Ni and NiO particles were made by a combustion synthesis process. The characteristics of synthesized powders were investigated with various kinds and amounts of fuels such as urea, citric acid and glycine. Ni phase particles without NiO phase were obtained through combustion synthesis process in air atmosphere with-out further calcinations process, when the content of glycine was 2.44 times of the stoichiometric ratio in the precursor solution. Primary particle sizes of synthesized Ni and NiO particles were about 20∼30 nm.