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Nanostructured Fe–12Co (wt%) powders were prepared by mechanical alloying in a planetary ball mill. The milling process was carried out at different milling conditions. The obtained powders were characterized by X‐ray diffraction, 57Fe Mössbauer spectrometry and magnetic measurements. The low and high speed ball‐milling conditions lead to the formation of a single and two‐bcc Fe(Co) structure, respectively, having different crystallite sizes, microstrains hyperfine parameters and magnetic properties. The average hyperfine magnetic field values: 〈B〉1 = 34.8 T and 〈B〉2 = 28.2 T of the two‐bcc Fe(Co) structure could be attributed to the nanocrystalline grains and to the grain boundaries, respectively. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)

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