Four Zn-Fe-Ni films were electrodeposited under potentiostatic deposition conditions on aluminum and steel plates. Their composition, corrosion property, and structure were evaluated as a function of the FeSO4 concentration in the electrolyte. Cyclic voltammetry of the individual metals was performed in conjunction with the SEM technique to study the electroplating process of the films. The results show that Zn-Fe-Ni alloys can be produced with good adhesive and anticorrosive properties, and all films have the same crystallographic structure as zinc, but with different crystallographic orientations.