The aim of this work was to prepare self-assembled films (SAF) via a layer-by-layer technique and to characterize the films by applying several instrumental techniques. The cationic system was composed of the organic polyelectrolyte poly(diallyldimethylammonium chloride) and the inorganic semiconductor cadmium selenide (CdSe), whereas the anionic system was composed of poly(acrylic acid) and nanoparticles of the photoactive semiconductor titanium dioxide (TiO2). Through measurements of the diffuse reflectance spectrum, absorption bands were observed in the near ultraviolet region for TiO2 and in the visible region for CdSe. The thicknesses of the SAF were determined through profilometry and scanning electron microscopy techniques, and the obtained values were on the order of microns. Finally, the SAF were irradiated with a Xe/Hg lamp, and the results indicated their potential for solar hydrogen production. (C) 2013 Elsevier B.V. All rights reserved.