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以正硅酸乙酯和氧氯化锆为原料 ,用溶胶 -凝胶法制备了无支撑ZrO2 -SiO2 膜。应用DTA -TG、XRD、SEM和BET等测试技术对无支撑ZrO2 -SiO2 膜的结构、表面形貌和孔径进行了表征 ,结果表明ZrO2 -SiO2 凝胶膜虽在 46 7℃开始出现少量单斜ZrO2 ,但在 5 0 0℃和 12 0 0℃热处理后的主晶相均为四方ZrO2 ,显然SiO2 的存在阻碍了四方相ZrO2 向单斜相ZrO2 转变的过程 ,ZrO2 -SiO2 膜具有比ZrO2 膜更高的热稳定性 ,在95 0℃烧结的无支撑ZrO2 -SiO2 膜孔径稍呈双峰分布 ,其最可几孔径为 3 .3 5nm。
Using orthosilicate and zirconium oxychloride as raw materials, an unsupported ZrO2-SiO2 membrane was prepared by sol-gel method. The structure, surface morphology and pore size of unsupported ZrO2 -SiO2 membranes were characterized by DTA-TG, XRD, SEM and BET techniques. The results showed that although the ZrO2-SiO2 gel films began to appear a few monoclinic ZrO2. However, the main crystalline phases after heat treatment at 500 ℃ and 1200 ℃ are all tetragonal ZrO2. Obviously, the presence of SiO2 hinders the transformation of tetragonal ZrO2 to monoclinic ZrO2. The ZrO2-SiO2 film has a higher resistivity than the ZrO2 film Higher thermal stability, the pore size of unsupported ZrO2-SiO2 film sintered at 95 0 C is slightly bimodal with the most probable pore size of 3.35 nm.