Hydroxyl radicals dominate reoxidation of oxide-derived Cu in electrochemical CO2 reduction

Shijia Mu, Honglei Lu, Qianbao Wu, Lei Li, Ruijuan Zhao, Chang Long () and Chunhua Cui ()
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Shijia Mu: University of Electronic Science and Technology of China
Honglei Lu: University of Electronic Science and Technology of China
Qianbao Wu: University of Electronic Science and Technology of China
Lei Li: University of Electronic Science and Technology of China
Ruijuan Zhao: University of Electronic Science and Technology of China
Chang Long: University of Electronic Science and Technology of China
Chunhua Cui: University of Electronic Science and Technology of China

Nature Communications, 2022, vol. 13, issue 1, 1-8

Abstract: Abstract Cuδ+ sites on the surface of oxide-derived copper (OD-Cu) are of vital importance in electrochemical CO2 reduction reaction (CO2RR). However, the underlying reason for the dynamically existing Cuδ+ species, although thermodynamically unstable under reductive CO2RR conditions, remains uncovered. Here, by using electron paramagnetic resonance, we identify the highly oxidative hydroxyl radicals (OH•) formed at room temperature in HCO3- solutions. In combination with in situ Raman spectroscopy, secondary ion mass spectrometry, and isotope-labelling, we demonstrate a dynamic reduction/reoxidation behavior at the surface of OD-Cu and reveal that the fast oxygen exchange between HCO3- and H2O provides oxygen sources for the formation of OH• radicals. In addition, their continuous generations can cause spontaneous oxidation of Cu electrodes and produce surface CuOx species. Significantly, this work suggests that there is a “seesaw-effect” between the cathodic reduction and the OH•-induced reoxidation, determining the chemical state and content of Cuδ+ species in CO2RR. This insight is supposed to thrust an understanding of the crucial role of electrolytes in CO2RR.

Date: 2022
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DOI: 10.1038/s41467-022-31498-8

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