Increasing demand for aluminum matrix composites (AMCs) in the manufacturing sector leads to the development of squeeze casted hybrid AMCs bearing superior mechanical attributes. Excessive hardness due to squeeze pressure and the presence of reinforcement particles makes the machining of AMCs challenging and results in excessive tool wear and inadequate surface finish. Wire electric discharge machining (WEDM) process has been preferred over conventional manufacturing processes for the machining of squeeze casted Al2024/Al2O3/W hybrid composite. This study investigates the selection of the most pertinent wire electrode for the precise machining of Al2024/Al2O3/W. Simple zinc-coated (NT) and cryogenic treated (CT) brass wire electrodes have been selected for machining. Scanning electron microscope (SEM) analysis of CT wire shows that cryogenic treatment enhances the soundness and stability by reducing microcavities in its microstructure. To analyze the effects of cryogenic treatment, the machining performance of CT wire has been compared with NT wire. Besides wire type, the influence of key input variables has also been analyzed on the imperative response measures including cutting speed (CS), surface roughness (SR) and kerf width (KW) to make the machining process more effective. Microstructural analysis of NT wire depicts a high concentration of micro-voids, micro-cracks, and deep craters, while the surface of CT has been observed relatively fine after the machining. Comparative analysis of both wire electrodes has declared that CT wire yields 26.96% and 15.10% superior results for CS and SR respectively, and 6.92% deprived results for KW than NT wire.