Electrodeposition of Ni–Fe Thin Films: Effect of Electrolyte Composition and Current Density on Structure, Morphology and Magnetic Properties

In the present study, the electrodeposition of thin Ni–Fe films obtained from aqueous electrolytes containing nickel (II) and iron (II) sulfates and chlorides is investigated. The study particularly emphasizes the influence of electrolyte additives—boric acid, chloride ions, and Na2EDTA—on the electrochemical behavior, microstructure, and magnetic properties of the deposited layers. Cyclic voltammetry revealed a partial alignment of the reduction potentials of nickel and iron and the suppression of the hydrogen evolution side reaction up to −1 V. Electrodeposition in galvanostatic mode in the range of 0.5 to 1.0 A/dm2 allows the formation of layers with iron contents between 20.5 wt. % to 41.4 wt. % and coating thickness from 1.3 to 3.0 µm. SEM and AFM observations demonstrated a pronounced dependence of the surface morphology on the current density, with higher current densities promoting the formation of dendritic structures. X-ray diffraction confirmed the dominance of a face-centered cubic (FCC) Ni-based solid solution, accompanied by minor contributions from non-stoichiometric Fe1−xO. All the obtained Fe-Ni films have soft magnetic properties. Increasing the current density and the boric acid concentration causes the coercive force and isotropy of the layers to improve. The results demonstrate that thin Ni-Fe films with controlled structure and morphology, with favorable soft ferromagnetic properties suitable for functional applications, could be electrodeposited from complex chloride–sulfate electrolytes by adjusting the current density.