Die-sink electric discharge machining (EDM) is essential for shaping complex geometries in hard-to-machine materials. This study aimed to optimize key input parameters, such as the discharge current, gap voltage, pulse-on time, and pulse-off time, to enhance the EDM performance by maximizing the material removal rate while minimizing the surface roughness, residual stress, microhardness, and recast layer thickness. AISI 316L stainless steel was chosen due to its industrial relevance and machining challenges, while a Ti-6Al-4V-SiCp composite electrode was selected for its thermal resistance and low wear. Using Taguchi’s L27 orthogonal array, this study minimized the trial numbers, with analysis of the variance-quantifying parameter contributions. The results showed a maximum material removal rate of 0.405 g/min and minimal values for the surface roughness (1.95 µm), residual stress (1063.74 MPa), microhardness (244.8 Hv), and recast layer thickness (0.47 µm). A second-order model, developed through a response surface methodology, and a feed-forward artificial neural network enhanced the prediction accuracy. Multi-response optimization using desirability function analysis yielded an optimal set of conditions: discharge current of 5.78 amperes, gap voltage of 90 volts, pulse-on time of 100 microseconds, and pulse-off time of 15 microseconds. This setup achieved a material removal rate of 0.13 g/min, with reduced surface roughness (2.46 µm), residual stress (1518.46 MPa), microhardness (259.01 Hv), and recast layer thickness (0.87 µm). Scanning electron microscopy further analyzed the surface morphology and recast layer characteristics, providing insights into the material behavior under EDM. These findings enhance the understanding and optimization of the EDM processes for challenging materials, offering valuable guidance for future research and industrial use.