Ti/Zn-TiO 2 electrodes were successfully prepared by the co-deposition method, on a titanium substrate, using an acidic zinc sulphate solution with TiO 2 nanoparticles in suspension. After electrodeposition, samples were heated in air at 450°C for 6 h. The X-ray diffraction analysis of the deposits point to the metal matrix modification from Zn to ZnO. In addition, the scanning electron microscopy results indicate that the films have a high surface area with a rich morphology, due to the appearance of ZnO needle-shaped grains. The voltammograms recorded, in Na 2 SO 4 solution, for these electrodes under illumination at λ0365 nm confirmed the films photoactivity. Photoelectrochemical degradation of Ibuprofen (Ibu) was achieved with the Zn-TiO 2 electrodes after thermal treatment. UV-Vis spectrometry, high-performance liquid chromatography (HPLC), chemical oxygen demand (COD) and total organic carbon (TOC) measurements were performed and data demonstrated that Ibuprofen was efficiently degraded. Absorbance at 220 nm, COD and TOC removals of 35%, 34% and 23%, respectively, were obtained after a 3 h period.