Room Temperature Nanographene Production via CO₂ Electrochemical Reduction on the Electrodeposited Bi on Sn Substrate

Electrochemical reduction of carbon dioxide (CO₂RR) to crystalline solid carbon at room temperature is challenging, but it is a providential CO₂ utilization route due to its indefinite storage and potential applications of its products in many advanced technologies. Here, room-temperature synthesis of polycrystalline nanographene was achieved by CO₂RR over the electrodeposited Bi on Sn substrate prepared with various bismuth concentrations (0.01 M, 0.05 M, and 0.1 M). The solid carbon products were solely produced on all the prepared electrodes at the applied potential -1.1 V vs. Ag/AgCl and were characterized as polycrystalline nanographene with an average domain size of ca. 3-4 nm. The morphology of the electrodeposited Bi/Sn electrocatalysts did not have much effect on the final structure of the solid carbon products formed but rather affected the CO₂ electroreduction activity. The optimized negative potential for the formation of nanographene products on the 0.05Bi/Sn was ca. -1.5 V vs. Ag/AgCl. Increasing the negative value of the applied potential accelerated the agglomeration of the highly reactive nascent Bi clusters in situ formed under the reaction conditions, which, as a consequence, resulted in a slight deviation of the product selectivity toward gaseous CO and H₂ evolution reaction. The Bi-graphene composites produced by this method show high potential as an additive for working electrode modification in electrochemical sensor-related applications.