NiFe electrodes are developed for the oxygen evolution reaction (OER) in an alkaline electrolyser based on an anion exchange membrane (AEM) separator and fed with diluted KOH solution as supporting electrolyte. This study reports on the electrochemical behaviour of two different NiFe-oxide compositions (i.e., Ni1Fe1-oxide and Ni1Fe2-oxide) prepared by the oxalate method. These catalysts are assessed for single-cell operation in an MEA including a Sustainion™ anion-exchange membrane. The electrochemical polarization shows a current density of 650 mA cm−2 at 2 V and 50 °C for the Ni1Fe1 anode composition. A durability test of 500 h is carried out using potential cycling as an accelerated stress-test. This shows a decrease in current density of 150 mA cm−2 mainly during the first 400 h. The performance achieved for the anion-exchange membrane electrolyser single-cell based on the NiFeOx catalyst appears promising. However, further improvements are required to enhance the stability under these operating conditions.