Zirconia has received much attention as catalysts for its high surface area and acid-base property. The textural and acid-base properties of ZrO2 depend on both, the synthesis procedure and the calcinations temperature. The aim of the present study is the preparation and characterization of nickel/cupper/zirconia and cobalt/cupper/zirconia microspheres using hydrolysis process. This process is based on homogeneous hydrolysis of droplets of a concentrated ZrO2(NO3)2-urea solution after adding hexamethyletetramine. Gelation was conduced successfully and the gel spheres were dried at 80 °C. The dried gel spheres were thermally treated at 550 °C. Characterization of the samples was performed using X-ray diffraction (XRD), BET nitrogen adsorption, scanning electron microscopy (SEM), thermogravimetric (TGA) and UV-Vis spectroscopy. The performance of the microspheres was investigated as catalysts in steam reforming of ethanol. Theses catalysts exhibit a good selectivity for hydrogen.