Anion exchange membrane water electrolysis (AEMWE) is an efficient, cost-effective solution to renewable energy storage. The process includes oxygen and hydrogen evolution reactions (OER and HER); the OER is kinetically unfavourable. Studies have shown that nickel (Ni)- iron (Fe) catalysts enhance activity towards OER, and cerium oxide (CeO₂) supports have shown positive effects on catalytic performance. This study covers the preliminary evaluation of Ni, Ni₉₀Fe₁₀ (at%) and Ni₉₀Fe₁₀/CeO₂ (50 wt%) nanoparticles (NPs), synthesized by chemical reduction, as OER catalysts in AEMWE using commercial membranes. Transmission electron microscopy (TEM) images of the Ni-based NPs indicate NPs roughly 4–6 nm in size. Three-electrode cell measurements indicate that Ni₉₀Fe₁₀ is the most active non-noble metal catalyst in 1 and 0.1 M KOH. AEMWE measurements of the anodes show cells achieving overall cell voltages between 1.85 and 1.90 V at 2 A cm⁻² in 1 M KOH at 50 °C, which is comparable to the selected iridium-black reference catalyst. In 0.1 M KOH, the AEMWE cell containing Ni₉₀Fe₁₀ attained the lowest voltage of 1.99 V at 2 A cm⁻². Electrochemical impedance spectroscopy (EIS) of the AEMWE cells using Ni₉₀Fe₁₀/CeO₂ showed a higher ohmic resistance than all catalysts, indicating the need for support optimization.