Keilbach Andreas, Döblinger Markus, Köhn Ralf, Amenitsch Heinz, Bein Thomas
Department of Chemistry and Biochemistry and Center for NanoScience (CeNS), University of Munich, Butenandtstrasse 5-13 (E), 81377 Munich, Germany.
Chemistry. 2009 Jul 6;15(27):6645-50. doi: 10.1002/chem.200802216.
Periodic mesoporous organosilica (PMO) mesophases based on bis(triethoxysilyl)ethane (BTSE) were synthesized within the confined tubular environment of anodic alumina membrane (AAM) channels. The resulting mesophases were investigated by transmission small angle X-ray scattering (SAXS), nuclear magnetic resonance (NMR), nitrogen sorption, and transmission electron microscopy (TEM). Two different surfactants--nonionic Brij 56 and ionic cetyltrimethylammonium bromide (CTAB)--were used in an acid-catalyzed evaporation-induced self-assembly (EISA) process. Brij 56 as the structure-directing agent (SDA) resulted in the formation of either the hexagonal circular or the cubic mesophase. While the hexagonal circular mesophase is common for such kinds of composites, the cubic mesophase has never been reported before. The template could be removed from the mesophases by template extraction and calcination after annealing the samples. When using CTAB as the SDA during EISA, the only mesophase observed was the hexagonal circular structure. This is in contrast to previous experiments and reports on pure silica mesophases, where the only mesophase formed with CTAB is hexagonal columnar.
基于双(三乙氧基硅基)乙烷(BTSE)的周期性介孔有机硅(PMO)中间相在阳极氧化铝膜(AAM)通道的受限管状环境中合成。通过透射小角X射线散射(SAXS)、核磁共振(NMR)、氮吸附和透射电子显微镜(TEM)对所得中间相进行了研究。在酸催化的蒸发诱导自组装(EISA)过程中使用了两种不同的表面活性剂——非离子型Brij 56和离子型十六烷基三甲基溴化铵(CTAB)。Brij 56作为结构导向剂(SDA)导致形成六方圆形或立方中间相。虽然六方圆形中间相对此类复合材料来说很常见,但立方中间相此前从未有过报道。在对样品进行退火后,可通过模板萃取和煅烧从中间相中去除模板。在EISA过程中使用CTAB作为SDA时,观察到的唯一中间相是六方圆形结构。这与之前关于纯二氧化硅中间相的实验和报道形成对比,在那些实验和报道中,与CTAB形成的唯一中间相是六方柱状。