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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TiOSO_4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 m~2/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 synthesis of mesoporous titania precursors was carried out under the influence of ultrasound, microwave and hydrothermal field respectively, using industrial titanyl sulfate as titanium source and composite template synthesis route. By adjusting the pH value of the reaction system to control the TiOSO_4 solution hydrolysis and polycondensation rate. After calcination, the anatase mesoporous titania was obtained. The products were characterized by XRD, nitrogen isothermal adsorption and desorption, particle size distribution, SEM, TEM, SAD and X-ray photoelectron spectroscopy (XPS). The results show that the external field with strong polarization and mild hydrothermal environment is conducive to the preparation of mesoporous titania with better structure. The ultrasonic vibration facilitates the formation of mesoscopic structure. Under microwave irradiation, the prepared mesoporous titania has a specific surface area of 146.6 m 2 / g, an average pore diameter of 2.57 nm and a grain size of 13.65 nm. Ultrasound, microwave and hydrothermal than the conventional synthesis method is more conducive to the formation and stability of the mesoporous structure.