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A comparative study on the synthesis mechanism and microstructural development of hierarchical porous mullite monoliths obtained by the sol-gel process with three different silicon sources

机译:三种不同硅源的溶胶-凝胶法制备分级多孔莫来石整体材料的合成机理和微观结构发展的比较研究

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摘要

Hierarchical porous mullite monoliths have been prepared via a sol-gel process accompanied by phase separation. Propylene oxide (PO) acted as an acid scavenger to mediate the gelation, poly(ethylene oxide) (PEO) as the phase-separation inducer and network former, aluminum chloride hexahydrate (AlCl3 center dot 6H(2)O) as the aluminum source. The route was improved by using hypotoxic tetraethylorthosilicate (TEOS) and nontoxic aqueous colloidal silica (Aq) instead of tetramethoxysilane (TMOS). The synthesis mechanism and microstructural development were comparatively investigated by scanning electron microscopy (SEM), thermogravimetry-differential thermal analysis (TG-DTA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and nitrogen adsorption-desorption. It was found that the mixing degree of precursors and concurrent process of gelation and phase separation are key elements to get well-defined hierarchical porous mullite monoliths. In addition, the monoliths with high relative crystallinity are more likely to be obtained under low transformation temperature in organic silicon sources system. (C) 2015 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
机译:已通过溶胶-凝胶法伴随相分离制备了分级的多孔莫来石整体料。环氧丙烷(PO)充当酸清除剂来介导凝胶化,聚环氧乙烷(PEO)作为相分离诱导剂和网络形成剂,六水合氯化铝(AlCl3中心点6H(2)O)作为铝源。通过使用次毒性的原硅酸四乙酯(TEOS)和无毒的水性胶体二氧化硅(Aq)代替四甲氧基硅烷(TMOS)改进了该路线。通过扫描电子显微镜(SEM),热重-差热分析(​​TG-DTA),X射线衍射(XRD),傅里叶变换红外光谱(FTIR)和氮吸附-脱附对合成机理和微观结构进行了比较研究。发现前驱体的混合程度以及同时发生的凝胶化和相分离过程是获得定义明确的分级多孔莫来石整体材料的关键因素。另外,在有机硅源系统中,在较低的转变温度下,更有可能获得具有较高相对结晶度的整料。 (C)2015 Elsevier Ltd和Techna Group S.r.l.版权所有。

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