Synthesis and characterization of an aliphatic monoimide-bridged polysilsesquioxane by the sol-gel route

Based on differential scanning calorimetry data, it was shown that the reaction of (3-triethoxysilylpropyl)succinic anhydride and (3-amino)propyltriethoxysilane at 110 A degrees C resulted in the formation of polyamic acid, whereas the thermal treatment at 220 A degrees C led to the generation of an aliphatic monoimide-bridged polysilsesquioxane as proved by FT-IR. X-ray powder diffraction studies showed a prominent reflection at 2 theta A = 6.66A degrees (d = 1.32 nm) revealing that a crystalline area is formed. Si-29 CP-MAS-NMR and C-13 CP-TOSS-MAS-NMR measurements proved that no cleavage of the Si-C bond occurred, and a highly condensed material was obtained.