Macromolecule‐Mediated Exfoliation of Two‐Dimensional Materials: Mechanisms, Advancements, and Perspectives

The scalable production of high‐quality two‐dimensional materials (2DMs) remains challenging due to the limited efficiency, poor controllability, and environmental concerns associated with conventional exfoliation methods. Macromolecule‐mediated exfoliation (MME) has emerged as an efficient and sustainable strategy for the preparation of 2DMs. By exploiting controlled force transmission and interfacial interactions, macromolecules enable effective layer separation while stabilizing exfoliated nanosheets and introducing surface functionality. This review summarizes recent progress in mechanically assisted exfoliation of 2DMs using natural and synthetic macromolecules, highlights underlying exfoliation mechanisms and macromolecular design principles, and discusses current challenges and future opportunities in this rapidly evolving field.