Void Formation/Elimination and Viscoelastic Response of Polyphenylsilsesquioxane Monolith.

Polyphenylsilsesquioxane (PhSiO) particles as an organic-inorganic hybrid were prepared using sol-gel method, and monolithic samples were obtained via a warm-pressing. The reaction mechanism of particles' polymerization and transformation to the monolith under the warm-press were investigated using solid state Si nuclear magnetic resonance (NMR) spectrometer, thermal gravimetric-differential thermal analyzer (TG-DTA), mass spectrometer (MS) and scanning electron microscope (SEM). Transparent and void-free monoliths are successfully obtained by warm-pressing above 180 °C. Both the terminal ⁻OH groups on particles' surface and warm-pressing are necessary for preparation of void-free PhSiO monolith. From the load-displacement measurement at various temperatures, a viscoelastic deformation is seen for PhSiO monolith with voids. On the other hand, an elastic deformation is seen for void-free PhSiO monolith, and the void-free monolith shows much higher breakdown voltage.