A series of NiCeOx mixed metal oxide catalysts with various Ce/(Ce + Ni) ratios were prepared using hydrothermal methods The NiCeOx catalyst with a 4% Ce/(Ni + Ce) molar ratio (NiCeOx-4) demonstrated excellent catalytic performance for propane oxidation. Furthermore, the preparation method strongly affected the morphology and surface structure of the NiCeOx-4 catalyst as well as its catalytic activity for propane oxidation. The NiCeOx-4 catalyst that was prepared with the hydrothermal method exhibited a better catalytic performance compared with catalysts that were prepared by the co-precipitation method, sol-gel method and physical mixing of pure NiO and CeO2 powders. The results demonstrated that Ni-containing CeO2 (NiCeOx) nanoparticles were located on the surface of the NiCeOx-4 catalyst that was prepared using the hydrothermal method. As a result, the NiCeOx-4 catalyst had strong reducibility, a large number of active oxygen species, and strong ability to break the C-H bond of propane, which led to higher catalytic activity for propane combustion.