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In-situ spectroscopic probe of the intrinsic structure feature of single-atom center in electrochemical CO/CO2 reduction to methanol

Ren Xinyi,Zhao Jian,Li Xuning,Shao Junming,Pan Binbin,Salamé Aude,Boutin Etienne,Groizard Thomas,Wang Shifu,Ding Jie,Zhang Xiong,Huang Wen-Yang,Zeng Wen-Jing,Liu Chengyu,Li Yanguang,Hung Sung-Fu,Huang Yanqiang,Robert Marc,Liu Bin

While exploring the process of CO/CO 2 electroreduction (CO x RR) is of great significance to achieve carbon recycling, deciphering reaction mechanisms so as to further design catalytic systems able to overcome sluggish kinetics remains challenging. In this work, a model single-Co-atom catalyst with well-defined coordination structure is developed and employed as a platform to unravel the underlying reaction mechanism of CO x RR. The as-prepared single-Co-atom catalyst exhibits a maximum methanol Faradaic efficiency as high as 65% at 30 mA/cm 2 in a membrane electrode assembly electrolyzer, while on the contrary, the reduction pathway of CO 2 to methanol is strongly decreased in CO 2 RR. In-situ X-ray absorption and Fourier-transform infrared spectroscopies point to a different adsorption configuration of *CO intermediate in CORR as compared to that in CO 2 RR, with a weaker stretching vibration of the C–O bond in the former case. Theoretical calculations further evidence the low energy barrier for the formation of a H-CoPc-CO – species, which is a critical factor in promoting the electrochemical reduction of CO to methanol.