The technology of p-type transparent semiconductors is utilized in various fields, and enhancing their performance holds industrial significance. Thus, improving the versatility and efficiency of the p-type transparent conducting oxides (TCO) has become critical for the semiconductor industries and technologies. To be used as hole carrier layes in optoelectronic devices, this study aimed to modify the physical features of nickel oxide (NiO) through a doping approach which may broaden and strengthen the usage of NiO. A cost-effective ultrasonic pyrolysis spray technique was employed for pure and lead (Pb) doped nickel oxide thin film production. The influence of the lead concentration on optical, structural, and morphological traits of the NiO nanostructures was examined via various analyses, including energy-dispersive X-ray spectroscopy (EDAX), scanning electron microscopy (SEM), Photoluminescence, UV–visible spectroscopy, X-Ray Diffraction, and Raman spectroscopy, were utilized to investigate the optical and structural characteristics of these films. In correlation, the X-Ray Diffraction results indicated that the Pb doping induced strain and altered lattice parameters of the grown nanostructures while the cubic phase of NiO maintained. The crystallite size of NiO samples ranged from 31.49 nm to 18.75 nm based on Pb doping concentration which was notably influenced by species and doping content. The UV–vis measurements demonstrated that optical parameters, such as optical band gap, were sensitive to Pb doping ratios. The Raman spectrum analysis confirmed the successful incorporation of Pb ions into NiO. Additionally, the intensity of the PL spectra decreased with increasing Pb content, offering potential applications as window layers in solar cells, smart windows, and other optoelectronic devices.