Zinc oxide and titanium dioxide composite thin films were prepared on Corning 7059 glass substrates by co-sputtering. The reactive gas-surroundings used was ultrahigh purity oxygen. To analyze the structural, optical and photocatalytic properties of the ZnO-TiO 2 samples, X-ray diffraction (XRD), atomic force microscopy (AFM), optical absorption, Raman spectroscopy and methylene blue bleaching were carried out at room temperature. XRD patterns indicate the presence of TiO 2 (anatase and rutile phases), ZnO, ZnTiO 3 , and Zn 2 TiO 4 crystalline structures. AFM images allow the observation of non-homogeneous surface in the ZnO-TiO 2 system, suggesting the separation of different crystalline phases in the composite. Raman studies exhibit different spectra in the films depending on the area analyzed, which can be interpreted as a result of the existence of well separated crystalline regions as seen in AFM images. The photocatalytic activity (PA) of TiO 2 -ZnO-ZnTiO 3 -Zn 2 TiO 4 composite, as expected for adequate coupling semiconductors, is larger than PA of ZnO and TiO 2 oxides, used as references. A simple proposal about the probable alignment of the conduction band, the valence band, and the Fermi level is included. E. García-Ramírez · M. Mondragón-Chaparro ESIME Azcapotzalco, Instituto Politécnico Nacional,