New superalloys are potential materials in aircraft and power plant industries because of their properties like high-temperature strength, creep life and resistance to corrosion and oxidation at elevated temperatures. Because of the superior properties of superalloys, machining them using the conventional processes is a difficult task that is associated with high cost and poor accuracy. In this study, an attempt has been made to machine NIMONIC 75 superalloy by the electro discharge machining (EDM) process, using the Taguchi-based Gray Relational Analysis method for multi-objective optimization of material removal rate (MRR), tool electrode wear rate (TEWR) and surface finish (SF). The experiments conducted were based on [Formula: see text] (2[Formula: see text]) orthogonal array. Six input parameters namely tool material, peak current, gap voltage, pulse on-time, pulse off-time and tool lift time were considered in this study. The validation results proved that the parametric setting of tool material as copper, peak current as 12[Formula: see text]A, gap voltage as 50[Formula: see text]V, pulse on-time as 200[Formula: see text][Formula: see text]s, pulse off-time as 15[Formula: see text][Formula: see text]s and tool lift time as 2[Formula: see text]s, yields optimized values of the performance characteristics. SEM images indicate the presence of numerous surface irregularities, whereas the XRD test shows the formation of various carbides on the EDMed surface.