Highly Efficient,Green, and Scalable β‐Cyclodextrin‐Assisted Aqueous Exfoliation of Transition‐Metal Dichalcogenides: MoS2 and ReS2 Nanoflakes

The β‐cyclodextrin‐assisted aqueous‐exfoliation method was used to prepare transition‐metal dichalcogenide (TMD) nanosheets, in a cheap, highly efficient, scalable and environmentally friendly manner. As study cases, MoS₂ and ReS₂ nanoflakes were prepared according to this method. Particularly, the effective exfoliation of ReS₂ crystals in an aqueous environment was observed for the first time. Moreover, exfoliated nanomaterials can be readily utilized in hydrogen evolution reactions (HERs) as noble‐metal‐free catalysts. This work provides new opportunities for highly efficient exfoliation of TMDs and other 2D nanomaterials into few‐layer nanosheets in aqueous media. Their production process showed high biocompatibility, broad applicability and excellent sustainability.