In the present work we report the preparation of nanocrystalline alloys, of composition Fe73.5Nb3Cu1Si13.5B9, formed directly by mechanical alloying of the constituents. Powders of the pure elements, in the appropriate proportions, were mixed in a Reitch planetary ball mill for upto 120 hours. The composition and the amount of the crystalline phases evolve during the milling and have been followed by Mossbauer Spectroscopy. A metastable FeSi solid solution is-formed with up to 18% Si content. This phase contains about 50% of the Fe present in the sample. At the same time other Fe disordered alloys-are produced. These are characterised by an inhomogeneous distribution of hyperfine fields.
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