The objective of this work was to perform a comprehensive analysis of the changes in the optical, structural, and nuclear radioactive attenuation properties of polyvinyl alcohol/lead oxide (PVA/PbO) films with different PbO contents (0.8, 1, 1.2, and 1.5 gm). The morphology of the prepared films was examined by scanning electron microscopy (SEM) and the results showed the homogeneous presence of PbO in the film image.  Infrared spectroscopy (FT-IR) study indicates a significant decrease in the polyvinyl alcohol (PVA) peaks by increasing PbO contents. The presence of PbO in the prepared films was also confirmed by energy-dispersive X-ray spectroscopy (EDX). Practical and theoretical techniques were used to accurately analyze the gamma-ray attenuation properties of the PVA series. Using Linear Attenuation Coefficient (LAC) values other relevant parameters such as MAC were calculated. From the results, we found that 1.5% g PbO, had a higher density (2.54 g/3cm), and higher LAC, MAC, and lower Half Value Layer ( HVL) values were observed. Moreover, the results of hardness experiments proved that the addition of PbO to a decrease in the flux.