Ultrafast microwave synthesis of Ti-based MXenes with high yields

We report a microwave-assisted method for synthesizing MXenes that accelerates hydrofluoric acid etching of MAX phases by ∼500-fold compared to conventional approaches. Ti₃C₂ and Ti₃CN MXenes were obtained from Ti₃AlC₂ and Ti₃AlCN within 3 minutes at 220 W, yielding ∼90% and 70% product, respectively. The process produces expanded, accordion-like structures that delaminate into flakes with mild ultrasonication, eliminating post-synthesis intercalation. Rapid, uniform heating and hydrogen evolution drive structural expansion and facilitate delamination. Structural and morphological analyses (XRD, XPS, TEM, SEM, DLS, AFM) confirmed their successful synthesis, while electrochemical testing showed performance comparable to conventionally prepared MXenes. This approach establishes a rapid, efficient, and high-yield route for scalable MXene production.