MXenes are a new, and growing, family of 2D materials with very promising properties for a wide variety of applications. Obtained from the etching of MAX phases, numerous properties can be targeted thanks to the chemical richness of the precursors. Herein, we highlight how etching agents govern surface chemistries of Ti 3 C 2 T x , the most widely studied MXene to date. By combining characterization tools such as X-ray diffraction, X-ray photoelectron, Raman and electron energy loss spectroscopies, scanning and transmission electron microscopies and a surface sensitive electrochemical reactionthe hydrogen evolution reaction, HERwe clearly demonstrate that the etching agent (HF, LiF/HCl or FeF 3 /HCl) strongly modifies the nature of surface terminal groups (F, OH and/or O), oxidation sensitivity, delamination ability, nature of the inserted species, interstratification, concentration of defects and size of flakes. Beyond showing how using these different characterization tools to analyze MXenes, this work highlights that the MXene synthesis routes can influence targeted applications.

TinCn−1Tx2D-sheets are functionalized using a new etching environment allowing the modification of their surface chemistry and production of rationalized TiO2@MXene nanocomposites.