Comprehensive synthesis of Ti3C2Tx from MAX phase to MXene

MXenes are a large family of two-dimensional materials that have attracted attention across many fields due to their desirable optoelectronic, biological, mechanical and chemical properties. There currently exist many synthesis procedures that lead to differences in flake size, defects and surface chemistry, which in turn affect their properties. Herein, we describe the steps to synthesize Ti3C2Tx—the most important and widely used MXene, from a Ti3AlC2 MAX phase precursor. The procedure contains three main sections: synthesis of Ti3AlC2 MAX, wet chemical etching of the MAX in hydrofluoric acid/HCl solution to yield multilayer Ti3C2Tx and its delamination into single-layer flakes. Three delamination options are described; these use LiCl, tertiary amines (tetramethyl ammonium hydroxide/ tetrabutyl ammonium hydroxide) and dimethylsulfoxide respectively. These procedures can be adapted for the synthesis of MXenes beyond Ti3C2Tx. The MAX phase synthesis takes about 1 week, with the etching and delamination each requiring 2 d. This protocol requires users to have experience working with hydrofluoric acid, and it is recommended that users have experience with wet chemistry and centrifugation; characterization techniques such as X-ray diffraction and particle size analysis are also essential for the success of the protocol. While alternative synthesis methods, such as minimally intensive layer delamination, are desirable for certain MXenes (such as Ti2CTx) or specific applications, this protocol aims to standardize the more commonly used hydrofluoric acid/HCl etching method, which produces Ti3C2Tx with minimal concentration of defects and the highest conductivity and serves as a guideline for those working with MXenes for the first time. MXenes are two-dimensional materials with diverse optoelectronic, biological, mechanical and chemical properties. This protocol describes how to prepare single-layer flakes of Ti3C2Tx, the most important and widely used MXene, from a Ti3AlC2 MAX phase precursor.