Towards Antimonene and 2D Antimony Telluride through Electrochemical Exfoliation

Two‐dimensional (2D) layered antimony (Sb) and antimony telluride (Sb₂Te₃) are two valuable materials for optoelectronic devices and thermoelectric applications. Preparing high‐quality sheets of these materials is the initial phase to promote their expected issues. Herein, micrometer‐sized few‐to‐multilayered sheets of Sb and Sb₂Te₃ have been obtained by electrochemical exfoliation. The layered rhombohedral Sb was exfoliated in Na₂SO₄ and Li₂SO₄ electrolytes by anodic–cationic intercalation, and Sb₂Te₃ was exfoliated in Na₂SO₄. These findings are important contributions for the solution‐based room‐temperature electrochemical exfoliation, which is stable under glove‐box‐free conditions, to further improve the production of high‐quality exfoliated sheets.