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Effect of Substrate and Pyrolysis Atmosphere of FeNx Materials on Electrocatalysis of the Oxygen Reduction Reaction

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Abstract

In this work, several PGM-free materials supported on three types of carbon blacks (Vulcan XC-72, Monarch-1000, and Ketjenblack EC-600JD) and pyrolysed on N2 and NH3 atmosphere are investigated as catalysts for the oxygen reduction reaction (ORR) in acid and alkaline electrolytes. The synthesized materials are characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), energy-dispersive X-ray analysis (EDX), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy. The electrochemical characterization shows that for all N2- and NH3-treated catalysts, the ORR activity is higher in alkaline than acidic conditions, though in both cases, the main reaction product is water, thus evidencing a predominant occurrence of a 4-electron oxygen reduction mechanism. Further, a reasonable relationship is established between Fe-Nx coordination (pyridinic-N) and pyrrolic-N contents and the ORR activity of catalysts in acid media (FeNx supported on Monarch-1000). In alkaline conditions, the iron coordination with pyridinic-N, coupled to a high carbon surface area (Ketjenblack), enhances the ORR activity regardless of the pyrolysis atmosphere. Finally, the ORR performance in alkaline medium of the FeNx/Ketjenblack catalyst pyrolysed under N2 atmosphere is essentially the same as that achieved for the benchmark catalyst (Pt/C), while the durability of the best catalysts evidence to be quite promising in both acidic and alkaline media, as shown by a standard accelerated stability test.

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Funding

The authors received financial support from the Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) and the São Paulo State Research Foundation (FAPESP grant numbers 2019/22183-6; 2014/22130-6; 2017/15304-6). RS also received CAPES scholarship (CAPES grant number 1614344).

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Authors and Affiliations

  1. São Carlos Institute of Chemistry, University of São Paulo, São Carlos, SP, 13560-970, Brazil

    Ulisses Alves do Rêgo, Ricardo Sgarbi & Edson A. Ticianelli

  2. Universidade Federal Do Maranhão, Grajaú, MA, 65940-000, Brazil

    Ulisses Alves do Rêgo

  3. Research Centre for Gas Innovation, University of Sao Paulo, Escola Politecnica, Ave Prof Mello Moraes 2231, Sao Paulo, SP, 05508030, Brazil

    Thiago Lopes

  4. Universidade Federal Do Maranhão, São Luis, MA, 65080-040, Brazil

    Clenilton Costa dos Santos & Auro A. Tanaka

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  1. Ulisses Alves do Rêgo
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do Rêgo, U.A., Sgarbi, R., Lopes, T. et al. Effect of Substrate and Pyrolysis Atmosphere of FeNx Materials on Electrocatalysis of the Oxygen Reduction Reaction. Electrocatalysis 12, 548–563 (2021). https://doi.org/10.1007/s12678-021-00671-w

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