aCrystalline cobalt oxides were prepared by a precipitation method using three different precipitation agents, IJNH 4 ) 2 CO 3 , Na 2 CO 3 and COIJNH 2 ) 2 . Cobalt oxide nanoparticles corresponding to a Co 3 O 4 loading of 30 wt% were also deposited over high-surface area nanocrystalline ceria by the same precipitation agents. The effect of calcination temperature, 350 or 650°C, on the morphological and structural properties was evaluated. Characterization by BET, XRD, SEM, TEM, Raman spectroscopy, H 2 -TPR, XPS and NH 3 -TPD was performed and the catalytic properties were explored in the methane oxidation reaction. The nature of the precipitation agent strongly influenced the textural properties of Co 3 O 4 and the Co 3 O 4 -CeO 2 interface. The best control of the particle size was achieved by using COIJNH 2 ) 2 that produced small and regular crystallites of Co 3 O 4 homogeneously deposited over the CeO 2 surface. Such a Co 3 O 4 -CeO 2 system precipitated by urea showed enhanced low-temperature reducibility and high surface Co 3+ concentration, which were identified as the key factors for promoting methane oxidation at low temperature. Moreover, the synergic effect of cobalt oxide and nanocrystalline ceria produced stable full conversion of methane in the entire range of investigated temperature, up to 700-800°C, at which Co 3 O 4 deactivation usually occurs.