Monocomponent, bicomponent and hybrid thin films containing metal oxides (SnO 2 , ZnO, CuO) and copper sulfide were obtained by spray pyrolysis deposition. The crystalline structure (X-ray diffraction), morphology (atomic force microscopy) and surface energy (contact angle) were correlated with the opto-electrical properties (transmittance, current density vs voltage, photocurrent, band energy diagrams). The samples show a predominant dispersive component of the surface energy and photosensitivity response under illumination. The photocatalytic activity was tested in methylene blue and methyl orange solutions and the highest value (around 45%) corresponds to the hybrid samples. Comparative adsorption studies in dark using similar dye solutions are presented.