A nanostructured Fe 65 Al 30 Sn 5 alloy has been synthesized by mechanical alloying of elemental Fe, Al, and Sn powders in a planetary ball mill. The structure and phase composition of the asmilled sample and the samples after subsequent heat treatment at 400°C, 500°C, and 800°C were investigated using X-ray diffraction, electron microscopy, 57 Fe and 119m Sn Mo¨ssbauer spectroscopy. We found that the as-milled sample is a nanocrystalline ternary bcc solid solution of the estimated composition Fe 62 Al 32.6 Sn 5.4. The samples of Fe 65 Al 30 Sn 5 after annealing are non-uniform materials that mainly comprise the ternary B2 ordered phase Fe 65 Al 30 Sn x , x Sn ≤ 1 at. pct. In addition to the dominant B2 ordered phase, we also identified chemically non-ordered regions, Sn and FeSn, FeSn 2 .