纳米单斜相ZrO_2的制备

Preparation of a Nano-sized ZrO_2 with Mon ℃linic Phase

沉淀法制备了ZrO2,重点考察了煅烧温度ZrO2粉体性质的影响,并用热重法-差示扫描量热法、X-射线衍射和N2物理吸附等手段对粉体进行了测试和表征。结果表明,随煅烧温度的升高,ZrO2的比表面积、平均孔径和孔容大幅度下降,微晶尺寸逐渐增大,单斜相ZrO2的含量增加,四方相的含量减少。1000℃时ZrO2粉体完全以单斜相存在。600℃煅烧2 h制得了单斜相为主的ZrO2粉体,其微晶尺寸为21.6 nm,比表面积为39.2 m2/g、平均孔径为11.7 nm,孔容为0.23 cm3/g。

ZrO2 was prepared by a precipitation method, and the influence of the calcination temperature on the nature of ZrO2 was investigated. The ZrO2 samples were characterized by thermogravimetry-differential scanning calorimetry, X-ray diffraction and N2 physisorption. The results showed that the BET surface area, pore volume and pore diameter decreased and the crystallite size increased with the increase of the calcination temperature. Moreover, the content of the mon℃ linic phase increased and the content of the tetragonal phase decreased with the calcination temperature. When the calcination temperature was 1000 ℃, ZrO2 completely existed as the mon℃ linic phase. The ZrO2 calcinated at 600 ℃was mainly present in the mon℃ linic phase. Its crystallite size was 21.6 nm. Its BET surface area, pore diameter and pore volume were 39.2 m2/g, 11.7nm and 0.23 cm3/g respectively.