Quasi-one-dimensional (quasi-1D) materials enjoy growing interest due to their unusual physical properties and promise for miniature electronic devices. However, the mechanical exfoliation of quasi-1D materials into thin flakes and nanoribbons received considerably less attention from researchers than the exfoliation of conventional layered crystals. In this study, we investigated the micromechanical exfoliation of representative quasi-1D crystals, TiS3 whiskers, and demonstrate that they typically split into narrow nanoribbons with very smooth, straight edges and clear signatures of 1D TiS3 chains. Theoretical calculations show that the energies required for breaking weak interactions between the two-dimensional (2D) layers and between 1D chains within the layers are comparable and, in turn, are considerably lower than those required for breaking the covalent bonds within the chains. We also emulated macroscopic exfoliation experiments on the nanoscale by applying a local shear force to TiS3 crystals in different crystallographic directions using a tip of an atomic force microscopy (AFM) probe. In the AFM experiments, it was possible to slide the 2D TiS3 layers relative to each other as well as to remove selected 1D chains from the layers. We systematically studied the exfoliated TiS3 crystals by Raman spectroscopy and identified the Raman peaks whose spectral positions were most dependent on the crystals’ thickness. These results could be used to distinguish between TiS3 crystals with thickness ranging from one to about seven monolayers. The conclusions established in this study for the exfoliated TiS3 crystals can be extended to a variety of transition metal trichalcogenide materials as well as other quasi-1D crystals. The possibility of exfoliation of TiS3 into narrow (few-nm wide) crystals with smooth edges could be important for the future realization of miniature device channels with reduced edge scattering of charge carriers.
2D carbides and nitrides (MXenes) are widely recognized for their exceptional promise for numerous applications. However, physical property measurements of their individual monolayers remain very limited despite their importance for revealing the intrinsic physical properties of MXenes. The first mechanical and electrical measurements of individual single‐layer flakes of Nb4C3Tx MXene, which are prepared via an improved synthetic method are reported. Characterization of field‐effect transistor devices based on individual single‐layer Nb4C3Tx flakes shows an electrical conductivity of 1024 ± 165 S cm−1, which is two orders of magnitude higher than the previously reported values for bulk Nb4C3Tx assemblies, and an electron mobility of 0.41 ± 0.27 cm2 V−1 s−1. Atomic force microscopy nanoindentation measurements of monolayer Nb4C3Tx membranes yield an effective Young's modulus of 386 ± 13 GPa, assuming a membrane thickness of 1.26 nm. This is the highest value reported for nanoindentation measurements of solution‐processable 2D materials, revealing the potential of Nb4C3Tx as a primary component for various mechanical applications. Finally, the agreement between the mechanical properties of 2D Nb4C3Tx MXene and cubic NbC suggests that the extensive experimental data on bulk carbides could be useful for identifying new MXenes with improved functional characteristics.
MXenes, two-dimensional transition metal carbides or nitrides, have recently shown great promise for gas sensing applications. We demonstrate that the sensitivity of intrinsically metallic Ti3C2T x MXene can be considerably improved via its partial oxidation in air at 350 °C. The annealed films of MXene sheets remain electrically conductive, while their decoration with semiconducting TiO2 considerably improves their chemiresistive response to organic analytes at low-ppm concentrations in dry air, which was used to emulate practical sensing environments. We demonstrate that partially oxidized MXene has a faster and a qualitatively different sensor response to volatile analytes compared to pristine Ti3C2T x . We fabricated multisensor arrays of partially oxidized Ti3C2T x MXene devices and demonstrate that in addition to their high sensitivity they enable a selective recognition of analytes of nearly the same chemical nature, such as low molecular weight alcohols. We investigated the oxidation behavior of Ti3C2T x in air in a wide temperature range and discuss the mechanism of sensor response of partially oxidized MXene films, which is qualitatively different from that of pristine Ti3C2T x .
The interfaces of layered trichalcogenide TiS3(001), with metals Au and Pt, were examined using X-ray photoemission spectroscopy. In spite of the fact that both Au and Pt are large work function metals, no evidence of Schottky barrier formation was found with this n-type semiconductor. Two- and four-terminal field-effect transistor measurements performed on exfoliated few-nm-thick TiS3 crystals using pure Au contacts indicate that Au forms an Ohmic contact on TiS3(001), with negligible contact resistance. The absence of appreciable Schottky barrier formation is attributed to strong interactions with sulfur at the metal-semiconductor interface.
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