Liquid‐Phase Plasma Bubbles Exfoliation of Few‐Layer Nanosheets for High‐Performance CO ₂ ‐to‐Formate Conversion

ABSTRACT Two‐dimensional (2D) materials have demonstrated excellent application prospects in electrocatalysis due to their unique anisotropy, high densities of exposed atoms, and tunable surface chemistry. However, the top‐down exfoliation of few‐layer nanosheets by breaking van der Waals interactions often introduces external intercalating molecules or solvent molecules, which adversely affect their performance in electrocatalytic reactions. Herein, we report a liquid‐phase plasma bubbles treatment method for the exfoliation and preparation of few‐layer Bi 2 Se 3 nanosheets. As no external intercalating molecules are introduced, and the as‐exfoliated few‐layer nanosheets possess a higher density of unsaturated bonds, they exhibit outstanding performance in the electrocatalytic carbon dioxide reduction reaction (CO 2 RR). The Faradaic efficiency for CO 2 electroreduction to formate exceeds 90%, with catalytic stability maintained for up to 100 h. Furthermore, this exfoliation method demonstrates broad applicability, successfully producing few‐layer MoS 2 , WS 2 , and WSe 2 nanosheets. This work provides a new strategy for the synthesis of high‐performance few‐layer nanosheets for electrocatalysis.