C 60 fullerene has been radiation grafted on bare and functionalized silica surface with mercaptopropyl moieties in toluene solution. The resulting fullerene-silica hybrid nanomaterials have been characterized by FT-IR and solid state 13 C CP-MAS NMR spectroscopy and compared to the radiolysis products of C 60 in toluene. It has been found that fullerene is grafted on silica surface but, because the radiation grafting has been conducted in toluene, fullerene results arylated from radicals derived from toluene radiolysis. The fullerene-silica hybrid nanomaterials cannot be extracted by warm decalin, demonstrating that the fullerene cage is chemically bonded on the silica surface. The thermal behavior of fullerene-silica hybrid nanomaterials has been studied by thermogravimetric analysis (TGA) and differential thermal analysis (DTA) in air flow.