pH对硅溶胶-凝胶-四乙基硅酸-三甲基氯硅兰(TEOS-TMCS)合成的影响

Artha Monica Andini, C. Azmiyawati, A. Darmawan
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引用次数: 0

摘要

以三甲基氯硅烷(TMCS)和四乙基硅酸盐(TEOS)为前驱体,完成了溶胶-凝胶法合成二氧化硅的研究。本研究的目的是确定pH值如何影响合成二氧化硅的性能。利用红外光谱(FTIR)、热重分析(TGA)和GSA对合成的疏水二氧化硅进行了表征,以确定pH调节对其官能团特征、热性能和孔隙形态的影响。TEOS/TMCS的比例固定为75:25,改变pH(4、6、7、8、10)和煅烧温度(未煅烧、300℃和500℃)。FTIR分析表明,随着煅烧温度的升高,干凝胶中C-H和Si-OH基团的数量减少。pH值为6时形成的干凝胶在其他pH值中具有最高的热稳定性。BET分析的结果表明,pH值的变化直接影响了表面的物理特性,使凝胶网络的刚性降低,更容易受到大气中孔隙体积和直径收缩的影响。同时,在碱性介质中,会发生连续的冷凝,使孔径和体积减小。高孔径和大体积意味着pH为7是制备干凝胶的理想条件。
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Effect of pH on the Synthesis of Silica Sol-Gel Tetraethylorthosilicate-Trimethylchlorosilan (TEOS-TMCS)
Sol-gel synthesis of silica employing the co-precursor trimethylchlorosilane (TMCS) and the precursor tetraethylorthosilicate (TEOS) was accomplished. The purpose of this investigation was to ascertain how pH affected the properties of synthetic silica. The synthesized hydrophobic silica was characterized using FTIR, TGA, and GSA to determine the effect of pH adjustment on the functional group characters, thermal properties, and pore morphology. The ratio between TEOS/TMCS was fixed at 75:25 and varied the pH (4, 6, 7, 8, and 10) and the calcination temperature (without calcination, 300℃ and 500℃). FTIR analysis showed that the number of C-H and Si-OH groups in the xerogel decreased with increasing calcination temperature. Xerogel formed at pH 6 provides the highest thermal stability among other pHs. The results from the BET analysis revealed that changes in pH directly affect the physical characteristics of the surface, making the resulting gel network less rigid and more susceptible to shrinkage of pore volume and diameter in the atmosphere. Meanwhile, in an alkaline medium, continuous condensation will occur so that the pore diameter and volume decrease. The high pore diameter and volume imply that pH 7 is ideal for preparing xerogels.
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