The effect of S doping on the physicochemical and photoelectrochemical properties of ZnO and Bi2O3 films has been studied. Two procedures were used for the synthesis of S-ZnO and S-Bi2O3 thin films on Ti mesh, obtaining lamellar shape nanocrystals for S-ZnO film. The presence of TiO2 anatase phase and wurtzite (ZnO and S-ZnO film) and TiO2 anatase and a mixture of α,β-Bi2O3 (Bi2O3 and S- Bi2O3) was observed. The inclusion of sulfur and nitrogen atoms as part of the lattice of the films was evidenced by XPS analysis. The photoelectrochemical performance of the composite films was obtained, with photocurrent densities of 350 µA cm-2 (1-S-ZnO) and 330 µA cm-2 (Bi2O3).