Preparation and characterization of perfluoroaulfonic resin/titaniaorganic-inorganic hybrid films were presented. The transparent hybrid films were prepared by hydrothermal treatment at low temperature of a mixed solution of tetrabutyl titanata and perfluorosulfonic resin with the help of acetylacetone. The charactarization was carried out by SEM, XRD, FT-IR, UV-Vis and TGA. The results showed that the perfiuorosulfonic resin/titania hybrid transparent films were composed of titania particles dispersed in the perfluorosulfonic resin matrix very well and the titania was of anatase phase. Its diameter decreased with increasing weight ratio of titania to perfluorosulfonic resin.