In recent years, electrochemical exfoliation of layered materials has attracted increasing attention owing to its wide feasibility in the fast and high-yield preparation of various two-dimensional (2D) nanomaterials. This process typically involves the use of an electric field to drive the intercalation of counter ions into the layered structure. The regulation of the interlayer chemistry plays a crucial rule in electrochemical exfoliation, yet it is often overlooked in existing review articles. To fill this gap, we present a summary of the most recent progress made in understanding the role of interlayer chemistry regulation in electrochemical, with a particular emphasis on the impact of redox reactions that lead to the electrochemical degradation of electrolytes and solvents, as well as the covalent modification necessary for creating 2D functional derivatives. The opportunities and challenges in this field are provided in the end, with a focus on the critical roles played by the electrochemical kinetics and interface observation in the development of large-scale industrial methods. These factors are pivotal for the continued progress and advancement of prospective techniques in this area.
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