Highly supersaturated nanocrystalline FexCu100−xalloys (10≤x≤95) have been prepared by mechanical alloying of elemental crystalline powders. The development of the microstructure is investigated by x‐ray diffraction, differential scanning calorimetry, and transmission electron microscopy. The results are compared with data for ball‐milled elemental Fe and Cu powders, samples prepared by inert gas condensation, and sputtered films. The deformation during milling reduces the grain size of the alloys to 6–20 nm. The final grain size of the powders depends on the composition of the material. Single‐phase fcc alloys withx≤60 and single‐phase bcc alloys withx≥80 are formed even though the Fe‐Cu system exhibits vanishingly small solid solubilities under equilibrium conditions. For 60≤x≤80, fcc and bcc solid solutions coexist. The alloy formation is discussed with respect to the thermodynamic conditions of the material. The role of the large volume fraction of grain boundaries between the nanometer‐sized crystals, as well as the influence of internal strains and stored enthalpies introduced by ball milling, is critically assessed.
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