This work deals with Ni catalysts supported on both mono and binary oxide prepared by a conventional wet impregnation method. The catalytic properties of the material were investigated in oxy-steam reforming of methane (OSRM) process. The physicochemical properties of the catalysts were extensively studied using techniques such as Temperature Programmed Reduction (TPR-H2), Temperature Programmed Desorption of Ammonia (TPD-NH3), Brunauer Emmett Teller Method (BET), X-ray Diffraction studies (XRD), Thermal Analysis coupled with Mass Spectrometry (TG-DTA-MS), Time of Flight Secondary Ion Mass Spectrometer (ToF-SIMS), X-ray Photoelectron Spectroscopy (XPS) and Scanning Electron Microscope with EDX detector (SEM-EDX). The catalytic activity results showed that the Ni/CeO2∙La2O3 (2:1) catalyst exhibited superior activity and high selectivity towards hydrogen formation in the studied process due to the high content of Ni species present on the catalyst surface. The low activity of the Ni catalysts supported on La2O3 or binary oxide with high content of lanthanum oxide is related to the strong interaction of NiO with support.