The FeCoNiCrMo_0.5Al_x system with x up to 2.13 was analyzed from the point of view of evolution of the phase composition and microstructure. Cast samples were synthesized by induction melting and analyzed by X-ray diffraction, energy dispersive spectroscopy, scanning electron microscopy, and Vickers microhardness test methods. Phase compositions of these alloys in dependance on Al concentration consist of FCC solid solution, σ-phase, NiAl-based B2 phase, and BCC solid solution enriched with Mo and Cr. Phase formation principles were studied. Al dissolves in a FeCoNiCrMo_0.5 FCC solid solution up to 8 at.%.; at higher concentrations, Al attracts Ni, removing it from FCC solid solution and forming the B2 phase. Despite Al not participating in σ-phase formation, an increase in Al concentration to about 20 at.% leads to a growth in the σ-phase fraction. The increase in the σ-phase was caused by an increase in the amount of B2 because the solubility of σ-forming Mo and Cr in B2 was less than that in the FCC solution. A further increase in Al concentration led to an excess of Mo and Cr in the solution, which formed a disordered BCC solid solution. The hardness of the alloys attained the maximum of 630 HV at 22 and 32 at.% Al.

In the present study, powder of FeCoCrNiMo_0.5Al_1.3 HEA was manufactured by gas atomization process, and then used for laser powder bed fusion (L-PBF) and microplasma spraying (MPS) technologies. The processes of phase composition and microstructure transformation during above mentioned processes and subsequent heat treatment were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and differential thermal analysis (DTA) methods. It was found that gas atomization leads to a formation of dendrites of body centered cubic (BCC) supersaturated solid solution with insignificant Mo-rich segregations on the peripheries of the dendrites. Annealing leads to an increase of element segregations till to decomposition of the BCC solid solution and formation of σ-phase and B2 phase. Microstructure and phase composition of L-PBF sample are very similar to those of the powder. The MPS coating has a little fraction of face centered cubic (FCC) phase because of Al oxidation during spraying and formation of regions depleted in Al, in which FCC structure becomes more stable. Maximum hardness (950 HV) is achieved in the powder and L-PBF samples after annealing at 600 °C. Elastic modulus of the L-PBF sample, determined by nanoindentation, is 165 GPa, that is 12% lower than that of the cast alloy (186 GPa).

One of the most promising applications of FeNiCoCrMoAl-based high-entropy alloy is the fabrication of protective coatings. In this work, gas-atomized powder of FeNiCoCrMo_0.5Al_1.3 composition was deposited via high-velocity oxygen fuel spraying. It was shown that in-flight oxidation of the powder influences the coating’s phase composition and properties. Powder oxidation and phase transformations were studied under HVOF deposition, and during continuous heating and prolonged isothermal annealing at 800 °C. Optical and scanning electron microscopy observation, energy dispersive X-ray analysis, X-ray diffraction analysis, thermogravimetric analysis, differential thermal analysis, and microhardness tests were used for study. In a gas-atomized state, the powder consisted of BCC supersaturated solid solution. The high rate of heating and cooling and high oxygen concentration during spraying led to oxidation development prior to decomposition of the supersaturated solid solution. Depleted Al layers of BCC transferred to the FCC phase. An increase in the spraying distance resulted in an increase in α-Al₂O₃ content; however, higher oxide content does not result in a higher microhardness. In contrast, under annealing, the supersaturated BCC solid solution decomposition occurs earlier than pronounced oxidation, which leads to considerable strengthening to 910 HV.

In this work, the effect of high-entropy alloy powder preparation on the coatings deposited via high-velocity oxygen fuel sprayings was studied. The powders of FeNiCoCrMo_0.5Al_1.3 composition were prepared by milling and gas atomization. The structures, porosity, phase composition, and microhardness of the coatings produced from mechanically alloyed and gas-atomized powders were compared. The influence of milling parameters on the powder phase composition and morphology was studied. Milling at 600 rpm for 1.5 h allowed the production of mechanically alloyed powder with a homogeneous distribution of Fe, Ni, and Al and thin lamellas enriched with Co, Cr, and Mo. Despite the difference in the feedstock powders’ phase compositions, the phase compositions of the coatings deposited from mechanically alloyed and gas-atomized powders are the same consisting of BCC, FCC solutions, and oxide. The amount of FCC solutions and oxide in the coating depends on the size distribution of the sprayed powder. It was found that the phase composition and the properties of the coatings deposited from the mechanically alloyed and gas-atomized powders of similar sizes are similar.