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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。
The non-agglomerated ZrO2-HfO2-Y2O3 nanocomposite powders were successfully prepared by reverse titration coprecipitation-azeotropic distillation using pure ZrOCl2.8H2O, HfOCl2.8H2O and Y (NO3) 3.6H2O as raw materials. The influence of preparation process on particle size and agglomeration state was analyzed by means of XRD, TEM and BET. The results show that the addition amount of dispersant PEG and the pretreatment of wet gel have little effect on the grain size of ZrO2-HfO2-Y2O3 composite powders, but significantly affect the dispersion of powders. Dispersing agent was added in an amount of 1% (mass fraction) and the dispersibility of the powder finally obtained under azeotropic distillation of wet gel was the best. The precursor precipitates were calcined at 500 ℃ for 1 h, and the ZrO2-HfO2-Y2O3 solid solution with high oxygen ion conductivity was obtained. The mean particle size of the powders was about 15 nm.