Department of Chemistry and Center for NanoScience (CeNS), University of Munich, Butenandtstrasse 5-13 (Gerhard-Ertl Building), 81377 Munich, Germany.
Chemistry. 2011 Aug 16;17(34):9463-70. doi: 10.1002/chem.201002278. Epub 2011 Jul 5.
Cubic and circular hexagonal mesoporous carbon phases in the confined environment of the pores of anodic alumina membranes (AAM) were obtained by organic-organic self-assembly of a preformed oligomeric resol precursor and the triblock copolymer templates Pluronic F127 or P123, respectively. Casting and solvent evaporation were followed by self-assembly and the formation of a condensed wall material by thermopolymerization of the precursor oligomers, thus resulting in mesostructured phenolic resin phases. Subsequent thermal decomposition of the surfactant and carbonization were achieved through thermal treatment at temperatures up to 1000 °C under an inert atmosphere. The resulting hierarchical mesoporous composite materials were characterized by small-angle X-ray scattering and nitrogen-sorption measurements. The structural features were directly imaged in TEM cross-sections of the composite membranes. For both structures, the AAM pores were completely filled and no shrinkage was observed due to strong adhesion of the carbon-wall material to the AAM pore walls. As a consequence, the pore size of the mesophase system stays almost constant even after thermal treatment at 1000 °C.
通过预聚物酚醛树脂的有机-有机自组装以及分别使用两亲性嵌段共聚物模板 Pluronic F127 和 P123,在阳极氧化铝膜(AAM)孔的受限环境中得到了立方和六方介孔碳相。浇铸和溶剂蒸发后,通过前驱体低聚物的自组装和缩合壁材料的形成,得到了介孔酚醛树脂相。随后,通过在惰性气氛下高达 1000°C 的热处理来实现表面活性剂的热分解和碳化。通过小角 X 射线散射和氮气吸附测量对所得的分级介孔复合材料进行了表征。在复合膜的 TEM 横截面中直接对结构特征进行了成像。对于这两种结构,AAM 孔都被完全填充,由于碳壁材料与 AAM 孔壁之间的强附着力,没有观察到收缩。因此,即使在 1000°C 的热处理后,介相体系的孔径仍几乎保持不变。