Combustion synthesis of CuFe2O4

Metallic ferrites are investigated as prospective materials for different applications especially as anodes in extractive metallurgy. CuFe₂O₄, one of the important ferrites, is envisaged for substituting the carbon anode in Hall-Heroult cells. A single step combustion process has been used for the synthesis of CuFe₂O₄ powder from cupric nitrate, ferric nitrate and urea. The experimental conditions for maximum conversion efficiency of the precursor powders have been optimized. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) have confirmed the formation, structure and homogeneity of the as-prepared powders. The detailed physical, electrical and structural characterization of the materials have been carried out for the specimens obtained on sintering at different temperatures up to 1000 °C.     

Molten salt synthesis of ZnNb2O6 powder

Pure ZnNb₂O₆ powder was successfully prepared by the molten salt synthesis method using Nb₂O₅ 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 ZnNb₂O₆ powder can be obtained by the molten salt synthesis method at 600 °C, and the SEM photographs show that the grains of the powder are rod-like particles.     

Molten salt synthesis of single-crystal Co3O4 nanorods

The synthesis of the single-crystal Co₃O₄ nanorods by molten salt approach was reported for the first time. The products were characterized by Transmission electron microscopy (TEM), X-ray diffraction (XRD), High-resolution transmission electron microscopy (HRTEM) and Selected-area electron diffraction (SAED). TEM results indicate that these nanorods have diameters of about 150 nm and lengths of about 2 μm. According to the analysis of the SAED and HRTEM results, we drew the conclusion that these nanorods grew along an unusual [− 1,− 1,15] direction by Ostwald ripening mechanism.     

Morphology-controlled synthesis of CdWO4 nanorods and nanoparticles via a molten salt method

Cadmium tungstate (CdWO₄) nanoparticles and nanorods have been successfully synthesized by a molten salt method at 270 °C, and the morphology of the nanocrystals can be controlled by adjusting such reaction conditions as the calcined time and the weight ratio of the salt to the CdWO₄ precursor. The resultant sample is a pure phase of CdWO₄ without any other impurities.     

Ultra-fast synthesis and enhanced photocatalytic properties of alpha-Fe2O3/ZnO core-shell structure

Spindle-like α-Fe₂O₃/ZnO core-shell structures were synthesized by a simple two-step method of microwave hydrothermal synthesis. The as-prepared products were characterized by X-ray diffraction, transmission electron microscopy, high-resolution TEM and selected area electron diffraction. Furthermore, photocatalytic activity was measured through the degradation of methyl orange solution. And the results of degradation reveal that the spindle-like α-Fe₂O₃/ZnO nanocomposites exhibit better photocatalytic activities (3.5 times improvement) than those of the pure spindle-like α-Fe₂O₃ under ultraviolet irradiation. A mechanism was proposed based on which the electrons excited in the photocatalytic process.     

新型氧化物(Ca_(0.85-x)Nd_xOH)_(1.16)CoO_2的水热合成及热电性能(英文)

采用水热法制备了一系列具有片状形貌的(Ca0.85OH)1.16CoO2热电材料,并研究了Nd掺杂对该材料结构及热电性能的影响.结果表明,所制备的样品均为p型材料,在473K以下,材料的热电系数随着Nd含量的增加而增大;Nd掺杂后,材料的载流子浓度和载流子迁移率均发生变化,因此材料的电导率随着Nd含量的增加先增大后减小;在573K时,(Ca0.75Nd0.1OH)1.16CoO2材料的功率因子达到7.06×10-5W/(m·K2).     

Preparation and electrical properties of Ca5Si3 and Sr5Si3 powders

Single phase Ca₅Si₃ and Sr₅Si₃ powders were prepared, and their electric and thermoelectric properties were investigated. The Ca₅Si₃ and Sr₅Si₃ powders are synthesized by exposure of the Si powders to Ca and Sr fluxes, respectively. It is found that both silicides show a p-type conduction and semiconductor-like behavior. The electronic band structures of the silicides are calculated using the first-principles total-energy calculation program in pseudopotential schemes with plane-wave basis functions. The calculated result predicts the possibility of a semiconductor-like property with a sharp pseudogap at the Fermi level for Ca₅Si₃, as experimentally obtained. The silicide would be expected to be a new semiconductor-like conducting material.     

Ca3Co4O9 ceramics consolidated by SPS process: Optimisation of mechanical and thermoelectric properties

Ca₃Co₄O₉ (349) thermoelectric (TE) oxide ceramics were successfully prepared by Spark Plasma Sintering process. The effects of the uniaxial pressure (30-100 MPa), the dwell temperature (700-900 °C) and the cooling rate were investigated. Microstructure analyses have revealed strong enhancements of the bulk density as the pressure level and the applied temperature during the SPS process are increased. Mechanical properties were investigated by using instrumented nanoindentation and three point bending tests. Hardness, elastic modulus, strength and fracture toughness were shown to improve drastically and depend on the processing parameters. Thermal expansion measurements reveal a noticeable anisotropy induced by unidirectional hot pressing. The mechanical, thermal and thermoelectric properties were correlated to the microstructure and crystallographic texture of the resulting ceramics.     

Electrical properties of thick-film NTC thermistor composed of Ni0.8Co0.2Mn2O4 ceramic: Effect of inorganic oxide binder

The thick-film NTC thermistors were prepared by screen printing Ni_0.8Co_0.2Mn₂O₄ ceramic on the alumina. The influence of inorganic oxide binder composition and thickness of thermistor layer on the thermistor constant and initial resistivity are studied. The relation between the resistivity (ρ) and the absolute temperature for the prepared thick-film thermistor comply with Arrhenius equation. The room temperature sheet resistivities of the thick films were in the range 0.56-7.45 MΩ cm and temperature sensitivity index in the range 1492-3335 K. Binder composition dependent agglomeration of microcrystallites is observed in the microstructure of the thick-film Ni_0.8Co_0.2Mn₂O₄ ceramic. The spinel ceramic was prepared by oxalate co-precipitation and sintering.     

Molten salt synthesis of Mo2C powder using a mechanically milled powder

A novel process for synthesizing ceramic powders in molten salt is presented. Dissimilar to the traditional mechanochemical process, the novel process is based on a chemical reaction in the liquid phase (molten salt). The results show that Mo₂C powder could be successfully synthesized using this method. The end-product was analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy-dispersion X-ray (EDX) spectroscopy. The mechanism of the reaction in molten salt is discussed.     

Controllable synthesis and magnetic property of BiMn2O5 crystals

Uniform submicron BiMn₂O₅ particles were prepared via a facile one-step hydrothermal route at low temperature. Bi(NO₃)₃, MnCl₂·4H₂O and KMnO₄ were used as starting materials; KOH as a pH adjustor and also as a mineralizer. Single-crystalline orthorhombic BiMn₂O₅ sample with controllable morphology was obtained. The microstructure strongly depends on the molar ratio of the starting materials, KOH concentration and reaction temperature. X-ray photoelectron spectroscopy shows the existence of Mn⁴⁺ state. Magnetic measurement indicates Néel temperature T_N at 44 K. The susceptibility above T_N obeys the Curie-Weiss law, χ = C/(T − θ), with θ = −350 K. The effective paramagnetic moment μ_eff = 4.66 μ_B/Mn, demonstrating the coexistence of mixed Mn³⁺ and Mn⁴⁺ valences.     

Large-scale fabrication of H2(H2O)Nb2O6 and Nb2O5 hollow microspheres

Hollow micro-sized H₂(H₂O)Nb₂O₆ spheres constructed by nanocrystallites have been successfully synthesized via a bubble-template assisted hydrothermal process. In the reaction process, H₂O₂ acts as a bubble generator and plays a key role in the formation of the hollow structure. An in situ bubble-template mechanism has been proposed for the possible formation of the hollow structure. The spherelike assemblies of these H₂(H₂O)Nb₂O₆ nanoparticles have been transformed into their corresponding pseudohexagonal phase Nb₂O₅ through a moderate annealing dehydration process without destroying the hierarchical structure. Optical properties of the as-prepared hollow spheres were investigated. It is exciting that the absorption edge of the hollow Nb₂O₅ microspheres shifts about 18 nm to the violet compared with bulk powders in the UV/vis spectra, indicating its superior optical properties.     

Combustion synthesis of Sr0.5Ba0.5Nb2O6 and effect of fuel on its microstructure and dielectric properties

Nano-sized Sr_0.5Ba_0.5Nb₂O₆ (SBN50) powder has been synthesized, at very short reaction time, for the first time by a novel combustion method. Ba(NO₃)₂ and Sr(NO₃)₂ were used as source of Sr and Ba, respectively, while Nb-oxalate was used as the source of niobium. Urea, hexamethyltetramine (HMT) and glycine were used as fuel. The crystallite sizes in the powder ranged between 14-125 nm. X-ray diffraction analysis showed complete SBN50 phase formation at 700 °C, when urea/HMT was used as fuel, and at 800 °C when glycine was used as fuel. Ferroelectric-paraelectric phase transition temperature (T_c) close to 40 °C was observed when urea and HMT were used and the T_c was −49 °C when glycine was used. When urea was used as fuel highest dielectric constant was observed for the pellets sintered at 1250 °C for 4 h. Low dielectric loss was observed when HMT was used as fuel. Larger grain sizes in the sintered pellets were observed when glycine was used as fuel.     

Combustion synthesis of La0.7Sr0.3Co0.5Fe0.5O3 (LSCF) porous materials for application as cathode in IT-SOFC

La_0.7Sr_0.3Co_0.5Fe_0.5O₃ (LSCF) porous materials have attracted a substantial interest for application as cathode in solid oxide fuel cells of intermediate temperature (IT-SOFC). This work investigates the effect of different propellants (urea, glycine, citric acid and sucrose) in the preparation of LSCF powders by the combustion method and also the influence of the sintering temperature on the porosity and electrical conductivity. TGA profiles of the as-prepared samples showed a lower weight loss for the sample prepared with glycine, associated with the higher combustion temperature. XRD patterns presented characteristic reflections of LSFC perovskite and a small formation of secondary phases, with nanometric crystallite sizes (9-20 nm). SEM analysis revealed the loose and porous structure of the powder materials. Densification studies were carried within 950-1100 °C, showing that porosity decreased with increasing sintering temperature. Electrical conductivity was measured in the temperature range 300-800 °C and correlated with the sintering temperature.     

Low temperature sintering and microwave dielectric properties of ZnTiNb2O8 ceramics with BaCu(B2O5) additions

The phases, microstructure and microwave dielectric properties of ZnTiNb₂O₈ ceramics with BaCu(B₂O₅) additions prepared by solid-state reaction method have been investigated using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The pure ZnTiNb₂O₈ ceramic shows a high sintering temperature of about 1250 °C. However, it was found that the addition of BaCu(B₂O₅) lowered the sintering temperature of ZnTiNb₂O₈ ceramics from above 1250 °C to 950 °C due to the BCB liquid-phase. The results showed that the microwave dielectric properties were strongly dependent on densification, crystalline phases and grain size. Addition of 3 wt% BCB in ZnTiNb₂O₈ ceramics sintered at 950 °C afforded excellent dielectric properties of ?_r = 32.56, Q × f = 20,100 GHz (f = 5.128 GHz) and τ_f = −64.87 ppm/°C. These represent very promising candidates for LTCC dielectric materials.     

Electrical properties of Ta2O5 thin films deposited on Cu

The electrical and dielectric properties of reactively sputtered Ta₂O₅ thin films with Cu as the top and bottom electrodes forming a simple metal insulator metal (MIM) structure, Cu/Ta₂O₅/Cu/n-Si, were studied. Ta₂O₅ films subjected to rapid thermal annealing (RTA) at 800°C for 30 s in N₂ ambient crystallized the film, decreased the leakage current density and resulted in reliable time-dependent dielectric breakdown characteristics. The conduction mechanism at low electric fields (<100 kV/cm) is due to Ohmic conduction; however, the Schottky mechanism becomes predominant at high fields (>100 kV/cm). Present studies demonstrate the use of Cu as a potential electrode material to replace the conventional precious metal electrodes for Ta₂O₅ storage capacitors.     

High energy density lithium ion batteries using Li2.6Co0.4 − xCuxN (anode) and Cu0.04V2O5 (cathode) electrode materials

Li_2.6Co_0.4 - xCu_xN (x = 0, 0.15) anode materials were prepared by conventional solid state reaction. Between both materials, Li_2.6Co_0.25Cu_0.15N exhibited better capacity retention than that of Li_2.6Co_0.4N. According to electrochemical impedance spectroscopy, the better cycling behavior of Li_2.6Co_0.25Cu_0.15N has been attributed to the improvement in interfacial compatibility between the electrode and electrolyte interface. A possible explanation to this was given. Li_2.6Co_0.4 - xCu_xN/Cu_0.04V₂O₅ full-cells were assembled to investigate the reliability of Li_2.6Co_0.4 - xCu_xN anode materials in practical applications. The Li_2.6Co_0.25Cu_0.15N/Cu_0.04V₂O₅ cell delivered a specific capacity of 260 mA h g^− 1, and a specific energy of 505.7 mW h g^− 1, which was much higher than that of C/LiCoO₂ lithium ion batteries.     

Molten salt synthesis of anisometric particles in the SrO-Nb2O5-BaO system

Acicular particles of KSr₂Nb₅O₁₅, Sr_0.5Ba_0.5Nb₂O₆, and SrNb₂O₆ were synthesized in the SrO-BaO-Nb₂O₅ system, using KCl or SrCl₂·6H₂O salts. In the SrCl₂·6H₂O + Nb₂O₅ system, acicular SrNb₂O₆ particles were formed by a solid state reaction between the salt and Nb₂O₅. Large, irregularly shaped (Sr-rich) Sr₂Nb₂O₇ particles formed with increasing reaction temperature and time. Small but finite solubility of SrO in the KCl + SrNb₂O₆ system favored the formation of acicular KSr₂Nb₅O₁₅ and blade-like Sr₂Nb₂O₇ particles (at higher temperatures). Uniformly sized, acicular KSr₂Nb₅O₁₅ particles were easier to reproduce compared to the formation of acicular Sr_0.5Ba_0.5Nb₂O₆ and SrNb₂O₆ particles.     

Ce掺杂Ca3Co4O9的高温热电性能

利用二次固相反应方法制备了Ce掺杂的Ca3Co4O9热电材料(CexCa3-xCo4O9,x=0、0.1、0.3),并测试了样品的微观结构和高温热电性能。测试结果表明,Ce替代Ca可有效调制Ca3Co4O9的热电参数;随着温度的升高,样品的电阻率和热导率降低,See-beck系数增大。在973K的温度下,Ce0.1Ca2.9Co4O9具有最高的热电性能(ZT=0.23)。     

Densification and properties of barium zirconate ceramics by addition of P2O5

The influences of P₂O₅ doping on the sintering behavior, phase formation and properties of barium zirconate ceramics were investigated. Unmodified BaZrO₃ was difficult to densify, even at 1600 °C. Only a porous microstructure could be obtained. However, doping BaZrO₃ with P₂O₅ markedly enhances its sinterability. 94.2% of theoretical density was achieved with the inclusion of 4 mol% P₂O₅ sintered at 1600 °C for 4 h. The bending strength of the samples sintered at 1600 °C for 4 h was improved by almost 8 times by the addition of 4 mol% P₂O₅. The average bending strength of 152.3 ± 16.7 MPa was obtained. The Vickers hardness of 4 mol% P₂O₅ modified BaZrO₃ reaches 8.8 ± 0.4 GPa.