Polystyrene (PS)--methacryloxypropyl trimethoxy silane (MPTMS) copolymer/zirconia (ZrO2) nanohybrid materials were successfully prepared by the combination of solvothermal and in situ synthesis methods, in which the comonomer was used as chemical bonding agent between the nanoparticles and the matrix, and acetylacetone (AcAc) was used as a size control agent of ZrO2 in the PS matrix. Then, a new transparency film with a relatively high refractive index (1.72) was successfully obtained, in which ZrO2 could be dispersed well in the PS-MPTMS matrix. Field emission scanning electron microscopy images indicated that AcAc was helpful in the dispersion of the nanoparticles, and smaller ZrO2 particles with no aggregation were obtained in the PS-MPTMS matrix. The structure and thermal properties of the hybrid films were investigated by Fourier transform infrared spectroscopy and thermogravimetric analysis, and the surface properties were also examined. (c) 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 130: 2320-2327, 2013