The nano-CeO2/ZnO catalysts were prepared using a novel combination of homogeneous precipitation with micro-emulsion for oxidative coupling of methane with CO2 as an oxidant. The prepared catalysts were compared with those prepared using the conventional impregnation. The catalysts prepared in two ways were characterized with FTIR, TEM, XRD and CO2-TPD. The effects of the reaction temperature, the amount of ZnO doped in the catalysts and the average size were investigated. The experimental investigation demonstrated that methane conversion over the nano-CeO2/ZnO catalysts prepared by the combined technique was higher than that obtained over catalysts prepared by the conventional impregnation. A better low-temperature activity has also been achieved over the nanocatalysts. There was no clear trend between the average size of nano-CeO2/ZnO catalysts and their catalytic performance but methane conversion increased with increasing fractal dimension of nanocatalysts. (C) 2004 Elsevier B.V. All rights reserved.