In the present study, twenty seven [(Fe–35wt%Mn)100−x–Cux] alloy samples were processed using high-energy ball milling, followed by uniaxial compaction under different processing conditions. The compressibility behavior in terms of relative density (RD) was examined with milling time (MT: 1 h, 5.5 h, and 10 h), ball-to-powder mass ratio (BPMR: 5:1, 10:1, and 15:1), milling speed (MS: 100 rev/min, 200 rev/min, and 300 rev/min), compaction pressure (CP: 25–1,100 MPa), and alloy composition (Cu content [CC]: 0 wt%, 5 wt%, 10 wt%). Particle size analysis using X-ray diffraction (XRD) and high-resolution scanning electron microscopy (HRSEM) combined with energy-dispersive X-ray spectroscopy (EDS) were applied for microstructural characterization. The experiments were conducted based on the central composite design of response surface methodology (RSM), and the results for the compaction behavior were examined with the input parameters. Analysis of variance (ANOVA) test was applied to determine the most significant input parameters. The attained results revealed that increasing ball milling parameters (MT, MS, and BPMR) resulted in significant enhancements in the microstructural features, such as improved elemental dispersion and occurrence of refined particles with substantial decrease in the crystallite size. On the other hand, increasing the input parameters exhibited a detrimental influence on the compactibility and RD of the alloys. In addition, increasing the CC resulted in a substantial improvement in the compressibility and RD of the developed alloys. The recommended combination of the studied variables includes MT for 5 h, MS for 150 rev/min, BPMR of 10:1, and 10 wt%Cu to attain an acceptable compromise of enhanced microstructure features, improved compaction response, and RD.
