Synthesis and characterization of Ti₃C₂T_x MXene with preserved MAX phase structure via optimized delamination

MXenes, an emerging family of two-dimensional (2D) transition metal carbides, are typically synthesized by etching MAX phases in fluoride-containing solutions. Conventional delamination methods often fail to recover all delaminated MXene flakes, leaving a significant portion trapped in sediment and reducing the overall yield. In this study, we investigated the recovery of sediment-trapped Ti₃C₂T_x MXene in the form of a film through a modified conventional method. The hexagonal MAX phase Ti₃AlC₂ was synthesized via pressureless sintering at 1450 °C for 3 h under flowing argon, followed by selective etching using a mixture of HF/HCl and subsequent washing with LiCl solution. The delaminated MXene was prepared in two distinct forms: (1) A colloidal solution with an average flake size of ~700 nm, suitable for solution-based applications. (2) A thin layer of hexagonal flakes (average size of ~10 μm) was deposited on a glass substrate via a transfer method (single dip-coating). X-ray diffraction (XRD) analysis corroborated the structural integrity of the MXene. Scanning electron microscopy (SEM) image of the MXene revealed the preservation of the hexagonal morphology inherited from the parent MAX phase, whereas Fourier-transform infrared (FTIR) and Raman spectroscopy identified hydrophilic surface functional groups (–O and –OH). By efficiently recovering sediment-trapped MXene without the addition of any external agents, this investigation not only increases yield but also enables simple and efficient deposition of Ti₃C₂T_x MXenes on the surface for advanced applications in electronics, energy storage, and sensor technologies.