doi:10.1016/j.cej.2025.171198engPakrieva, EkaterinaHernandez-Ferrer, JavierMartinez, GemaBalas, FranciscoGarcía-Bordeje, EnriqueAnson-Casaos, AlejandroSimonelli, LauraBartolome, FernandoBenito, Ana M.Maser, Wolfgang K.Hueso, Jose L.Santamaria, Jesus3-component (N, Fe, Co) atomically dispersed ORR catalysts prepared by laser-driven decomposition of organic precursorsART-2025-147024The sluggish kinetics of the oxygen reduction reaction (ORR) remain a key bottleneck for the commercialization of proton exchange membrane fuel cells (PEMFCs), driving the search for efficient, non-precious metal catalysts. Herein, we present a laser-assisted pyrolysis strategy for the synthesis of nitrogen-doped carbon (NC) materials, both metal-free and containing atomically dispersed Fe and Co, using aerosolized phthalocyanine precursors and a near-instantaneous rapid decomposition under a high-energy laser beam, while preventing metal aggregation. A single-step post-synthetic thermal activation under an NH₃/N₂ atmosphere further tailors the textural and surface properties, without requiring ammonia co-feeding during laser pyrolysis, acid etching, or multiple treatments, marking a significant improvement over our previously reported single atom (Fe-N/C) protocols. The resulting Fe_Co/NC_tr catalyst exhibits high specific surface area, enhanced microporosity, improved graphitization, and increased abundance of electrochemically beneficial nitrogen sites. Compared to our earlier reported Fe–N/C catalysts, Fe_Co/NC_tr delivers significantly higher limiting current densities and enhanced durability in alkaline media. Overall, the developed Fe_Co/NC catalyst exhibits good ORR catalytic activity and outstanding long-term stability in alkaline media, comparable to the state-of-the-art commercial Pt/C catalysts. Cyanide poisoning tests confirm the essential role of atomically dispersed Fe2+ and Co2+ as active ORR sites.2025http://zaguan.unizar.es/record/16522710.1016/j.cej.2025.171198http://zaguan.unizar.es/record/165227oai:zaguan.unizar.es:165227info:eu-repo/grantAgreement/ES/AEI/CEX2023-001286-Sinfo:eu-repo/grantAgreement/ES/AEI/PID2020-114926RB-I00info:eu-repo/grantAgreement/ES/AEI/PID2023-146481OB-I00info:eu-repo/grantAgreement/ES/DGA/T03-23Rinfo:eu-repo/grantAgreement/ES/UZ-DGA/T57-23Rinfo:eu-repo/grantAgreement/ES/MICINN/CNS2022-135911info:eu-repo/grantAgreement/ES/MICINN/JDC2022-049007-Iinfo:eu-repo/grantAgreement/ES/MICINN/PID2022-139671OB-I00Chemical Engineering Journal 526 (2025), 171198 [13 pp.]by-nc-ndhttps://creativecommons.org/licenses/by-nc-nd/4.0/deed.esinfo:eu-repo/semantics/openAccess