Nanostructured cobalt materials have recently attracted considerable attention due to their potential applications in high-density data storage, magnetic separation and heterogeneous catalysts. The size as well as the morphology at the nano scale strongly influences the physical and chemical properties of cobalt nano materials. In this study, cobalt nano particles synthesized by a a polyol process, which is a liquid-phase reduction method, were investigated. Cobalt hydroxide (Co(OH)2), as an intermediate reaction product, was synthesized by the reaction between cobalt sulphate heptahydrate (CoSO4·7H2O) used as a precursor and sodium hydroxide (NaOH) dissolved in DI water. As-synthesized Co(OH)2 was washed and filtered several times with DI water, because intermediate reaction products had not only Co(OH)2 but also sodium sulphate (Na2SO4), as an impurity. Then the cobalt powder was synthesized by diethylene glycol (DEG), as a reduction agent, with various temperatures and times. Polyvinylpyrrolidone (PVP), as a capping agent, was also added to control agglomeration and dispersion of the cobalt nano particles. The optimized synthesis condition was achieved at 220oC for 4 hours with 0.6 of the PVP/Co(OH)2 molar ratio. Consequently, it was confirmed that the synthesized nano sized cobalt particles had a face centered cubic (fcc) structure and with a size range of 100-200 nm.