Conventionally, the synthesis of MXene requires the use of hydrofluoric acid, either on its own or mixed with other acids (e.g., HCl, H2SO4), or the use of reagents that release HF in situ (e.g., LiF + HCl, known as the MILD approach, and NH4HF2) to remove the A layer from the MAX precursor. However, HF is extremely hazardous to humans and the environment. Furthermore, the aggressiveness of HF causes unavoidable damage to the basal plane of the MXene layer, resulting in a small flake size of the delaminated MXenes. A few hydrothermal approaches have been reported to etch the MAX phase to MXene. Gentile et al. reported the hydrothermal etching of Ti3C2 using HBF4 as an etchant. Yet, the etching mechanism was still based on the decomposition of HBF4 to HF upon heating to 60 °C. Another example, inspired by the Bayer process used in bauxite refining for the isolation of aluminium oxide, Li et al. reported a fluorine-free synthesis of Ti3C2Tx via alkali treatment, which involves the use of 27.5 M of NaOH at 270 °C for 12 hours. Peng et al. reported a hydrothermal etching of MAX phases (Ti3AlC2 and Nb2AlC) by 12 M HCl and 0.5 M NaBF4 for up to 32 hours at 180 °C. Alternatively, non-aqueous approaches such as molten salt and halogen etching have also been reported. However, the abovementioned approaches require harsh reaction conditions, making them costly and difficult to scale up. Amongst all other approaches, electrochemical etching of MAX phases is particularly promising.