Jaehyeok Doh

This research aims to enhance MXene (Ti 3 C 2 T x ) synthesis from MAX phases (Ti 3 AlC 2 ) through a hydro‐solvothermal exfoliation process, with a focus on reducing time and temperature requirements. Prior hydrothermal studies have encountered challenges due to high reaction temperatures. In comparison to previous research, this work achieves superior results at lower temperatures. Two optimized MXene preparation routes are investigated and the etchant's impact on MXene surface chemistry is analyzed. Comprehensive X‐ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive X‐ray Spectroscopy (EDS), X‐ray Photoelectron Spectroscopy (XPS), Fourier transform infrared (FTIR), Raman spectroscopy, and Atomic Force Microscopy (AFM) analyses provide insights into hydrosolvothermal synthesis (H‐Ti 3 C 2 T x ) multilayers(ML), confirming/challenging recent spectroscopic assignments. Remarkably, hydro‐solvothermal treatment induces significant changes in surface composition, increasing hydroxyl (─OH) groups without oxidation and reducing fluorine (─F) groups on the H‐ Ti 3 C 2 T x surface. These study's results hold promise for applications in energy storage and electromagnetic wave shielding. This research accomplishes three main objectives: i) secures hydrothermal synthesis of two‐ dimensional (2D) MXenes, ii) efficiently utilizes lithium fluroide‐ hydrochloric acid (LiF−HCl) etching for high‐quality MXene flakes with minimal defects, and iii) understands hydro‐solvothermal kinetics. This approach advances MXene synthesis with enhanced material quality and production efficiency (>98%), in a more eco‐friendly and safer manner. This eco‐conscious synthesis underscores MXene's versatility and eco‐friendly methods' significance, reshaping MXene exploration and sustainable material synthesis, with potential implications for future electrochemical applications.