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We report the pyrolysis of NiFe‐containing nanocrystals, which leads to 10.2±2.4 nm NiFe alloy particles embedded in carbon with an exceptional area specific exchange current density of 0.048 mA cmNi−2 toward the alkaline hydrogen oxidation reaction (HOR). The high activity primarily originates from optimized hydrogen and hydroxyl adsorption strength due to alloying effect between Ni and Fe.
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