LAUSR

© 2020 Wiley-VCH GmbH Aggregation-induced emission (AIE) luminogens are an important type of advanced functional materials with fantastic optical properties and have found potential applications in organic electronics, biochemistry, and molecular imaging. Herein, this article presents a novel application of AIE luminogens (AIEgens) for efficient exfoliation of layered transition metal dichalcogenides (TMDs, such as MoS2 and WSe2). From the 1H NMR spectroscopic analysis, the designed AIEgens can insert into the space between layers of MoS2 in ethanol solution and the dynamic molecular rotation against the weak interactions affords large-scale few-layer MoS2 nanosheets (7–8 layers) with enhanced smoothness. The 3D AIEgens play a significant role in preserving the crystal lattice of MoS2 even at high pressure (>15 GPa). More importantly, the new approach can also be used for exfoliation of WSe2 to achieve large-scale few-layer nanosheets. The present work thus provides a facile and high yielding synthetic method for accessing on a large scale 2D layered materials with enhanced properties for high-technology applications.