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The process of co-deposition of Ni with Mo from alkaline electrolytes was studied by taking linear and cyclic polarization curves of Pt electrode at various concentrations of initial components and potential scan rates. Solutions of Na2MoO4∙2H2O and NiSO4∙7H2O were used as sources of ions of the main components in NH4OH electrolyte. It was found that codeposition of nickel with molybdenum goes through the oxide formation stage, and a solid solution of these two metals is deposited on the cathode surface. The film obtained at constant current on Ni electrode under optimal conditions was found amorphous, but additional thermal treatment at 500 °C for one hour made it polycrystalline. This was confirmed by peaks in X-ray diffraction patterns, corresponding to NiMoO4, Ni, and MoO3. The proposed electrolyte and electrolysis conditions allow to obtain thin films with molybdenum content ranging from 17.1 to 50.9 at.%. The co-deposition of Ni with Mo is limited by diffusion of these ions to the cathode surface. The knowledge of the mechanism of co-deposition of Ni and Mo will make possible a selection of optimal conditions for deposition of alloys of the required composition with satisfactory electrocatalytic properties.

Study of electrochemical deposition of Ni-Mo thin films from alkaline electrolytes