To advance the MXene field, it is crucial to optimize each step of the synthesis process and create a detailed, systematic guide for synthesizing high‐quality MXene that can be consistently reproduced. In this study, a detailed guide is provided for an optimized synthesis of titanium carbide (Ti 3 C 2 T x ) MXene using a mixture of hydrofluoric and hydrochloric acids for the selective etching of the stoichimetric‐Ti 3 AlC 2 MAX phase and delamination of the etched multilayered Ti 3 C 2 T x MXene using lithium chloride at 65 °C for 1 h with argon bubbling. The effect of different synthesis variables is investigated, including the stoichiometry of the mixed powders to synthesize Ti 3 AlC 2 , pre‐etch impurity removal conditions, selective etching, storage, and drying of MXene multilayer powder, and the subsequent delamination conditions. The synthesis yield and the MXene film electrical conductivity are used as the two parameters to evaluate the MXene quality. Also the MXenes are characterized with scanning electron microscopy, x‐ray diffraction, atomic force microscopy, and ellipsometry. The Ti 3 C 2 T x film made via the optimized method shows electrical conductivity as high as ≈21,000 S/cm with a synthesis yield of up to 38 %. A detailed protocol is also provided for the Ti 3 C 2 T x MXene synthesis as the supporting information for this study.

Inside Back Cover In article number 2300030, Anasori and co-workers present a detailed guide for the optimized synthesis of titanium carbide (Ti3C2Tx) MXene and investigate the effects of selective etching and delamination conditions. The resulting Ti3C2Tx MXene film exhibits high electrical conductivity (≈21,000 S/cm) and a synthesis yield of 38 %. This study also provides a detailed step-by-step recipe for high-quality Ti3C2Tx MXene synthesis.