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以正硅酸乙酯和钛酸丁酯为原料,用溶胶-凝胶法制备SiO2-TiO2复合膜。采用TG-DTG、FT-IR和AFM等测试技术对膜的热稳定性、凝胶膜热处理前后的结构变化和复合膜的表面微观形貌进行表征。实验结果表明:分级干燥或者保持65%相对湿度的直接干燥可以得到无裂纹的凝胶膜;复合膜的热稳定较好,650℃以后没有明显的质量损失;焙烧过程中,不同升温区间采用不同的升温速率,以防止膜开裂;复合膜在制备过程中形成了Si-O-Ti键,经烧结后Si-O-Ti键位置没有发生明显位移;原子力显微镜分析表明,膜表面完整无缺陷,薄膜平均孔径约为50nm。

SiO2-TiO2 composite membranes were prepared by sol-gel process using tetraethoxy silicone(TEOS) and tetrabutyl titivate(TBOT) as raw materials.Thermal stability,structural transformation before and after heat treatment,surface morphologies of composite membranes were characterized by means of thermogravimetry-derivative thermogravimetry(TG-DTG),Fourier transform infrared(FT-IR) spectroscopy and atomic force microscopy(AFM) etc.The results show that gradual drying or directly drying under relative humidity 65% can get gel membranes without cracks;composite membrane's thermal stability is good,there is no significant mass loss after being heat treated at 650℃;In the process of sintering,different heating rates are set in different temperature ranges in order to prevent membranes cracking;Si-O-Ti bond forms during the preparation process,and the position doesn't displace obviously after being sintered.Atomic force microscopy analysis shows that membrane surfaces are integrit,and membrane pore size is about 50nm.

参考文献

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[4] Carl Blanchet;Pascal Joly;Michel Granier;Gerard F. Lanneau;Marc Cretin;Michel Persin;Oleg Melnyk;Jean-Olivier Durand .Synthesis and chemical reactivity of semicarbazide-supported silicas[J].Tetrahedron letters: The International Journal for the Rapid Publication of Preliminary Communications in Organic Chemistry,2003(22):4191-4194.
[5] Chang JW.;Marrero TR.;Yasuda HK. .Continuous process for propylene/propane separation by use of silver nitrate carrier and zirconia porous membrane[J].Journal of Membrane Science,2002(1/2):91-102.
[6] 余定华,何杰,杨万秀.微波辐射法制备TiO2/丝光沸石薄膜光催化剂的研究[J].安徽大学学报(自然科学版),2004(02):59-65.
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