In the present study, NiO and Cu-doped NiO nanoparticles were successfully synthesized by wet chemical method at room temperature using sodium hydroxide (NaOH) as precipitating agent. The as-prepared Cu-doped NiO powder samples were subjected to three different calcination temperatures such as, 350 °C, 450 °C and 550 °C in order to investigate the impact of calcined temperatures on the phase formation, particle size and band gap evolution. The phase formation and crystal structure information of the prepared nanomaterials were examined by X-ray powder diffraction (XRD). XRD revealed the face-centered cubic (FCC) structure. Average crystalline size of pure and doped samples estimated using Scherer formula was found to be 15 nm and 9 nm respectively. With increase in the calcination temperature from 350 °C to 550 °C for the Cu doped NiO samples the particle size of the nanoparticles was found to increase from 4 nm to 9 nm respectively. The optical study for both pure and doped NiO nanoparticles was performed using an UV–Vis spectrophotometer in the wavelength range of 200–800 nm. The strong absorption in the UV region confirms the band gap absorption in NiO and was estimated from the UV–Vis diffuse reflectance spectra via Tauc plot. Systematic studies were also carried out to study the effect of calcination on the optical transmittance. Samples were also investigated using Raman and Fourier Transform Infrared Spectroscopy (FTIR). Furthermore, morphology of the pure NiO and Cu-doped NiO Nanoparticles were examined by scanning electron microscope (SEM).