In this work Pb 0.05 Fe 0.95 nanostructured alloy was prepared by high energy ball milling under argon atmosphere. X-ray diffraction (XRD), differential scanning calorimetry (DSC) and Mössbauer measurements were performed in the milled samples to study the alloying process and the structural variation with milling time. XRD and DSC results of Pb 0.05 Fe 0.95 alloy indicate the presence of free Pb metal for milling times shorter than 20 h. On the other hand, XRD and Mössbauer results show that the final Pb 0.05 Fe 0.95 alloy (sample milled for 310 h) is constituted by four nanocrystalline phases: b.c.c.-Fe, possibly with Pb impurities trapped in it, Fe/Pb phase and finally two Fe oxide phases (Fe 1−x O and Fe 3 O 4 ). The relative areas corresponding to these phases in the Mössbauer spectrum are 58% for the b.c.c.-Fe, 12% for the b.c.c. Fe/Pb alloy, and 30% for the Fe oxide phases. The Fe/Pb phase, with approximate composition Fe 0.71 Pb 0.29 , is being reported for the first time and it is also shown that this phase is thermally stable up to 650 K.