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Abstract Copper (Cu) has been regarded as a highly efficient electrocatalyst for the conversion of CO2 into a multicarbon product. However, the catalytic mechanism and the active sites of Cu catalysts under operating conditions still remain elusive. Yang's team applied systematic operando characterization techniques to provide a quantitative analysis of the valence states and the chemical environment of Cu nanocatalysts under electrochemical reaction conditions, which clearly reveal the evolution of Cu nanocatalysts before and after the entire electrochemical CO2 reduction.