CuO-SiO2 catalysts were prepared by the sol-gel technique and calcined at two temperatures, 673 and 1073 K, Characterization of the catalysts was achieved by BET, FTIR, TPR, dissociative N2O adsorption, XPS, HRTEM, and reactivity toward NO + H-2. As a function of the calcination temperature, characterization techniques showed: textural (BET), morphological and structural (HRTEM), reducibility (TPR, XPS), dispersion, and catalytic reactivity (NO + H-2) differences between samples. Both samples showed remarkable stability during on-stream experiments. The microstructure of the catalysts as a consequence of the preparation method allows the understanding of the catalytic behavior of calcined and reduced samples as well as the stability toward sintering, (C) 1999 Academic Press.