In this paper, the possibility of production of Cu matrix nano-composite powder containing 10, 37 and 54 wt.% NiO using mechano-chemical reduction of different copper oxides (CuO and Cu2O) was studied. Structural evolutions were characterized by X-ray diffraction. Also, the microstructure was characterized by scanning electron microscopy and transmission electron microscopy. Particular attention has been paid to the reaction mechanism and kinetics using differential scanning calorimetry. It was found that the reactions completed gradually between 5 to 22h of milling. Formation of Cu2O and Cu(Ni) solid solution, as intermediate phases, were observed during the reaction. It was found that, the initial excess Cu delayed reduction reaction and decreased the final crystallite size up to 18nm. Microstructural results showed that relatively large nano-composite agglomerates powder composed of uniform dispersion of NiO nano-particles in nano-crystalline Cu matrix were obtained. Kinetic study revealed that CuO reduction to Cu through two-steps reaction with lower activation energies in each step had higher rate, compared to one-step reduction of Cu2O.