The preparation and characterization of different catalysts containing equal amounts of Ni (0.660 wt.%) and Rh (0.022 wt.%) and their catalytic performances and stability in CPO of methane in hard reaction conditions have been investigated. All the catalysts were obtained from hydrotalcite-type precursors (HT), prepared according to different methodologies: (a) impregnation of the active phase on a support derived from a HT precursor, (b) coprecipitation, inserting Ni and Rh inside the HT precursor, or (c) coprecipitation on a support (alpha-Al2O3) of a HT precursor containing the active metals. The different present phases as a function of the preparation method have been identified. The observed scale of activity in CPO of methane may be attributed to the dispersion of the metal particles and to the different surface area values of the catalysts. (c) 2006 Elsevier B.V. All rights reserved.