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The co-precipitation and in situ modified Hummers’ method was used to synthesize Nickel Spinal Ferrites (NiFe) nanoparticles and NiFe coated with Thermally Reduced Graphene Oxide (TRGO) (NiFe-TRGO) nanoparticles, respectively. By using polyvinyl chloride (PVC), tetrahydrofuran (THF), and NiFe-TRGO, the nanocomposite film was synthesized using the solution casting technique with a thickness of 0.12–0.13 mm. Improved electromagnetic interference shielding efficiency was obtained in the 0.1–20 GHz frequency range. The initial assessment was done through XRD for the confirmation of the successful fabrication of nanoparticles and DC conductivity. The microstructure was analyzed with scanning electron microscopy. The EMI shielding was observed by incorporating a filler amount varying from 5 wt.% to 40 wt.% in three different frequency regions: microwave region (0.1 to 20 GHz), near-infrared (NIR) (700–2500 nm), and ultraviolet (UV) (200–400 nm). A maximum attenuation of 65 dB was observed with a 40% concentration of NiFe-TRGO in nanocomposite film.