(Pr1-xNdx)0.6Sr0.4Co0.8Fe0.2O3-δ体系双稀土阴极材料的氧化学扩散系数及电学性能的研究

采用固相反应法合成了(Pr1-xNdx)0.6Sr0.4Co0.8Fe0.2O3-δ(x=0.2、0.4、0.6、0.8)钙钛矿氧化物系样品,采用XRD分析物相结构,采用XPS分析化学状态,用电导弛豫法研究了(Pr1-xNdx)0.6Sr0.4Co0.8Fe0.2O3-δ系样品的氧化学扩散性能.实验结果表明,(Pr1-...     

中温固体电解质LaGaO3的制备

分别采用固相反应法、凝胶燃烧法分别制备了镓酸镧基固体电解质粉体(La0．9Sr0.1Ga0．8Mg0．2O3-δ)．讨论了煅烧温度对粉体物相的影响,比较了两种方法所制备粉体的特点．X射线衍射分析表明．固相反应法制备需经1250℃下预烧15h,1500℃下煅烧24h．得到La0．9Sr0.1Ga0．8Mg0．2O3-δ粉体颗粒尺寸在1μm,而凝胶燃烧法仅需在1400℃煅烧10h可以合成La0．9Sr0.1Ga0．8Mg0．2O3-δ粉体,粉体颗粒尺寸150nm。     

聚合物协助燃烧法合成La0.8Sr0.2Co0.5Fe0.5O3-δ纳米粉体

为开发新型高性能中温固体氧化物燃料电池阴极材料,以La、Sr、Co和Fe的硝酸盐、葡萄糖和丙烯酰胺为原料,在pH=8-10的碱性条件,通过聚合物协助燃烧法制备了La0.8 Sr0.2 Co0.5 Fe0.5 O3-δ(LSCF)钙钛矿相纳米粉体.用XRD、SEM和TEM表征了LSCF粉体的相结构和微观形貌,结果显示,在...     

LSCF系钙钛矿型致密透氧膜的制备及其透氧性能

通过柠檬酸-EDTA络合法合成了不同的A位Sr取代的LSCF系钙钛矿型粉体材料La0.1Sr0.9Co0.8Fe0.2O3-δLa0.3Sr0.7Co0.8Fe0.2O3-δLa0.5Sr0.5Co0.8Fe0.2O3-δ和La0.8Sr0.2Co0.8Fe0.2O3-δ采用XRD测试手段对粉体及膜片的晶体结构进行了表征.用静压片法制备透氧膜,并测定了LSCF系钙钛矿膜的透氧量,分析了温度和A位Sr不同掺杂量等因素对膜透氧性能的影响.结果表明,该系列膜的透氧量均随着温度升高而增大,随着Sr掺杂量的增加而增大.并在850℃下对透氧膜100h透氧稳定性进行实验研究,结果表明,膜片的透氧量随时间没有明显变化,表现出良好的稳定性.     

溶胶凝胶法制备超细负热膨胀性ZrW2O8粉体

以溶胶凝胶法制备负热膨胀材料ZrW2O8粉体并与固相法制备的粉体相比较.对其前驱体进行热重-差热分析(TG-DSC)、以X射线粉末衍射(XRD)、透射电镜(TEM)、扫描电子显微镜(SEM)分别对粉体进行物相分析和形貌观测.结果表明溶胶凝胶法比固相法合成温度低,于610℃合成单一立方结构ZrW2O8粉体,并且粉体颗粒比固相法小,为100nm;ZrW2O8粉体有很好的负热膨胀特性,以高温X射线衍射分析,在室温约500℃范围内,溶胶凝胶法制备的粉体的热膨胀系数为-5.93×10-6/K;比固相法(-6.31×10-6/K)的略低.     

阴极材料Ba0.5Sr0.5Co0.8Fe0.2O3-δ的制备和性能

用共沉淀法合成了具有单一的立方型钙钛矿结构的新型阴极材料Ba0.5Sr0.5Co0.8Fe0.2O3-δ,研究了材料的电导率和热膨胀系数与温度的关系.结果表明,前驱体在1100℃煅烧3 h后形成具有单一的立方型钙钛矿结构尺寸小于1 μm的Ba0.5Sr0.5Co0.8Fe0.2O3-δ粉末;在500～600℃致密材料的电导率高于100 S/cm,热膨胀系数随着温度的升高从13.62×10-6逐渐增大到18.75×10-6,当温度超过700℃后急剧增大.致密材料热膨胀系数在高温下剧增的主要原因是材料中比较大的氧损失.     

LnBaCo2O5+δ(Ln=Gd,Nd,Sm,Pr)-Ba0.5Sr0.5Co0.8Fe0.2O3-δ双相混合导体透氧膜的制备及性能测试

用固相反应法制备了LnBaCo2O5+δ(Ln=Gd,Nd,Sm,Pr)-Ba0.5Sr0.5Co0.8Fe0.2O3-δ(质量比为1:1)4种双相混合导体膜.通过XRD分析可知,除了PrBaCo2O5+δ和Ba0.5Sr0.5Co0.8Fe0.2O3-δ(BSCF)复合时发生明显反应外,其它3种复合膜在复合过程中均显示了良好的化学兼容性.4种双相膜在850℃时透氧率最高的是NdBa-(Co2O5+δ-Ba0.5Sr0.5Co0.8Fe0.2O3-δ膜(约为0.28mL/(cm2·min)).     

新型中温固体氧化物燃料电池阴极材料Ba0.5Sr0.5Co0.8Fe0.2O3-δ的制备

碳酸共沉淀法合成了新型中温固体氧化物燃料电池（ITSOFC）阴极材料Ba0.5Sr0.5Co0.8Fe0.2O3-δ（BSCF）.利用XRD、DSC、TG、SEM和EDX等手段研究了不同煅烧温度对产物相结构、形貌和成分的影响.结果表明,前驱体经过1000℃煅烧2h后,产物形成了钙钛矿结构,但存在少量BaO或SrO杂相.随着煅烧温度提高,产物中的杂相逐渐消失,产物的晶体结构在1180℃条件下转变为单一的立方型钙钛矿结构,其化学组成为Ba0.51Sr0.49Co0.72Fe0.19O3-δ,而且颗粒均匀,基本在10 μm以下.     

溶胶凝胶法制备超细负热膨胀性ZrW2O8粉体

以溶胶凝胶法制备负热膨胀材料ZrW2O8粉体并与固相法制备的粉体相比较.对其前驱体进行热重-差热分析(TG-DSC)、以X射线粉末衍射(XRD)、透射电镜(TEM)、扫描电子显微镜(SEM)分别对粉体进行物相分析和形貌观测.结果表明溶胶凝胶法比固相法合成温度低,于610℃合成单一立方结构ZrW2O8粉体,并且粉体颗粒比固相法小,为100nm;ZrW2O8粉体有很好的负热膨胀特性,以高温X射线衍射分析,在室温约500℃范围内,溶胶凝胶法制备的粉体的热膨胀系数为-5.93×10-6/K;比固相法(-6.31×10-6/K)的略低.     

纳米(Ba,Sr)TiO_3粉体材料的制备

采用溶胶 -凝胶工艺制备了 (Ba ,Sr)TiO3凝胶 ,并利用微波烧结技术对凝胶进行合成和烧结。结果表明 ,获得的 (Ba ,Sr)TiO3粉体颗粒较细 ,与传统固相反应合成法相比 ,其钙钛矿相的合成温度由 110 0℃降至 90 0℃ ;粉体的颗粒尺寸在 5 0nm附近     

Microwave assisted semi-solvothermal synthesis of nanocrystalline barium titanate

In an endeavor to synthesize tetragonal nanocrystallites of BaTiO3 at much reduced reaction time, we explored the possibility of performing microwave assisted semi-solvothermal reaction by using Ba(OH)2 . 8H2O and amorphous titanium hydrous gel as precursors and 1,4-butanediol and water as solvent. Typically, such a microwave assisted reaction was accomplished within 2 hrs at 220 degrees C as against 12 hrs required in conventional approach. The crystallized BaTiO3 powders (microwave assisted as well as conventionally processed for reference) were characterized by X-ray diffraction, thermal analysis, infrared spectroscopy, Raman spectroscopy, scanning electron microscopy, transmission electron microscopy, and atomic force microscopy. We have detected metastable cubic phase by XRD while locally symmetric tetragonal phase by Raman spectroscopy in case of conventional semi-solvothermal processing. On the contrary, we could detect co-existence of tetragonal and cubic phases by XRD and only tetragonal phase by Raman spectroscopy in case of microwave assisted semi-solvothermal processing. The TEM analysis indicates typical particle size distribution in the range of approximately 20 to 80 nm for conventionally processed powder while that in the range of approximately 20 to 50 nm for microwave processed powder. HRTEM images evince the distortion from an ideal cubic structure in case of microwave processed powder which can be correlated with anisotropic lattice contraction during the microwave induced heating. AFM analysis exhibited relatively less aggregation of nanoparticles for microwave assisted process.     

机械合金化制备FeSiAl合金粉末的研究

采用机械合金化的方法制备了FeSiAl合金粉末样品。以硅钢粉和铝粉为原料,按摩尔分数Fe3Si0.4Al0.6配比,研究其机械合金化过程,并对机械合金化的机制进行探讨。用激光粒度仪、X射线衍射(XRD)和扫描电子显微镜分析材料的粒度、形貌和结构。研究表明,Fe3Si0.4Al0.6混合粉末球磨30h后,粉末粒径可达18μm;Fe3Si0.4Al0.6混合粉末经高能球磨20h后,形成具有bcc结构的α固溶体;球磨继续进行,合金化的粉末和晶粒不断细化。     

TiO2微波碳热合成纳米TiC及其转化过程研

以TiO₂和纳米炭黑为原料, 机械干法混合后, 在Ar气氛下微波碳热合成纳米TiC。合成产物通过XRD和SEM进行表征, 研究了TiO₂粒径、反应温度、保温时间对微波碳热合成纳米TiC物相、显微形貌和TiO₂自身转化率的影响。实验结果表明, 微波碳热还原合成纳米TiC经1300℃保温40 min和1400℃保温30 min可使TiO₂充分反应, 且粒径为40 nm的TiO₂的转化率可达到98.2%, 合成的TiC粒度分布均匀, 平均粒径约小于100 nm。此外, 根据固相扩散机制对不同反应温度下两种粒径TiO₂转化率随时间的变化进行了Avrami方程拟合, 并绘制了两种粒径TiO₂的转化曲线, 为TiO₂与纳米炭黑微波合成纳米TiC提供理论参考。     

Solid phase preparation of submicron-sized SrTiO3 crystallites from SrO2 nanoparticles and TiO2 powders

Submicron-sized SrTiO₃ crystallites were prepared by a low temperature solid state method. The proposed preparation method involved two simple steps: firstly, SrO₂ nanoparticles of 35–90 nm were precipitated from the reaction of Sr(NO₃)₂ and H₂O₂ in an alkalescent aqueous solution (pH = 8) under the ambient condition; secondly, perovskite phase SrTiO₃ with a minor amount of SrCO₃ impurity were produced by heating the mixture of excessive SrO₂ nanoparticles and commercial TiO₂ powders in air at 700 °C for 10 h, which could be easily washed with 1 mol/l HNO₃ aqueous solution and distilled water to yield pure SrTiO₃ crystallites with the size of about 125–320 nm. The phase, purity and size of the as-obtained product were characterized by means of powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and field emission scanning electron microscopy (FESEM).     

The effects of hydroxide gel drying on the characteristics of co-precipitated zirconia-hafnia powders

Mixed zirconia-hafnia (Hf_0.25Zr_0.75O₂) powders of fine particle size and narrow particle-size distribution can be prepared via co-precipitation routes using mixed zirconium and hafnium salts as the starting materials. The characteristics of the resultant zirconia-hafnia powders are dependent strongly on the dehydration route by which the co-precipitated hydroxide gels are dried. Zirconium-hafnium hydroxide gels are formed when zirconium and hafnium oxynitrates are co-precipitated in an ammonia solution of pH 10.5. The co-precipitated hydrous gels were dried by three very different routes including organic solvent dehydration, microwave drying, and conventional infrared heating lamp drying. The dried hydroxides were then calcined at various temperatures in the temperature range 550–1150 °C, followed by ball milling to remove large soft-particle agglomerates. The resultant zirconia-hafnia powders were characterized for crystallite size, particle size, particle-size distribution, particle morphology, and the degree of powder agglomeration, using experimental techniques such as X-ray diffraction, BET surface area, differential thermal analysis, thermo-gravimetric analysis, sedigraph, scanning and transmission electron microscopy. Hard particle aggregates, which cannot be effectively eliminated using ball milling, occur in the zirconia-hafnia powders processed via either the microwave drying or conventional infrared heating lamp drying routes. In contrast, the organic solvent dehydration route resulted in an almost aggregate-free powder of fine crystallite and particle sizes. Therefore, the zirconia-hafnia powder processed via the organic solvent dehydration route exhibited high sinterability on sintering at 1300 °C.     

Combustion synthesis and microwave absorption property of SiC(Fe) solid solution powder under different reaction time

SiC(Fe) solid solution powders were synthesized via combustion reaction of the Si and C system in a 0.1 MPa nitrogen atmosphere using iron as the dopant and PTFE as the chemical activator, under different reaction time. The microstructures of prepared powders have been characterized by the SEM, EDS, XRD and Raman spectra, respectively. Results indicate that the prepared powders have fine spherical particles and narrow particle size distribution. The electric permittivities of SiC samples were determined in the frequency range of 8.2–12.4 GHz. Results show that the permittivity of SiC decreases with the increasing reaction time. The Fe doped SiC powder with reaction time of 45 min with 2 mm or 2.5 mm thickness exhibit the best microwave absorption properties in the X-band range(8.2–12.4 GHz). A method to predict absorbing property in the other frequency range has been presented.     

Synthesis of MgNb2O6 by coprecipitation

A simple coprecipitation technique was used successfully to synthesize fine powders of MgNb₂O₆ (MN) phase. An aqueous mixture of ammonium carbonate and ammonium hydroxide was used to precipitate Mg²⁺ and Nb⁵⁺ cations as carbonate and hydroxide respectively under basic conditions. This precipitate on heating at 750 °C produced MN powders. For comparison MN powders were prepared by the traditional solid state method. The phase content and the lattice parameters were studied by powder X-ray diffraction (XRD). Particle size and morphology of the particles were studied by scanning electron microscopy (SEM).     

A coprecipitation technique to prepare NaNbO3 and NaTaO3

A simple coprecipitation technique has been used successfully for the preparation of pure, ultrafine, single phases of NaNbO₃ (NN) and NaTaO₃ (NT). An alcoholic solution of ammonium carbonate and ammonium hydroxide was used to precipitate Na⁺ and Nb⁵⁺ (or Ta⁵⁺) cations under basic conditions as carbonate and hydroxide, respectively. On heating at 700°C, these precursors produce respective products. For comparison, both NN and NT powders were also prepared by the traditional solid state method. The phase purity and lattice parameters were studied by powder X-ray diffraction (XRD). The particle size and morphology were studied by scanning electron microscopy (SEM).     

Low-Temperature Synthesis of Ultrafine La0.7Sr0.3MnO3 Powder via Chelate Homogenization

Ultrafine La_0.7Sr_0.3MnO₃ powders were prepared via homogenization in chelate solutions, followed by the calcination of solid precursors at 700°C in air or oxygen, and their phase composition and average particle size were determined. The solid precursors were obtained from a solution of polynuclear La, Sr, and Mn chelates (diethylenetriaminepentaacetates) by three procedures: (1) gelation of the solution, followed by air drying of the resultant gel; (2) gelation followed by microwave dehydration; and (3) microwave dehydration of the solution. The results demonstrate that the way in which the chelate solution is converted into solid foams has little effect on the phase composition and particle size of the powders. At the same time, the phase composition and particle size of the reaction products depend on the calcination atmosphere (air or oxygen). Calcination in oxygen (700°C, 10 h) ensures the preparation of phase-pure La_0.7Sr_0.3MnO₃ powders, with an average particle size of 30 nm, from the three precursors.     

Cr掺杂Ba0.5Sr0.5Co0.8Fe0.1Cr0.1O3-δ钙钛矿型膜的透氧性能研究

采用固相反应法合成了钙钛矿型Ba0.5Sr0.5Co0.8Fe0.2-xCrxO3-δ(x=0.00,0.10)透氧膜粉体。利用XRD和SEM研究了Ba0.5Sr0.5Co0.8Fe0.2-xCrxO3-δ(x=0.00,0.10)的晶体结构和烧结性能,考察了在700~850℃范围内Ba0.5Sr0.5Co0.8Fe0.2-xCrxO3-δ(x=0.00,0.10)膜片的氧渗透性能。结果表明,它们均显示出优良的透氧性能,850℃时的透氧量分别为1.05mL/(min.cm2)、0.85mL/(min.cm2)。透氧稳定性的研究表明,Cr掺杂Ba0.5Sr0.5-Co0.8Fe0.1Cr0.1O3-δ在800℃时显示出较高的稳定性,证实用Cr离子部分取代Ba0.5Sr0.5Co0.8Fe0.2O3-δ的Fe离子能明显提高钙钛矿的结构稳定性。