Publication date: 15th December 2025
Ti3AlC2, a typical MAX phase compound, serves as the parent structure of Ti3C2Tx MXenes, the most extensively studied member of the MXene family for diverse applications. Despite the growing interest, most experimental studies on Ti3AlC2 rely on polycrystalline samples, limiting the accurate determination of its intrinsic physical properties. The synthesis of large, high-quality single crystals remains a significant challenge, yet it is essential for probing fundamental electronic, optical, and transport behaviours. In this work, we report the first successful growth of high-quality large Ti3AlC2 single crystals via a TiAl3 flux-assisted approach. The crystals exhibit excellent structural quality, with individual flakes exceeding 1 cm in length and basal-plane surface areas reaching up to ~36 mm2. Hall measurements on individual flakes reveal a high carrier density of ~1021 cm-3, while polarisation-resolved Raman spectra show a nearly circular intensity pattern, indicating optical isotropy within the basal plane. To investigate surface characteristics, scanning tunnelling microscopy was performed on freshly cleaved crystals, revealing non-flat surface topography influenced by cleavage termination. First-principles calculations indicate that cleavage predominantly occurs between Ti–Al layers and reveal distinct surface-dependent band structures and Fermi surfaces. A nearly regular hexagonal Fermi contour corresponds to the Al-terminated surface, while a star-like sixfold modulated contour is associated with the Ti-terminated surface. Chemical etching of these MAX phase crystals yields millimetre-scale Ti3C2Tx flakes, which can be mechanically exfoliated onto chips. Raman spectra exhibit a strong G-band peak at ~1550 cm-1, with no discernible D-band, indicating ultralow-defect sp2-like carbon structures. Two-terminal devices fabricated from these flakes display symmetric I–V characteristics and negligible gate modulation across 2.5 μm channels, confirming metallic behaviour and good electrical contact. This work establishes a scalable route to large Ti3AlC2 single crystals, offering new insights into their intrinsic properties, laying a solid foundation for future MXene-based device technologies.
This work was supported by ERC-CZ program (project LL2101) from the Ministry of Education Youth and Sports (MEYS) and used large infrastructure from the project Advanced Functional Nanorobots (reg. No. CZ.02.1.01/0.0/0.0/15_003/0000444 financed by the EFRR). We also gratefully acknowledge the Czech computer infrastructure Metacentrum provided by the e-INFRA CZ project (ID: 90254), supported by the Ministry of Education, Youth and Sports of the Czech Republic. M.V. further acknowledge the support from the Czech Science Foundation (GACR No. 23-08083M). F.M.O. acknowledges the support from the Czech Science Foundation (GA ČR No. 25-16769S). This work was supported by Ministry of Education Youth and Sports (MEYS), project Advanced Multiscale Materials for Key Enabling Technologies (AMULET) from Programme Johannes Amos Comenius, co-funded by EU (CZ.02.01.01/00/22_008/0004558).
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