Shajesh P, Smitha S, Aravind P R, Warrier K G K
Materials & Minerals Division, National Institute for Interdisciplinary Science and Technology, Industrial Estate, Trivandrum 695019, India.
J Colloid Interface Sci. 2009 Aug 15;336(2):691-7. doi: 10.1016/j.jcis.2009.04.023. Epub 2009 Apr 14.
Highly porous organic inorganic hybrid networks have been prepared from tetraethoxysilane (TEOS) and 3-glycidoxypropyltrimethoxysilane (GPTMS) precursors by drying at ambient pressure. Hydrolysis-condensation reactions of the alkoxy groups on the precursors provide the inorganic network and polymerization of the epoxy group on GPTMS, the organic network. The effects of varying the molar ratios, water/OR, and TEOS/GPTMS (precursor ratio) on the gel structure were investigated. Infrared spectroscopy, thermal analysis, nitrogen adsorption measurements, and tunneling electron microscopy were used to characterize the structure and porosity features of the hybrids. At low precursor ratios, the organic networking is characterized by highly cross-linked polymer chains of low molecular weight and at high precursor ratios it consists of mainly linear chains of high molecular weight. Organic networking reinforces the inorganic network at high precursor ratios and the monoliths effectively withstand the stress produced during drying at ambient pressure. But as the proportion of the organic precursor increases, there is a higher shrinkage of the gel network, increasing the density of the dried gel. Variation in precursor ratio affects the volume of larger pores, while varying water content influences the volume of smaller pores. Monolithic gels with low shrinkage and density could be prepared through ambient pressure drying by this method.
通过在常压下干燥,由四乙氧基硅烷(TEOS)和3-缩水甘油氧基丙基三甲氧基硅烷(GPTMS)前驱体制备了高度多孔的有机-无机杂化网络。前驱体上烷氧基的水解缩合反应形成无机网络,而GPTMS上环氧基的聚合形成有机网络。研究了改变摩尔比、水/OR和TEOS/GPTMS(前驱体比例)对凝胶结构的影响。使用红外光谱、热分析、氮吸附测量和隧道电子显微镜来表征杂化物的结构和孔隙率特征。在前驱体比例较低时,有机网络的特征是低分子量的高度交联聚合物链,而在前驱体比例较高时,它主要由高分子量的线性链组成。在高前驱体比例下,有机网络增强了无机网络,整体材料能够有效承受常压干燥过程中产生的应力。但是随着有机前驱体比例的增加,凝胶网络的收缩率更高,干燥凝胶的密度增加。前驱体比例的变化影响较大孔隙的体积,而水含量的变化影响较小孔隙的体积。通过这种方法可以通过常压干燥制备具有低收缩率和密度的整体凝胶。