Abstract Fe-ZrO 2 and Cu-ZrO 2 xerogels were prepared by a sol-gel method. The effect of the hydrolysis catalyst during the gelation step, namely H 2 SO 4 or NH 4 OH, on the properties of the resulting materials was investigated by XRD, BET, TGA/DTA, TPD of ammonia, FTIR, and TPR. Fe-ZrO 2 and Cu-ZrO 2 xerogels, with sulfuric acid introduced as the hydrolysis catalyst, mainly crystallyzed in the tetragonal phase and exhibited larger surface area and acid amount than those obtained with NH 4 OH. Ammonia TPD shows that