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Insights into Electrocatalytic Oxygen Evolution over Hierarchical FeCo<sub>2</sub>S<sub>4</sub> Nanospheres

Ching‐Wen LiaoDepartment of Materials and Mineral Resources Engineering, Institute of Mineral Resources Engineering, National Taipei University of Technology, Taipei 106344, TaiwanSheng-Yu ChenInstitute of Chemistry, Academia Sinica, Taipei 115201, TaiwanLiang‐Ching HsuNational Synchrotron Radiation Research Center, Hsinchu 300092, TaiwanChia-Wei LinDepartment of Materials and Mineral Resources Engineering, Institute of Mineral Resources Engineering, National Taipei University of Technology, Taipei 106344, TaiwanJeng‐Lung ChenNational Synchrotron Radiation Research Center, Hsinchu 300092, TaiwanChun‐Hong KuoDepartment of Applied Chemistry, National Yang Ming Chiao Tung University, Hsinchu 300093, TaiwanYu‐Hsu ChangDepartment of Materials and Mineral Resources Engineering, Institute of Mineral Resources Engineering, National Taipei University of Technology, Taipei 106344, Taiwan

2021en

ABI

Annotatsiya

In this work, a system of spinel FeCo2S4-catalyzed oxygen evolution reaction (OER) is studied. The hierarchical FeCo2S4 nanospheres (HNSs) are synthesized by a two-step hydrothermal method on Ni foam (NF) by vulcanizing Fe–Co precursors with different concentrations of Na2S. Since FeCo2S4 HNSs have the advantages of a large exposed surface area and high dispersity on the Ni foam, the FeCo2S4/NF heterostructure is used as a working electrode for OER in an electrochemical system. The catalysis results represent that the performance of FeCo2S4/NF in OER correlates with the vulcanized HNS surfaces made with different concentrations of Na2S, where the 0.1 M FeCo2S4/NF catalyst is the optimized condition to exhibit the lowest OER overpotential. Besides, the structures of FeCo2S4 HNSs are stable after a 12 h OER durability test. In the results of in situ X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) measurements with the FeCo2S4/NF electrode, the mechanism of FeCo2S4-catalyzed water splitting is through the formation of MOOH (M = metal) followed by the release of O2, the so-called indirect pathway, in the alkaline condition. Co has the major role to play in the OER reaction, while Fe holds its electronic state. Moreover, the reason for sulfide-assisted OER is the reduced charge-transfer barrier in the HNS structure that benefits MOOH generation.

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DOI: 10.1021/acssuschemeng.1c06658

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