The use of precious metal electrocatalysts in clean electrochemical energy conversion and storage applications is widespread, but the sustainability of these materials, in terms of their availability and cost, is constrained. In this research, iron triadbased bimetallic nitrogen-doped carbon (M−N−C) materials were investigated as potential bifunctional electrocatalysts for the oxygen reduction reaction (ORR) and oxygen evolution reaction (OER). The synthesis of bimetallic FeCo−N−C, CoNi−N−C, and FeNi−N−C catalysts involved a precisely optimized carbonization process of their respective metal−organic precursors. Comprehensive structural analysis was undertaken to elucidate the morphology of the prepared M−N−C materials, while their electrocatalytic performance was assessed through cyclic voltammetry and rotating disk electrode measurements in a 0.1 M KOH solution. All bimetallic catalyst materials demonstrated impressive bifunctional electrocatalytic performance in both the ORR and the OER. However, the FeNi−N−C catalyst proved notably more stable, particularly in the OER conditions. Employed as a bifunctional catalyst for ORR/OER within a customized zinc−air battery, FeNi−N−C exhibited a remarkable discharge−charge voltage gap of only 0.86 V, alongside a peak power density of 60 mW cm −2 . The outstanding stability of FeNi−N−C, operational for about 55 h at 2 mA cm −2 , highlights its robustness for prolonged application.