Single ZrO 2 and mixed CeO 2–ZrO 2 oxides with different CeO 2/ZrO 2 ratios were prepared by the sol–gel method and the CeO 2 by precipitation. The prepared support were impregnated with an aqueous solution of NiCl 2·6H 2O at an appropriate concentration to yield 3 wt.% of nickel respectively in the catalysts. Catalytic materials were characterized by BET (N 2 adsorption–desorption), SEM-EDS, XRD and TPR. The oxidative steam reforming of methanol (OSRM) reaction was investigated on these catalysts for H 2 production as a function of temperature. Depending of the CeO 2/ZrO 2 ratio; the catalysts composition has a significant influence on the surface area (BET), reduction properties and methanol conversion. XRD patterns of the Ni-base catalysts showed well defined diffraction peaks of the metallic Ni except on the Ni/CeO 2 catalyst, suggesting that on this sample all of the active phase was highly dispersed. Ni/Ceria-rich catalysts were vastly active for OSRM, giving a total CH 3OH conversion at 325 °C with GHSV = 0.3 × 10 5 h −1. They also showed close selectivity toward H 2, with high selectivity to CO 2 in all range of temperatures, this suggests that the reverse WGS reaction does not occur on these samples. It seems that the nickel is the phase mainly responsible of hydrogen production although the CeO 2/ZrO 2 support reduces the CO formation.