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Fully dense bulk nanocomposites have been obtained by a novel two-step severe plastic deformation process in the immiscible Fe–Cu system. Elemental micrometer-sized Cu and Fe powders were first mixed in different compositions and subsequently high-pressure-torsion-consolidated and deformed in a two-step deformation process. Scanning electron microscopy, X-ray diffraction and atom probe investigations were performed to study the evolving far-from-equilibrium nanostructures which were observed at all compositions. For lower and higher Cu contents complete solid solutions of Cu in Fe and Fe in Cu, respectively, are obtained. In the near 50% regime a solid solution face-centred cubic and solid solution body-centred cubic nanograined composite has been formed. After an annealing treatment, these solid solutions decompose and form two-phase nanostructured Fe–Cu composites with a high hardness and an enhanced thermal stability. The grain size of the composites retained nanocrystalline up to high annealing temperatures.

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