Abstract
We report the synthesis and structural studies of new hybrid organic–inorganic porous materials with flexible siloxane spacers with different lengths bonded to polyhedral oligomeric silsesquioxane (POSS) cages. Positron annihilation lifetime spectroscopy (PALS) was used to measure the pore sizes of two polymers. For sample 1, which has a shorter linker, the free volume diameters were found to be 5.32 ± 0.06 A, 8.28 ± 0.05 A, and 10.42 ± 0.05 A at 25 °C. The first value represents the POSS cage, while the others describe the space between linkers. For polymer 2, the appropriate diameters are 4.96 ± 0.04 A and 7.96 ± 0.06 A for the POSS cage and linker spacing, respectively. This sample is extremely well organized and homogeneous. The evolution of the free volume sizes as a function of temperature in the range from −20 °C to +60 °C was investigated. Solid-state NMR spectroscopy (SS NMR) was employed to study the structure and molecular dynamics of the polymers. The signal assignment was performed using 1H M...
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