Double iron and aluminum carbides were prepared by mechanical alloying from elemental powders, with a ball-to-powder weight ratio 20:1. The samples were milled for 1, 3, 5, 10, 15, 20 and 25 h. The alloy progress for each milling time was evaluated by X-ray diffraction (XRD) and 57 Fe Mössbauer spectroscopy. Once the alloy was consolidated two sorts of paramagnetic sites and a magnetic distribution were detected according to the Mössbauer fit. The majority doublet could correspond to Fe 3 AlC 0.5 carbide as X-ray diffraction suggest, and the other could be Fe 3 AlC 0.69 ; the magnetic distribution corresponding to Fe 3 Al phase, Fe 7 C 3 and Fe 5 C 2 single carbides. The hyperfine parameters are reported.