A series on nanocrystalline Fe 100-x Cr x alloys prepared by mechanical alloying was investigated with Xray diffraction (XRD), scanning electron microscopy (SEM) and Mössbauer spectroscopy (MS) techniques. XRD and SEM were used to structurally characterize the samples whereas MS permitted phase analysis as well as determination of the Debye temperature, D . Concerning the latter, an enhancement relative to bulk D -values was revealed in the range of 40 x 50. In a sample of Fe 55.5 Cr 44.5 two phases were detected viz. (1) crystalline and magnetic with D =572 (56) K and (2) amorphous and paramagnetic with D =405 (26) K.