Nickel Oxide (NiO) is an important transition metal oxide with cubic lattice structure. NiO is thermally stable that is suitable for tremendous applications in the field of optic, ceramic,glass, electro-chromic coatings, plastics, textiles, nanowires, nanofibers, electronics,energy technology, bio-medicine, magnetism and so on. In this present study, NiO nanoparticles were successfully synthesized by sol-gel technique. Nano-sols were prepared by dissolving Nickel-Chloride [NiCl2.6H2O] in NaOH solvent and were converted into nano structured gel on precipitation. A systematic change in preparation parameters like calcination temperature, time, pH value has been noticed in order to predict the influence on crystallite size. Then the prepared samples were characterized by the X-ray Diffraction Spectroscopic (XRD), UV-VIS Spectroscopy, Fourier Transform Infra-Red Spectroscopy (FTIR), Energy Dispersive X-ray Spectroscopy (EDX), Scanning Electron Microscopy (SEM) and Particle Size Analyzer (PSA). From XRD, the average crystalline-size has been calculated by Debye-Scherrer Equation and it was found to be 12.17 nm and the band gap energy of Nickel oxide (NiO) from UV studies reveals around 3.85 eV. Further, EDX and FTIR studies, confirm the presences of NiO nanoparticles. The SEM study exhibits the spherical like morphology of Nickel oxide (NiO). Further from PSA, the mean value of NiO nanoparticles has been determined.