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Polyvinyl Alcohol (PVA)/Polyvinylpyrrolidone (PVP) (50/50) blends consisting of various concentrations of (0%, 2%, 4%, 8%, 12%, 16%) Molybdenum trioxide nanoparticles (MoO3) have been prepared by solvent casting technique. The structural studies were carried out using FTIR and XRD. The optical properties were studied using UV Visible and fluorescence spectroscopy. The energy gap of the films found decreasing with the increase in doping concentration.. The maximum Young's modulus of 1477.73 MPa is observed for the blend with 12 wt% MoO3. The AFM analysis indicates that the surface roughness of the films increases upon doping with MoO3 nanoparticles. The dc conductivity is increased from 7.19 × 10−8 S/cm for the pureblend to 5.49 × 10−7 S/cm for PVA/PVP blend with 12 wt%MoO3 nanofiller. The thermal stability of the films found increased upon doping. The prepared films were explored for supercapacitor applications as separator. [ABSTRACT FROM AUTHOR]