Influence of Process Control Agents, Mill Type, and Elemental Substitution on the Mechanosynthesis of Selected High-Entropy Alloys

High-entropy alloys (HEAs) are a transformative class of materials with remarkable structural and functional properties. Solid-state processing techniques, such as high-energy ball milling, are being increasingly used for their production. In these processes, the use of a process control agent (PCA) seems to be essential to prevent excessive cold welding and agglomeration; however, the influence of different PCAs on alloy formation remains insufficiently understood. This study systematically examined the effects of the PCA type, milling configuration, and elemental substitution on HEAs mechanosynthesis. A non-equiatomic alloy, Al10Cr12Fe35Mn23Ni20 (selected for its known single-phase Face Center Cubic (FCC) behavior), was used to explore the PCA and mill-type effects. The alloy was synthesized in a planetary mill (Fritsch Pulverisette 7) and a vibratory mill (SPEX 8000M) using diverse PCAs, including liquid (methanol, ethanol, isopropyl, and n-heptane) and solid (stearic acid and sodium chloride) agents. In addition, lightweight equiatomic alloys MgAlTiNi(Co,Cr,Fe) were used to explore the influence of different PCAs and the effect of elemental substitution under similar PCA conditions as those used with the equiatomic alloy. The products were characterized using X-ray diffraction, scanning electron microscopy, thermogravimetric analysis, and differential thermal analysis techniques. The results highlighted that the PCA selection, milling configuration, and alloy chemistry influenced the phase evolution, particle size distribution, and thermal behavior. The results provide insights into the mechanosynthesis of selected high-entropy alloys produced under different PCA and milling conditions.