Abstract: TiO₂/Perfluorosulfonated Resin(PSR) hybrid films were prepared at low-temperature by steam-hydrothermal treatment. Their crystal structure, surface morphology and structure were characterized by XRD, AFM and FT-IR,respectively, and the effects of PSR and TiO₂ in the film on their performance after hydrothermal treatment were analyzed. The valuations of photocatalytic activities of thin films were carried out by degradation of methyl orange in water solution under UV irradiation. The results showed that the hybrid films prepared at low temperature with steam-hydrothermal treatment had high reactivity for degradation of methyl orange and the addition of PSR could significantly increase the photocatalytic reactivity.