AlxCoCrCuFeNi high-entropy alloys were synthesised through mechanical alloying and spark plasma sintering. Different alloys were produced by varying the aluminium content (x = 0.5, 1.5, 2.5 and 4). The influences of the milling duration on the evolution of microstructure, constituent phases and morphology were studied. Increasing milling time resulted in grain refinement and higher solid solution homogenisation characterised by a high internal strain. As a consequence of aluminium addition, the microstructure of materials evolved from face centered cubic (FCC) and body centered cubic (BCC) phases to FCC, BCC and ordered BCC phases. Both mechanical alloying and SPS conditions as well as aluminium content led to grain refinement and variations of mechanical properties. In particular, hardness increased with increasing aluminium content. The aluminium percentage and the evolution of consequent phases are responsible for the microstructural stability at high temperatures. In addition, with Al content increase, the further synergy of strength and ductility along with a more pronounced strain hardening was obtained.
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