An in situ exploration of how Fe/N/C oxygen reduction catalysts evolve during synthesis under pyrolytic conditions

Shuhu Yin, Hongyuan Yi, Mengli Liu, Jian Yang, Shuangli Yang, Bin-Wei Zhang, Long Chen, Xiaoyang Cheng, Huan Huang, Rui Huang, Yanxia Jiang (), Honggang Liao () and Shigang Sun
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Shuhu Yin: Xiamen University
Hongyuan Yi: Xiamen University
Mengli Liu: Xiamen University
Jian Yang: Chongqing University
Shuangli Yang: Xiamen University
Bin-Wei Zhang: Chongqing University
Long Chen: Xiamen University
Xiaoyang Cheng: Xiamen University
Huan Huang: Chinese Academy of Sciences
Rui Huang: Xiamen University
Yanxia Jiang: Xiamen University
Honggang Liao: Xiamen University
Shigang Sun: Xiamen University

Nature Communications, 2024, vol. 15, issue 1, 1-9

Abstract: Abstract In pursuing cheap and effective oxygen reduction catalysts, the Fe/N/C system emerges as a promising candidate. Nevertheless, the structural transformations of starting materials into Fe- and N-doped carbon catalysts remains poorly characterized under pyrolytic conditions. Here, we explore the evolution of Fe species and track the formation of Fe–N4 site development by employing diverse in-situ diagnostic techniques. In-situ heating microscopy reveals the initial formation of FeOx nanoparticles and subsequent internal migration within the carbon matrix, which stops once FeOx is fully reduced. The migration and decomposition of nanoparticles then leads to carbon layer reconstruction. Experimental and theoretical analysis reveals size-dependent behavior of FeOx where nanoparticles below 7 nm readily release Fe atoms to form Fe–N4 while nanoparticles with sizes >10 nm tend to coalesce and impede Fe–N4 site formation. The work visualizes the pyrolysis process of Fe/N/C materials, providing theoretical guidance for the rational design of catalysts.

Date: 2024
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DOI: 10.1038/s41467-024-50629-x

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