The Influence of Oxygen Concentration during MAX Phases (Ti₃AlC₂) Preparation on the α-Al₂O₃ Microparticles Content and Specific Surface Area of Multilayered MXenes (Ti₃C₂Tx).

The high specific surface area of multilayered two-dimensional carbides called MXenes, is a critical feature for their use in energy storage systems, especially supercapacitors. Therefore, the possibility of controlling this parameter is highly desired. This work presents the results of the influence of oxygen concentration during Ti₃AlC₂ ternary carbide-MAX phase preparation on α-Al₂O₃ particles content, and thus the porosity and specific surface area of the Ti₃C₂Tx MXenes. In this research, three different Ti₃AlC₂ samples were prepared, based on TiC-Ti₂AlC powder mixtures, which were conditioned and cold pressed in argon, air and oxygen filled glove-boxes. As-prepared pellets were sintered, ground, sieved and etched using hydrofluoric acid. The MAX phase and MXene samples were analyzed using scanning electron microscopy and X-ray diffraction. The influence of the oxygen concentration on the MXene structures was confirmed by Brunauer-Emmett-Teller surface area determination. It was found that oxygen concentration plays an important role in the formation of α-Al₂O₃ inclusions between MAX phase layers. The mortar grinding of the MAX phase powder and subsequent MXene fabrication process released the α-Al₂O₃ impurities, which led to the formation of the porous MXene structures. However, some non-porous α-Al₂O₃ particles remained inside the MXene structures. Those particles were found ingrown and irremovable, and thus decreased the MXene specific surface area.