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多孔 3D 纳米结构中的结构-性能关系:使用乙醇作为溶剂制备的环氧交联硅气凝胶。

Structure-property relationships in porous 3D nanostructures: epoxy-cross-linked silica aerogels produced using ethanol as the solvent.

机构信息

NASA Glenn Research Center, 21000 Brookpark Road, Cleveland, Ohio 44135, USA.

出版信息

ACS Appl Mater Interfaces. 2009 Apr;1(4):894-906. doi: 10.1021/am900014z.

Abstract

Cross-linking silica aerogels with organic groups has been shown to improve the strength over un-cross-linked aerogels by as much as 2 orders of magnitude. Previous cross-linking chemistry has been developed using solvents specifically chosen to dissolve the monomers and accommodate the reaction temperature. Because the process of making the aerogels requires so much solvent, it is of interest to consider less toxic solvents such as ethanol to increase safety and enhance scale up. To this end, two different epoxy precursors with suitable solubility in ethanol were evaluated as cross-linkers for silica gels prepared from (3-aminopropyl)triethoxysilane and tetraethylorthosilicate. In addition, 1,6-bis(trimethoxysilyl)hexane (BTMSH) was used as an additive in the underlying silica structure to add flexibility to the aerogels. It was found that the ethanol-derived aerogels exhibited more shrinkage than those prepared from other solvents but that including BTMSH in the aerogels significantly reduced this shrinkage. Inclusion of BTMSH also imparted the ability of the aerogel monoliths to recover elastically when compressed up to 50% strain. In addition, optimized cross-linked aerogels prepared in this study have mechanical properties comparable to those using other more undesirable solvents and cross-linkers.

摘要

用有机基团交联二氧化硅气凝胶已被证明可以将未交联气凝胶的强度提高 2 个数量级。以前的交联化学方法是使用专门选择的溶剂来溶解单体并适应反应温度。由于制备气凝胶需要大量溶剂,因此考虑使用毒性较小的溶剂(如乙醇)来提高安全性并提高规模是很有意义的。为此,评估了两种不同的在乙醇中具有适当溶解度的环氧前体,作为由(3-氨丙基)三乙氧基硅烷和正硅酸乙酯制备的硅胶的交联剂。此外,1,6-双(三甲氧基硅基)己烷(BTMSH)被用作底层硅胶结构中的添加剂,以增加气凝胶的柔韧性。结果发现,与用其他溶剂制备的气凝胶相比,由乙醇制备的气凝胶收缩率更高,但在气凝胶中加入 BTMSH 显著降低了这种收缩率。BTMSH 的加入还赋予了气凝胶整体在压缩至 50%应变时弹性恢复的能力。此外,本研究中制备的优化交联气凝胶具有与使用其他更不理想的溶剂和交联剂相当的机械性能。

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