This paper systematically reports the thermodynamic characteristic and phase evolution of immiscible Cr–Mo binary alloy during mechanical alloying(MA) process. The Cr–35Mo(in at%) powder mixture was milled at 243 and258 K, respectively, for different time. For comparative study, Cr–15Mo and Cr–62Mo powder mixtures were milled at 243 K for 18 h. Solid solution Cr(Mo) with body-centered cubic(bcc) crystal structure and amorphous Cr(Mo) alloy was obtained during MA process caused by high-energy ball milling. Based on the Miedema's model, the free-energy change for forming either a solid solution or an amorphous in Cr–Mo alloy system is positive but small at a temperature range between 200 and 300 K. The thermodynamical barrier for forming alloy in Cr–Mo system can be overcome when MA occurs at 243 K, and the supersaturated solid solution crystal nuclei with bcc structure form continually, and three supersaturated solid solutions of Cr–62Mo, Cr–35Mo and Cr–15Mo formed. Milling the Cr–35Mo powder mixture at 258 K, the solid solution Cr(Mo) forms firstly, and then the solid solution Cr(Mo) transforms into the amorphous Cr(Mo)alloy with a few of nanocrystallines when milling is prolonged. At higher milling temperature, it is favorable for the formation of the amorphous phase, as indicated by the thermodynamical calculation for immiscible Cr–Mo alloy system.
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