Thin film bilayers of TiO2/CuO with intentionally varied thickness of the top layer of TiO2(25–150 nm) were grown by means of sequential rf magnetron reactive sputtering from Cu and Ti metallic targets in a flow rate-controlled Ar + O2 gas mixture. XRD diffraction in GID configuration, SEM top and cross-sectional images, EDS combined with SEM, XRR profiles, UV–VIS-NIR spectrophotometry and synchrotron soft radiation XAS in TEY mode were used to characterize crystal structure, morphology, the mode of growth, chemical composition, density and roughness as well as the optical and electronic properties of the synthesized thin film bilayers. CuO bottom layer turned out to crystallize in a monoclinic structure while TiO2 top layer remained amorphous. Film roughness of CuO decreased from about 12 nm with the increasing thickness of TiO2 thin film to about 1–2 nm. X-ray absorption spectroscopy demonstrated a presence of Cu+ and Cu2+ in TiO2 top layer of TiO2/CuO heterostructure. The photoelectrochemical measurements revealed that thin film bilayers of TiO2/CuO behaved as photocathodes in the process of water splitting. The photocurrent density was found to be an increasing function of the top TiO2 layer thickness.
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