Post Iron Decoration of Mesoporous Nitrogen‐Doped Carbon Spheres for Efficient Electrochemical Oxygen Reduction

Abstract Iron–nitrogen–carbon (Fe–N–C) catalysts are considered as the most promising nonprecious metal catalysts for oxygen reduction reactions (ORRs). Their synthesis generally involves complex pyrolysis reactions at high temperature, making it difficult to optimize their composition, pore structure, and active sites. This study reports a simple synthesis strategy by reacting preformed nitrogen‐doped carbon scaffolds with iron pentacarbonyl, a liquid precursor that can effectively form active sites with the nitrogen sites, enabling more effective control of the catalyst. The resultant catalyst possesses a well‐defined mesoporous structure, a high surface area, and optimized active sites. The catalysts exhibit high ORR activity comparable to that of Pt/C catalyst (40% Pt loading) in alkaline media, with excellent stability and methanol tolerance. The synthetic strategy can be extended to synthesize other metal–N–C catalysts.