Several methods (impregnation, oxalate gel-coprecipitation and conventional aqueous coprecipitation) have been comparatively examined for the preparation of binary Cu/ZrO2 catalysts for the catalytic production of hydrogen by steam reforming of methanol (SRM). A variety of techniques including N-2 adsorption, XRD, N2O chemisorption, XRD, H-2-TPR, and XPS were used to characterize the physical and chemical properties of the as-obtained catalysts. The results show that the preparation method significantly affects the component dispersion, microstructural properties and the resulting catalytic performance with respect to methanol conversion, H-2 production and CO concentration. The catalyst with higher specific copper surface area and component dispersion shows higher activity for methanol conversion at lower temperature. The best Cu/ZrO2 catalyst has been prepared by an oxalate gel-coprecipitation method, which shows much higher catalytic activity and enhanced long-term stability in the SRM reaction as compared to the catalysts prepared by conventional aqueous-coprecipitation and impregnation methods. (c) 2005 Elsevier B.V. All rights reserved.