The nano-NiO powder was prepared by sol-gel method combining heat treatment technology and its structure and morphology were explored. In addition, the NiO powder electrochemical properties were tested by constant current charging and discharging. The results show that the stable performance sol can be composed by nickel acetate as source of nickel and PAA as chelating agent. Nano-NiO powder of crystal structure integrity, particle uniformity can be prepared by the sol. The gel decomposes completely and gradually forms nanocrystal at 430οC. Its grain size is gradually increasing when the annealing temperature rise. The nano-NiO powder sintered at 600°C exhibits uniform particle, integrity crystal structure, low aggregation and superior electrochemistry performance and may be used in Li-ion battery as the anode material.