Photocatalytic activities of TiO2 films were experimentally studied. TiO2 films with different crystal structures (amorphous, anatase, rutile) were prepared by a Low Pressure Metal Organic Chemical Vapor Deposition (LPMOCVD) at different reaction temperatures and also by a Sol-Gel method using TTIP (Titanium Tetra Iso-Propoxyde). The Effect of CVD preparation method, CVD reaction conditions, crystal structure and wave-length of UV light on the photocatalytic decomposition rate of methylene blue in aqueous solution were studied. First, the characteristics of CVD preparation of TiO2 films, such as the CVD film growth rate, crystal structure and morphology of the grown TiO2 films, were experimentally studied as a function of CVD reaction temperature. Secondly, photocatalytic activities of TiO2 films were evaluated by using two types of photo-reactors. The results indicated that TiO2 films prepared by CVD exhibit higher photocatalytic activity than a catalyst prepared by the Sol-Gel method. Among the CVD grown TiO2 films, anatase and rutile showed high photocatalytic activities. However, amorphous TiO2 films showed lower activities. The activity of the photocatalysts of anatase films was excellent under all types of UV-Iamps. The activity of CVD-prepared anatase films was four to seven times higher than that of photocatalyst films prepared by the Sol-Gel method.