The growing demand for efficient and sustainable energy storage systems has driven significant interest in the development of high-performance electrode materials for supercapacitors. In this study, polyaniline (P)/nickel ferrite (N) composites were synthesized to overcome the limitations of individual components and enhance electrochemical performance. While polyaniline offers excellent pseudocapacitive behaviour, its poor cyclic stability remains a challenge. Conversely, N, a spinel-type transition metal oxide, provides superior structural stability and redox activity. Nanocomposites were prepared by varying aniline: N ratios (1,0.05, 1,0.10, 1,0.15) via insitu polymerization. Structural and morphological characterizations using FTIR, and XRD confirmed the composite formation, while FESEM analysis revealed uniform distribution of N nanoparticles on branched P rods. Electrochemical measurements conducted in 1 M H₂SO₄ within a 0.0–0.8 V potential window demonstrated an impressive specific capacitance of 513 F/g at 1 A/g for PN0.10 and also obtained cyclic stability (600 cycles, at 4 A/g) with good capacitance retention (99%). This signifies the composite’s potential as a high-performance electrode material, paving the way for next-generation energy storage devices.