<p>This study aims to evaluate the effect of reduced graphene (rG) oxide and titanium nitride (TiN) nanoparticle synthesis parameters on the electrochemical performance of polyaniline (PANI) nanocomposite as a supercapacitor electrode material. In the preparation of the PANI nanocomposites, 20&#xa0;wt.% rG and 10 wt.% TiN were used as reinforcements via solution mixing with the use of ultrasonication and subsequent heat treatment. The ultrasonication time, heat treatment temperature, and holding time were the synthesis parameters modified in this study to obtain the optimum fabrication parameters. The nanocomposite powders were examined using Fourier transform infrared spectroscopy, scanning electron microscopy, and x-ray diffraction. The thermal characteristics were measured using a thermal gravimetric analyzer. Using the Taguchi optimization method, the best processing parameters resulted in specific capacitance of approximately 346 F g⁻¹ at 0.5 A g⁻¹ and coulombic efficiency of 99.8% after 500 charge–discharge cycles. Thus, this study identified the optimal ultrasonication and heat treatment parameters for PANI/rG/TiN nanocomposites, providing a foundation for future research in advanced engineering materials for energy storage applications. Additionally, it establishes a standardized framework for ultrasonication and heat treatment processes, ensuring consistent and comparable results across studies on PANI/rG/TiN nanocomposites.</p>