超细氢氧化锆颗粒制备试验研究

Investigation on Preparation of Ultrafine Zirconium Hydroxide Particles

利用溶胶-凝胶法制备超细氢氧化锆颗粒并用BET比表面积测试,系统地研究了超声分散、陈化条件、干燥温度、反应温度等制备条件对氢氧化锆活性的影响。利用TEM、HRTEM对所制得的氢氧化锆样品进行表征。试验表明:采用溶胶-凝胶法可以制得直径为10nm左右的氢氧化锆颗粒,颗粒由厚度约为1nm、直径约为4nm的片状分子堆积构成。制备比表面积较高的氢氧化锆样品的最佳工艺参数:反应温度为60℃,超声振荡周期为1∶3,超声分散的时间为15min,陈化温度为60℃,陈化时间为30min,干燥温度为100℃。

In this study, ultrafine zirconium hydroxide particles are prepared with sol-gel method. With BET, the influences to their activities from different conditions, like ultrasonic dispersion, aging conditions, desiccating temperatures and reaction temperatures, are researched systematically. Also, the samples are characterized by TEM and HRTEM. It reveals that zirconium hydroxide particles with a diameter of about 10 nm are prepared with sol-gel method, and such particles are constructed by several plate-like molecules with a thickness of 1nm and a diameter of 4 nm. The optimal preparation conditions for zirconium hydroxide with high activity are concluded that reaction temperature is 60℃, ultrasonic time is 15min with a period of 1 ： 3, aging teperature is 60℃,aging time is 30min, and desiccating temperature is 100℃.