以正硅酸乙酯（TEOS）、硝酸铁和银酸铵为原料，用溶胶－凝胶法制备了Fe－Si－O和Mo－O溶胶，通过浸渍－提拉法，分别制得了Fe－Si－O薄膜（以载玻片为基板）和MO－Fe－Si－O薄膜（以多孔α－Al2O3为基质材料）．考察了制备工艺条件对Fe－Si－O成膜的影响，采用DTA、XRD和SEM等技术研究了热处理条件对Mo－Fe－Si－O薄膜结构的影响．结果表明：溶胶粘度、衬底材质、浸渍时间、提拉速度等是影响Fe－Si－O成膜的主要因素；溶胶－凝胶法制备的Mo－Fe－Si－O／α－Al2O3无机复合膜热处理温度达到650℃以上，即能形成比较明显的结晶相，薄膜经高温焙烧（700℃）－冷却反复5次，膜表面没有出现剥离和开裂现象．
Fe-Si-O and Mo-O sols were prepared by sol-gel process by using Si(OC2H5)4 (TEOS), Fe(NO3)3·9H2O and (NH4)6·Mo7O24·4H2O.
The Fe-Si-O membrane(on the microscope slide) and Mo-Fe-Si-O membrane (on the α-Al2O3 support) were obtained by diploid-circle-
dipping-coating. The effect of process conditions on the Fe-Si-O membrane and the influence of thermal treatment process on the Mo-Fe-Si-O membrane were studied
by DTA, XRD and SEM technique. The results indicated that the major factors affecting the Fe-Si-O membrane were sol viscosity, substrates,
dipping-coating time, withdrawal speed etc, and Mo-Fe-Si-O/α-Al2O3 membrane obtained by sol-gel method must be sintered at above 650℃
to form perfectly cubic phase structure. The membrane surfaces were crack-free after five times sintering at 700℃-cooling at 25℃
procedures.
参考文献
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