A new organic/inorganic hybrid polymer POSS/PMMA was prepared by atom transfer radical polymerization (ATRP), in which Octa(γ -chloropropyl) polyhedral oligomeric silsesquioxane (POSSCl) was used as a crosslink agent to incorporate poly(methyl methacrylate) (MMA). The structure and composition of the composite was characterized using various techniques, including Fourier transform infrared spectroscopy (FTIR), 1
H NMR, X-ray diffraction (XRD) as well as gel permeation chromatography (GPC). All the results indicated that POSS molecule was successfully incorporated into the PMMA matrix. The thermal stability property of the composite was investigated by thermal gravimetric analysis (TGA).The results showed that the composite displayed good thermal stability and higher temperatures at maximum weight loss rate (T max ) than that of the pure PMMA homopolymer, which may be attributed to the incorporation of rigid silica cube.