Nickel oxide (NiO) nanoparticles of nominal size range 16 nm and 25 nm were obtained by controlling the calcination temperature. These particles were prepared by the precipitation method. Structural, optical and morphological characterizations were done by X-ray powder diffraction, UV–vis diffuse reflectance spectroscopy and scanning electron microscopy. Studies of magnetic measurements (up to 60 kOe) and temperature variations from 2 K to 300 K of the NiO nanoparticles were investigated. Particles of 16 nm exhibited a weak ferromagnetic component and hysteresis loop. There is a increase in coercivity H c and the remanence M r at 8 K accompanied by an exchange bias H E. H E monotonically tends to zero as the particles size varied from 16 nm to 25 nm. The hysteresis loop and the size dependent χ are interpreted with the uncompensated surface spins, whereas the transition at 30 K is suggested to be Néel temperature T N of the spins in the core of the 16 nm particles. In addition, the increasing temperature cannot showed an approach to saturation in the magnetization curve, it indicates the possibility of an asperomagnetism and/or spin glass behavior of the NiO nanoparticles.