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This study proposing an environmentally friendly and lead (Pb)-free alternative in the form of electrospun mats of Bi2O3/WO3/PVA for X-ray shielding. By varying Bi2O3 filler loading (0–20 wt%) while keeping WO3 filler constant at 10 wt%, the study examined density, thickness, and mass attenuation coefficient (µ) of the fabricated mats. X-ray attenuation was evaluated across different X-ray energy levels (16.61–25.27 keV) using X-ray fluorescence (XRF) unit. Meanwhile, the surface morphology and nanoparticle dispersion within the PVA nanofiber mat were observed through Field Emission Scanning Electron Microscope (FESEM). Results demonstrated improved X-ray attenuation with increased Bi2O3 filler loadings, except for mats containing 20 wt% Bi2O3 and 10 wt% WO3 (mat B5) due to coagulation and porosity issues. The electrospun mat with 15 wt% Bi2O3 and 10 wt% WO3 (mat B4) exhibited the highest X-ray attenuation. Thus, electrospun mat B4 is proposed as a promising candidate for environmentally friendly X-ray shielding material. [ABSTRACT FROM AUTHOR]