The study of galvanostatic iron electrodeposition on nickel substrate was carried out in order to establish the most suitable experimental conditions to obtain pure iron fragile layers to be removed and transformed into powder. Under current density of 40 mA cm(-2) the deposits obtained were satisfactory to be transformed into a powder. In the light of the cathodic polarization phenomena and Scanning Electron Microscopy (SEM) graphs an explanation has been offered for the various trends observed during the investigation. The optimum storage conditions for the iron powder was found to be in vacuum using the Schlenk technique. The results led to conclude that the use of stainless steel as anode must be avoided since the presence of Mn is not beneficial for the performance of iron electrodes in charge/discharge reactions in Ni/Fe batteries.