Two-dimensional (2D) layered antimony (Sb) and antimony telluride (Sb 2 Te 3 )a re two valuable materials for optoelectronic devices and thermoelectric applications. Preparing high-quality sheets of thesem aterials is the initial phase to promotet heir expected issues. Herein, micrometer-sized few-to-multilayered sheetso fS ba nd Sb 2 Te 3 have been obtained by electrochemical exfoliation. The layered rhombo-hedralS bw as exfoliated in Na 2 SO 4 and Li 2 SO 4 electrolytes by anodic-cationic intercalation, and Sb 2 Te 3 was exfoliated in Na 2 SO 4 .T hese findings are important contributions for the solution-based room-temperature electrochemical exfoliation, whichi ss table under glove-box-free conditions, to further improve the productiono fh igh-quality exfoliated sheets. exfoliated switchingv oltage in 4and 10 min. In the insert the height profilesa long the x axis of some selected sheets.