以工业硫酸氧钛为钛源,采用复合模板合成路线,分别于超声,微波和水热外场作用下合成了介孔二氧化钛前驱体.通过调节反应体系的pH值来控制TiOSO4液的水解和缩聚速率.煅烧脱除模板后得到锐钛型的介孔二氧化钛.产物采用XRD,氮等温吸附脱附,粒度分布,SEM,TEM,SAD和X射线能谱分析(XPS)等技术进行了表征.结果表明:具有强极化作用和温和水热环境的外场利于制备结构更佳的介孔二氧化钛;超声振动利于介观结构的形成.在微波辐照下,所制得介孔二氧化钛的比表面积为146.6 m2/g,平均孔径2.57 nm,晶粒尺寸13.65 nm.超声、微波和水热较常规合成方法更利于形成和稳定介孔结构.
The precursors of mesoporous titania were synthesized via composite templates route from industrial TiOSO4 solution under ultrasonic, microwave and hydrothermal field effect. The rate of hydrolysis and condensation of TiOSO4 solution was controlled by adjusting the pH value of the reacting system. Mesoporous titania with anatase phase was obtained after templates removal by calcinations. The as-prepared powder was characterized by XRD, N2 isothermal adsorption and desorption method, particle size distribution, SEM, TEM, SAD and XPS. External field with enhancing polar action and soft hydrothermal condition is adaptive to prepare better mesoporous titania. Ultrasonic vibration promotes the formation of mesoporous structure. Under microwave irradiation, mesoporous TiO2 was synthesized with BET surface area 146.6 m2/g,average pore diameter 2.57 nm and crystal size 13.65 nm. Ultrasonic, microwave irradiations and hydrothermal condition are better than conventional method in forming mesopore and stabilizing the structure.
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