The Properties of YSZ Electrolyte Sintering at 1300℃

The properties of yttria stabilized zirconia(YSZ) related to the sintering process were discussed.YSZ nano-powders about 40-100 nm as raw material,the sub-micrometer grain sizes such as 0.4-3 μm in YSZ were gotten by sintering process at 1300 ℃,which was performed at 1000 ℃ for 2 h,then raised the temperature at the rate of 50 ℃/h to 1400 ℃,then decreased directly to 1300 ℃ in 30 minutes,finally at 1300 ℃ for 5-20 hours.The ratio of bigger grain size becomes larger as the holding time increasing at 1300 ℃.The grains less than 1 μm are about 50%,eg,43.2%,52.2% and 51.1% related to 1300 ℃ holding 5 hours,8 hours and 10 hours,respectively.As YSZ grain size became small,the electrical conductivities did not decrease,even increased,about 0.20 s/cm at 1000 ℃.The reduced sintering temperature and time were benefited to co-fire with the electrodes in electrode-supported SOFCs.     

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.     

Spark plasma sintering of undoped SnO<Subscript>2</Subscript> ceramics

Various parameters in spark plasma sintering(SPS),such as sintering temperature,holding time,heating rate,and pressure,were adopted to investigate their effects on the densification of pure SnO2 power.The obtained experimental data show that the SPS process enhances densification.The high-density undoped SnO2 ceramics (96.6% of theoretical) was obtained at much lower temperature (1000℃),within a much shorter time,compared to the conventional sintering process.The high-density undoped SnO2 ceramics (96.6% of theoretical) were obtained by SPS,under the condition of temperature:1000℃,pressure:40MPa,heating-rate:200℃/min,and holding time:3min     

Sintering and dielectric properties of fine-grained BaTiO_3 ceramics

A new sintering method, spark plasma sintering (SPS), is described for the sintering of fine-grained BaTiO_3 ceramics. Dense ceramics with fine grain size of near 170 nm are obtained using SPS at low temperature of 900℃ without holding time. The dielectric measurements of various grain size specimens show that the dielectric constants decrease with the reduce of grain size, and diffuse phase transition showed in the dielectric-temperature spectra. The variation in dielectric properties with grain size is explained.     

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.     

Effect of quenching and partitioning process on MA constituent in Nb-bearing HSLA steel

The effect of quenching-partitioning (Q-P) process on martensite-austenite (MA) constituent is investigated by the thermo-analysis simulator for a niobium-bearing HSLA steel. The process includes quenching from 950 ℃ to the intermediate temperature of 350-550 ℃ at the rate of 30 ℃/s and subsequent reheating at the rate of 20-50 ℃/s and partitioning at 660-800 ℃. The microstructure is characterized by nano probe, EBSD, colored metallograph, optical microscope and graphic analytic method. The results show that the improvement of distribution homogeneity of MA in microstructure, the diminishment of the MA average grain size and increment of the MA volume fraction is caused by the intermediate temperature decrease, the reheating rate increase and a proper partitioning temperature. The volume fraction of MA is up to 7.9% while the sample is quenched to 450 ℃, reheated at 50 ℃/s and partitioned at 750 ℃. The grain is granular or equiaxed in shape and the average grain size of MA is about 0.77-1.48 μm after treated by Q&P process. The grains tend to be coarse and with sharpy-angle as the intermediate temperature is up and the reheating rate and the partitioning temperature rises. The MA volume fraction depends on the untransformed austenite volume fraction after quenching and carbon diffusion time and temperature during partitioning process.     

Effect of Spark Plasma Sintering on Microstructures and Properties of Al-Fe Alloy

2024 Aluminum alloy powder （ 60wt% ） and Fe-based amorphous powder （ 40 wt% ） were adopted. They were mechanical machined for 48hours after being mixed. Bulk material was gained after Spark Plasma Sintering. The sintering parameters included sintering holding time. 300℃ - 800 ℃ were adopted while the temperature, heating or cooling rates, pressure and heating or cooling rate was 100℃/min and with the pressure of 50 MPa in the experiments. The holding time was 10 min or 20 min at different temperatures, respectively. Bulk materials after sintering were examined by Scanning Electron Microscopy and X-Ray Diffraction. The micro-hardness and relative density also were tested. The sintering temperature had the most significant influence on the microstructure and property of the bulk material. The influence of holding time came second while the heating or cooling rates and pressure were fixed. The density became larger with the increase of the temperature. The compactness was best at 500℃. The pressure and generation of high-temperature phases were the factors which affected the density and the comoactness.     

Effects of activated sintering process on properties and microstructure of W-15Cu alloy

The effects of activated sintering technology of H2 atmosphere sintering on the microstructure and properties of W-15Cu alloy using ultrafine W-15Cu composite powder fabricated by spray drying calcining-continuous reduction technology were investigated.The experimental results showed that W-15Cu alloy,consolidated by activated sintering technology of H2 atmosphere sintering for 1 h at 1300 ℃,with 98.5 % relative density,transverse rupture strength 1218 MPa,Vickers hardness HV0.5 378,average grain size about 1.2 μm and thermal conductivity 192 W/m·K,was obtained.In comparison to the normal sintering process,activated sintering process to W-15Cu alloy could be achieved at lower sintering temperature.Furthermore,better properties in activated sintered compacts were obtained,and activated sintering process resulted in finer microstructure and excellent properties.     

Characterization of YSZ Ceramic Nanopowders Synthesized at Different Temperatures via Polyacrylamide Gel Method

Tetragonal zirconia (T-ZrO_2) ceramic nanopowders stabilized with 3 mol% Y_2O_3 were synthesized via polyacrylamide gel method,using ZrOCl_2?8H_2O and Y(NO_3)_3?6H_2O as raw materials.The effect of temperature on phase composition and morphology of YSZ nanopowders and sintering behavior of YSZ ceramics was investigated by X-ray diffraction (XRD),scanning electron microscopy (SEM) and Vickers hardness tester.The aging-resistance of YSZ ceramics was measured by means of aging experiments.The results demonstrated that the phase composition of YSZ ceramic nanopowders had no obvious change and it was composed of T-ZrO_2.Particle size of well-dispersed YSZ ceramic nanopowders increased from 17 to 35 nm with increasing calcining temperature from 600 to 800 ℃.There was noticeable negative correlation between calcining temperature and the relative density of YSZ ceramic at the same sintering temperature.The aging experiments showed that water vapor facilitated tetragonal to monoclinic phase transformation,and the sample that had smaller grain size exhibited better aging-resistance.It can be concluded that when the calcining temperature is 600 ℃ and sintering temperature is 1 550 ℃,the relative density and hardness of YSZ ceramic arrive at the peak of 96.64% and 11.135 GPa respectively,and it has less microcracks and excellent aging-resistance.     

Effects of sintering additives on preparation of CaF2 transparent ceramics

The effects of different sintering addictives on the preparation of CaF2 transparent ceramics were studied. Transparent CaF2 ceramics were fabricated by vacuum sintering and hot isostatic pressing (HIP) method, using CaF2 nanopowders synthesized by chemical precipitation method as raw materials. The nanopowders and transparent ceramics were studied using X-ray diffraction, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and spectrophotometer. The experimental results indicated that the obtained nanopowders presented normal distribution with grain size about 30 nm; transmittance of CaF2 transparent ceramics was 39% and 26% at 1100 nm for LiF and NaF as sintering addictives, respectively, with corresponding mean grain size 188 μm and 44 μm. Loss of transmission could be attributed to the residual closed porosity. Sintering mechanism was liquid-phase sintering at pre-stage, then solid-phase sintering at later stage, as well as solid solution of lithium ions and sodium ions in the CaF2 lattice structure.     

Effect of solid-solution temperature on the microstructure of Fe-Ni based high strength low thermal expansion （HSLTE） alloy

The influence of solid-solution temperature on the dissolution of carbide precipitates, the average grain size and the microhardness of the austenite matrix in an Fe-Ni based high strength low thermal expansion （HSLTE） alloy was investigated to obtain the proper temperature range of the solid-solution process. The XRD analysis, microstructure observations, and the theoretical calculations showed that the Mo-rich M2C-type precipitates in the Fe-Ni based HSLTE alloy dissolve completely at about 1100℃. The average grain size of the studied alloys increases from 14 to 46 μm in the temperature range of 1050 to 1200℃. The microhardness of the matrix decreases gust for the sake of solid-solution treatment, but then increases later with increasing solution temperature because of the solution strengthening effect.     

Effect of thermal treatment on microstructure and phase of partially-stabilized zirconia

ZrO2-MgO-Y2O3-CaO-Al2O3 composites with a multiphase microstructure were fabricated by die pressing process and sintered at various thermal programs. The microstructure of this polycrystalline was examined to clarify the role of Al2O3 on grain growth. Environmental scanning electron microscopy (ESEM) micrographs revealed that spinel was beneficial to refine grain. The effect of thermal treatment on the formation of monoclinic phase was discussed. It can be found that, the grain size and the fraction of the monoclinic phase in this partially stabilized zirconia(PSZ) increases after heat treatment at 1 150 ℃. The temperature of heat- treatment, not the time for holding, is the governing factor of the fraction of monoclinic phase.     

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.     

Effect of Sintering Time on Structure and Properties in CuO-doping KNN-LS-BF Piezoelectric Ceramics

The 0.6 mol% CuO-doping 0.996(0.95 Na_(0.5)K_(0.5)NbO_3-0.05 LiSbO_3)-0.004 FeBiO_3(KNN-LSBF-CuO) piezoelectric ceramics were synthesized by a solid-state reaction technique, and the structure and piezoelectric properties dependence of sintering time in KNN-LS-BF-CuO ceramics were studied. It is found that all the samples sintered for various time are perovskite structure mixed with orthorhombic symmetry phase and tetragonal phase, but the sintering time has significant influences on the crystalline and properties. When the sintering time increases from 2 hours to 6 hours, the grain of KNN-LS-BF-CuO ceramics becomes more homogeneous and more tight-arrangement. The experimental results reveal that the longer sintering time than 4 hours is beneficial for improving partial properties, such as d_(33), tgδ, and Q_m, but is adverse to ε_r and k_p, the KNNLS-BF-CuO ceramics with optimum properties can be synthesized for 6 hours at 1 060 ℃.     

Grain Boundary Distribution Evolution of 00Cr12Ti FSS during Annealing

The texture and grain boundary of 00Cr12 Ti FSS have a close correlation with properties and should be controlled to optimize the performance of steel sheets. In this paper, the macrotexture evolution during recrystallization annealing was investigated by XRD, the microtexture and grain boundary distribution evolution during recrystallization annealing were investigated by EBSD. The results showed that the γ fiber texture were mainly generated by replacing α fiber texture in recrystallization process. But with the holding time extending, γ fiber texture transferred to other texture after the holding time got to a certain degree. The major CSLs in 00Cr12 Ti FSS after recrystallization are Σ3 and the frequency of Σ3 climb up and then decline with the holding time extending. Σ11 plays an important role in the process of recrystallized γ fiber texture formation.     

Low-temperature Rapid Synthesis of Ultrafine Hafnium Carbide Ceramic Powders

Nano hafnium carbide(HfC) powders were synthesized by sol-gel combining hightemperature rapid heat treatment process using citric acid and hafnium tetrachloride as the raw materials. The effects of ball milling treatment on the phase and morphology of pyrolysis products(HfO_2-C) and final HfC product were investigated and the influences of heat treatment temperature and holding time on the structure and properties of the synthesized hafnium carbide powders were also studied. The experimental results showed that the HfO_2-C powders with good uniformity and small particle size were prepared by controlling the milling time. Pure HfC powders with an average particle size of 500 nm were obtained at 1 700 ℃ with a holding time of 3 min, and the oxygen content was about 0.69 wt%, lower than that of the hafnium carbide powders prepared by SPS(0.97%).     

Effects of deformation parameters on formation of pro-eutectoid cementite in hypereutectoid steels

Brittle pro-eutectoid cementite that forms along prior-austenite in hypereutectoid steels is deleterious to mechanical properties. The optimum process parameters which suppress the formation of pro-eutectoid cementite in hypereutectoid steels with carbon content in the range of 0.8%-1.3% in mass fraction, were investigated. Pro-eutectoid cementite formation is effectively hindered by increasing the deformation temperature and decreasing the amount of strain. Transformation at lower temperatures close to the nose of the cooling-transformation diagram also reduces the tendency of the formation of pro-eutectoid cementite. Control of prior-austenite grain size and grain boundary conditions is important. Due to larger number of nucleation sites, finer prior-austenite grain size results in the acceleration of transformation to pro-eutectoid cementite. However, large prior-austenite and straight boundaries lead to less nucleation sites of pro-eutectoid cementite. The cooling rate and carbon content should be reduced as much as possible. The transformation temperature below 660 °C and the strain of 0.5 at deformation temperature of 850 °C are suggested.     

Effects of pre-strain and baking parameters on the microstructure and bake-hardening behavior of dual-phase steel

In a typical process, C-Mn steel was annealed at 800℃ for 180 s, and then cooled rapidly to obtain the ferrite-martensite microstructure. After pre-straining, the specimens were baked and the corresponding bake-hardening （BH） values were determined as a function of pre-strain, baking temperature, and baking time. The influences ofpre-strain, baking temperature and baking time on the microstructure evolution and bake-hardening behavior of the dual-phase steel were investigated systematically. It was found that the BH value apparently increased with an increase in pre-strain in the range from 0 to 1%; however, increasing pre-strain from 1% to 8% led to a decrease in the BH value. Furthermore, an increase in baking temperature favored a gradual improvement in the BH value because of the formation of Cottrell atmosphere and the precipitation of carbides in both the ferrite and martensite phases. The BH value reached a maximum of 110 MPa at a baking temperature of 300℃. Moreover, the BH value enhanced significantly with increasing baking time from 10 to 100 min.     

Relation between powder size and electrolyte properties in nano YSZ system

YSZ (yttria stabilized zirconia) electrolyte properties made from different sizes of nano powders were investigated. As a result, the sample marked KD with the smallest size (10 nm) of first particles and the sample marked TH with narrow distribution and the smallest median diameter Mmcd of 0.49μm have the best sintering properties and the highest electrical conductivity. There is a very well correlation between the density and the electrical conductivity of YSZ, that is, the samples with a higher density have a higher electrical conductivity. The area resistance of YSZ electrolyte made in the experiment, such as TH of 0.483 Ω.cm^2, is much lower than that of the sample D of 1.300 Ω.cm^2 made in Germany at 850℃. The complex resistance of YSZ electrolyte made in the experiment at the grain, grain boundary and electrode in the range of 300-750℃ decreases greatly compared to the sample made in Germany by shown in the complex impedance plot.     

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 ℃.