Synthesis and characterization of Ti ₃ C ₂ T _<i>x</i> MXene with preserved MAX phase structure via optimized delamination

MXenes, an emerging family of 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 overall yield. In this study, we investigate the recovery of sediment-trapped Ti₃C₂T_x MXene in the form of a film through a modified conventional method. The hexagonal MAX phase&nbsp;Ti₃AlC₂&nbsp;was synthesized via pressureless sintering at&nbsp;1450°C for 3 hours&nbsp;under flowing argon, followed by selective etching using a mixture of&nbsp;HF/HCl&nbsp;and subsequent washing with&nbsp;LiCl solution. The delaminated MXene was prepared in two distinct forms: (1) A&nbsp;colloidal solution&nbsp;with an average flake size of&nbsp;~700 nm, suitable for solution-based applications. (2) Thin layer of Hexagonal flakes&nbsp;(average size&nbsp;~10 μm) deposited on a glass substrate via transfer method (single dip-coating). XRD analysis&nbsp;corroborated the structural integrity of MXene. SEM imaging&nbsp;of MXene showed the preservation of the hexagonal morphology inherited from the parent MAX phase, while&nbsp;FTIR and Raman spectroscopy&nbsp;identified hydrophilic surface functional groups (-O&nbsp;and&nbsp;-OH).&nbsp;By efficiently recovering sediment-trapped Mxene without the addition of any external agents, this investigation not only&nbsp;enhances yield&nbsp;but also enables &nbsp;simple and efficient deposition of Ti₃C₂T_x&nbsp;MXenes on the suface for advanced applications in&nbsp;electronics, energy storage, and sensor technologies.