The present study used ultra-sonication approach to manufacture ZnO/NiFe2O4 (ZNF) and casting technique to prepare ZnO/NiFe2O4-Cs/PVP nanocomposite films. The successful creation of these nanocomposites with a significant decrease in the % crystallinity of the polymer blend with doping agent was verified by XRD results. ZNF and the Cs/PVP chains interacted in the polymer nanocomposites, as seen by the spectra of the FTIR. To determine the direct and indirect optical band gaps, tauc graphs were studied using data from UV-Vis analysis. The results indicate that while the Urbach energy was found to increase, the optical band gaps decreased as the weight percentage of the nanofiller increased. Using a thermogravimetric approach, the thermal stability of the produced PNCs has been investigated. Conductivity experiments demonstrated that when the nanofiller ZNF content increased to 2.5 wt%, so did AC conductivity, the dielectric loss, and the dielectric constant. The correlation between the mechanism of conduction and the amount of nanoparticles indicates that an increase in the percentage of ZNF in nanocomposites could increase their conductivity, with values ranging from 3.72 x 10-12 for pure blend to 7.72 x 10-8 S/cm for 2.5%ZNF-Cs/PVP at 100 Hz. The dielectric measurements for the nanocomposite films showed an increase in dielectric losses and dielectric constant, which is indicative of the films' enhanced dielectric polarization. The results of characterization point to possible uses of these polymer nanocomposites in flexible optoelectronic and magneto-electronic applications and energy storage devices.