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The synthesis and characterization of PVA-chitosan-NiO, PVA-chitosan-TiO2, and PVA-chitosan-TiO2@NiO films have opened avenues for tailoring materials with specific electrical, dielectric, and optical properties. The synergistic effects arising from the combination of polymers and metal oxides offer a platform for further optimization and application-specific tuning. The synthesis process successfully incorporated NiO and TiO2 nanoparticles into the PVA-chitosan matrix, creating three distinct films: PVA-chitosan-NiO, PVA-chitosan-TiO2, and PVA-chitosan-TiO2@NiO. Structural analyses, including X-ray diffraction (XRD) and scanning electron microscopy (SEM), revealed well-defined nanostructures with crystalline metal oxide dispersions. Dielectric characterization demonstrated frequency-dependent behavior, elucidating the influence of metal oxides on dielectric constants and loss tangents. Cole–Cole plots provide insights into relaxation processes and can guide applications in capacitors and energy storage devices. Conductivity measurements highlight the enhanced electrical performance of NiO and TiO2. This study provides a foundation for future research on the development of advanced functional materials for a wide range of technological applications. The insights gained from this work contribute to the growing body of knowledge on polymer-metal oxide composites and pave the way for innovations in electronic, optoelectronic, and energy-related technologies.