context: On the basis of the change in the direction of the exfoliating voltage, electrochemical exfoliation of 2D antimony, bismuth and their compounds can be divided into DC voltage exfoliation and square-wave voltage exfoliation. DC voltage exfoliation uses a DC power supply to provide the voltage, and the voltage direction does not change during the exfoliation process. The process of preparing 2D antimony, bismuth and their compounds by the DC voltage exfoliation method is similar to that of cathode exfoliation graphene. The exfoliation process was conducted by using a large block of antimony or bismuth or its compound as the cathode and platinum wire or foil as the anode and in an organic solution. This process applies a voltage to the bulk of antimony, bismuth and their compounds at the cathode, drives the insertion of cations in the electrolyte, and uses jet force that produces hydrogen to promote the peeling of antimony, bismuth and their compounds. In 2017, Li et al. illustrated the possible mechanism of cathodic exfoliation to prepare 2D Sb nanosheets in 0.5 M Na2SO4 solution. Driven by the voltage, the Na+ intercalation layer that accumulates at the negative electrode enters the interlayer of the bulk Sb crystal. Because a large amount of the Na+ intercalation layer enters the interlayer of the Sb crystal, the exfoliation of Sb is eventually promoted by the expansion force (Fig. 4a). Furthermore, the positive and negative voltage and the size of the electrolyte cations affect the efficiency of exfoliation.