Manufacture of high-dispersed W-Cu composite powder by mechano-thermal process

In order to improve the process of co-reduction of oxide powder, a new mechano-thermal process was designed to produce high-dispersed W-Cu composite powder by high temperature oxidation, short time high-energy milling and reduction at lower temperature. The particle size, oxygen content and their sintering abilities of W-Cu composite powder in different conditions were analyzed. The results show that after a quick milling of the oxide powder for about 3-10 h, the reduction temperature of the W-Cu oxide powder can be lowered to about 650 ℃ from 700-750 ℃ owning to the lowering of particle size of the oxide powder. The average particle size of W-Cu powder after reduction at 650 ℃ is about 0. 5μm smaller than that reduced at 750 ℃. After sintering at 1 200℃ for 1 h in hydrogen atmosphere, the relative density and thermal conductivity of final products (W-20Cu) can attain 99. 5% and 210 W ·m-1· K-1 respectively.     

Synthesis and Microstructure of Partly-oriented Bismuth Layer Structure Ferroelectrics Ceramics SrBi4Ti4O15

SrBi4Ti4O15 powder was synthesized by conventional solid state synthesis （ CS ） and molten salt synthesis （ MSS ） . MSS method can synthesize plate-like SrBi4Ti4O15 at lower temperature （900℃） than CS method. Plate-like form becomes more distinct when the synthesis temperature increases. This would help cause the grain orientation of the ceramics after sintering. The sintered samples of MSS had grain orientation at （0,0, 10） plane. The degree of （0,0,10） grain orientation F was 62.1% . Hot pressing made （0,0,10） grain orientation more distinct （ F = 85.7% ）. The microstructures of the sintered samples were detected by SEM. Due to the grain orientation the density of samples fabricated by MSS was lower than that of prepared by CS.     

Synthesis of PZT power by wet-dry method and its structure

To prepare PZT powder at lower temperature, lead zirconate titanate (PZT) powder (x(Zr)/x(Ti)=56?44) was prepared by wet-dry method. Glycol was used as the solvent, and zirconium oxychloride was used as zirconium source. The properties and structure of the powder were analyzed by XRD, SEM and Sedimentograph. The effects of sintering parameter such as sintering temperature, keeping time and heating-up velocity on structure of PZT power were investigated. The results show that homogeneous PZT with single-phase perovskite structure can be obtained after sintering at 730 ℃ for 2 h, and the average size of PZT powder is about 113 nm.     

Dielectric Properties of （AgxNa1-x）（NbyTa1-y）O3 System Prepared by Liquid Method

The dielectric properties of （AgxNa1-x）（NbyTa1-y）O3 were investigated, and its dielectric loss and capacitance were measured. The dielectric properties of nanometer （AgxNa1-x）（NbyTa1-y）O3 ceramic prepared by liquid method were better than that by conventional solid method. The average grain size of the nanometer powder（34 nm） obtained by citrate-gel method was small near 500 nm and homogeneous and the microstructure was dense and uniform. In addition, the sintering temperature had a great effect on properties. The dielectric properties of resultant samples were as follows： ε〉500, tgδ〈6 10^-4, αc〈 10 ppm/℃, ρv〉1 012Ω·cm.     

Low Temperature Synthesis of Nano Porous 12CaO?7Al_2O_3 Powder by Hydrothermal Method

Single-phase insulating 12CaO?7Al_2O_3(C12A7) powder was synthesized using an optimized hydrothermal method. Pure phase of C12A7 was got at a comparatively lower temperature(c.a. 300 ℃) than that has been previously reported. The crystallite size of the synthesized C12A7 powder was 7±2 nm. The surface area values calculated for all the samples at a synthesis temperature range of 250-800 ℃ for 5 h were in the range of about 19-24 m~2/g, with pore sizes of 12-20 nm. This low-temperature-based synthetic strategy along with nano porous structures and a high surface area value can facilitate catalyst application.     

Preparation of BN／SiO2 ceramics by PIP method

The precursor infiltration and pyrolysis(PIP) method for preparation of BN/SiO2 composites was used to improve mechanical properties, dielectric properties and feasibility of high temperature dielectric parts with large dimensions and complex shapes. In the processing procedure, the porous BN ceramic matrix was first successfully prepared by compacting the mixed powders of B and BN and then sintering them at a certain temperature under normal pressure of N2. The polycarbosilane(PCS) solution was vacuum infiltrated into porous BN ceramics at the room temperature and then at 800℃ in the air to depolimerize out amorphous SiO2, and sintered further at 1 300℃ in N2 to get BN/SiO2 composites. The microstructure of materials was studied by means of X-ray diffraction and electron probe micro analysis. The thermo-decomposition mechanism of PCS was investigated by a TG-DTA and infrared (IR) spectrum analysis. The flexural strengths were measured by the three-point bending method. The dielectric constant and the loss tangent were measured by the wave-guide method. The results show BN/SiO2 composites were fabricated. The obtained composites posses a flexural strength of 61.96 - 93.31 MPa, the dielectric constant in the range of 3.50 - 3.78 and the order of magnitude of the loss tangent at 10^-3 , which are good for the high tempera turedielectric parts with large size and complex shapes.     

Preparation of ZAO powder and investigation on its infrared emissivity

According to the basic infrared stealth mechanism of low infrared emissivity powders,the ZAO powder materials were prepared by liquid coprecipitation method,and the starting materials were Zn( NO3) 6H2O and Al( NO3) 39H2O. The process parameters were obtained,and the relationship between technology parameters and infrared emissivity was investigated. The temperature of thermal treatment,crystal structure and surface micrograph of ZAO powder was analyzed by the help of TG-DTA,XRD and SEM. The infrared stealth performance of ZAO powder was studied by IR-2 emissivity spectroscopy. Results showed that the infrared emissivity was the lowest when pH was 8. 0,calcination temperature was 1100 ℃,calcination time was 2 h,and the Al2O3doping content was 3% ( mass percentage) . The crystal structure of doped ZAO powder was lead-zinc, and there exists distortion of crystal lattice in nanocrystalline ZnO. The average particle size was 10 μm. The lowest infrared emissivity reached to 0. 61 at between 8 μm and 14 μm. It means that the ZAO powders will be excellent infrared stealthy materials.     

Shape memory effect during preparation of alumia ceramic tubes

Pure alumina ceramic tube and 95 alumina ceramic(the ceramic with 95.84% alumina) tube were prepared by using self-prepared alumina micrometer powder without agglomeration as raw material. The ceramic green was shaped by isostatic pressing and sintered at different temperature from 800 to 1 600 ℃ for 2 h. The 95 ceramic tube sintered at 1 550 ℃ for 2 h had mean particle size of 4 μm, bend strength of 437 MPa and volume density of 3.714 g/cm3. Shape memory effect during sintering was observed. XRD results showed that no phase transition occurred during shape memory process, which indicated that shape memory effect was not caused by phase transition. Several probable causes of the alumina ceramic shape memory effect were discussed in this paper.     

GRAIN GROWTH IN NANOSIZE AIN POWDERS

The nanosize AlN particles wereprepared by evaporation-condensation method in DCarc nitrogen plasma. Aluminium of high purity(99. 999% ) was evaporated and nitrided in nitro-gen plasma by use of high temperature and high re-activity of plasma gas. The purity of nanosize AlNparticles is more than 98% (wt%) and the averageparticle size is about 50nm. The grain growth ofnanosize AlN particle is also studied. The resultsshow that the nanosize AlN particle begins to growup at 900℃ and the grain growth increase rapidlyat 1100℃. When the temperature is increased to1600℃, the surface of nanosize AlN particle hasbeen sintered softly. Results will be beneficial to prepare AlN ceramics.     

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.     

Phase structure and electrical properties of La<Subscript>2</Subscript>O<Subscript>3</Subscript>-doped BiInO<Subscript>3</Subscript>-PbTiO<Subscript>3</Subscript> ceramics with high curie temperature

The phase structure and electrical properties of pure and La2O3-doped Bi-InO3-PbTiO3 （BI-PT） ceramics were studied respectively. In （1 -x）BI-xPT （x=0.72-0.80） ceramics, the stability of tetragonal phase increased with increasing x, and pure perovskite structure was obtained for x=-0.80 ceramics. The phase transition temperature range was between 575 ℃ and 600 ℃ for x=0.72-0.80 ceramics, higher than that of PT （-490 ℃）. The c/a ratio almost linearly decreased with increasing La2O3 content in x-0.80 ceramics. It is believed that Pb^2＋ vacancies were formed by La^3＋ substituting Pb^2＋ in La2O3-doped BI-PT ceramics. Tc shifted to lower temperature by 30 ℃/mol% La2O3. The maximum dielectric constant 8557 around 559 ℃ was exhibited in 0.5mol%-doped BI-0.80PT ceramics. La2O3-doped ceramics could be poled resulting from decreasing of c/a ratio and improving of dielectric loss and resistivity. The maximum piezoelectric coefficient d33 was 12 pC/N for 2mol%-doped BI-0.80PT ceramics.     

Microstructures and mechanism of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/Al composites fabricated by the reaction between SiO<Subscript>2</Subscript> and molten aluminum

Al₂ O₃/Al composite was fabricated by the reaction between SiO₂ and molten aluminum. The microstructures of the composite obtained under different reaction conditions were analyzed. The formation mechanism of the composite microstructure was discussed. Results show that the reaction kinetics is influenced remarkably by the reaction temperature, reaction time and the quantity of SiO₂. The morphologies of Al₂O₃ have different features, depending on the reaction temperature. The composite has equaxed Al₂O₃ grains when materials reacted below 1200°C, and the composite is composed of a large number of fine Al₂O₃ grains and aluninum. The composite has a frame-shaped Al₂O₃ microstructure at the reaction temperature of above 1250°C. CHENG Xiao-min: Born in 1964 Funded by the National Natural Science Foundation of China (No. 91522)     

Crystal growth,structure and properties of bismuth triborate BiB<Subscript>3</Subscript>O<Subscript>6</Subscript> crystal

BiB₃O₆ (BIBO) single crystals with size of 46×23×10 mm³ and weight of 26.0 g have been successfully grown by top-seeded method. Problems encountered in the growth process of this crystal have been discussed in detail, and the methods of growing high-quality large crystals have been put forward. The relationship between their structure and properties is studied. The space group of monoclinic BiB₃O₆ is C2 and the cell parameters are a=7.1203(7) Å, b=4.9948(7) Å, c=6.5077(7) Å, β=105.586(8)″, and V=222.93(5) ų. The density of BIBO is 4.8965 g/cm³. The Mohs’s scale of hardness is 5.5–6. There is no cleavage face in the crystal. The transmittance of BIBO is about 80 percent in the range from visible coherent light to near-infrared light. The ultraviolet cutoff wavelength is at 276 nm. BiB₃O₆ is a biaxial crystal and has two sets of axes, and the relative orientation of (X, Y, Z) with regard to (a, b, c) is: X//b, (Y, c)=47.2°, (Z, a)=31.6°, determined by X-ray analysis combined with polarized microscopy. Second-harmonic-generation (SHG) experiments were carried out for the first time. In type I phase-matching (PM) directions (11.1°, 90°) and (168.9°, 90°), SHG conversion efficiencies of two directions for 1.064 μm light are up to 67.7% and 58%, respectively. We have also obtained the third-harmonic-generation (THG) of 1.064 μm. The comparative experiments between BIBO and KTP were carried out on conversion efficiency, transmittance and hardness. All the above results indicate that BiB₃O₆ is a kind of excellent nonlinear optical (NLO) crystal.     

Synthesis and electrochemical properties of Cr-doped Li<Subscript>3</Subscript>V<Subscript>2</Subscript>(PO<Subscript>4</Subscript>)<Subscript>3</Subscript> cathode materials for lithium-ion batteries

Cr-doped Li₃V₂(PO₄)₃ cathode materials Li₃V_2−x Cr _x (PO₄)₃ were prepared by a carbothermal reduction(CTR) process. The properties of the Cr-doped Li₃V₂(PO₄)₃ were investigated by X-ray diffraction (XRD), scanning electron microscopic (SEM), and electrochemical measurements. Results show that the Cr-doped Li₃V₂(PO₄)₃ has the same monoclinic structure as the undoped Li₃V₂(PO₄)₃, and the particle size of Cr-doped Li₃V₂(PO₄)₃ is smaller than that of the undoped Li₃V₂(PO₄)₃ and the smallest particle size is only about 1 μm. The Cr-doped Li₃V₂(PO₄)₃ samples were investigated on the Li extraction/insertion performances through charge/discharge, cyclic voltammogram (CV), and electrochemical impedance spectra(EIS). The optimal doping content of Cr was that x=0.04 in the Li₃V_2−x Cr _x (PO₄)₃ samples to achieve high discharge capacity and good cyclic stability. The electrode reaction reversibility was enhanced, and the charge transfer resistance was decreased through the Cr-doping. The improved electrochemical performances of the Cr-doped Li₃V₂(PO₄)₃ cathode materials are attributed to the addition of Cr³⁺ ion by stabilizing the monoclinic structure. Funded by the Guangxi Natural Science Foundation(No. 0832259) and the National Basic Research Program of China (No. 2007CB613607)     

Dielectric Properties of B2O3 Doped MgTiO3-CaTiO3 System Ceramics

The dielectric ceramics with a main crystal phase of MGTiO3 and additional crystal phase of CaTiO3 were prepared by the conventional electronic ceramics technology .the strucures of MgTiO3 are ilmenitetype,and belong to hexagonal syngony.the ratio of MgTiO3 to Ca TiO3 doping on the dielectric properties of MGTiO3-CaTiO3(MCT)ceranics were inrestigated.the addition of B2O3 decreases the sintering temperatnre and results in rapid desification without obrious negative effect on the Q values of the system(Q=1/tan ).B2O3 exists as liquid phase in the sintering process,promoting the reactions as a singering agent.     

Orientation of Bi<Subscript>3.2</Subscript>La<Subscript>0.8</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> ferroelectric thin films with different annealing schedules

Fatigue-free Bi_3.2La_0.8Ti₃O₁₂ ferroelectric thin films were successfully prepared on p-Si (100) substrates using metalorganic solution deposition process. The orientation and formation of 5-layers thin films were studied under different processing conditions using XRD. Experimental results indicate that increase in annealing time at 700 °C after preannealing for 10 min at 400 °C can remarkably increase (200)-orientation of the films derived from the precursor solutions with two contents of citric acid. Meanwhile, high content of citric acid increases the film thickness and is conducive to the a-orientation of the films with the preannealing, and low concentration of the solution is conducive to the c-orientation of the films without the preannealing.     

Manufacture Process of 8Y2O3 Stabilized ZrO2 from Nano Powders

The manufacture process of 8 mol% Y2O3 stabilized ZrO2 ( YSZ ) from nano powders, including the forming and sintering stages, was studied. During the forming process of YSZ powders, the relative density of YSZ increases lineally with the forming press, and the sintering linear shrinkage of YSZ to the forming press compiles to the parabola trend. When the forming press exceeding 500MPa, the samples with lower shrinkage and high density were obtained. The sintering temperature of YSZ decreases greatly because of the small size and high active surface of YSZ powders. As a result, the beginning sintering temperature of YSZ made in the experiment is as low as 825℃, and the end sintering temperature is 1300-1350℃ . The relative density of YSZ ceramic by solid sintering at 1300-1350℃ is more than 97% , with little and small pores in the uniform microstructure.     

Effect of matrix composition on physical properties of Al<Subscript>3</Subscript>CON in-situ reaction reinforced corundum composite

60% white corundum used for aggregate, 5% aluminium powder for fixed additions and 35% various additives for matrix were prepared for specimens 1#,2#,3#. They were mixed uniformly with the suitable resin as a binder and pressed under pressure of 315 ton forging press, then dried at 200℃ for 24 h. Effects of various additives on 1500 ℃×2 h creep properties of Al3CON reinforced corundum composite were researched. The experimenal results show that creep coefficients of specimens 1#,2#,3# at 1500 ℃×2 h are 1.4×10^- 4, -9.4×10^-4, -22.6×10^-4, respectively. Crushing strength of the slide plate added with suitable additive A after fired at 1500 ℃ ×3 h reaches to 225 MPa, the creep rate is positive all the time from 0% to 0.014% at 1500 ℃ for 2 h. The microstructure result analysis shows that reinforced phases of Al3CON fiber composite have been formed after fired with Al powder in coke at high temperatures for specimen 1#, and the strength of the composite is increased. The hot modulus of rupture is up to 59 MPa at 1400 ℃ and the RUL is obviously higher than that at 1700 ℃. Its service life is two times as that of Al2O3-C slide plate when used in the process of pouring steel. The mechanism of creep rate resistance of the composites can be discovered by means of SEM and EDAX analysis. It is concluded that the active Al3CON and Al2O3 multiphases that were formed by N2 in gas, C, Al and Al2O3 inside the matrix of the composites during in-situ reaction,which gives the composites outstanding creep rate resistance for the dense zone resuiting from Al3CON oxidation that inhibits contraction at the high temperature. Besides, the matrix will turn into the multiphase with high refractoriness, N content and its Al3CON reinforced fiber will further increase accordingly. In addition, Al3CON formed by Al2O3 and C, Al in the matrix with N2 in gas will inhibit the creep rate and also greatly improve the creep rate resistance of the composites.     

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 of Fe-Al Intermetallie /TiC-Al2O3 Ceramie Composites from llmenite by SHS

Fe-Al intermetallic/TiC-Al2O3 ceramic composites were successfully prepared by selfpropagating high-temperature synthesis （SHS） from natural ilmenite, aluminium and carbon as the raw materials. The effects of carbon sources, preheating time and heat treatment temperature on synthesis process and products were investigated in detail, and the reaction process of the FeTiO3-Al-C system was also discussed. It is shown that the temperature and velocity of the combustion wave are higher when graphite is used as the carbon source, which can reflect the effect of the carbon source structure on the combustion synthesis; Prolonging the preheating time or heat treatment temperature is beneficial to the formation of the ordered intermetallics; The temperature and velocity of the combustion wave are improved, but the disordered alloys are difficult to eliminate with the preheating time prolonged. The compound powders mainly containing ordered Fe3Al intermetallic can be prepared through heat treatment at 750 ℃.