Fe-Mn alloy films have been prepared by electrodeposition in an organic bath containing FeCl2+MnCl2 in dimethyl formamide. The electroreduction of Mn(II) was irreversible and the diffusion coefficient of Mn(II) was calculated to be 8.0 x 10(-11) m(2) s(-1) at 298 K. An amorphous film of Fe-Mn was obtained by potentiostatic electrolysis. The Mn content varied from 4.8 at.% to 72.3 at.% with increase in the applied cathodic potential. Scanning electron microscope investigation showed that the deposited film was homogeneous and consisted of spherical particles. Nano-sized pores were observed in the surface of these particles. After heat treatment at 773 K, large crystal grains formed and X-ray diffraction patterns indicate that solid solution of Mn in gamma-Fe occurred. The alloying temperature of the Fe-Mn film was determined to be 10 13 K using differential thermal analysis. (c) 2007 Elsevier B.V. All rights reserved.