NiO nanoparticles were fabricated by sol-gel route using ammonium hydroxide and nickel nitrate as precursors. The NiO nanoparticles were calcinated at 400 °C and 1000 °C. The nanoparticles were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), vibrating sample magnetometer (VSM), thermogravimetry analysis/differential thermal analysis (TGA/DTA). The structural properties were evaluated by X-ray diffraction (XRD). XRD confirmed the formation of well-crystallized and high purity NiO phase. The XRD showed that the peaks were sharpened and the crystallite size increased as the calcination temperature increased. The average crystallite size ranged from 12 nm to 20 nm, when calcined at temperatures 400 °C and 1000 °C, respectively. Fourier transform infrared spectroscopy (FT-IR) revealed the chemical composition and confirmed the formation of NiO nanoparticles. The nanoparticles showed paramagnetic behavior.