硅锆复合膜的制备与表征-高校化学工程学报.pdf

20 3 No.3 Vol.20 2006 6 Journal of Chemical Engineering of Chinese Universities June 2006 1003-9015(2006)03-0443-06 , , , ( , 300072) - TG-DTA XRD BET SEMTEM AFM 25 () 700~900 - O648.22 TQ174.758.11 TQ028.8 A Preparation and Characterization of Silica-Zirconia Composite Membranes ZHANG Bao-quan, ZHANG Bao-feng, XU Li-ming, LIU Xiu-feng (School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China) Abstract: The defect-free silica-zirconia composite membrane was prepared by sol-gel method. The surface morphology, pore size distribution and crystal structure of the membrane were investigated by using thermogravimetric analysis and differential thermal analysis (TGA-DTA), X-ray diffraction (XRD), gas adsorption analyzer (BET), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and atomic force microscopy (AFM), etc. The zirconium nitrate is more suitable to be used as the precursor than zirconium oxychloride to get stable zirconyl oxalate sol with uniform particles. Silica was used as the stabilization agent. The defect-free composite membrane was obtained when 25% silica (in volume) is added. Pure zirconia is ready to transform from tetragonal to monoclinic phase at 600~650ºC, however, the crystal transformation is prohibited by the interaction between silica and zirconia, which also leads to increase the crystallization temperature of the silica. The preliminary results demonstrate that only tetragonal zirconia appears at 700~900, and the size of which does not change with temperature. Key words: zirconium nitrate; silicon