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Bimetallic sulfides are expected to realize efficient CO2 electroreduction into formate over a wide potential window, however, they will undergo in situ structural evolution under the reaction conditions. Therefore, clarifying the structural evolution process, the real active site and the catalytic mechanism is significant. Here, taking Cu2SnS3 as an example, we unveiled that Cu2SnS3 occurred self‐adapted phase separation toward forming the stable SnO2@CuS and SnO2@Cu2O heterojunction during the electrochemical process. Calculations illustrated that the strongly coupled interfaces as real active sites driven the electron self‐flow from Sn4+ to Cu+, thereby promoting the delocalized Sn sites to combine HCOO* with H*. Cu2SnS3 nanosheets achieve over 83.4 % formate selectivity in a wide potential range from −0.6 V to −1.1 V. Our findings provide insight into the structural evolution process and performance‐enhanced origin of ternary sulfides under the CO2 electroreduction. [ABSTRACT FROM AUTHOR]

Carbon dioxide (CO2) conversion is promising in alleviating the excessive CO2 level and simultaneously producing valuables. This work reports the preparation of carbon nanorods encapsulated bismuth oxides for the efficient CO2 electroconversion toward formate production. This resultant catalyst exhibits a small onset potential of −0.28 V vs. RHE and partial current density of over 200 mA cm−2 with a stable and high Faradaic efficiency of 93 % for formate generation in a flow cell configuration. Electrochemical results demonstrate the synergistic effect in the Bi2O3@C promotes the rapid and selective CO2 reduction in which the Bi2O3 is beneficial for improving the reaction kinetics and formate selectivity, while the carbon matrix would be helpful for enhancing the activity and current density of formate production. This work provides effective bismuth‐based MOF derivatives for efficient formate production and offers insights in promoting practical CO2 conversion technology. [ABSTRACT FROM AUTHOR]