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, MoS 2 and ReS 2 nanoflakes were prepared according to this method. Particularly, the effective exfoliation of ReS 2 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.