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A nanocrystalline face-centered cubic (fcc) solid solution of 6% Fe in Cu was prepared by high-energy ball milling, and annealed at temperatures from 200 to 360°C to induce chemical unmixing. The chemical state of the material was characterized by three-dimensional atom probe microscopy, Mössbauer spectrometry and X-ray powder diffractometry. The unmixing was heterogeneous, with iron atoms forming...
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