Any industry that manufactures dies, punches, molds, and machine components from difficult-to-cut materials, such as Inconel, titanium, and other super alloys, largely relies on wire electrical discharge machining (WEDM). In the current study, the effect of the WEDM process parameters on Inconel 600 alloy with untreated zinc and cryogenically treated zinc electrodes was investigated. The controllable parameters included the current (IP), pulse-on time (Ton), and pulse-off time (Toff), whereas the wire diameter, workpiece diameter, dielectric fluid flow rate, wire feed rate, and cable tension were held constant throughout the experiments. The significance of these parameters on the material removal rate (MRR) and surface roughness (Ra) was established using the analysis of the variance. The experimental data acquired using the Taguchi analysis were used to analyze the level of influence of each process parameter on a particular performance characteristic. Their interactions with the pulse-off time were identified as the most influential process parameter on the MRR and Ra in both cases. Furthermore, a microstructural analysis was also performed via scanning electron microscopy (SEM) to examine the recast layer thickness, micropores, cracks, depth of metal, pitching of metal, and electrode droplets over the workpiece surface. In addition, energy-dispersive X-ray spectroscopy (EDS) was also carried out for the quantitative and semi-quantitative analyses of the work surface and electrodes after machining.