Mechanical milling (MM) was performed on Cr72Fe28 alloy. X-ray diffraction and Mössbauer spectroscopy were used to follow the progress of the structural variation. The experimental results indicate that the milled powders are composed of two disordered components with random close-packed and random loose-packed structures, and a small amount of crystalline component. The crystallization of the material starts at a temperature of 800 K. © 1993.