract the structure and lattice parameters from the XRD analysis results, we first apply the pseudo-Voigt model function to the experimental data obtained from XRD analysis and then the Rietveld algorithm is used in order to optimize the model function to estimate the true intensity values. Our simulated intensities are in good agreement with the experimental peaks, therefore, all structural parameters such as crystallite size and lattice constant are achieved through this simulation. Magnetic analysis reveals that the synthesized functionalized NPs have a saturation magnetization almost equal to that of pure nanoparticles (PNPs). It is also found that the presence of the turmeric causes a small reduction in coercivity of the functionalized NPs in comparison with PNP. Our TGA and FTIR results show that the turmeric is bonded very well to the surface of the NPs. So it can be inferred that a nancomposite (NC) powder of turmeric and nanoparticles is produced. As an application, the anti-arsenic characteristic of turmeric makes the synthesized functionalized NPs or NC powder a good candidate for arsenic removal from polluted industrial waste water. Project supported by the University of Guilan and the Iran Nanotechnology Initiative Council.

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.

Thermal behavior and phase transformation of ZrO{sub 2}–10%SiO{sub 2} precursor powder prepared by a co-precipitation route without adding stability agent

Energy Technology Data Exchange (ETDEWEB)

Chu, Hsueh-Liang [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Hwang, Weng-Sing [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Institute of Nanotechnology and Microsystems Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Wang, Cheng-Li [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Wang, Moo-Chin, E-mail: mcwang@kmu.edu.tw [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China); Lee, Kuen-Chan [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China); Huang, Hong-Hsin [Department of Electrical Engineering, Cheng Shiu University, 840 Cheng Ching Road, Niaosong, Kaohsiung 83347, Taiwan (China); Lee, Huey-Er, E-mail: huerle@kmu.edu.tw [School of Dentistry, College of Dental Medicine, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 807, Taiwan (China); Department of Dentistry, Kaohsiung Medical University, 100 Tzyou 1st Road, Kaohsiung 807, Taiwan (China)

2014-12-15

Highlights: • The precursor powders contained about 68.3 wt% ZrO{sub 2}, which corresponds to ZrO{sub 2}·1/8 H{sub 2}O. • The exothermic peak temperature of tetragonal ZrO{sub 2} formation occurred at 1014 K. • The activation energy of ZrO{sub 2}–10%SiO{sub 2} precursors crystallization is 993.7 kJ/mol. • Only the tetragonal ZrO{sub 2} formed when the precursor calcined at 1173–1373 K for 2 h. • As calcined at 1473 K for 2 h, tetragonal ZrO{sub 2} fully converted to monoclinic ZrO{sub 2}. - Abstract: Thermal behavior and phase transformation of ZrO{sub 2}–10%SiO{sub 2} precursor powder prepared by a co-precipitation route without adding stability agent has been studied using different thermal analysis/thermogravimetry (DTA/TG), X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), nano beam electron diffraction (NBED), high-resolution TEM (HRTEM) and energy-dispersive X-ray spectrometer (EDS). The TG results show that four weight loss regions were from 298 to 443 K, 443 to 743 K, 743 to 793 K and 793 to 1400 K. The DTA result shows that the ZrO{sub 2} freeze-dried precursor powders crystallization at 1014 K. The activation energy of 993.7 kJ/mol was obtained for tetragonal ZrO{sub 2} crystallization using a non-isothermal process. The XRD result shows that only a single phase of tetragonal ZrO{sub 2} appears when the freeze-dried precursor powders after calcination between 1173 and 1373 K for 2 h. Moreover, when calcined at 1473 K for 2 h, the phase transformation from tetragonal ZrO{sub 2} fully converted to monoclinic ZrO{sub 2} occurred.

Thermoluminescence in HfO{sub 2}:Eu{sup 3+} powders irradiated in UV; Termoluminiscencia en polvos de HfO{sub 2}:Eu{sup 3+} irradiados en el UV

Energy Technology Data Exchange (ETDEWEB)

Ceron R, P. V. [Universidad de Guanajuato, Division de Ciencias e Ingenierias, Loma del Bosque No. 103, Col. Lomas del Campestre, 37150 Leon, Guanajuato (Mexico); Montes R, E.; Rivera M, T.; Diaz G, J. A. I.; Guzman M, J. [IPN, Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Legaria, Av. Legaria 694, Col. Irrigacion, 11500 Ciudad de Mexico (Mexico)

2016-10-15

Various inorganic compounds synthesized for photo luminescent applications have also presented a thermoluminescent (Tl) response, for example the metal oxides doped with rare earths. This property extends the use of these materials to the radiation dosimetry. For this reason, in this work the Tl response is presented in HfO{sub 2}:Eu{sup 3+} powders synthesized by the hydrothermal path, exposed to ultraviolet (UV) radiation of 254 nm. The kinetic parameters of its brightness curve were also calculated using the Chen expressions and the analysis method based on the shape of the curve. For the powders irradiated for 10 min the highest Tl response corresponds to the sample with 5% of the impurity, which is 6.5 times higher than the signal corresponding to the intrinsic sample. Its bright curve shows a main peak with a maximum in 148 degrees Celsius and a second order kinetics. Another test with the same material shows the Tl response against the exposure time, with a maximum in the 3 minutes. These calculations and tests constitute a first approach for the study of these powders as Tl dosimeter for UV radiation. (Author)

Characteristics of LiMO2 (M = Co, Ni, Ni0.2Co0.8, Ni0.8Co0.2) powders prepared from solution of their acetates

International Nuclear Information System (INIS)

Arof, A.K.

2008-01-01

Stoichiometric quantities of the acetates of lithium, cobalt and nickel were dissolved in distilled water and stirred with a magnetic stirrer. After complete dissolution was obtained, the solutions were heated at 120 deg. C under continuous stirring until some dark colored powder materials were formed. These precursor materials were divided into three batches and heated at 250 deg. C (for 24 h), 370 deg. C (for 24 h) and 800 deg. C for 10 h. The precursor and calcined samples were X-rayed. The X-ray diffractograms for the prepared samples were compared to that of commercialized samples and those published in the literature. The Bragg peak with Miller indices (0 0 3) in the diffractogram of the LiNi 0.8 Co 0.2 O 2 prepared sample showed a lower intensity compared to the (1 0 4) peak. The ratio of the (0 0 3) to (1 0 4) peaks for the LiNi 0.2 Co 0.8 O 2 sample is 1.56. Lattice parameters showed that the LiCoO 2 and LiNi 0.2 Co 0.8 O 2 samples produced by the method in the present investigation have potential to exhibit good electrochemical performance when used as electrodes in lithium ion batteries

Photocatalytic performance of pure anatase nanocrystallite TiO2 synthesized under low temperature hydrothermal conditions

International Nuclear Information System (INIS)

Sayilkan, Funda; Erdemoglu, Sema; Asiltuerk, Meltem; Akarsu, Murat; Sener, Sadiye; Sayilkan, Hikmet; Erdemoglu, Murat; Arpac, Ertugrul

2006-01-01

Photocatalytic performance of a hydrothermally synthesized pure anatase TiO 2 with 8 nm average crystallite size for decomposition of Reactive Red 141 was examined by investigating the effects of UV-light irradiation time, irradiation power, amount of TiO 2 and initial dye concentration. Change in the UV absorbance of the dye during irradiation was monitored. One wt.% TiO 2 in 30 mg/l Reactive Red 141 aqueous solution was found adequate for complete decolorization in 70 min at 770 W/m 2 irradiation power. It was realized that, compared to Degussa P-25, the synthesized nano-TiO 2 can be repeatedly used as a new catalyst. The results also proved that Reactive Red 141 is decomposed catalytically due to the pseudo first-order reaction kinetics

Preparation of UO{sub 2}, ThO{sub 2} and (Th,U)O{sub 2} pellets from photochemically-prepared nano-powders

Energy Technology Data Exchange (ETDEWEB)

Pavelková, Tereza [Czech Technical University in Prague, Faculty of Nuclear Sciences and Physical Engineering, Břehová 7, 115 19 Praha 1 (Czech Republic); Čuba, Václav, E-mail: vaclav.cuba@fjfi.cvut.cz [Czech Technical University in Prague, Faculty of Nuclear Sciences and Physical Engineering, Břehová 7, 115 19 Praha 1 (Czech Republic); Visser-Týnová, Eva de [Nuclear Research and Consultancy Group (NRG), Research & Innovation, Westerduinweg 3, 1755 LE Petten (Netherlands); Ekberg, Christian [Nuclear Chemistry/Industrial Materials Recycling, Chalmers University of Technology, SE-412 96 Göteborg (Sweden); Persson, Ingmar [Department of Chemistry and Biotechnology, Swedish University of Agricultural Sciences, P.O. Box 7015, SE-750 07 Uppsala (Sweden)

2016-02-15

Photochemically-induced preparation of nano-powders of crystalline uranium and/or thorium oxides and their subsequent pelletizing has been investigated. The preparative method was based on the photochemically induced formation of amorphous solid precursors in aqueous solution containing uranyl and/or thorium nitrate and ammonium formate. The EXAFS analyses of the precursors shown that photon irradiation of thorium containing solutions yields a compound with little long-range order but likely “ThO{sub 2} like” and the irradiation of uranium containing solutions yields the mixture of U(IV) and U(VI) compounds. The U-containing precursors were carbon free, thus allowing direct heat treatment in reducing atmosphere without pre-treatment in the air. Subsequent heat treatment of amorphous solid precursors at 300–550 °C yielded nano-crystalline UO{sub 2}, ThO{sub 2} or solid (Th,U)O{sub 2} solutions with high purity, well-developed crystals with linear crystallite size <15 nm. The prepared nano-powders of crystalline oxides were pelletized without any binder (pressure 500 MPa), the green pellets were subsequently sintered at 1300 °C under an Ar:H{sub 2} (20:1) mixture (UO{sub 2} and (Th,U)O{sub 2} pellets) or at 1600 °C in ambient air (ThO{sub 2} pellets). The theoretical density of the sintered pellets varied from 91 to 97%. - Highlights: • Photochemically prepared UO{sub 2}/ThO{sub 2} nano-powders were pelletized. • The nano-powders of crystalline oxides were pelletized without any binder. • Pellets were sintered at 1300 °C (UO{sub 2} and (Th,U)O{sub 2}) or 1600 °C (ThO{sub 2} pellets). • The theoretical density of the sintered pellets varies from 91 to 97%.

Characterization of oxalate-based 237NpO2 powder

International Nuclear Information System (INIS)

Rankin, D.T.; Burney, G.A.; Smith, P.K.; Sisson, R.D.

1976-01-01

238 Pu, a radioisotope heat source, is produced by irradiating reactor targets containing 237 NpO 2 . The neptunium oxide is obtained by precipitating and calcining 237 Np(IV) oxalate. The effects of oxalate precipitation parameters on particle morphology and size distribution of 237 NpO 2 powder were established to provide process controls for fabricating reactor targets

Synthesis, Structure, and Rigid Unit Mode-like Anisotropic Thermal Expansion of BaIr2In9.

Science.gov (United States)

Calta, Nicholas P; Han, Fei; Kanatzidis, Mercouri G

2015-09-08

This Article reports the synthesis of large single crystals of BaIr2In9 using In flux and their characterization by variable-temperature single-crystal and synchrotron powder X-ray diffraction, resistivity, and magnetization measurements. The title compound adopts the BaFe2Al9-type structure in the space group P6/mmm with room temperature unit cell parameters a = 8.8548(6) Å and c = 4.2696(4) Å. BaIr2In9 exhibits anisotropic thermal expansion behavior with linear expansion along the c axis more than 3 times larger than expansion in the ab plane between 90 and 400 K. This anisotropic expansion originates from a rigid unit mode-like mechanism similar to the mechanism of zero and negative thermal expansion observed in many anomalous thermal expansion materials such as ZrW2O8 and ScF3.

Characterization of UO{sub 2}, a) Characterization of UO{sub 2} powder; b) Investigation of U-O system by DDK and TGA methods; Karakterizacija UO{sub 2}, a) Karakterizacija praha UO{sub 2}; b) Ispitivanje sistema U-O metodama DDK i TGA

Energy Technology Data Exchange (ETDEWEB)

Ristic, M M [Institute of Nuclear Sciences Vinca, Laboratorija za reaktorske materijale, Beograd (Serbia and Montenegro)

1962-10-15

The objectives of the study of U-O powder system were: detailed characterization of the UO{sub 2} powder which will be used for studying the sintering process, and more detailed properties of the U-O system (thermodynamic aspects of oxidation kinetics). Study of the physical and chemical properties of UO{sub 2} powder were performed and then oxidation kinetics of UO{sub 2} {yields}U{sub 3}O{sub 7} was investigated. Detailed qualitative DDK analysis was done. Owing to the TGA equipment there was a possibility to obtain U{sub 3}O{sub 7} study of U{sub 3}O{sub 7} {yields} U{sub 3}O{sub 8} oxidation was possible.

Preliminary study in development of glass-ceramic based on SiO2-LiO2 system, starting of different SiO2 starting powders

International Nuclear Information System (INIS)

Daguano, J.K.M.F.; Santos, F.A.; Santos, C.; Marton, L.F.M.; Conte, R.A.; Rodrigues Junior, D.; Melo, F.C.L.

2009-01-01

In this work, lithium disilicate glass-ceramics were developed starting of the rice ash- SiO 2 and Li 2 CO 3 powders. The results were compared with glass ceramics based on the lithium disilicate obtained by commercial SiO 2 powders. Glass were melted at 1580 deg C, and annealed at 850 deg C. X-Ray diffraction and scanning electron microscopy were used for characterization of the materials, and hardness and fracture toughness were evaluated using Vickers indentation method. Glasses with amorphous structure were obtained in both materials. After annealing, 'rice-ash' samples presented Li 2 SiO 3 and residual SiO 2 as crystalline phases. On the other side, commercial SiO 2 - Samples presented only Li 2 Si 2 O 5 as crystalline phases and the better results of hardness and fracture toughness. (author)

(Bi, Pb).sub.2, Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x superconductor and method of making same utilizing sinter-forging

Science.gov (United States)

Chen, Nan; Goretta, Kenneth C.; Lanagan, Michael T.

1998-01-01

A (BiPb).sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x (Bi223) superconductor with high J.sub.c, phase purity, density and mechanical strength is formed from Bi2223 powder which is synthesized from a mixture of Bi.sub.2 O.sub.3, PbO, SrCO.sub.3, CaCo.sub.3 and CuO. The mixture is milled, then dried and calcined to synthesize the Bi2223 powder with the desired phase purity. The calcination is performed by heating the dried mixture for 50 hours at 840.degree. C. The partially synthesized powder is then milled for 1-4 hours before calcining further for another 50 hours at 855.degree. C. to complete the synthesis. After calcination, the Bi2223 powder is cold pressed to a predetermined density and sinter forged under controlled temperature and time to form a Bi2223 superconductor with the desired superconducting properties.

(Bi, Pb){sub 2}Sr{sub 2}Ca{sub 2}Cu{sub 3}O{sub x} superconductor and method of making same utilizing sinter-forging

Science.gov (United States)

Chen, N.; Goretta, K.C.; Lanagan, M.T.

1998-10-13

A (BiPb){sub 2}Sr{sub 2}Ca{sub 2}Cu{sub 3}O{sub x}(Bi223) superconductor with high J{sub c}, phase purity, density and mechanical strength is formed from Bi2223 powder which is synthesized from a mixture of Bi{sub 2}O{sub 3}, PbO, SrCO{sub 3}, CaCo{sub 3} and CuO. The mixture is milled, then dried and calcined to synthesize the Bi2223 powder with the desired phase purity. The calcination is performed by heating the dried mixture for 50 hours at 840 C. The partially synthesized powder is then milled for 1--4 hours before calcining further for another 50 hours at 855 C to complete the synthesis. After calcination, the Bi2223 powder is cold pressed to a predetermined density and sinter forged under controlled temperature and time to form a Bi2223 superconductor with the desired superconducting properties. 5 figs.

Thermal analysis of formation of nano-crystalline BaTiO3 using Ba(NO32 and TiO2

Directory of Open Access Journals (Sweden)

Md. Jawed Ansaree

2015-12-01

Full Text Available The reaction of Ba(NO32 with TiO2 was studied by thermogravimetric (TG and differential scanning calorimetric (DSC techniques up to 1000 °C and in nitrogen atmosphere. It was found that the formation of BaTiO3 takes place above 600 °C and that precursor mixing time and heating rate have no effect on the reaction temperature. BaTiO3 powder was prepared by calcination of Ba(NO32 and TiO2 precursor mixture at 800 °C for 8 h. X-ray diffraction analysis of the synthesized BaTiO3 confirmed the formation of tetragonal phase with lattice parameters a = 3.9950±0.0003 Å and c = 4.0318±0.0004 Å. Thermal analysis of the synthesized BaTiO3 powder showed weight loss within temperature range 40–1000 °C of only 0.40%. This small amount of weight loss was connected with some impurity phase, and identified as BaCO3 using Fourier transform infrared (FTIR technique.

Heat generation ability in AC magnetic field of nano MgFe2O4-based ferrite powder prepared by bead milling

International Nuclear Information System (INIS)

Hirazawa, Hideyuki; Aono, Hiromichi; Naohara, Takashi; Maehara, Tsunehiro; Sato, Mitsunori; Watanabe, Yuji

2011-01-01

Nanosized MgFe 2 O 4 -based ferrite powder having heat generation ability in an AC magnetic field was prepared by bead milling and studied for thermal coagulation therapy applications. The crystal size and the particle size significantly decreased by bead milling. The heat generation ability in an AC magnetic field improved with the milling time, i.e. a decrease in crystal size. However, the heat generation ability decreased for excessively milled samples with crystal sizes of less than 5.5 nm. The highest heat ability (ΔT=34 o C) in the AC magnetic field (370 kHz, 1.77 kA/m) was obtained for fine MgFe 2 O 4 powder having a ca. 6 nm crystal size (the samples were milled for 6-8 h using 0.1 mm φ beads). The heat generation of the samples was closely related to hysteresis loss, a B-H magnetic property. The reason for the high heat generation properties of the samples milled for 6-8 h using 0.1 mm φ beads was ascribed to the increase in hysteresis loss by the formation of a single domain. Moreover, the improvement in heating ability was obtained by calcination of the bead-milled sample at low temperature. In this case, the maximum heat generation (ΔT=41 o C) ability was obtained for a ca. 11 nm crystal size sample was prepared by crystal growth during the sample calcination. On the other hand, the ΔT value for Mg 0.5 Ca 0.5 Fe 2 O 4 was synthesized using a reverse precipitation method decreased by bead milling. - Research Highlights: →The crystal and particle size for MgFe 2 O 4 based ferrite were decreased by bead milling. →The highest heat ability was obtained for MgFe 2 O 4 having a ca. 6 nm crystal size. →This high heat generation ability was ascribed to the increase in hysteresis loss. →Hysteresis loss was increased by the formation of a single domain.

The effect of anion on the magnetic properties of nanocrystalline NiO synthesized by homogeneous precipitation

International Nuclear Information System (INIS)

Ranga Rao Pulimi, V.; Jeevanandam, P.

2009-01-01

The effect of using different anions (nitrate, chloride, sulfate, and acetate) during the precursor synthesis, by homogeneous precipitation, on the magnetic properties of the final product (nanocrystalline NiO), has been studied. The precursors and the oxide were characterized by various analytical techniques including powder X-ray diffraction, FT-IR spectroscopy, thermal gravimetry (TGA), and magnetic measurements. The synthesized NiO samples possess crystallite size in the range, ∼2-6 nm, depending on the anion of the nickel salt. The nickel oxide nanoparticles exhibit superparamagnetic behavior. Acetate and sulfate anions lead to NiO with higher saturation magnetization (∼1.2-1.8 emu/g), while chloride and nitrate anions lead to NiO nanoparticles with lower saturation magnetization (∼0.1-0.4 emu/g) values. The observed magnetic behavior has been attributed to the size effect.

The effect of anion on the magnetic properties of nanocrystalline NiO synthesized by homogeneous precipitation

Energy Technology Data Exchange (ETDEWEB)

Ranga Rao Pulimi, V. [Department of Chemistry, Indian Institute of Technology Roorkee, Roorkee 247667 (India); Jeevanandam, P. [Department of Chemistry, Indian Institute of Technology Roorkee, Roorkee 247667 (India)], E-mail: jeevafcy@iitr.ernet.in

2009-09-15

The effect of using different anions (nitrate, chloride, sulfate, and acetate) during the precursor synthesis, by homogeneous precipitation, on the magnetic properties of the final product (nanocrystalline NiO), has been studied. The precursors and the oxide were characterized by various analytical techniques including powder X-ray diffraction, FT-IR spectroscopy, thermal gravimetry (TGA), and magnetic measurements. The synthesized NiO samples possess crystallite size in the range, {approx}2-6 nm, depending on the anion of the nickel salt. The nickel oxide nanoparticles exhibit superparamagnetic behavior. Acetate and sulfate anions lead to NiO with higher saturation magnetization ({approx}1.2-1.8 emu/g), while chloride and nitrate anions lead to NiO nanoparticles with lower saturation magnetization ({approx}0.1-0.4 emu/g) values. The observed magnetic behavior has been attributed to the size effect.

Redox reaction between graphene oxide and In powder to prepare In2O3/reduced graphene oxide hybrids for supercapacitors

Science.gov (United States)

Xu, Xiaoyang; Wu, Tao; Xia, Fengling; Li, Yi; Zhang, Congcong; Zhang, Lei; Chen, Mingxi; Li, Xichuan; Zhang, Li; Liu, Yu; Gao, Jianping

2014-11-01

A facile and quick route for the chemical reduction of graphene oxide (GO) using In powder as a reductant has been established. The reduction of GO by In powder is traced by UV-visible absorption spectroscopy, and the obtained reduced graphene oxide (rGO) is analyzed. The In3+ ions produced during the reaction between the GO and the In powder are chemically transformed to In2O3 and then form In2O3/rGO hybrids. The In2O3/rGO hybrids are used as electrode materials and their electrochemical performance are studied using cyclic voltammetry and galvanostatic charge/discharge. The In2O3/rGO hybrids demonstrate excellent electrochemical performance and their highest specific capacitance is 178.8 F g-1 which is much higher than that of either In2O3 or rGO. In addition, the In2O3/rGO hybrids are also very stable.

The magnetic and colloidal properties of CoFe2O4 nanoparticles synthesized by co-precipitation.

Science.gov (United States)

Gyergyek, Sašo; Drofenik, Miha; Makovec, Darko

2014-01-01

Magnetic CoFe(2)O(4) nanoparticles were synthesized by co-precipitation at 80 °C. This co-precipitation was achieved by the rapid addition of a strong base to an aqueous solution of cations. The investigation of the samples that were quenched at different times after the addition of the base, using transmission electron microscopy (TEM) coupled with energy-dispersive X-ray spectroscopy (EDXS) and X-ray powder diffractometry, revealed the formation of a Co-deficient amorphous phase and Co(OH)(2), which rapidly reacted to form small CoFe(2)O(4) nanoparticles. The nanoparticles grew with the time of aging at elevated temperature. The colloidal suspensions of the nanoparticles were prepared in both an aqueous medium and in a non-polar organic medium, with the adsorption of citric acid and ricinoleic acid on the nanoparticles, respectively. The measurements of the room-temperature magnetization revealed the ferrimagnetic state of the CoFe(2)O(4) nanoparticles, while their suspensions displayed superparamagnetic behaviour.

Photocatalytic degradation of diethyl phthalate using TiO{sub 2} nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Singla, Pooja, E-mail: pooja.singla@thapar.edu; Pandey, O. P., E-mail: pooja.singla@thapar.edu; Singh, K., E-mail: pooja.singla@thapar.edu [School of Physics and Materials Science, Thapar University, Patiala-147004 (India)

2014-04-24

TiO{sub 2} nanoparticles predominantly in rutile phase are synthesized by ultrasonication assisted sol-gel method. TiO{sub 2} powder is characterized using X-ray powder diffraction and UV-vis diffuse reflectance. TiO{sub 2} is used as catalyst in photocatalytic degradation of Diethyl Phthalate. TiO{sub 2} exhibits good photocatalytic activity for the degradation of diethyl phthalate.

Facile synthesis of core-shell Cu2O@ ZnO structure with enhanced photocatalytic H2 production

Science.gov (United States)

Zhang, Yong-Hui; Jiu, Bei-Bei; Gong, Fei-Long; Lu, Kuan; Jiang, Nan; Zhang, Hao-Li; Chen, Jun-Li

2018-05-01

Core-shell Cu2O@ZnO composites were synthesized successfully based on a one-pot hydrothermal method in the presence of dioctyl sulfosuccinate sodium salt (AOT) surfactant. The Cu2O can be converted to rough core-shell Cu2O@ZnO structure by adjusting the amount of zinc powder added. The as-synthesized Cu2O@ZnO composites exhibited excellent photocatalytic activity and the amount of H2 generated using these composites was 4.5-fold more than that produced with Cu2O cubes. A possible photocatalytic mechanism for the Cu2O@ZnO composites with enhanced photocatalytic activity could be the separation by ZnO of the effective charge carriers.

Syntheses and characterizations of LiFePO4 powders

OpenAIRE

Jugović, Dragana; Kuzmanović, Maja; Mitrić, Miodrag; Cvjetićanin, Nikola; Uskoković, Dragan

2011-01-01

The olivine type compositions LiMPO4 (M = Fe, Mn, Co) are among the most attractive materials for the positive electrode of lithium-ion battery. The benefits of using LiFePO4 are excellent cycle life, high structural stability, low cost and environmental friendliness. Here will be presented our efforts to obtain LiFePO4 powders through several synthesis methods. The differences in phase purity, microstructure, morphology, and electrochemical performances of synthesized powders were investigat...

Synthesis, characterization and degradation activity of Methyl orange Azo dye using synthesized CuO/α-Fe2O3 nanocomposite

Directory of Open Access Journals (Sweden)

Mohsen Mehdipour Ghazi

2017-04-01

Full Text Available This study investigated the photo-degradation of methyl orange (MO as a type of azo dye using a CuO/α-Fe2O3 nanocomposite. A CuO/α-Fe2O3 powder with a crystalline size in the range of 27-49 nm was successfully prepared using simple co-precipitation along with a sonication method. The characterization of the synthesized sample was done via XRD, FE-SEM, EDS, FTIR and DRS analyses. The Tauc equation revealed that the band gap of the nano composite in the direct mood was 2.05 ev, which is in the visible light range. The effect of operating factors containing dye concentration, photocatalyst dosage and pH on dye degradation efficiency was measured. Response Surface Method (RSM was employed to specify the parameter effects. The photocatalytic activity of the CuO/α-Fe2O3 nanocomposite was evaluated by degradation of MO under visible light irradiation. The results showed that the pH value played a very effective role in the dye degradation process efficiency. Also, the photocatalytic degradation of MO obtained was equal to 88.47% in the optimal values.

Neutron powder diffraction study of nuclear and magnetic structures of oxidized and reduced YBa2Fe3O8+w

International Nuclear Information System (INIS)

Karen, P.; Kjekshus, A.; Huang, Q.; Karen, V.L.; Lynn, J.W.; Rosov, N.; Natali Sora, I.; Santoro, A.

2003-01-01

YBa 2 Fe 3 O 8+w has been investigated by neutron powder diffraction as function of temperature and oxygen nonstoichiometry close to the limits of the homogeneity range, -0.24 0) in the structural layers of Y, or by creating oxygen vacancies (w 2 Cu 3 O 6+w' upon oxidation. The effects of nonstoichiometry on these related crystal structures are discussed in terms of bond-valence sums. The cooperative magnetic structure for all compositions is based on a larger cell related to the nuclear cell by the transformation matrix (11-bar0/110/002), having orthorhombic symmetry when the nuclear structure is tetragonal and monoclinic symmetry when the nuclear structure is orthorhombic. The iron moments are coupled antiferromagnetically in all three directions, the Neel temperature is almost constant as a function of w (T N ∼660 K), and so is also the low-temperature saturation moment μ AF ∼4.0μ B

K{sub 2}MnF{sub 5}·H{sub 2}O as reactant for synthesizing highly efficient red emitting K{sub 2}TiF{sub 6}:Mn{sup 4+} phosphors by a modified cation exchange approach

Energy Technology Data Exchange (ETDEWEB)

Han, Tao, E-mail: danbaiht@126.com; Wang, Jun; Lang, Tianchun; Tu, Mingjing; Peng, Lingling

2016-11-01

As reactant for synthesizing K{sub 2}TiF{sub 6}:Mn{sup 4+} phosphors, the cross-shaped and cuboid-shaped K{sub 2}MnF{sub 5}·H{sub 2}O powders were prepared by the simple chemical method. Based on the reaction mechanism, oxidizing K{sub 2}MnF{sub 5}·H{sub 2}O (Mn{sup 3+}) to Mn{sup 4+} by KMnO{sub 4} (Mn{sup 7+}), a modified cation exchange approach for synthesizing highly efficient red emitting K{sub 2}TiF{sub 6}:Mn{sup 4+} phosphor was proposed. The obtained K{sub 2}TiF{sub 6}:Mn{sup 4+} (2.7–5.3 at.%) phosphors have the size of 30–80 μm with a rough surface, their emission spectra consist of five narrow bands extending from 580 to 660 nm with the strongest peak at 634.8 nm, whose relative emitting intensity depends on the molar ratio of KMnO{sub 4} to K{sub 2}MnF{sub 5}·H{sub 2}O (the platform value = 3.2), and two broad excitation bands are peaking at ∼365 nm and ∼460 nm. The internal quantum yield of our synthesized K{sub 2}TiF{sub 6}:Mn{sup 4+} phosphors is up to 82.5%, which is higher than the commercial CaAlSiN{sub 3}:Eu{sup 2+} value, their excitation bands peak at ∼460 and ∼365 nm are consistent with those of Y{sub 3}A{sub 5}O{sub 12}:Ce{sup 3+} phosphors and their emission bands are more suitable for the sensitivity curve of photopic human vision. In addition, our synthesized phosphors show better thermal quenching properties. These findings show a large potential of the synthesized K{sub 2}TiF{sub 6}:Mn{sup 4+} phosphors for commercialization. - Highlights: • We synthesize the cross-shaped and cuboid-shaped K{sub 2}MnF{sub 5}·H{sub 2}O. • K{sub 2}MnF{sub 5}·H{sub 2}O is as a reactant for synthesizing K{sub 2}TiF{sub 6}:Mn{sup 4+} phosphors. • K{sub 2}TiF{sub 6}:Mn{sup 4+} will improve the current white LED with high CRI for indoor lighting.

A potential route to synthesize imporous MgB{sub 2} bulks by pretreatment of B powder at ambient pressure

Energy Technology Data Exchange (ETDEWEB)

Pan, X F; Zhou, J D; Zhao, Y [Key Laboratory of Magnetic Levitation and Maglev Trains (Ministry of Education of China), Superconductivity R and D Center (SRDC), Mail Stop 165, Southwest Jiaotong University, Chengdu, Sichuan 610031 (China); Cheng, C H [Superconductivity Research Group, School of Materials Science and Engineering, University of New South Wales, Sydney, 2052 NSW (Australia)], E-mail: yzhao@home.swjtu.edu.cn

2009-04-15

Imporous MgB{sub 2} bulks with a density of 1.82 g cm{sup -3} have been synthesized by pretreatment of B powder in an in situ solid-state reaction at ambient pressure. The results show that the MgB{sub 2} with B powder pretreatment has a significant improvement in J{sub c}, B{sub irr}, microstructure and intergranular coupling, but with no decrease of T{sub c}. At 20 K and 4 T, the J{sub c} is enhanced by 4 times by the pretreatment of the B powder. For the B pretreated MgB{sub 2}, the B{sub irr} at 20 K reaches 5 T and J{sub c} at 10 K and 6 T reaches 2200 A cm{sup -2}, compared to 4.2 T and 670 A cm{sup -2} for the B-not-pretreated MgB{sub 2}. It is argued that the small amounts of highly dispersed carbon in B powder may enhance the mobility of B particles during the reaction of B and Mg, which avoids the formation of voids in the positions of Mg particles.

In-Situ Synchrotron Radiation Study of Formation and Growth of Crystalline CexZr1-xO2 Nanoparticles Synthesized in Supercritical Water

DEFF Research Database (Denmark)

Tyrsted, Christoffer; Becker-Christensen, Jacob; Hald, Peter

2010-01-01

-zirconia system, the growth of ceria and zirconia nanoparticles is fundamentally different under supercritical water conditions. For comparison, ex situ synthesis has also been performed using an in-house supercritical flow reactor. The resulting samples were analyzed using PXRD, small-angle X-ray scattering......In situ synchrotron powder X-ray diffraction (PXRD) measurements have been conducted to follow the nucleation and growth of crystalline CexZr1-xO2 nanoparticles synthesized in supercritical water with a full substitution variation (x = 0, 0.2, 0.5, 0.8, and 1.0). Direction-dependent growth curves...... are determined and described using reaction kinetic models. A distinct change in growth kinetics is observed with increasing cerium content. For x = 0.8 and 1.0 (high cerium content), the growth is initially limited by the surface reaction kinetics; however, at a size of ∼6 nm, the growth changes and becomes...

Zeolitic adsorbent synthesized from powdered waste porcelain, and its capacity for heavy metal removal

International Nuclear Information System (INIS)

Wajima, T.; Ikegami, Y.

2006-01-01

A zeolitic adsorbent was synthesized from powdered waste porcelain kept at 80 o C for 24 h. The product contained the zeolite phases Na-P1 and hydroxysodalite. The product with the highest cation exchange capacity (CEC) was synthesized using 4 M NaOH and the sample weight / volume of alkali solution ratio was 1/4. The highest CEC obtained for the product was almost 1900 mmol/kg, which is the same as that of natural zeolite. The product with the highest CEC was tested for its ability to remove heavy metals (Fe, Cu, Ni, Zn, Pb, Cd, Mn, Cr, Al, B,Mo) from an acidic solution (pH 2). The product can neutralize the acidic solution to almost pH 7, and the capacity of the product for the removal of heavy metals is higher than that of the natural zeolite, except for Mo and B. (authors)

Synthesis and characterization of superconducting YBCO powder

International Nuclear Information System (INIS)

Praveen, B.; Karki, T.; Krishnamoorthi, J.

2008-01-01

Full text: Superconducting yttrium barium copper oxide power has been synthesized through solid state sintering method - milling and sintering - using Y 2 O 3 , BaCo 3 and CuO powders. XRD result of the milled and sintered powder reveals that the powder that has formed contains YBa 2 Cu 3 O 6.5 superconducting phase. Results obtained by SEM/EDAX show the distribution of the different elements. Experiments carried out by intermediate firing and final annealing in oxygen controlled atmosphere show the diffusion of oxygen in preformed YBa 2 Cu 3 O 6.5 and their results are discussed

Fabrication and properties of La{sub 2-x}Gd{sub x}Hf{sub 2}O{sub 7} transparent ceramics

Energy Technology Data Exchange (ETDEWEB)

Wang, Zhengjuan [State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Zhou, Guohong, E-mail: sic_zhough@mail.sic.ac.cn [State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); Zhang, Fang; Qin, Xianpeng [State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); Ai, Jianping [State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Wang, Shiwei, E-mail: swwang51@mail.sic.ac.cn [State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China)

2016-01-15

La{sub 2-x}Gd{sub x}Hf{sub 2}O{sub 7} (x=0–2.0) transparent ceramics were fabricated through vacuum sintering from nano-powders synthesized by a simple combustion method. The phase composition of the powders and final ceramics, the in-line transmittance, microstructures and density of the ceramics were investigated. With the increasing of Gd content, the ceramics maintained the cubic pyrochlore structure, and the lattice parameters decreased, whilst the densities increased linearly. All the ceramics were transparent. The highest in-line transmittance was 76.1% at 800 nm (x=1.2). With high density (7.91–8.88 g/cm{sup 3}) and effective atomic number, some of the La{sub 2-x}Gd{sub x}Hf{sub 2}O{sub 7} (x=0–2.0) transparent ceramics are promising candidates for scintillator hosts. - Highlights: • A new series of La{sub 2-x}Gd{sub x}Hf{sub 2}O{sub 7} transparent ceramics were fabricated by vacuum sintering using combustion-synthesized powders. • All the ceramics are transparent and the in-line transmittance can reach to 76.1% at 800 nm when x=1.2. • The Gd content has effects on the crystal structure, in-line transmittance, microstructures and densities of the ceramics. • With high density (7.91~8.88 g/cm3) and effective atomic number, some of the La2-xGdxHf2O7 transparent ceramics are promising candidates for scintillator hosts.

Low-temperature synthesis of ZrB2 powder from oxides using Na

Directory of Open Access Journals (Sweden)

Haruhiko Morito

2017-12-01

Full Text Available ZrB2 was synthesized by heating a mixture of ZrO2, B2O3, and Na in a molar ratio of 1:1:5 at 873–1273 K. While unreacted ZrO2 remained in the sample synthesized at 873 K, single phase ZrB2 powders were obtained at temperatures ≥1073 K. The diameters of the ZrB2 particles obtained at 1073 and 1273 K were 0.1–20 and 10–100 μm, respectively. Single phase ZrB2 was also obtained at 873 K when the starting material was rich in B2O3 and Na (ZrO2:B2O3:Na = 1:5:15. This route yielded fine particle aggregates of ZrB2, which were found to be <0.1 μm in size.

Directed laser processing of compacted powder mixtures Al2O3-TiO2-Y2O3

Directory of Open Access Journals (Sweden)

Vlasova M.

2013-01-01

Full Text Available The phase formation, microstructure and surface texture of laser treated ternary powder mixtures of Al2O3-TiO2-Y2O3 had been studied. Rapid high temperature heating and subsequent rapid cooling due to the directed movement of the laser beam forms concave ceramic tracks. Phase composition and microstructure of the tracks depends on the Al2O3 content and the TiO2/Y2O3 ratio of the initial mixtures. The main phases observed are Y3Al5O12, Y2Ti2O7, Al2O3 and Al2TiO5. Due to the temperature gradient in the heating zone, complex layered structures are formed. The tracks consist of three main layers: a thin surface layer, a layer of crystallization products of eutectic alloys, and a lower sintered layer. The thickness of the crystallization layer and the shrinkage of the irradiation zone depend on the amount of Y3Al5O12 and Al2O3 crystallized from the melt.

Microwave hydrothermal synthesis and characterization of PZT 52/48 powders

International Nuclear Information System (INIS)

Teixeira, G.F.; Gasparotto, G.; Santos, N.A.; Zaghete, M.A.; Varela, J.A.; Longo, E.

2009-01-01

Full text: Lead Zirconate Titanate (PZT) is a ceramic witch has great interest because of their ferroelectric, piezoelectric, and other electrical properties. In this work Pb(ZrxTi1-x)O3 powders were synthesized by microwave hydrothermal synthesis (M-H) at 180°C without excess lead content. This method allows obtaining particles whit nanometer size, good stoichiometric controls, high purity and crystalline degree at low temperatures and short times of synthesis. Powders were synthesized with molar concentration of 0.15 mol.L -1 during different times: 30 min, 2, 4, 6 and 8 h. After that the powders were characterized by X-ray diffraction (XRD), Field Emission Gun (FEG) and photoluminescence (PL). Through analysis it is observed that the crystalline phase of PZT is obtained from 2 hours of synthesis and this same time also presents more intense PL emission. (author)

Enhanced PL and EL properties of Alq3/nano-TiO2 with the modification of 8-vinyl POSS

Science.gov (United States)

Li, Jie; Xie, Bing; Xia, Kai; Zhao, Chunmao; Li, Yingchun; Hu, Shengliang

2018-04-01

In this study, tris (8-hydroxyquinoline) aluminum/nano-titanium dioxide (Alq3/nano-TiO2) composites were synthesized using a simply in-situ process with 8-vinyl polyhedral oligomeric silsesquioxane (POSS) as a modifier. The as-prepared Alq3/nano-TiO2 composites were characterized by X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS) and ultraviolet visible (UV-vis) absorption spectra. The effect of modification on luminescence properties for the samples was studied by photoluminescence (PL) spectra, electroluminescence (EL) spectra and time-resolved luminescence decay curves. Organic light emitting diodes (OLEDs) with the corresponded emitting layer structure were investigated. The results show that the amphiphilicity of the 8-vinyl POSS leads to well-dispersion state of the nano-TiO2 in the Alq3. Adding a proper weight percentage of 8-vinyl POSS is beneficial for the PL and EL properties enhancement of the composites. OLED using the Alq3/nano-TiO2 with 1 wt% 8-vinyl POSS emitting layer has the low turn-on voltage (4.7 V at 1 cd/m2), high maximum luminance (7463 cd/m2 at 8.75 V), and high luminous efficiency (1.13 cd/A at 100 mA/cm2). Adding 1 wt% 8-vinyl POSS in Alq3/nano-TiO2 can increase the EL intensity by a factor of 37.1 at 8 V. These values are better than those for OLEDs using the Alq3 emitting layer. The increase in luminance and current efficiency stability can be attributed to the energy transfer process between the Alq3 and the nano-TiO2, and the suppression of the self-quenching by caged 8-vinyl POSS molecules.

Sol-gel synthesis and densification of aluminoborosilicate powders. Part 2: Densification

Science.gov (United States)

Bull, Jeffrey; Selvaduray, Guna; Leiser, Daniel

1992-01-01

Aluminoborosilicate (ABS) powders, high in alumina content, were synthesized by the sol-gel process utilizing four different methods of synthesis. The effect of these methods on the densification behavior of ABS powder compacts was studied. Five regions of shrinkage in the temperature range 25-1184 C were identified. In these regions, the greatest shrinkage occurred between the gel-to-glass transition temperature (T sub g approximately equal to 835 C) and the crystallization transformation temperature (T sub t approximately equal 900 C). The dominant mechanism of densification in this range was found to be viscous sintering. ABS powders were amorphous to x-rays up to T sub t at which a multiphasic structure crystallized. No 2Al2O3.B2O3 was found in these powders as predicted in the phase diagram. Above T sub t, densification was the result of competing mechanisms including grain growth and boria fluxed viscous sintering. Apparent activation energies for densification in each region varied according to the method of synthesis.

Plasma Synthesized Doped Boron Nanopowder for MgB2 Superconductors