In the present work the synthesis of multicomponent nanocrystalline Al0.1- 0.5(Mn)CoCrFeNi HEA powder feedstocks by mechanical alloying (MA) through high energy ball milling to produce HEA coatings with cold spraying were studied. Pure (>99.5) elemental powders of Al (Mn), Co, Cr, Cu, Fe & Ni were mixed in predetermined ratios and mechanically alloyed under Ar gas in a Planetary Ball Mill. MA HEA powder feedstocks were characterized by optical microscopy, SEM+EDAX, XRD & XPS to determine powder particle size, shape & distribution, particle surface condition, chemical composition, crystal & phase structures & microstructures. MA-processed Al-HEA powder feedstocks exhibited tri-modal particle size distribution (PSD) while Mn-HEA had four distinct PSD modes. Fine size fraction of the MA- HEA powders contained A2/B2 (BCC) harder phases with lattice parameters of 2.8831 and .2.8690 Å, respectively and coarse size fraction contained (ductile) softer A1 phase/Cu-rich regions combined (FCC) having a lattice parameter of 3.6181 Å. The ratio of the phases varied depending on the Al and Mn contents in the powder. For higher aluminium contents, there was more disordered A2/B2 phases and less disordered A1 phase in Al0.1–0.5 HEA powder feedstocks. A1 phase contained Fe, Cr, Co and Ni; A2 phase contained Fe, Cr; and B2 phase contained Al, Ni elements in Al0.1–0.5 HEA powder feedstocks. There were passive surface oxide films on the rough surfaces of MA HEA powder feedstocks consisting of a main mixture of surface oxides such as Al2O3, MnO, Cr2O3, Mn2O3, and minor oxides such as CuO, Fe2O3, NiO, Fe3O4, and a few CoCr2O4 spinel oxide. Dual FCC-dual BCC phase prediction of thermodynamic stable phase formation criteria reported in the literature on MA-HEA powder feedstocks were consistent with the experimental results of the present study.
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