Abstract In this work we report the magnetic and structural properties obtained by Mössbauer spectrometry, Vibrating Sample Magnetometry and X‐ray diffraction, of powder of Nd 2 Fe 14 B prepared by mechanical alloying. The mixtures were ball milled during 48 hours and submitted to heat treatments between 500 and 900 °C under an argon atmosphere. Structural parameters were derived from high statistics X‐ray patterns. The Mössbauer spectra registered at 300 K for samples without heat treatment were fitted by means of a sextet and a hyperfine field distribution, associated to a residual pure iron phase (α‐Fe) and a disordered iron‐based phase, respectively. From the spectra at 300 K the formation of the Fe 3 C phase is observed for samples heat treated at 900 °C. A quenching above 900 °C accelerates the formation of the Fe 3 C phase. The hysteresis loops allow to conclude that these samples behave as soft ferromagnets. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)