Effect of glycerol on monolithicity, density, microhardness and sintering temperature of TMOS silica aerogels

A. Venkateswara Rao , G.M. Pajonk , D. Haranath , P.B. Wagh
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引用次数: 10

Abstract

In continuation of our earlier work on silica aerogels, the experimental results on monolithicity, bulk density and Vickers hardness of glycerol modified silica aerogels as a function of sintering temperatures are reported. The molar ratios of methanol (MeOH) solvent, glycerol (G) additive, ammonia (NH4OH) catalyst and water (H2O) to the tetramethoxysilane (TMOS) precursor were found to be best in between the ranges: 6–12, 0.3–0.83, 3.6 × 10−2–1.0 × 10−1 and 4–8, respectively, for the production of monolithic silica aerogels. The best quality silica aerogels in terms of monolithicity, transparency and low density have been obtained with the molar ratio of 1TMOS:0.83G:12MeOH:4H2O:3.6 × 10−3 NH4OH, respectively. The aerogels of this molar ratio have been characterized by density, Vickers hardness measurements and scanning electron microscopic observations as a function of sintering temperatures. The pore size distribution was found to shift towards the narrow pore radii as the temperature increased above 260°C. The results have been supported by the particle and pore sizes observed using scanning electron microscopy technique and BET surface analyses.

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甘油对TMOS二氧化硅气凝胶的整体度、密度、显微硬度和烧结温度的影响
在我们早期二氧化硅气凝胶研究的基础上,本文报道了甘油改性二氧化硅气凝胶的整体密度、体积密度和维氏硬度随烧结温度的变化规律。甲醇(MeOH)溶剂、甘油(G)添加剂、氨(NH4OH)催化剂和水(H2O)与四甲基氧基硅烷(TMOS)前驱体的摩尔比分别在6-12、0.3-0.83、3.6 × 10−2-1.0 × 10−1和4-8范围内是制备整体硅气凝胶的最佳原料。当摩尔比为1TMOS:0.83G:12MeOH:4H2O:3.6 × 10−3 NH4OH时,得到了整体质量、透明度和低密度最好的二氧化硅气凝胶。这种摩尔比的气凝胶已经通过密度、维氏硬度测量和扫描电镜观察作为烧结温度的函数来表征。在260℃以上,随着温度的升高,孔隙尺寸分布向窄孔半径方向偏移。用扫描电子显微镜技术和BET表面分析观察到的颗粒和孔隙大小支持了这一结果。
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Author index Subject index Contents Investigation of organosilanes as structure-directing agents in zeolite synthesis The influence of gel properties on the kinetics of crystallization and particulate properties of MFI-type zeolities. I. The influence of time and temperature of gel ageing on the particulate properties of silicalite-1 microcrystals
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