NiO nanoparticles have been prepared by a simple and efficient chemical precipitation method with the aid of a surfactant. In this method, NiO2 (nickel peroxide) was first prepared by oxidation of nickel (II) nitrate with hypochlorite solution. The as-prepared NiO2 was then easily converted to nanosized NiO merely by treating it with ethanol at room temperature. The fabricated NiO nanoparticles were characterized by XRD, TEM, and EDX techniques. The effect of three different surfactants viz., SLES, CTAB and Triton X-100 on the formation of NiO nanoparticles was also studied.