NiO nanoparticles with average particle size of 25 nm were successfully prepared by anodic arc plasma method. The composition, morphology, crystal microstructure, specific surface area, infrared spectra, and particle size distribution of product were analyzed by using X-ray diffraction (XRD), transmission electron microscopy (TEM) and the corresponding selected area electron diffraction (SAED), Fourier transform infrared (FTIR) spectrum, and Brunauer-Emmett-Teller (BET) N2 adsorption. The experiment results show that the NiO nanoparticles are bcc structure with spherical shape and well dispersed, the particle size distribution ranging from 15 to 45 nm with the average particle size is about 25 nm, and the specific surface area is 33 m2/g. The infrared absorption band of NiO nanoparticles shows blue shifts compared with that of bulk NiO.