Influence of Mechanical Alloying on the Microstructure and Solid Solubility of Binary and Ternary Fe‐Based and Cu‐Based Nanostructured Alloys Powders

This research presents copper‐ and iron‐based binary and ternary systems synthesized using the mechanical alloying (MA) technique under various processing conditions, using a PM400 planetary mill. Structural and microstructural properties were investigated by X‐ray diffraction (XRD) and scanning electron microscopy (SEM), while differential thermal analysis (DTA) and Mössbauer spectroscopy were employed to assess phase evolution. The results reveal the formation of nanostructured phases and composite structures, with significant grain refinement (approximately 10–11 nm). Systematic variations observed in lattice parameters provide quantitative evidence of enhanced solid‐state solubility. In the Cu–Fe–Co system, iron and cobalt atoms substitute copper lattice sites, enhancing iron solubility, and DTA confirms the formation of a solid solution after prolonged milling, which agrees with XRD results. In Fe–Al and Fe–Al–Sn alloys, aluminum solubility increases significantly under non‐equilibrium conditions, producing a disordered bcc solid solution that evolves into the ordered B2 FeAl phase with iron contents above approximately 40 at.%. Mössbauer spectroscopy reveals a magnetic sextet, detected after 8 h of milling. Additionally, a growing paramagnetic FeAl(Sn) fraction is observed with continued milling, confirming solubility enhancement. Furthermore, results indicate that solid‐state solubility increases with milling time due to stress‐assisted atomic diffusion, eventually reaching saturation after prolonged milling.