The LM24–7.5ZrB2–2.5FA hybrid composite presents machining difficulties as it has excellent durability and low-temperature conductivity, making it challenging to machine using standard methods. In spite of this aspect, Electrical Discharge Machining (EDM) is well-suited for machined materials made of aluminum alloys, including LM24–7.5ZrB2–2.5FA. LM24 aluminum alloy-based hybrid composite prepared using 7.5wt% of zirconium diboride (ZrB2) and 2.5wt% of Fly Ash (FA) by stir casting route. This study explores the machinability of the hybrid composite and the primary goal is to establish a connection between the process variable’s key efficiency indicators, which include Material Removal Rate (MRR), Surface Roughness (SR), and Tool Wear Rate (TWR), which collectively reflect dimensional accuracy and machining efficiency. The experimentation involves three adjustable process parameters, namely pulse current (I), pulse-on time (TonTon), and pulse-off time (ToffToff). These variables are subjected to variation, and a total of 20 experimental runs are set up utilizing the Response Surface Methodology (RSM) and a full-factorial Central Composite Design (CCD). Analysis of Variance (ANOVA) is employed to determine which operating variables substantially influence performance characteristics. The analysis reveals that current has a strong influence on MRR, SR, and TWR by 49.5%, 37.7%, and 36.1%, respectively, followed by pulse-on time and pulse-off time. The developed quadratic regression models for MRR, SR, and TWR demonstrated good performance in predicting the responses, as evidenced by the R2R2 values of 0.9030, 0.9890, and 0.9302 obtained from ANOVA results.