This work reports aspect related to chemical capping synthesis of nano-sized particles of nickel o xide. It is a simp le, novel and cost effective method. The average particle size, specific surface area, crystallin ity index are estimated fro m XRD analysis. The structural, functional groups and optical characters are analyzed with using of SEM, FTIR and UV-visib le techniques. XRD studies confirm the p resence of high degree of crystallin ity nature of nickel o xide nanoparticles. Their particle size is found to be 12 n m and specific surface area (SSA) is 74m2 g-1. The optical band gap energy value 3.83ev has also been determined fro m UV-Vis spectrum.