Novel methods for the preparation of metal‐supported materials are desired for better catalytic performance and selectivity. In this article, Ni supported on multiwall nanotubes (Ni/MWNTs) is synthesized with electrodeposition method for electrocatalytic CO2 reduction reaction (CO2RR). The sample drying time after electrodeposition is found critical to oxidize Ni for better activity, and higher Ni oxidation state is required for CO2RR. The loading effect study proves that higher current density is achieved from small Ni clusters than that from large nano particles. This work provides a pioneer approach to synthesize small Ni clusters using electrodeposition method for electrocatalytic CO2 conversion.
Electrochemical reduction reaction of CO2 (CO2RR) is a promising technology for alleviating the global warming caused by the emission of CO2. This technology, however, is still in the stage of finding efficient catalysts. The catalysts must be able to convert CO2 to other carbon‐based products with high activity and selectivity to valuable chemicals. In this review, previous development of heteroatom‐doped metal‐free carbon materials (H‐CMs) is briefly summarized. Recent progress of CO2RR promoted by metal single‐atom catalysts (M‐SACs) is then discussed with emphasis on the synthesis of M‐SACs, the catalytic performance, and reaction mechanisms. The high temperature pyrolysis method and electrodeposition are attracting attentions recently to prepare M‐SACs with high metal loading on N‐doped carbon materials, a very active M‐SACs system for the CO2RR. Theoretical calculations of free energy change on active sites, the Operando X‐ray absorption near edge structure (XANES), and Bader charge analysis reveal a significant role of metal oxidation state and charge transfer between metal atoms and absorbed CO. The challenges and perspectives for the extensive applications of M‐SACs in CO2RR are also discussed in this review.
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