纳米Bi2O3-Y2O3快离子导体的制备

以共沉淀法制备的纳米(75mol%Bi2O3+25mol%Y2O3)混合粉体作为原料,通过无压反应烧结工艺制备了纳米Bi2O3-Y2O3快离子导体.对烧结过程中高导电相(纳米δ-Bi2O3)的形成规律研究表明固溶反应发生在烧结过程的初期,在烧结过程中晶粒生长规律符合(D-Do)2=K·t抛物线方程.用模式识别技术对δ-Bi2O3相生成的工艺条件进行优化的工艺参数优化区为Y＞-1.846X+3.433(X=0.0059T+0.0101t,Y=-0.0059T+0.0101t,式中,T为烧结温度,t为烧结时间).在T=600℃,t=2h无压反应烧结条件下,纳米晶Bi2O3-Y2O3快离子导体材料的相对密度可达96%以上,并且微观结构致密均匀,很少有残留气孔和裂纹,平均晶粒尺寸在100nm以下.     

纳米氧化铋基材料高温相变的研究

以分析纯Bi(NO3)3·5H2O和Y(NO3)·6H2O为原料制备纳米β-Bi2O3和Bi2O3-Y2O3(75%(摩尔分数)Bi2O3 25%(摩尔分数)Y2O3)粉体,平均粒度分别为40和30nm.经TG-DTA、高温XRD以及高温拉曼的研究结果表明,亚稳态的纳米β-Bi2O3粉体在升温过程中于420℃先向低温稳定的α-Bi2O3转变,在720℃时向δ-Bi2O3相转变,降温过程则是由δ→β→α.由于纳米Bi2O3具有很高的活性,使得相变温度比微米Bi2O3有所降低.纳米Bi2O3-Y2O3复合粉体升温过程中,Y2O3的固溶反应在较低温度(400℃)开始,500℃时β-Bi2O3完全转变为δ相,同时Y2O3完全固溶到δ-Bi2O3晶体中.Y2O3的掺杂使得Bi2O3的β→δ相转变温度大幅降低.     

微波烧结Al2O3/SiC纳米复合陶瓷的研究

以分析纯Al(NO3)3.9H2O·NH3.H2O和50 nm的SiC粉体为原料,采用溶胶-凝胶法制备干凝胶,经热处理合成Al2O3/SiC纳米复合粉体。利用微波烧结制备Al2O3/SiC纳米复合陶瓷,并与常规烧结比较,分析了两种烧结方法对制备试样的力学性能影响。结果表明,与常规烧结相比,微波烧结可以提高Al2O3/SiC纳米复合陶瓷的强度和韧性,改善材料的显微结构,促进致密化和晶粒生长。     

化学沉淀法合成纳米Bi2O3粉末

以Bi(NO3)3 为原料,利用化学沉淀法合成Bi2O3 粉体,发现最佳的工艺条件为:反应温度为90℃,反应时间为 2h, Bi(NO3 )3 溶液的质量浓度为300g/L。XRD分析结果表明产物为α Bi2O3。TEM和激光粒度分析表明,Bi2O3 粉体粒径约为 60nm,颗粒呈球形, 且分布均匀。将 Bi2O3 粉体置于空气中 6个月后测试未见团聚现象。反应机理是液 液反应的进行,实现了纳米Bi2O3 的生成。     

非化学计量Bi2O3对制备Bi4Ti3O12粉体影响的研究

制备晶粒形貌生长各向异性的中间化合物Bi4Ti3O12粉体是采用流延成型和模板晶粒生长(TGG)等工艺方法制备(Na0.5Bi0.5)TiO3基无铅压电织构陶瓷的关键技术.以NaCl-KCl熔盐法制备了生长各向异性的Bi4Ti3O12粉体,利用X射线衍射和扫描电子显微镜研究了非化学计量Bi2O3对粉体相结构和微观形貌的影响,优化了制备Bi4Ti3O12粉体的工艺参数,并探讨了Bi4Ti3O12粉体在熔盐中的生长机理.研究表明,随着Bi2O3过量程度的增加,所得Bi4Ti3O12粉体颗粒的平均尺寸和均匀程度均增加,当Bi2O3过量7.5%时达到最佳值,其平均粒径为8～10 μm.     

湿化学法制备 Y2O3纳米粉及透明陶瓷

以Y(NO3)3溶液和NH3·H2O为原料,制备了Y2O3纳米粉体.先驱沉淀物的化学组成为Y2(OH)5NO3·H2O.研究了pH值及滴加过程对先驱沉淀物形貌及Y2O3产物烧结性的影响.正向滴定,pH值较低时(pH=7.9),先驱沉淀物为片状结构;pH值较高时(pH=10.0),先驱沉淀物片层状结构特性减轻,并且颗粒变的细小.反向滴加时,片层状结构特征消失,主要为块状晶粒.先驱沉淀物为片状结构时,得到的粉体活性较高.添加适量的(NH4)2SO4能够减轻Y2O3粉体的团聚,沉淀的同时控制pH值在9以下,所得到的粉体具有更好的烧结性能.采用得到的Y2O3纳米粉,不加入任何烧结助剂,经1700℃真空烧结4h得到了透明Y2O3陶瓷.     

氮掺杂Bi2O3光催化剂的制备及其可见光催化性能

以硝酸铋和六次甲基四胺为原料,采用沉淀法合成了不同氮掺杂量的Bi2O3(N-Bi2O3)粉体,并采用XRD、FT-IR、XPS、UV-Vis、PL手段对其晶相结构和光谱特征等进行了表征.研究结果表明,未掺杂Bi2O3为单斜相α-Bi2O3,氮掺杂Bi2O3则为四方相β-Bi2O3和Bi5O7NO3组成的混晶,氮原子替代了Bi2O3晶格中部分氧原子,形成了Bi N键而稳定存在.氮掺杂能促进β-Bi2O3的生成.与未掺杂Bi2O3粉体相比,氮掺杂样品的吸收带边发生了明显红移,荧光强度明显减弱.甲基橙在可见光下的降解实验表明,氮掺杂Bi2O3具有良好的可见光催化活性.     

钛酸铋纳米粉体的水热合成研究

讨论了水热合成条件(原料种类、摩尔配比、反应温度和晶化时间)对水热法制备钛酸铋粉体结构和形貌的影响,以Bi(NO3)3·5H2O和TiCl4为原料,NaOH为矿化剂,在180～230℃和2～12h的水热条件下,制备出Bi4Ti3O12纳米粉体.XRD结果表明它是典型的层状钙钛矿结构.TEM观察表明,Bi4Ti3O12纳米晶是方形片状的,无团聚,晶粒边长分布为80～250nm,平均长度约200nm.     

无团聚ZrO2-HfO2-Y2O3复合纳米粉体的制备

以分析纯ZrOCl2·8H2O、HfOCl2·8H2O和Y(NO3)3·6H2O为原料,采用反向滴定共沉淀-共沸蒸馏法成功地制备出无团聚的ZrO2-HfO2-Y2O3复合纳米粉体.借助XRD、TEM、BET等手段分析了制备工艺对粉体粒径和团聚状态的影响.研究表明,分散剂PEG的加入量及前驱体湿凝胶的处理方式对最终制备的ZrO2-HfO2-Y2O3复合粉体的晶粒度影响不大,但显著影响粉体的分散状态.分散剂加入量为1%(质量分数)并对湿凝胶共沸蒸馏处理条件下最终获得的粉体的分散性最好.前驱体沉淀经500℃焙烧1h后,生成了具有高氧离子电导率的立方晶型ZrO2基ZrO2-HfO2-Y2O3固溶体,粉体的平均粒径约为15nm.     

TiAl-Al2O3纳米粉体的机械活化-放电等离子原位烧结

用机械活化-放电等离子烧结(MA-SPS)方法原位制备TiAl-Al2O3材料.MA后得到晶粒度小于25nm的纳米粉体,其中Al2O3起到机械活化和细化晶粒的作用,促使粉体快速纳米化;SPS原位烧结后得到密度为3.73g/cm3的(α2 γ)双相组织,组成相的晶粒度小于130nm.     

Plasma spraying of Al2O3 and Al2O3Y2O3

A microstructural study has been carried out of plasma-sprayed Al₂O₃ and mixed and sintered Al₂O₃Y₂O₃. In order to ascertain the degree of metastability achieved by plasma spraying, these results are compared with a similar experiment utilizing a CO₂ laser for melting and the hammer-and-anvil technique for quenching of the same materials. X-ray diffraction methods were used to determine the obtained phases and crystal structures. In addition, transmission electron microscopy was used to confirm the phases present and to study their morpology. The porosity was studied with both mercury intrusion porosimetry and small angle neutron scattering. The addition of Y₂O₃ is shown to decrease the porosity from 15% to 7.5%. Adhesion is likewise related to the addition of Y₂O₃ and it is seen that adhesion of the mixture is measurably improved over that of pure Al₂O₃. The implication of these results is discussed.     

Microstructure and Strength of Al2O3/Al2O3 Joints Bonded with ZnO-Al2O3-B2O3-SiO2 Glass-Ceramic

ZnO-Al2O3-B2O3-SiO2 （ZABS） glass powder was used as interlayer to join alumina ceramics. The effect of joining temperature on the microstructure and strength of joints was investigated. The results showed that the ZABS glass can react with alumina substrate to form a layer of ZnAl2O4 at Al2O3/glass interface. Bending test exhibited that low joining temperature （1150℃） led to low joint strength due to the formation of pores in the interlayer, originated by high viscosity of the glass. High joining temperature （1250 ℃） also resulted in low joint strength, because of large CTE （coefficient of thermal expansion） mismatch between amorphous interlayer and alumina substrate. Therefore, only when the joining temperature was appropriate （1200℃）, defect-free interface and high joint strength can be obtained. The optimum joint strength reached 285 MPa, which was the same as the base material strength.     

Surface tension of PbO-B2O3 and Bi2O3-B2O3 glass melts

The surface tensions of xPbO-(100?x) B₂O₃ (x = 30–80 mol%) and xBi₂O₃-(100?x) B₂O₃ (x = 0–100 mol%) melts were measured using the ring method over the temperature range 973 to 1373 K. The compositional and temperature dependences of surface tension were investigated. Addition of PbO and Bi₂O₃ to B₂O₃ increased the surface tensions of their respective PbO-B₂O₃ and Bi₂O₃-B₂O₃ melts. The surface tension showed a maximum at 60 mol% PbO in the PbO-B₂O₃ melts and at 70–80 mol% Bi₂O₃ in the Bi₂O₃-B₂O₃ melts. The temperature coefficient of surface tension was examined on the basis of its relationship to the structure, and it was suggested that the temperature coefficient of surface tension decreases with an increasing content of four-coordinated boron.     

Preparation of pressureless-sintered SiC-Y2O3-Al2O3

Sintering additives were prepared from aluminium hydroxide and yttrium hydroxide. These additives were soluble in water and resulted in a binder. A -SiC powder was mixed with the additive solution and sintered at 2150° C without pressure. The oxides formed from the additive promoted sintering. The sintered body contained no pores. Aluminium, silicon, and yttrium oxide were precipitated in the sintered body.     

Some physical properties of V2O5-Fe2O3 and V2O5-Fe2O3-Li2O systems

Various methods have been used to study the physical properties of the V₂O₅-Fe₂O₃ and V₂O₅-Fe₂O₃-Li₂O systems, including X-ray, electron microscope, Mössbauer effect, NMR and thermogravimetric measurements. The iron ions are approximately equally distributed in substitutional and interstitial sites in the V₂O₅ lattice. The maximum number of iron ions dissolved in the V₂O₅ matrix corresponds to 4 mol % Fe₂O₃. In all the samples a quantity of Fe₂O₃ which has not been included in lattice is observed. The V₂O₅-Fe₂O₃ and V₂O₅-Fe₂O₃-Li₂O systems are formed from solid solutions mixed with very small Fe₂O₃ particles. The analysis of the charge compensation of iron ions suggests that V₂O₅ is a quasi-amorphous semiconductor. Irradiation of V₂O₅-based samples with an electron beam induces the V₂O₅ platelets to convert to the VO _x phase.