<p>In this study, NiCu and NiFe based electrocatalysts cocatalyzed with CeO₂ nanorods for ethanol electrooxidation reaction (EOR) in alkaline medium were synthesized and their electrochemical performances were investigated in detail. In all samples, the amount of CeO₂ nanorods was kept constant (20 wt%), and the ratios of Ni and second metal (Cu or Fe) were systematically changed. The obtained nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). Electrochemical performance evaluations were carried out by cyclic voltammetry (CV), linear sweep voltammetry (LSV) and chronoamperometry (CA) methods. EOR activities of catalysts with different Ni: Cu and Ni: Fe ratios were compared and the highest performing compositions were determined for each system. According to CV analysis, NiCu-CeO_2NRs-2 had the highest current density (21.63&#xa0;mA cm⁻²) and the lowest onset potential (444 mV) among Cu-containing combinations. Among Fe-containing combinations, NiFe-CeO_2NRs-2 was observed as the best performing catalyst combination with a current density of 27.71 mV cm⁻² and an onset potential of 387 mV. The effect of temperature on electrocatalytic activity was also investigated by electrochemical measurements at different temperatures on catalysts with these optimum compositions. The study reveals the effect of different metal ratios and temperature conditions on EOR performance and evaluates the performance potential of NiCu and NiFe based systems cocatalyzed with CeO₂.</p>