TiO 2 and TiO 2 /MoO 3 particulate films were successfully prepared using a Langmuir-Blodgett technique. The as-deposited films were characterized by X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and electron probe microanalysis (EPMA). The results indicate that the TiO 2 and TiO 2 /MoO 3 films are composed of separate layers of TiO 2 and MoO 3 particles. Furthermore, the photocatalytic activity of the films was evaluated from the decomposition of a stearic acid film under ultraviolet and visible light irradiation. It was found that photocatalytic activity is significantly enhanced by the layer structure of the TiO 2 /MoO 3 film, compared to the single layer TiO 2 film.