Rapid Electrothermal Heating and Molten Salt Etching to Produce Ti₃C₂ MXenes

Rapid, out‐of‐oven techniques for MXene synthesis are of great interest and would allow for easier production of this exciting class of 2D materials. MXenes are typically synthesized by etching MAX phases with strong acids for long times, sometimes exceeding 40 h. Electrothermal synthesis techniques can reduce the heating time of materials; here Joule heating with molten salt etching precursors is utilized to etch MAX phase into multilayered (ML) Ti 3 C 2 T x MXenes. An inert environment is used to etch the MAX phase in 30 min at 750–800 °C. SEM/EDS and XRD confirmed etching of the material. XPS, FTIR, and Raman are compared to conventional LiF‐HCl ML‐ Ti 3 C 2 T x , showing similar spectra to Joule heated ML‐Ti3C2Tx material. Most importantly, this new out‐of‐oven Ti 3 C 2 T x synthesis decreased etching time by 98% from molten salt etching and reduced energy usage from 1.56 × 10 7 to 1.01 × 10 6 J g −1 per batch, paving the way for the commercialization of MXene etching.