This study was conducted to investigate the characteristics of the AlCrCuFeNi high-entropy alloy (HEA) synthesized through mechanical alloying (MA). In addition, effects of Process Control Agent (PCA) amount and milling time were investigated using X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). The results indicated that the synthesized AlCrCuFeNi alloy is a dual phase (FCC + BCC) HEA and the formation of the phases is strongly affected by the PCA amount. A high amount of PCA postponed the alloying process and prevented solid solution formation. Furthermore, with an increase in the PCA amount, lattice strain decreased, crystallite size increased, and the morphology of the mechanically alloyed particles changed from spherical to a plate-like shape. Additionally, investigation of thermal properties and annealing behavior at different temperatures revealed no phase transformation up to 400 °C; however, the amount of the phases changed. By increasing the temperature to 600 °C, a sigma phase (σ) and a B2-ordered solid solution formed; moreover, at 800 °C, the FCC phase decomposed into two different FCC phases.

Plasma electrolytic oxidation (PEO) coatings were grown on AZ31 Mg alloy in a silicate-based electrolyte containing KF using unipolar and bipolar (usual and soft-sparking) waveforms. The coatings were dual-layered consisting of MgO, MgF₂ and Mg₂SiO₄ phases. Surface morphology of the coatings was a net-like (scaffold) containing a micro-pores network, micro-cracks and granules of oxide compounds. Deep pores were observed in the coating produced by unipolar and usual bipolar waveforms. The soft-sparking eliminated the deep pores and produced the lowest porosity in the coatings. It was found that the corrosion performance of the coatings evaluated using EIS in 3.5 wt. % NaCl solution is mostly determined by the inner layer resistance, because of its higher compactness. After 4 days of immersion, the inner layer resistances were almost the same for all coatings. However, the coatings produced by unipolar and usual bipolar waveforms showed sharp decays in inner layer resistances after 1 week and even the barrier effect of outer layer was lost for the unipolar-produced coating after 3 weeks. The low-frequency inductive loops appeared after a 3-week immersion for all coatings indicated that the substrate was under local corrosion attack. However, both coatings produced by soft-sparking waveforms provided the highest corrosion performance.