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Catalysts play a vital role in electrochemical reduction of CO 2 to valuable products. Only based on effective catalysts, CO 2 electrolysis process can be advanced toward industrial application. In this work, we present a Sb-Cu 2 O material synthesized via one-pot microwave-assisted solvothermal route. The Sb-Cu 2 O derived bimetallic catalyst achieves a highest CO selectivity of 96% and good CO partial current densities of 37.3 and 74.0 mA cm−2 at − 0.8 and − 1.2 V vs. reversible hydrogen electrode (RHE), respectively. The Sb-Cu catalyst also displays good stability at current densities ranging from 5.6 to 100 mA cm−2. Additionally, for the first time, a complete theoretical study reveals the critical roles of Sb in selective CO 2 conversion to CO on this bimetallic material, including stabilizing stepped Cu surfaces selective for the reaction, lowering energy barriers for the formation of key intermediate and favouring CO desorption. [Display omitted] • Sb-Cu 2 O material is synthesized via a one-pot microwave-assisted route. • Sb is uniformly distributed and promotes the formation of nanocrystalline Cu 2 O. • The derived Sb-Cu shows outstanding performance for the CO 2 RR to CO. • Enhancing local CO 2 concentration is demonstrated to boost CO formation rate. • Theoretical study reveals the critical roles of Sb in CO formation on Sb-Cu. [ABSTRACT FROM AUTHOR]