Effect of the Substrate Materials in the Fabrication of an Electrode Based on Mixed Nickel‐Iron Oxide Electrocatalyst

Abstract The effect of different substrate materials in the fabrication of an electrode intended for use in the water oxidation reaction is investigated. The electrocatalyst is nickel‐iron oxide (NiFeOx) which is deposited by chronoamperometry on nickel, iron, titanium, and stainless steel substrates. The process of electrodeposition is optimized to achieve the lowest overpotential for the water oxidation reaction. The four electrodes are characterized by scanning electron microscopy (SEM), X‐ray photoelectron spectroscopy (XPS), and glow‐discharge optical emission spectroscopy (GDOES) to describe the effect of the substrate on the nature of the electrocatalyst layer. Electrochemical tests in 1 m NaOH are applied on the four electrodes to assess the stability and the retention of the electrocatalytic properties of the whole electrode. All electrodes show similar overpotential of ≈0.3 V at 10 mA cm⁻² implying that the substrate do not affect the electrocatalytic activity of the NiFeOx. After use, the overpotential increases in a range of 30–50 mV for nickel, iron, and titanium substrates, while stainless steel retains the lowest overpotential with an increase of 10 mV. This limited variation can be the effect of smaller NiFeOx nanoparticles compared to other substrates. XPS analysis reveals that after galvanostatic electrolysis, the oxidation state of Fe shifts slightly from Fe(II) to Fe(III), likely Fe₃O₄ and Fe₂O₃, while NiO/Ni₂O₃ change partially to Ni(OH)₂.