This work demonstrates a new sol-gel approach for synthesizing PbO2-doped zirconia using zircon mineral precursors. The streamlined methodology enables straightforward fabrication of the doped zirconia composites. Comprehensive materials characterization was performed using XRD, SEM, and TEM techniques to analyze the crystal structure, microstructure, and morphology. Quantitative analysis of the XRD data provided insights into the nanoscale crystallite sizes achieved, along with their relationship to lattice imperfections. Furthermore, the gamma-ray shielding capacity for the PbO2-doped zirconia samples was estimated by the Monte Carlo simulation, which proves an increase in the gamma ray shielding properties by raising the Pb concentration. The linear attenuation coefficient increased between 0.467 and 0.499 cm−1 (at 0.662 MeV) by increasing the Pb content between 11 and 21 wt%. By increasing the Pb content to 21 wt%, the synthesized composites' lead equivalent thickness reaches 2.49 cm. The radiation shielding properties for the synthesized composites revealed a remarkable performance against low and intermediate γ-ray photons, with radiation shielding capacity of 37.3 % and 21.4 % at 0.662 MeV and 2.506 MeV, respectively. As a result, the developed composites can be employed as an alternative shielding material in hospitals and radioactive zones.