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In this work, the influence of the synthesis conditions on the structure, morphology, and electrocatalytic performance for the oxygen evolution reaction (OER) of Mn-Co-based films is studied. For this purpose, Mn-Co nanofilm is electrochemically synthesised in a one-step process on nickel foam in the presence of metal nitrates without any additives. The possible mechanism of the synthesis is proposed. The morphology and structure of the catalysts are studied by various techniques including scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and transmission electron microscopy. The analyses show that the as-deposited catalysts consist mainly of oxides/hydroxides and/or (oxy)hydroxides based on Mn²⁺, Co²⁺, and Co³⁺. The alkaline post-treatment of the film results in the formation of Mn-Co (oxy)hydroxides and crystalline Co(OH)₂ with a β-phase hexagonal platelet-like shape structure, indicating a layered double hydroxide structure, desirable for the OER. Electrochemical studies show that the catalytic performance of Mn-Co was dependent on the concentration of Mn versus Co in the synthesis solution and on the deposition charge. The optimised Mn-Co/Ni foam is characterised by a specific surface area of 10.5 m²·g⁻¹, a pore volume of 0.0042 cm³·g⁻¹, and high electrochemical stability with an overpotential deviation around 330–340 mV at 10 mA·cm⁻²_geo for 70 h.