Dielectric tunable properties of BaTi<Subscript>4</Subscript>O<Subscript>9</Subscript>-doped Ba<Subscript>0.6</Subscript>Sr<Subscript>0.4</Subscript>TiO<Subscript>3</Subscript> microwave composite ceramics

BaTi₄O₉-doped Ba_0.6Sr_0.4TiO₃ (BST) composite ceramics were prepared by the conventional solid-state reaction and their structure, dielectric nonlinear characteristics and microwave dielectric properties were investigated. The secondary phase of the orthorhombic structure Ba₄Ti₁₃O₃₀ is formed among BST composite ceramics with the increase of BaTi₄O₉. At the same time, a duplex or bimodal grains size distribution shows fine grains in a coarse grain matrix. The degree of frequency dispersion of dielectric permittivity below T _m is increased initially and then decreased with respect to BaTi₄O₉. As the BaTi₄O₉ content increases, the tunability of composite ceramics decreases, while the Q value increases. Interestingly, 70 wt% BaTi₄O₉-doped BST has a tunability ∼4.0% (under 30 kV/cm biasing) versus a permittivity ∼68 and quality factor ∼134.1 (at ∼3.2 GHz). Supported by the Ministry of Science and Technology of China through 973-project (Grant No. 2009CB623302), the Cultivation Fund of the Key Scientific and Technical Innovation Project, Ministry of Education of China (Grant No.707024), Shanghai Committee of Science and Technology (Grant No. 07DZ22302), and Shanghai Foundation Project under 06JC14070     

Cu<Subscript>2</Subscript>ZnSnS<Subscript>4</Subscript> thin films prepared by sulfurizing different multilayer metal precursors

Cu₂ZnSnS₄ (CZTS) thin films were successfully fabricated on glass substrates by sulfurizing Cu-Sn-Zn multilayer precursors, which were deposited by ion beam sputtering and RF magnetron sputtering, respectively. The structural, electrical and optical properties of the prepared films under various processing conditions were investigated in detail. Results showed that the as-deposited CZTS thin films with the precursors by both ion beam sputtering and RF magnetron sputtering have a composition near stoichiometric. The crystallization of the samples, however, has a strong dependence on the atomic percent of constituents of the prepared CZTS films. A single phase stannite-type structure CZTS with a large absorption coefficient of 10₄/cm in the visible range could be obtained after sulfurization at 520°C for 2 h. The samples relative to the RF magnetron sputtering showed a low resistivity of 0.073 Ωcm and band gap energy of about 1.53 eV. The samples relative to the ion beam sputtering exhibited a resistivity of 0.36 Ωcm and the band gap energy is about 1.51 eV. Supported by the National Natural Science Foundation of China (Grant No. 10574106), the Planned Science and Technology Project of Guangdong Province (Grant No.2003C05005) and the Natural Science Fund of Zhanjiang Normal University (Grant No.200801)     

Domain structure and defects of highly ordered Bi<Subscript>4</Subscript>Si<Subscript>3</Subscript>O<Subscript>12</Subscript> micro-crystals

Highly ordered Bi₄Si₃O₁₂ micro-crystals were prepared at normal atmosphere. Phase identification of the prepared crystals was accomplished by X-ray diffractometer (XRD). Domain structure and defects were characterized by environmental scanning electron microscopy (ESEM). XRD shows that the obtained micro-crystals are of eulytite structure with chemical formulation of Bi₄Si₃O₁₂. A highly ordered growth pattern is confirmed due to the faster growth of the {124} faces than that of the {204} faces by ESEM. The growing process of the domain structure is of pollen parent and filial generation pattern. The filial generations of Bi₄Si₃O₁₂ crystals are generated from the pollen parent. Cracks generate from the defect areas and propagate along the {124} faces due to their lower binding energy under a proper temperature gradient, contributing to the total transcrystalline fracture. It is confirmed that the generation and development of the voids in the crystal grains can be developed when unmatched dimensions of the two opposite faces are formed. And the development of the voids is dependent on the dimensions and orientations of the two opposite faces. Supported by the Innovation Research Team Funds of Shaanxi University of Science & Technology (Grant No. SUST-A04)     

Microstructure and Thermal Properties Analysis of （1-x）As2S3-x CdBr2 Glass System

The homogeneous glass sample for the ( 1 - x ) As2S3-xCdBr2, where x=0. 015,0. 035,0.05, was prepared by the conventional melt-quenched method. Amorphoas ( 1 - x ) As2S3-xCdBr2 alloys were determined by X-ray diffraction, thermal compreheasive analysis and Raman scattering. The glass transittion temperature (TR) deereases a bit with the addition of CdBr2 . Based on the experimental data, the microstrtucture is considered to be the discrete molecule species of AsBr3 and Cd - S atomic bonds or clusters are honigeneously dispersed in a disordered polymer network formed by AsS3 pyramids interlinked by sulfur bridges.     

Effect of Grain Size of CaCO3 and SiO2 on the Formation of C3S Under Different Conditions

The effect of grain size of CaCO3 and SiO2 on the formation of C3S under various conditions, such as rapid heating rate（800 ℃/min）, normal heating rate（30 ℃/min） and in the presence or absence of ZnO, was studied. The results show that the decomposition temperature of CaCO3, the temperature of appearance of liquid phase and the f-CaO content descend when the grain size of CaCO3 and SiO2 becomes smaller, which attributes to the reactive activity enhancement of powders due to the decrease of the particle size. When the grain size of CaCO3 and SiO2 is below 1 μm, the rate of the formation of C3S is greatly raised. A rapid sintering rate and the presence of ZnO have an important effect on the formation of C3S and can lower the temperature of the formation of C3S by about 50 ℃.     

Microstructure and wear behaviour of laser-induced thermite reaction Al<Subscript>2</Subscript>O<Subscript>3</Subscript> ceramic coatings on pure aluminum and AA7075 aluminum alloy

Wear-resistant laser-induced thermite reaction Al2O3 ceramic coatings can be fabricated on pure Al and AA7075 aluminum alloy by laser cladding （one-step method） and laser cladding followed by laser re-melting （two-step method） using mixed powders CuO-Al-SiO2 in order to improve the wear properties of aluminum and aluminum alloy, respectively. The microstructure of the coatings was characterized by scanning electron microscopy （SEM） and X-ray diffraction （XRD）. The wear resistance of the coatings was evaluated under dry sliding wear test condition at room temperature. Owing to the presence of hard α-Al2O3 and γ-Al2O3 phases, the coatings exhibited excellent wear resistance. In addition, the wear resistance of the coatings fabricated by two-step method is superior to that of the coatings fabricated by one-step method.     

Crystallization of Fe78Si6B13 Bulk Crystaline/Amorphous （c/a） Composite

A metallic crystalline/amorphous （c/a） bulk composite was prepared by the slow cooling method after remelting the amorphous Fe78Si9B13 ribbon. By X-ray diffraction （XRD）, differential scanning calorimetry （DSC） and scanning electron microscope （SEM）, the composite consists of the primary dendrite α-Ee （without Si） as well as the amorphous matrix. After being anneal at 800 K, the uniform spheroid particles are formed in the c/a composite, which does not form in the amorphous ribbon under the various annealing process. Energy dispersive analysis of X-rays （EDAX）, SEM and XRD were applied to give more detailed information. The formation and evolution of the particle may stimulate the possible application of the Fe-matrix amorphous alloy.     

Conformation of Organic Chain in Phase Transition of Hybrid （Cl2H25NH3）2MnCl4

The structural change in phase transition of hybrid （Cl2H25NH3）2MnCl4 was investigated. The temperature and the structures of the phase transition is investigated by thermal gravimetry （TG） and differential scanning calorimetry （DSC）, infrared spectrum （IR） and X-ray diffraction （XRD）. The results suggest that the phase transition is reversible and the structural change arises from the conformation change of the organic chain. The interlayer distance increases when the hybrid transforms from low temperature phase to high temperature phase. This is explained by the diffusion of gauche-bond along the organic chains and they move away from each other when the phase transition occurs. Combining the experimental data with theoretical calculation, we propose that organic chain of the hybrid in high temperature phase is the conformation of gauche-bond alternating with trans bond （noted as GTG＇TGTG＇TGTG＇T）.     

Molten Salt Synthesis of Ba（ Mgl／3Nb2／3 ）O3 Powder

The single-phrase Ba(Mgl/3Nb2/3)O3(BMN) powder was saccessfully prepared by the KCImolten salt synthesis(MSS) method. The temperature for single-phase BMN powders by MSS was about 400℃ lower than that by the solid-phase method. The average particle size (APS) was about 0.91,u.m at 900℃ and increased with increasing synhesis temperature. Based on the APS, the activation energy for particle growth in theMSS, whose value was 64. 1kJmol^-1.was attained. The sinterability of the powder prepared by MSS method wasbetter than that pretared by solid-phase method.     

Nanocomposite films of V<Subscript>2</Subscript>O<Subscript>5</Subscript>−MoO<Subscript>3</Subscript> xerogel with poly ethylene oxide intercalation

Poly ethylene oxide (PEO)_x−V₂O₅−V₂O₅−MoO₃ (x=0, 0.5, 1) films were prepared by the sol-gel method. The synthesis and structure of the films were investigated by XRD, TG-DTA, FTIR, etc. The results show that V₂O₅−MoO₃ xerogel has a layered structure and its interlayer space increased from 1.3181 nm at x=0 to 1. 7898 nm at x=1 after the nanocomposite films were dried, and PEO in the interlayer changes the interface structure by forming hydrogen bonds with V=0 bands. CV measurement indicates that the intercalation of PEO improves insertion/extration properties of Li⁺ ions in the interlayer. ZHENG Jin-xia: Born in 1976 Funded by the National Natural Science Foundation of China (No. 50172036) and Natural Science Foundation of Hubei Province(No. 2001ABB083)     

Preparation and Properties of Dip-coated CeO2-TiO2 Thin Golden Glass Film

The golden and ultraviolet-absorbed CeO2-TiO2 film was prepared on soda-lime glass substrate with the thickness of 2 mm via the sol-gel method. The transmission spectra in range of 200 nm-800 nm were measured, and the crystallization, the abrasion and acid resistance were also investigated. The appropriate sol contents and heat-treatment schedule were determined. The results indicate that the appropriate molar ratio of Ce/Ti was 3：5 to 5：6. The ultraviolet-absorbance ability increased with the increase of the Ce/Ti molar ratio, but when the Ce/Ti molar ratio was higher than 1.5, the homogeneity of the film was deteriorated. With the increase of heat-treatment temperature, the main wavelengths of the color of the coated glasses were equal, but the color＇ s saturation decreased; the transmission peaks were the same, while the intensity of the peaks decreased. The roughness, abrasion and acid resistance of the film were also enhanced at the same time. The appropriate heat- treatment temperature may be 340℃.     

Synthesis,characterization and catalytic application of H<Subscript>3</Subscript>PW<Subscript>12</Subscript>O<Subscript>40</Subscript>/MCM-48 in the esterification of methacrylic acid with n-butyl alcohol

A novel environmental friendly catalyst, H3PW12O40/MCM-48, was prepared by impregnation method. The catalysts were characterized by means of XRD and FT-IR. The synthesis of n-butyl methacrylate catalyzed by H3PW12O40/MCM-48 was studied with methacrylic acid and n-butyl alcohol as reactants. H3PW12O40/MCM-48 is an excellent catalyst for synthesizing n-butyl methacrylate and Keggin structure of H3PW12O40 kept unchanged after being impregnated on surface of the molecular sieve support. Effects of n（methacrylic acid）：n（n-butyl alcohol）, catalyst dosage, cyclohexane（water-stripped reagent） and reaction time on yields of the product were investigated. The optimum conditions have been found, that is, molar ratio of acid to alcohol is 1：1.6, mass ratio of catalyst used to the reactants is 0.5% and reaction time is 2.0 h. Under these conditions, the yield of n-butyl methacrylate can reach 93.7%.     

Thermoelectric Properties and Electronic Structure of Ca3Co2O6

The nanosized Ca3Co2O6 powder was synthesized via sol-gel process.The phase composition was characterized by means of X-ray diffraction.Polycfrystalline swnples of Ca3Co2O6 were prepared by a sintering procedure of nanosized power.The seebeck cofficient and electrical conductivity of the samples were measured from 450K up to 750 K.The results show that the Seebeck coefficient increases with the increasing temperature.The electronic structures were calculated using the self-cwtsistent full-potential linearized augmentedc plane-wave (LAPW) method within the density functional theory.The relationship between thermoelectric property and electronic structures was discussed.     

Surface organic modification of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> magnetic nanoparticles

The surface organic modification of Fe3O4 nanoparticles with silane coupling reagent KH570 was studied. The modified and unmodified nanoparticles were characterized by FT-IR, XPS and TEM. The spectra of FT-IR and XPS revealed that KH570 was coated onto the surface of Fe3O4 nanoparticles to get Fe-O- Si bond and an organic coating layer also was formed. Fe3O4 nanoparticles were spheres partly with mean size of 18,8 nm studied by TEM, which was consistent with the result 17.9 nm calculated by Scherrer＇s equation. KH570 was adsorbed on surface and formed chemistry bond to be steric hindrance repulsion which prevented nanoparticles from reuniting. Then glycol-based Fe3O4 magnetic liquids dispersed stably was gained.     

Enhanced Low-field Magnetoresistence in the Absence of Mn Content in Polycrystalline La0.67Ca0.33MnO3

Magnetic and electrical transport properties of the La0.67Ca0.33Mn1-xO3 （x=0-0.16）, which were prepared by the sol-gel method followed by sintering treatment at 1 450, 1 100 and 900 ℃, respectively, were investigated. Experimental results show that, with the increase of x, the resistivity of samples increases and the insulator-metal transition temperature shifts towards lower temperature. Meanwhile, the intrinsic megnetoresistance effect is weakened and the extrinsic magnetoresistance is enhanced. For the samples with x=0.16 and 0.10 sintered at 1 100 ℃ and 900 ℃, respectively, low field magnetoresistance as high as about 50% can be observed. Furthermore, for the samples sintered at 1 100 ℃ and 900 ℃, the grain size is not only controlled by about sintering temperature, but also by the absence of Mn content x.     

Controlled synthesis and magnetic properties of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> walnut spherical particles and octahedral microcrystals

Magnetite Fe₃O₄ walnut spherical particles and octahedral microcrystals were successfully synthesized from K₄ [Fe (CN)₆], K₃ [Fe (CN)₆] and NaOH reagents via a simple hydrothermal process. And the uniform morphology of octahedral microcrystals was obtained in the presence of ethylene glycol. The morphology and structure of products were characterized by powder X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The results showed that the Fe₃O₄ walnut spherical particles and octahedral microcrystals were single crystals with the face-center cubic structure and with size distributions from 2.2 to 8.6 μm and 1.6 to 12.5 μm, respectively. Their magnetic properties were detected by a vibrating sample magnetometer at room temperature. The walnut spherical particles exhibited a ferromagnetic behavior with the coercive force (Hc), saturation magnetization (Ms) and remanent magnetization (Mr) being 150.57 Oe, 97.634 and 12.05 emu/g, respectively. For the octahedral microcrystals they were 75.28 Oe, 101.90 and 6.69 emu/g, respectively. Different sizes of walnut spherical particles were controlled synthesized through adjusting the NaOH concentration. It was found that ethylene glycol molecules have a significant effect on the formation of Fe₃O₄ octahedra. A possible mechanism was also proposed to account for the growth of these Fe₃O₄ products. Supported by Fund of weinan Teachers University (Grant No. 08YKZ008), the National Natural Science Foundation of China (Grant No. 20573072) and Doctoral Fund of Ministry of Education of China (Grant No. 20060718010)     

In-situ TEM Study on Mierostruetural Evolution of Nanostruetured TiO2

The effect of electron beam on the microstructures and phase transformation of nanostructured TiO2 heat treated at various temperatures for different time was studied by in-situ TEM and SAED. Anatase ex-situ heated at 250℃ and 360℃ transformed to rutile while irradiated by the electron beam. With the increasing sizes and distribution of the powders on the amorphous carbon, the process of phase transformation by the electron beam was encumbered. These evolutions may be due to the changes of vacuum atmosphere and the properties of powders.     

Effect of Al<Subscript>2</Subscript>O<Subscript>3</Subscript> content on residual stress and properties of CAS glass-ceramics

The structure and properties of the glass-ceramics were tested with X-ray diffraction testing instrument,correlative software,and other modern testing means.Then the effect of Al2O3 content on internal stresses in CaO-Al2O3-SiO2 glass-ceramics was studied deeply.In order to study the relationship of Al2O3 to the residual stress of CaO-Al2O3-SiO2 glass-ceramics,X-ray diffraction ＂sin2ψ＂ was used.The means utilized the x radial incidence produced from cathode radial tube,and took the space between crystals as measurement of strain.When the stresses produced,the space between crystals changed and the diffraction peak moved during Bragg diffraction.The magnitude of movement is related to the stresses.The experimental results show the residual stress is considerably high and Al2O3 can influence the mechanical properties of this material hugely.     

Preparation and characterization of nanocomposite MgFe<Subscript>2</Subscript>O<Subscript>4</Subscript>/SiO<Subscript>2</Subscript>

Nanocomposites MgFe₂O₄/SiO₂ were successfully synthesized by the sol-gel method in the presence of N, N-dimethylformamide (DMF). The formation of pure MgFe₂O₄ was confirmed by powder X-ray diffraction (XRD) and electron diffraction. The structural evolution of MgFe₂O₄ nanocrystals was followed by powder X-ray diffraction and IR absorption spectroscopy. The formation of spinel structure of MgFe₂O₄ started at 800 °C, and completed at 900 °C. The transmission electron microscopy (TEM) measurements suggest that the particle sizes increase with the increasing annealing temperature, and the mean particle sizes of the spherical samples annealed at 800 °C, 900 °C and 1 050 °C are ca. 3 nm, 8 nm and 11 nm, respectively. Magnetization measurements at room temperature and 78 K indicate superparamagnetic nature of these MgFe₂O₄ nanocrystals. Funded by the National Natural Science Foundation of China(No. 30771676), the Natural Science Foundation of Jiangsu Province (No. BK20081842), and the Foundation of Nanjing Bureau of Personal for the Returned Overseas Chinese Excellent Scholars     

Optical and magnetic properties of Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>/SiO<Subscript>2</Subscript> nano-composite films

Fe₂O₃/SiO₂ nano-composite films were prepared by sol-gel technique combining heat treatment in the range of 100–900 °C. The particle size was observed by FE-SEM. Optical properties of the films were investigated by UV-visible spectra. Structural and magnetic characteristics were investigated through FT-IR and VSM. The transparency of the Fe₂O₃/SiO₂ nano-composite films decreased with the content of the Fe₂O₃. Water and organic solvent in the films were evaporated with heat treatment, so the transparency of the films was enhanced under high temperature. It is also found that the saturation magnetization (M _s) of the films increases with the temperature. As the content of the Fe₂O₃ increases, when the content of the Fe₂O₃ is around 30wt%, the M _s of the films has a maximum value.