水热法制备稳定氧化锆纳米粉体  

The Hdrothermal Preparation of Stable Zirconia Nano Powder

作　　者：徐高峰 宋红章[1] 杨德林[1] 

机构地区：[1]郑州大学物理工程学院材料物理教育部重点实验室,郑州450001

出　　处：《表面技术》2017年第9期95-100,共6页Surface Technology

摘　　要：目的制备分散性好、粒径分布窄的稳定氧化锆纳米粉体。方法采用水热法制备氧化锆纳米粉体,考察水热时间、p H值、温度和有机添加剂丙三醇,对氧化锆粉体颗粒粒径、结晶度及稳定性的影响。通过XRD和SEM分析技术对不同条件下制备的样品进行表征。结果结晶度随着水热反应温度的升高而提高,形核速率在250℃时快速增加,粒径在150~250℃出现先长大后减小的规律。反应溶液的p H值影响样品的结晶度,通过调节溶液p H值可以减小粉体颗粒之间的团聚,改善粉体的分散性。水热反应进程越充分,样品的平均粒径越大。加丙三醇后,在反应条件为200℃、p H=10、t=12 h时制备钇掺杂量3%的氧化锆粉体,于1000℃煅烧12 h,得到分散性好、粒径分布窄的单立方相纳米氧化锆粉体颗粒。结论通过设定水热法反应温度、p H值、时间,可以制备粒径可控的稳定氧化锆纳米粉体,且钇掺杂可有效提高氧化锆的稳定性。加入丙三醇可以有效地改善粉体的分散性和稳定性,煅烧稳定氧化锆纳米粉体可以有效减小粉体粒径分布和提高粉体的结晶度。To study the preparation method of stable powder of zirconia, which was good dispersion and narrow size distri- bution. In the experiment, stable zirconia nano powder were prepared by hydrothermal hydrolysis process. The effect of hydro- thermal time, pH, temperature and organic additive glycerol on the particle size, crystalline and stability of the zirconia powder were investigated experimentally. The preparation samples of nano zirconia powder under different hydrothermal conditions were characterized by using XRD and SEM analysis technology. The crystallinity rises with the increase of the hydrothermal temperature. With the increase of the hydrothermal temperature from 150 ~C to 250 ~C, the particle diameter increases first, and then decreases because nucleation rate increases rapidly; The pH values of the reaction solution influence the crystallinity of sample. Selecting a suitable pH value can reduce reunion between powder particles and improve the dispersion of powder. The average partical size of the samples increases with reaction progresse. Zirconia powder doped with 3% Y and Glycerol prepared at 200 ℃, pH=10, t=12 h and then calcining them at 1000 ~C for 12 h, has good dispersion, narrow particle size distribution, and a single cubic phase. The samples of nano stable zirconia powde of controllable particle size were prepared by setting the hy- drothermal hydrolysis conditions, and Yttrium doped effectively improve the stability of zirconia. The addition of glycerol could improve evidently the stability and dispersion of zirconia powder, calcination stabilized zirconia nano powder could effectively reduce partical size distribution and improve the crystalline.

关 键 词：氧化锆 水热法 纳米粉体 粒径 结晶度 稳定性 

分 类 号：TQ134.12[化学工程—无机化工]