采用正硅酸乙酯和氧氯化锆,通过溶胶-凝胶法,以有机改性硅酸盐技术和水置换法相结合在 80℃条件下制备 ZrO2-SiO2 无开裂干凝胶.使用 TG-DTA 研究了干凝胶在加热过程中的热量和质量变化,根据 TG-DTA 曲线选择合适的温度对 10ZrO2-90SiO2(质量分数)干凝胶进行了热处理,并进行了 XRD 和 IR 分析,确定了干凝胶的析晶情况以及材料结构中各种基团的振动情况.采用有机改性硅酸盐技术和水置换法相结合可以减少凝胶在热处理过程中的开裂程度,ZrO2 的含量对胶凝时间和凝胶的颜色有很大的影响,当热处理温度升高时,析晶倾向越来越明显,达到 1150℃时出现晶体转变.
The dried gels without cracks were prepared under 80℃ with Si(OC2H5)4 and ZrOCl2*6H2O by the sol-gel method using the organically modified silicates technology combining with the water displacement method. The thermal and gravimetric changes of 10ZrO2*90SiO2 during heating were determined by TG-DTA. The heat treatment was carried out under different temperature according to the TG-DTA curve. The vibrating spectra of all cluster were studied by IR and the separating out of 10ZrO2*90SiO2 crystal was studied by XRD. The results show that the organically modified silicates technology and water exchanging method could reduce the crack of the dried gel occurring during the heating treatment. The gravimetric content of ZrO2 has an important effect on the gelating time and color of the gel. The tendency of the crystalline becomes more and more clear with the heating temperature increasing, when the heating temperature reaches 1150℃, the crystal conversion happens.
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