Effects of drying method on preparation of nanometer α-Al2O3

Ammonium aluminum carbonate hydroxide （AACH） precursor was synthesized by the precipitation reaction of aluminum sulfate and ammonium carbonate. Then the precursor was dealt with five drying methods including ordinary drying, alcohol exchange, vacuum freeze-drying, glycol distillation, n-butanol azeotropic distillation respectively and calcined at 1 200℃ for 2 h to get α-Al2O3. The effects of drying methods on preparation of nanometer α-Al2O3 were discussed, and the optimal drying method was confirmed. The structural properties of powders were characterized by XRD, SEM and BET measurements. The results show that vacuum freeze-drying, glycol distillation and n-butanol azeotropic distillation can prevent the powders from aggregating, and among them the n-butanol azeotropic distillation is the best method. The nanometer α-Al2O3 powder with non-aggregation can be manufactured using n-butanol azeotropic distillation and the average particle size is about 40 nm.     

Coprecipitation preparation and voltage sensitive characteristics of doped ZnO varistor

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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.     

Effect of anions on preparation of ultrafine α-Al2O3 powder

Ultrafine alumina power was obtained by calcining the precursor at 1 200 ℃ for 2 h, which was prepared by homogeneous precipitation method using aluminium salts and urea as raw materials. The effects of anions on the morphology, particle size, surface area and configuration of the precursors were studied. The results show that the reactions of urea with aluminium nitrate and aluminium chloride result in agglomerates gels with bad filtering performance, the morphology is fibrillar. Aluminium sulphate-urea reactions result in the direct formation of amorphous powders with good filtering performance, of which morphology are regular spherical particles with larger granularity and smaller surface area. The reaction of mutual compound of aluminium sulphate and aluminium nitrate with molar ratio of 40:60 with urea can produce precursor with good filtering performance, spherical morphology, and uniform granularity distribution in the particle size range of 2-3 μm.     

Preparation of AgSnO2 composite powders by hydrothermal process

Silver-tin oxide powders were synthesized by the hydrothermal method with Ag（NH3）2^＋ solution and Na2SnO3 solution as raw materials and Na2SO3 as reductant. The precipitation conditions of Na2SnO3 solution and the reduction conditions of Ag（NH3）2^＋ were also investigated. The powders prepared were characterized by differential thermal analysis （DTA）, X-ray diffraction analysis （XRD）, scanning electron microscope （SEM） and energy spectrum analysis, The results show that pH value of the solution is a key parameter in the formation of Sn（OH）4 precipitate and the reduction reaction of Ag（NH3）2^＋ can release H^＋ ions, which results in synchronous precipitation of Sn（OH）6^2- as Sn（OH）4. The reduction of Ag（NH3）2^＋ and precipitation of Na2SnO3 occur simultaneously and the coprecipitation of silver and tin oxide is reached by the hydrothermal method. The silver-tin oxide composite powders have mainly flake shape of about 0.3 μm in thickness and there exists homogeneous distribution of tin oxide and silver in the powder synthesized.     

纳米级二氧化钛超细粉的制备

采用醇盐的乙醇溶液，制备了纳米锐钛矿相二氧化钛粉体．通过TEM和XRD分析测试手段，对所得粉体进行了表征．TiO2粒子外观呈球形，粒径为5～10nm．用此制备工艺新技术，操作简单，无污染，易于实现工业化．     

Sand-wear resistance of brush electroplated nanocomposite coating in oil and its application to remanufacturing

Sand-wear resistance of nano scale alumina particle reinforced nickel matrix composite coating (n-Al₂O₃/Ni) prepared by brush electroplating technique was investigated via wear tests in sand-contaminated oil lubricant, comparing with that of AISI1045 steel and brush electroplated Ni coating. Effects of testing load, sand content and sand size on worn volume of the three materials, and also coating surface roughness on worn volume of the brush electroplated coatings were accessed. Results show that the worn volume of all the three materials increases with increasing of testing load, sand content and sand size. In the same conditions, n-Al₂O₃/Ni composite coating has the smallest worn volume while AISI1045 steel has the largest because of the n-Al₂O₃ particle effects. As to n-Al₂O₃/Ni and Ni coatings, the surface-polished coatings have obviously lower worn volume than the as-plated coatings. The brush electroplated n-Al₂O₃/Ni composite coating was employed to remanufacture the sand-worn bearing seats of a heavy vehicle and good results were gained. Foundation item: Project (50235030) supported by the National Natural Science Foundation of China; Project (51489020104ZD0401) supported by the National Key Laboratory for Remanufacturing; Project(51418060105JB3058) supported by National Defence Foundation     

Synthesis of polycrystalline Yb:Gd3Ga5O12 nanopowders by homogeneous precipitation method

The Ytterbium doped gadolinium gallium garnet [Yb³⁺:Gd₃Ga₅O₁₂, Yb:GGG] precursor powders were synthesized via homogeneous precipitation method using Yb₂O₃, Ga₂O₃, Gd₂O₃ and ammonium bicarbonate [NH₄HCO₃] as precipitator, and ammonium sulfate [(NH₄)₂SO₄] as additive. The evolution of phase composition and micro-structure of the powders were characterized by — TG DTA, XRD, IR, and TEM. The results indicate that all precursor powders completely transform to Yb:GGG phase by calcining at 900 °C for 8 h, the resultant powders are well dispersed and have smaller particle size approximately 80 nm owing to the electrostatic effect.     

两种不同方法制备TSAG纳米粉体的对比研究

采用溶胶-凝胶法和共沉淀法制备TSAG纳米粉体,利用XRD和SEM等测试手段对不同方法合成的TSAG纳米粉体进行表征,并根据谢乐公式计算出粉体粒径大小。结果表明共沉淀法经1200℃煅烧6h可得纯度高,平均晶粒尺寸为49.7nm的TSAG粉体,溶胶-凝胶法经1000℃煅烧3h可得纯度高,平均晶粒尺寸为23.25nm的TSAG粉体。从煅烧温度、保温时间以及制备所得粉体粒径大小对这两种方法进行比较。相较于共沉淀法,采用溶胶-凝胶法可获得晶相更纯,粒径更小,颗粒分布均匀,分散性能好的TSAG粉体,且此方法更省时节能。     

Structure transition of nano-titania during calcination

1　INTRODUCTIONTitaniahasthreecrystallines :brookite ,anataseandrutile .Theirbasicstructuralunitisthesame[TiO6 ]octahedron ,buttheirlatticestructuresaredifferent .Forexample ,brookitebelongstorhombiccrystallo series ,whilerutileandanatasebelongtosquarecrystallo series .Thoughrutileandanatasearethesamecrystallo series ,theirsymmetricalelementsandunit cellparametersaredifferent[1] .Inrecentyears ,muchattentionhasbeenpaidtophasetransformationoftitaniaparticle ,especiallytothetemperatureofph…     

NaF改性纳米TiO2粉体光催化性能

对P25型纳米TiO2粉体光催化降解罗丹明B的光催化过程的动力学分析表明,光催化降解为一级反应.以反应速率常数为评价指标,确定了光催化降解的最优条件为罗丹明B初始质量浓度为10 mg/L,灯与液面距离6 cm,液层厚度6 cm,TiO2加入量0.4 g/L.采用浸渍法制备了NaF掺杂改性的P25型纳米TiO2粉体.焙烧使样品的晶体颗粒长大,会导致纳米粉体的量子尺寸效应下降,NaF掺杂改性使F-进入TiO2晶格,取代了O位,从而造成了晶格畸变,使光生载流子增多,抵消了纳米粉体的量子尺寸效应下降的影响,表现为样品光催化活性提高.NaF最佳掺杂质量分数为3%.NaF掺杂量过多时,光生载流子产生量较大,纳米颗粒表面电子和空穴相邻较近,电子和空穴的复合几率增加,样品光催化性能下降.     

Modification of nano-TiO2 by Al2O3 in-situ coating

A novel technology of in-situ coating Al₂O₃ on the surface of H₄TiO₄ was developed to prevent the aggregation of nano-TiO₂ powders and improve the dispersibility and thermal stability in the way of forming a uniform coating layer. The heterogeneous nucleation was conducted to prepare the precursor of nano-TiO₂ and then Al₂O₃ was coated on the surface of precursor. The effects of Al₂O₃ in-situ coating on the properties of nano-TiO₂ were investigated. The results show that H₄TiO₄ can be dispersed well under alkaline condition (pH 8.5) and the heterogeneous nucleation can be controlled easily. The optimized uniform coating layer is obtained by adding 5% (mass fraction) and 10% of Al₂O₃ and the aggregation of nano-TiO₂ powders is effectively inhibited and the dispersibility is obviously improved. The crystal sizes of TiO₂ powders are 12.3, 11.4 and 8.7 nm after coating 0,5% and 10% of Al₂O₃ respectively. Al₂O₃ on the surface of particulates in amorphous phase could increase the thermal stability of nano-particles after calcined at 550 °C. Foundation item: Project(04GK2007) supported by Hunan Industrial Key Project of Science and Technology     

Morphology and tribological properties of Ni/n-SiO2 composite coatings by pulse-reverse current brush-plating

Ni/n-SiO₂ composite coating was electrodeposited by brush-plating with pulse-reverse current(RC). The morphology, hardness, and tribological properties of the coating were investigated and compared with those of Ni and composite coatings electrodeposited with direct current (DC). The results indicate that Ni/n-SiO₂ composite coating electrodeposited by RC, because of RC and the nano powders, has denser coating, finer crystal grains, higher hardness (HV650.0, nearly 1.5 times higher than that of Ni coating electrodeposited by DC) and lower friction coefficient (nearly 0.62), as a result, in the wearing experiment, the Ni/n-SiO₂ composite coating electrodeposited by RC has the least worn loss. So this kind of coating has better wear resistance. And RC electro brush-plating can be used as a new technology of brush-plating in the area of wear resistance. Foundation item: Project (50235030) supported by the National Natural Science Foundation of China; Project (51489020104JS9102) supported by the National Key Laboratory for Remanufacturing     

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…     

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.     

聚乙烯吡咯烷酮/溶剂辅助合成SnO_2纳米晶体

采用溶剂热方法合成了均分散SnO2纳米晶体。首先探索了在同一溶剂中,形成均分散SnO2纳米晶体的最佳反应条件:聚乙烯吡咯烷酮(PVP-k30)的质量浓度为5g.L-1,SnCl4.5H2O的浓度为0.14mol.L-1,反应温度为180℃,反应时间为24h。在保持最佳反应条件的基础上,还研究了不同溶剂中PVP-k30与溶剂之间相互作用对产物形貌、结晶性及吸光性能的影响,结果表明:在PVP-k30的乙醇溶剂中,物质之间的相互作用促使产物形成花簇状结构;而在N,N-二甲基甲酰胺(DMF)或DMF与乙醇(体积比为1∶1)溶剂中,产物的形貌为链状结构;花簇状产物的结晶性能与吸光性能要优于链状结构产物。     

Solvothermal preparation and characteristics of Sn-doped In2O3

Sn-doped In2O3 （ITO） nanopowders were prepared in ethanol solvent by solvothermal process. The effects of the solvothermal temperature, coprecipitation pH value and SnO2 content on the products phase and microwave absorption were investigated by X-ray diffractometry and microwave reflectance. ITO nanopowders with cubic structure can be respectively prepared at 250 and 270 ℃ for 6 h. The prepared product is InOOH or the mixture of InOOH and In3Sn4O12 when the solvothermal temperature is below 250℃. With rising solvothermal temperature and prolonging time, the absorption of the ITO powders gradually decreases. The products are ITO nanopowders by coprecipitating at pH=9 or 11, but ITO powders with Sn3O4 at pH=6. The absorption of powders prepared at pH=6 is better than that at any other pH value. The products are all ITO nanopowders and crystal size reduces with increasing SnO2 content. The microwave absorption of ITO nanopowders with SnO2 content of 8% （mass fraction） is the best among samples with different SnO2 contents.     

Preparation and structure characteristics of nano-Bi2O3 powders with mixed crystal structure

The nano-Bi2O3 powders were prepared by a chemical precipitation method with Bi(NO3)3, HNO3 and NaOH as reactants. The structural characteristics and morphology of nano-Bi2O3 powders were investigated by X-ray diffraction and transmission electron microscopy, respectively. The results show that under the optimum condition that 300g/L Bi(NO3)3 reacts at 90℃ for 2 h, the Bi203 powders with 60 nm on the average and 99.5% in purity are obtained. The prepared nano-Bi2O3 powders contain a mixed crystal structure of monoclinic and triclinic instead of traditional structure of monoclinic α-Bi2O3. And the mixed crystal structure is stable in air. The reason for the appearance of the mixed crystal structure may be that the ionic radius ratio of Bi^3 to O^2- changes easily during the formation of nano-Bi2O3 particles by a chemical precipitation method.     

Microstructure and Properties of CePO4 Ceramic

Cerium phosphate powders were synthesized by direct solid liquid reaction of cerium dioxide and phosphate acid at the Ce ： P ratio of 1 ： 1. Phase-pure and fine grain size CePO4 powers could be obtained by calcining the as received powders at the temperature higher than 600 ℃ . It is demonstrated that the grain size and morphology of the CePO4 powders were calcined at various temperatures. An interesting layered crystal structure and a series of microcracks that cross and occur along the extrusion stress direction on the extruded surface inside CePO4 were observed. The ductility and machinabililty of CePO4 ceramic are attributed to the layered structure. Continuous machining debris was observed on the turned surface.     

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