This work aims to extend the application field of sol-gel process from conventional oxides, carbides, sulfides to metallic nanocrystalline materials. Metallic ions were coordinated with chelating agents of citric acid (CA) and ethylene diamine tetraacetic acid (EDTA) in aqueous solution. Then the solutions were dried at 383 K, resulting in the formation of sol and gel. Heating treatments of dried gels were then carried out with protection of N 2 atmosphere. Ni and Ni 3 Sn alloy nanoparticles were obtained by this sol-gel method in the range of 623-823 K. The as-prepared Ni and Ni 3 Sn alloy nanoparticles have average grain sizes of 15 and 30 nm, and have face-centred-cubic (fcc) crystalline phase. Our results provide new insight into the application of conventional sol-gel method.