Electrochemical Performance of a Hybrid NiCo₂O₄@NiFelt Electrode at Different Operating Temperatures and Electrolyte pH

Transition metals such as nickel and cobalt as an alternative to Pt and Pd can be used for oxygen evolution reactions (OERs) and hydrogen production reactions (HERs) in alkaline environments, facilitating green hydrogen production as a sustainable alternative to fossil fuels. In this study, an NiCo₂O₄ catalyst was produced by a sono-hydrothermal method using urea as a hydrolysis agent. The electrochemical performance of the catalyst-coated NiFelt electrode was evaluated at different KOH concentrations (0.25, 0.5, and 1 M) and four operating temperatures in the interval of 20–80 °C. The electrode characteristics were investigated via electrochemical spectroscopy (cyclic voltammetry, EIS, multistep chronopotentiometry, multistep chronoamperometry) using two different reference electrodes (Ag/AgCl and Hg/HgO), to obtain insight into the anodic and cathodic peaks. XRD, SEM, EDS, and TEM analyses confirmed the purity, structure, and nanoscale particle size (20–45 nm) of the NiCo₂O₄ catalyst. The electrode showed symmetric CV with Ag/AgCl, making this reference electrode more appropriate for capacitance measurements, while Hg/HgO proved advantageous for EIS in alkaline solutions due to reduced noise. The overpotential of the catalyst-coated NiFelt decreased by 108 mV at 10 mA/cm² compared to bare NiFelt, showing a good potential for its application in anion exchange membranes and alkaline electrolyzers at an industrial scale.