亚微米球形ZrO_2颗粒材料的水热法合成及表征

Solvothermal synthesis of sub-micron spherical zirconia particles

以Zr(NO_3)_4·5H_2O和CO(NH_2)_2为原料,乙醇为溶剂,通过水热法合成亚微米级球形ZrO_2颗粒;用扫描电子显微镜(SEM)、X射线衍射仪(XRD)、傅里叶红外光谱仪(FT-IR)、热重-差热分析仪(TGA-DTA)、紫外-可见光吸收光谱仪(UVVis)对ZrO_2颗粒进行分析表征,研究工艺条件对球形ZrO_2颗粒尺寸和形貌的影响。结果表明:通过水热法合成的球形ZrO_2颗粒粒径分布较窄,添加适量的表面活性剂、无机盐溶液及水对产物的尺寸与形貌具有一定的影响;添加适量水可获得粒径分布更窄的球形ZrO_2颗粒,且热处理对球形ZrO_2颗粒的粒径大小和形状影响不大。

Sub-micron spherical ZrO_2 particles were prepared by the solutions C_2H_5OH containing CO（NH_2）_2 and Zr（NO_3）_4·5H_2O via the solvothermal treatment at 100 ℃. Scanning electron microscopy（SEM）, X-ray diffraction（XRD）, Fourier transform infrared（FT-IR） spectroscopy, thermogravimetric and differential thermal analysis（TGA-DTA）, and UV-vis spectra were used to characterize the samples. The influence of preparation conditions on the final product was investigated. The experimental results indicate that sub-micron spherical ZrO_2 particles prepared via the solvothermal treatment possess narrow particle size distribution.The surfactants, inorganic salt solution and water have some effect on size and shape of products. The spherical ZrO_2 particles with narrow particle size distribution can be obtained by adding appropriate amount of water, and the spherical shape remained during the heat treatment.