Kobler Johannes, Möller Karin, Bein Thomas
Department of Chemistry and Biochemistry and Center for NanoScience (CeNS), University of Munich, Butenandtstrasse 5-13 (E), D-81377 Munich, Germany.
ACS Nano. 2008 Apr;2(4):791-9. doi: 10.1021/nn700008s.
The synthesis and characterization of colloidal mesoporous silica (CMS) functionalized with vinyl-, benzyl-, phenyl-, cyano-, mercapto-, aminopropyl- or dihydroimidazole moieties is reported. Uniform mesoporous particles ranging in size from 40 to 150 nm are generated in a co-condensation process of tetraethylorthosilicate (TEOS) and organotriethoxysilanes (RTES) in alkaline aqueous media containing triethanolamine (TEA) in combination with cetyltrimethylammonium chloride (CTACl) serving as a structure-directing agent. The materials are obtained as colloidal suspensions featuring long-term stability after template removal by ion exchange with an ethanolic solution of ammonium nitrate or HCl. The spherical particles exhibit a wormlike pore system with defined pore sizes and high surface areas. Samples are analyzed by a number of techniques including TEM, SEM, DLS, TGA, Raman, and cross-polarized (29)Si-MAS NMR spectroscopy, as well as nitrogen sorption measurements. We demonstrate that co-condensation and grafting methods result in similar changes in the nitrogen adsorption behavior, indicating a successful internal lining of the pores with functional groups through both procedures.
报道了用乙烯基、苄基、苯基、氰基、巯基、氨丙基或二氢咪唑部分官能化的胶体介孔二氧化硅（CMS）的合成与表征。在碱性水介质中，以四乙氧基硅烷（TEOS）和有机三乙氧基硅烷（RTES）在含有三乙醇胺（TEA）并以十六烷基三甲基氯化铵（CTACl）作为结构导向剂的条件下进行共缩合过程，生成尺寸范围为40至150 nm的均匀介孔颗粒。通过与硝酸铵或HCl的乙醇溶液进行离子交换去除模板后，这些材料以具有长期稳定性的胶体悬浮液形式获得。球形颗粒呈现出具有确定孔径和高表面积的蠕虫状孔系统。通过多种技术对样品进行分析，包括透射电子显微镜（TEM）、扫描电子显微镜（SEM）、动态光散射（DLS）、热重分析（TGA）、拉曼光谱、交叉极化（29）Si - 魔角旋转核磁共振（MAS NMR）光谱以及氮吸附测量。我们证明共缩合和接枝方法导致氮吸附行为发生类似变化，表明通过这两种方法孔内均成功地形成了官能团内衬。
