Ce-containing MCM-41 mesoporous materials with large surface area and ordered pore structure system have been possible to be synthesized through a surfactant-assisted approach. The textural properties and structural regularity of the materials varied with the Si/Ce molar ratio. It is found that the band at 970 cm-1 in the FTIR spectrum of the Ce-MCM-41 mesoporous materials might be used as an indicator of the formation of the Ce-O-Si bond and its intensity as a measure of a degree of cerium ion substitution in the framework of Si-MCM-41. When Ni was loaded on the Ce-MCM-41 support, the Ni/Ce-MCM-41 catalysts show high catalytic activity which has strong temperature dependence. The methane conversion over these catalysts reached 60-75 % with a 100 % selectivity towards hydrogen.