Ni promoted MoO2 nanoparticles were synthesized by combining spray pyrolysis and solvothermal cracking process. First, polycrystalline MoO3 microparticles were prepared by spray pyrolysis at 600 oC. Then nano-sized Ni- MoO2 particles were formed by solvothermal cracking process after adding Ni precursor, which disassembled polycrystalline MoO3 microparticles into crystalline grains by thermal expansion and shattered them into Ni-MoO2 nanoparticles by the subsequent solvothermal polyol reduction process. TPR profiles of Ni-MoO2 nanoparticles presented the decrease of reducibility of MoO2 with addition of Ni promoter. Catalytic partial oxidation of n-dodecane was conducted at various temperatures from 450 °C to 850 °C using Ni-MoO2 nanoparticles and pure MoO2 nanoparticles. H2 yield of all the Ni-MoO2 nanoparticles was higher than that of pure MoO2 nanoparticles at 850 °C. Specially, 7 and 10mol% Ni-MoO2 nanoparticles showed desirable catalytic performance of ca. 60% of H2 yield. This is mainly attributed to the existence of polymolybdate with addition of Ni and Ni2+ species partly located in the polymolybdate layer without formation of bulk Ni phase.