Stoichiometric compositions of NiO were prepared by the standard chemical co-precipitation method to inspect the effect of the calcination temperature on structures, morphology, and physical properties. The samples were calcined at three different temperatures viz. 350 °C, 550 °C, and 650 °C for 5 h. X-ray diffraction analysis confirmed the cubic (Fm-3m) structure of the prepared samples. The average crystalline size increases from 41 nm to above 100 nm as the calcination temperature increases in the same time period. In Fourier transform infrared spectra, the spectral absorption bands were observed at ~413, 434, and 444 cm–1. The bandgap energy of NiO particles is decreased from 3.6 eV to 3.41 eV as the calcination temperature increases. The magnetic analysis confirms that the magnetization value of NiO is invariably decreased with a rise in the calcination temperature.