Fe-Mn alloy films have been prepared by electrodeposition for the first time. The electrode process of MnII reduced in MnCl2 + DMF and the electrodeposition of Fe-Mn in FeCl2 + MnCl2 + DMF were studied by cyclic voltammetry. The MnII + 2e = Mn reaction was irreversible and the diffusion coefficient of MnII was calculated to be 1.2 x10-6 cm2 s-1 at 25{degree sign}C. An amorphous film of Fe-Mn was obtained by potentiostatic electrolysis. SEM, EDAX experiments show that the film is homogeneous, dense and adheres firmly to the copper substrate. The content of Mn varies from 4.8 at.% to 72.3 at.% with the increase of the cathodic (deposition) potential. XRD patterns of the film after heat treatment at 500{degree sign}C indicate that solid solution of Mn in g- Fe occurs. The alloying temperature of the Fe-Mn alloy film is about 740{degree sign}C, determined by DTA experiments.
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