This study presents the utilization of mill scale waste, which has attracted much attention due to its high content of magnetite (Fe3O4). This work focuses on the extraction of Fe3O4 from mill scale waste via magnetic separation, and ball milling was used to fabricate a microwave absorber. The extracted magnetic powder was ground-milled using two different techniques: (i) a conventional milling technique (CM) and (ii) mechanical alloying (MM) process. The Fe3O4/CM samples were prepared by a conventional milling process using steel pot ball milling, while the Fe3O4/MM samples were prepared using a high-energy ball milling (HEBM) method. The effect of milling time on the structural, phase composition, and electromagnetic properties were examined using X-ray diffraction (XRD) and a vector network analyzer (VNA). XRD confirmed the formation of magnetite after both the magnetic separation and milling processes. The results revealed that Fe3O4 exhibited excellent microwave absorption properties because of the synergistic characteristics of its dielectric and magnetic loss. The results showed that the Fe3O4/CM particle powder had a greater absorption power (reflection loss: