无团聚ZrO_2-HfO_2-Y_2O_3复合纳米粉体的制备  

Preparation of agglomeration-free nanosized ZrO_2-HfO_2-Y_2O_3 composite powders

作　　者：石刚[1] 甄强[1,2] 李榕[1] 陈瑞芳[1] 严凯[1] Rose-Noelle VANNIER 

机构地区：[1]上海大学材料科学与工程学院 [2]上海大学纳米科学与技术研究中心 [3]法国法国里尔科技大学国家高等化学学院晶体化学及固体物理化学实验室,UPRESA-CNRS 8012 ENSCL-USTL,BP 108,59652 Villeneuve d’Ascq Cedex,法国

出　　处：《功能材料》2006年第7期1130-1133,共4页Journal of Functional Materials

基　　金：国家自然科学基金资助项目(20101006);上海市纳米专项基金资助项目(0452nm073)

摘　　要：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。Agglomeration-free naonsized ZrO2-HfO2-Y2O3 composite powders were successfully synthesized by the reverse titration coprecipitation- heterogeneous azeotropic distillation process with analytically pure ZrOCl2·8H2O、HfOCl2·8H2O and Y（NO3）3·6H2O as raw materials. The effect of synthesis conditions on the size and dispersity of composite powders was also investigated by means of XRD, TEM and BET. The experimental results showed that the quantity of PEG as dispersant and the processing mode of precursor hydrate wet gels affected the average grain size of composite powders slightly, but changed the dispersity of the powders noticeably. Nanosized composite powders with the best dispersity can be obtained by the combination of the addition of 1wt% PEG as dispersant into aqueous ammonia solution before coprecipitation and the heterogeneous azeotropic distillation of hydrate wet gels. After the precursor gels were calcined at 500℃ for 1 h, ZrO2-HfO2-Y2O3 cubic solid solution with high oxygen ionic conductivity was attained and the average particle size of the powders was about 15nm.

关 键 词：氧化锆 氧化铪 纳米粉末 共沉淀法 分散性 

分 类 号：TF123[冶金工程—粉末冶金]