The growing demand for sustainable and efficient energy storage technologies has stimulated extensive research on advanced electrode materials for capacitor and supercapacitor applications. In this work, polyaniline/graphene oxide (PANI/GO) nanocomposites were successfully fabricated via a facile in situ polymerization approach to improve the electrochemical performance of capacitor electrodes. The influences of polymerization reaction time and aniline (ANI) monomer content on the structural, morphological, and electrochemical characteristics of the synthesized nanocomposites were systematically examined. The prepared PANI/GO nanocomposites were deposited onto fluorine-doped tin oxide (FTO) conductive glass substrates and dried prior to characterization. The morphology, structural features, and chemical composition of the samples were investigated using Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). Electrochemical performance was evaluated by cyclic voltammetry (CV). The results demonstrated that the sample synthesized with a reaction time of 1 h and aniline monomer content of 1 mL exhibited the highest specific capacitance of 20.08 F g⁻¹. The improved electrochemical performance was mainly attributed to the synergistic interaction between PANI and GO, where GO provided a large specific surface area and abundant active sites for PANI deposition, thereby enhancing charge transfer and capacitive behavior. These findings suggest that PANI/GO nanocomposites possess considerable potential as promising electrode materials for high-performance capacitor and energy storage applications.