Preparation and sintering of nano Fe coated Si3N4 composite powders

Fe/Si₃N₄ composite powder was synthesized by the heterogeneous precipitation-thermal reduction process, and then pressed into flakes under a pressure of 10 MPa. Flakes were sintered by pressureless and hot-pressing at 1 600 °C under 0.1 MPa N₂. The chemical composition, phases and microstructure of composite powder and sintered flakes were investigated by energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results show that the structure of composite powders is Si₃N₄ coated by nano Fe. The crystal phases of sintered flakes by pressureless are Fe(Si) compound, SiC and Si₃N₄. The crystal phases of the sintered samples by hot-pressing are Fe, Fe(Si) compound and Si₃N₄. It is found that crystal phases flakes obtained by pressureless and hot-pressing are very different. Foundation item: Project(50804016) supported by the National Natural Science Foundation of China     

Phase composition, transition and structure stability of functionally graded cemented carbide with dual phase structure

The phase composition, phase transition and phase structure transformation of the wire-cut section of functionally graded WC-Co cemented carbide with dual phase structure were investigated by XRD phase analysis. It is shown that the composition of η phase in the core zone is Co3W3C （M6C type）. The structure of cobalt based solid solution binder phase is fcc type. At the cooling stage of the sintering process, the phase transition of η phase, i.e. M6C→M12C and the martensitic phase transition of the cobalt based solid solution binder phase, i.e. fcc→hcp are suppressed, which facilitates the strengthening of the alloy. Because the instantaneous temperature of the discharge channel is as high as 10 000 ℃ during the wire cutting process, the processed surface is oxidized. Nevertheless, the oxide layer thickness is in micro grade. In the oxide film, η phase is decomposed into W2C and CoO, and cobalt based solid solution binder is selectively oxidized, while WC remains stable due to the existence of carbon containing liquid organic cutting medium.     

Pressureless sintered 3Y-TZP/20%Al2O3 composite ceramic

Nanometer 3Y-TZP/20%Al₂O₃ (mass fraction) composite powders prepared by the chemical coprecipitation method were pressureless sintered at 1550 °C for 2 h. Effects of calcining temperatures at 800 °C, 1 000 °C, and 1 200 °C on phase structure, relative density, and Vicker’s hardness of the sintered bodies were studied. The results show that 1 000 °C was the optimal calcining temperature, and the powder calcined was composed of tetragonal zirconia with the Scherrer crystalline size of 6.3nm. The relative density was up to 98.5% under pressureless sintering, and the sintered body was t-ZrO₂ (without m-ZrO₂)+α-Al₂O₃ with the average size of 0.4 μm. Foundation item: State Key Laboratory for Powder Metallurgy(No.9706-36) Biography of the first author: YIN Bang-yao, born in 1966, majoring in advanced ceramic materials.     

Preparation and properties of 4.25Cu-0.75Ni／NiFe2O4 cermet

4.25Cu-0.75Ni/NiFe₂O₄ cermets were prepared by doping NiFe₂O₄ ceramic matrix with the mixed powders of Cu and Ni or Cu-Ni alloy powder as the electrical conducting metallic elements. The effects of technological parameters, such as the adding modes of metallic elements, the ball milling time, the sintering time and the sintering temperature, on the relative density and resistivity of the cermets were studied. The results show that the resistivity of 4.25Cu-0.75Ni/NiFe₂O₄ cermets decreases with increasing temperature, and has a turning point at 590 °C, which is similar to that of NiFe₂O₄ ceramic. The sintering temperature and adding modes of metallic elements have a great influence on the properties of 4.25Cu-0.75Ni/NiFe₂O₄ cermets. When the sintering temperature increases from 1200 °C to 1300 °C, the relative density increases from 89.86% to 95.33%, and the resistivity at 960 °C decreases from 0.11 Ω · cm to 0.03 Ω · cm, respectively. When the metallic elements are added with the mixed powders of Cu and Ni, the cermets of finely and uniformly dispersed metallic phase, high density and electric conductivity are obtained. The relative density and resistivity at 960 °C are 90.23% and 0.04 Ω · cm respectively for the cermet samples sintered at 1200 °C for 2 h, which are both better than those of the cermets prepared under the same technique conditions but with the metallic elements added as 85Cu-15Ni alloy powders. Foundation item: Project (G1999064903) supported by the National Key Fundamental Research and Development Program of China; project(2001AA335013) supported by the National High Technology Research and Development Program of China; project (50204014) supported by the National Natural Science Foundation of China     

Preparation of Superfine-Cemented Carbide by Spark Plasma Sintering

92WC-8Co puwder mixture with superfine-tungsten carbide was respectively sintered by spark plasma sintering（ SPS ） and sintering isostutic pressure （SIP）. Complete dense samples with 200 nm WC grains and 94.2HRA hardness were prepared by spark plasma sintering at 1 150 ℃ and under 4.5 kN for 5 minutes. SIP was carried out at 1 400 ℃ for 30 minutes with a result of 300-400 nm WC grains and 93 HRA hardness. The results show that sintering temperature is greatly decreased by SPS, sintering time is largely shortened and WC grain growth is effectively retarded. Micropores and drawb（wks in superfine-cemented carbide made by SPS are greatly declined, which is very useful to improving nwehanical properties.     

Preparation and Characterization of LiMn1.8Co0.2O3.95F0.05 by the Combustion-assisted Soft Route

LiMn1.8Co0.2O3.95F0.05 powder was prepared by heating the ignited LiMn1.8Co0.2O3.95F0.05 precursor gel using lithium acetate, magnesium acetate, cobalt acetate, lithium fluoride, citric acid and glycol as raw materials. The influence of the calcination temperature on the stractural and electrochemical properties of LiMn1. 8 Co0.2 O3.95 F0.05 was investigated by X-ray diffraction, scanning electron microscopy, and galvanostatic charge-discharge experiments. The powders prepared under different conditions are of good crystallinity. The discharge capacity of LiMn1. 8 Co0.2 O3.95 F0.05 powder inereased from 92 mAh/g to 105mAh/ g as the calcination temperature inereasedfrom 750 ℃ to 850 ℃ . The capacity of LiMn1. 8 Co0.2 O3.95 F0.05 heated at 750 ℃ , 800 ℃, 850 ℃ for 4 haurs remained at 95.2% , 97%, 94.2% , respectively, after being cycled 20 times, suggesting that the multiple substitution of Co and F for Mn and O results in a good cycling behavior.     

Die wall lubricated warm compaction behavior of non-lubricant admixed iron powder

The phenomena of die wall lubricated warm compaction of non-lubricant admixed iron powders were researched, and its mechanism of densification was discussed. Water atomized powder obtained from the Wuhan Iron and Steel Corporation was used. With compacting and sintering, compared with cold compaction, the density of warm compacted samples increases by 0.07 - 0. 22 g/cm^3 at the same pressed pressure. The maximum achievable green density of warm compacted samples is 7.12 g/cm^3 at 120℃, and the maximum sintered density is 7.18 g/cm^3 at 80℃. Compared with cold compaction, the ejection force of warm compaction is smaller; the maximum discrep- ancy is about 7 kN. The warm compacted mechanism of densification of iron powders can be obtained： heating the powder contributes to improving plastic deformation of powder particles, and accelerating the mutual filling and rearrangement of powder particles.     

Structural evolution and stability of mechanically alloyed Fe-Ni nanocrystalline

The structural evolution and stability of Fe100-xNix(x=10, 20, 35, 50) alloys prepared by mechanical alloying were investigated through X-ray diffraction analysis and transmission electron microscopy. The intrinsic conditions of preparation determining phase stability in nanocrystalline were clarified. After being milled for 120 h, the powders of Fe90Ni10 and Fe80Ni20 consist of a single α(bcc) phase, Fe30Ni30 powders are a single γ(fcc), and for Fe65Ni35 powders there is co-existence of α and γ phases. The as-milled Fe80Ni20 powders annealed at 680 ℃ exhibits the stability of high-temperature γ phase at room temperature, which is consistent with the theoretical prediction.     

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.     

Preparation and properties of crystallizable Glass/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composites for LTCC material

The investigated low temperature Co fired ceramics(LTCC) composite of 60wt% CaO-Al2O3-B2O3-SiO2 glass and 40wt% α-Al2O3 as a filler is a non-reactive system, which is a critical part of the low temperature Co fired ceramics process. Through a study on densification process, the phase transformation and microstructure can be revealed. Its composites typically consist of CaO-Al2O3-B2O3-SiO2 glass and α-Al2O3 powders of average particle size (D50=3.49 mm). The sintering behavior, phase evaluation, sintered morphology, and microwave dielectric properties were investigated. In the fire range of 800 to 900 ℃, the composites were crystallized after completion of densification. It is found that the composites start to densify at 825 ℃, simultaneously, the dielectric constant (εr) reaches its maximum. With increasing heat-treatment temperatures, due to the loose microstructure of the material, tanδ increases slightly. The last of the sintered samples were identified as partly Anorthite at 850 ℃. At that temperature it has εr of 7.9 and tanδ less than 1×10-3, and can be used as a promising LTCC material.     

Sintering and phase transformation of 7wt% calcia-stabilized zirconia ceramics

Calcia stabilized zirconia(CSZ) ceramics were prepared with 7wt% calcia-stabilized zirconia powder by pressureless sintering technology. The crystal phases of the sintered samples were studied by X-ray diffraction(XRD) and Raman spectroscopy techniques, and the microstructures of the fracture surfaces were observed by scanning electron spectroscopy(SEM). The phase compositions and the lattice parameters of cubic calcia-stabilized zirconia were calculated by XRD patterns. As the sintering temperature increasing from 1400 °C to 1600 °C, the monoclinic zirconia content decreases gradually, finally all monoclinic phase transforms to cubic calcia-stabilized zirconia, which is determined to be Ca_0.134Zr_0.866O_1.866. It is revealed that monoclinic zirconia is the main factor causing minute cracks on the surface of sintered samples, and the combination of the XRD patterns and Raman spectra is an effective way to research the phase transformations of zirconia. Funded by the National Natural Science Foundation of China(No.10574102)     

Preparation of TiAl/Ti2AlC Composites with Ti/Al/C Powders by In-situ Hot Pressing

TiAl/Ti2AlC composites were prepared by in-situ hot pressing of TilAl/C powders mixtures and sintered at different temperatures were investigated by X- ray diffraction （ XRD ） of samples. The reaction procedure of Ti-Al-C system could be divided into three stnges. Below 900℃ , Ti reacts with Al to form TiAl intermetallics ; above 900 ℃ , C reacts with remain Ti to form TiC triggered by the exothermal reaction of Ti and Al ; TiAl reacts with TiC to produce dense TiAl/Ti2AlC compasites.In the holding stage, ternary Ti2AlC develops to layered polycrystal and composites pyknosis in the meanwhile. The mechanism of synthesis and microstructure was especially discussed.     

Preparation of ITO nano-powders by hydrothermal-calcining process

1 INTRODUCTIONSn-doped In2O3(ITO) is one kind of n-typesemiconductor material[1].It has excellent electro-optical properties , such as electrical conductivityand high transparency under visible light[2],andiswidely used in electronic , transparent electrode ,solar cells and electro-irradiance , especially inscreen display[3 ,4].Recently nearly half of the met-al indium has been used to prepare ITO materialsin the developed countries[5], such as Japan, A-merica ,France and so on.So the…     

Fabrication of Ti2AlC by Spark Plasma Sintcring from Elemental Powders and Thermodynamics Analysis of Ti-M-C System

A ternary-layered carbide Ti2AlC material could be synthesized by spark plasma sintering（SPS） technology using elemental powder mixture of Ti, Al and active carbon. By means of XRD and SEM, phases were identified and microscopically evaluated. The experimental results show that the main phase in the product was fully crystallized Ti2AlC with small particle size when sintered at 1200℃. The synthesis temperature of SPS was 200-400℃ lower than that of hot pressing （HP） or hot isostatic pressing （HIP）. Through thermodynamics calculations, the mechanism of Ti2AlC was studied by calculating changes of Gibbs free energy of reactions.     

Sintering of the NiFe2O4-10NiO/xNi Cermet

The sintering behavior of NiFe2 O4-10NiO/xNi cermet which was used as the most prospective inert anode materials for aluminum electrolysis was studied by examining the effects of raw powder particle size, sintering temperature, and the contents of Ni. The results show that fine particle size enables the powder to have high driving force for sintering. High temperature is beneficial to densification, but the ultra-high temperature does harm to the improvement of the density. The samples of NiFe2O4-10NiO/SNi has the highest relative density of 97.28 % when it is sintered at 1 350 ℃, but it decreases to 95.23 % when sintered at 1 400 ℃. Low addition of Ni has a great help to the sintering of NiFe2 O4-10NiO matrix. When the samples are sintered at 1 350 ℃ and the mass fraction of Ni is 5%, the highest relative density is gained, but the density decreases with the further increase of Ni contents. The low density of the sintered samples of NiFe2 O4-10NiO/17Ni is attributed to the high volume fraction of pores.     

Effect of additives on the sintering of amorphous nano-sized silicon nitride powders

Amorphous nano-sized silicon nitride powders were sintered by liquid phase sintering. The influences of the additives of Y₂O₃ and Al₂O₃ prepared by two different ways, the polyacrylamide gel method and the precipitation method, were investigated. The grain sizes of the additives prepared by the first method were finer than those of prepared by the latter method. When sintered at the same temperature, 1700°C, the average grain size of the silicon nitride is 0.3 μm for the sample with the former additives, which is much finer than the one with the latter additives. The density of additives prepared by precipitation method is clearly lower than those of prepared by polyacrylamide gel method. Funded by the National Postdoctoral Foundation of China(No.20060400787)     

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.     

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

Nanometer RuO2-SnO2 was 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.     

Oxidation performance of Fe-Al/WC composite coatings produced by high velocity arc spraying

Fe-Al intermetallics with remarkable high-temperature intensity and excellent erosion, high-temperature oxidation and sulfuration resistance are potential low cost high-temperature structural materials. But the room temperature brittleness induces shape difficult and limits its industrial application. The Fe-Al intermetallic coatings were prepared by high velocity arc spraying technology with cored wire on 20G steel, which will not only obviate the problems faced in fabrication of these alloys into useful shapes, but also allow the effective use of their outstanding high-temperature performance. The Fe-Al/WC intermetallic composite coatings were prepared by high velocity arc spraying technology on 20G steel and the oxidation performance of Fe-Al/WC composite coatings was studied by means of thermogrativmetic analyzer at 450, 650 and 800°C. The results demonstrate that the kinetics curve of oxidation at three temperatures approximately follows the logarithmic law. The composition of the oxidized coating is mainly composed of Al₂O₃, Fe₂O₃, Fe₃O₄ and FeO. These phases distribute unevenly. The protective Al₂O₃ film firstly forms and preserves the coatings from further oxidation. Foundation item: Project(50235030) supported by the National Natural Science Foundation of China; Project(98BK014) supported by the Foundation of State Economy Trade Committee of China     

Effect of cobalt loading on reducibility, dispersion and crystallite size of Co／Al2O3 Fischer-Tropsch catalyst

Co/Al2O3 Fischer-Tropsch synthesis catalysts with different cobalt loadings were prepared using incipient wetness impregnation method. The effects of cobalt loading on the properties of catalysts were studied by means of X-ray diffraction (XRD), temperature programmed reduction (TPR), hydrogen temperature programmed desorption (H2-TPD) and O2 titration. Co-support compound formation can be detected in catalyst system by XRD.For the Co/Al2O3 catalysts with low cobalt loading, CoAl2O3 phase appears visibly. Two different reduction regions can be presented for Co/Al2O3 catalysts, which belong to Co3 O4 crystallites (reduction at 320 ““C) and cobalt oxidealumina interaction species (reduction at above 400℃). Increasing Co loading results in the increase of Co3 O4 crystallite size. The reduced Co/Al2O3 catalysts have two adsorption sites, and cobalt loading greatly influences the adsorption behavior. With the increase of cobalt loading, the amount of low temperature adsorption is increased, the amount of high temperature adsorption is decreased, and the percentage reduction and cobalt crystallite size are increased.