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采用溶胶-凝胶法制备TiO_2凝胶物质,对原料钛酸正丁酯、水、冰乙酸和乙醇各成分用量进行研究,以水热合成法对凝胶物质进行处理,成膜后对两种膜层质量进行观察对比。探索确定了形成凝胶状TiO_2膜层形成的最佳条件,各原料用量钛酸正丁酯∶水∶冰乙酸∶乙醇=4.50∶1.50∶1.00∶20.00(体积比,mL)。将凝胶状TiO_2在烘箱中160℃加热16h进行水热合成。在实验室环境下,将凝胶状TiO_2、水热合成后内酯状TiO_2分别进行了如下处理:乙醇稀释、离心过滤沉淀两次,然后用上层溶液在洁净的玻璃表面形成包覆膜层,然后将两种膜层分别放置在空气中自然干燥和烘箱中匀速升温烘干,并通过扫描电子显微镜观察了水热合成处理后形成的TiO_2膜层微观结构,发现凝胶状TiO_2膜层易开裂、脱落,使用效果不理想,经水热合成法处理的膜层分布均匀、完整、性质稳定。水热合成法制备TiO_2膜层条件在实验室条件下易实现,膜层质量稳定、不开裂,达到使用要求。
The TiO 2 gel was prepared by sol-gel method. The amount of each component of raw materials, such as n-butyl titanate, water, glacial acetic acid and ethanol, was studied. The gel material was treated by hydrothermal synthesis method. The quality of the film was observed and compared. The optimal conditions for the formation of gel-like TiO 2 film were explored. The content of each raw material n-butyl titanate: water: glacial acetic acid: ethanol = 4.50: 1.50: 1.00: 20.00 (volume ratio, mL). The gelatinous TiO_2 was heated in an oven at 160 ℃ for 16h to synthesize hydrothermally. In the laboratory environment, the gel-like TiO_2, hydrothermally synthesized lactone-like TiO_2 were treated as follows: diluted with ethanol, centrifuged and precipitated twice, then the upper solution in the clean glass surface coating layer formed, Then, the two kinds of films were placed in the air, respectively, and dried in an oven at a constant speed. The microstructure of the TiO 2 films formed after hydrothermal synthesis was observed by scanning electron microscopy. The gel-like TiO 2 film was found to be easily cracked , Off, the use of results is not satisfactory, the hydrothermal synthesis of the film distribution process is uniform, complete, stable in nature. Hydrothermal synthesis of TiO 2 film conditions easy to achieve in laboratory conditions, the film quality is stable, not cracking, to meet the requirements.