In this study we incorporated various amounts of a double-decker silsesquioxane (DDSQ) into phenolic/DDSQ hybrids, which we prepared from a bifunctionalized phenolic DDSQ derivative (DDSQ-4OH), phenol, and CH2O under basic conditions (with DDSQ-4OH itself prepared through hydrosilylation of nadic anhydride with DDSQ and subsequent reaction with 4-aminophenol). We characterized these phenolic/DDSQ hybrids using Fourier transform infrared spectroscopy; 1H, 13C, and 29Si nuclear magnetic resonance spectroscopy; X-ray photoelectron spectroscopy (XPS); and thermogravimetric analysis. The thermal decomposition temperature and char yield both increased significantly upon increasing the DDSQ content, with the DDSQ units providing an inorganic protection layer on the phenolic surface, as confirmed through XPS analyses. We obtained carbon/DDSQ hybrids from the phenolic/DDSQ hybrids after thermal curing and calcination at 900 °C; these carbon/DDSQ hybrids displayed electrochemical properties superior to those of previously reported counterparts.

In this study the authors used an unusual linear symmetric poly(ethylene oxide-b-caprolactone) (PEO-b-PCL) diblock copolymer as a template within phenolic/double-decker silsesquioxane (DDSQ) hybrids to synthesize mesoporous phenolic/DDSQ materials having Frank-Kasper (FK) phases (e.g., , A15, H, and Z phases). These FK structures are the first to have been prepared using a block copolymer and the first to exist in mesoporous materials. The authors' mesoporous carbon/DDSQ hybrids displayed high capacitance (764 F g −1 at a current of 0.5 A g −1 and 98.4% capacitance retention over 2000 cycles), arising from their high surface areas, high pore volumes, and tunable concentrations of N, O, and Si heteroatoms.