Raman spectroscopy is one of the most useful tools for the analysis of twodimensional (2D) materials. While MXenes are a very large family of 2D transition metal carbides and nitrides, there have been just a few Raman studies of materials from this family. Here, we report on a systematic study of the most widely used and most important MXene to date: Ti 3 C 2 T x . By synthesizing material using different methods, we show that Raman spectra of Ti 3 C 2 T x are affected not only by the composition and surface groups but also by intercalated species and stacking. Due to a plasmonic peak of Ti 3 C 2 T x around 785 nm, resonant conditions are achieved, enabling us to observe an extra peak at ∼120 cm −1 , when excited with a red diode laser. We report differences in Raman spectra collected from single flakes of Ti 3 C 2 T x , colloidal solutions, and multilayer films. Lastly, we show how an undesirable photoluminescent background could serve as evidence of material degradation, which leads to the formation of defective titania and amorphous carbon. This study shows how Raman spectroscopy can be used for the characterization of important emerging 2D materials: MXenes.
Figure S1. (a) Blocks of Ti3AlC2 (top) and Al-Ti3AlC2 (bottom), (b) mass loss during the washing of Al-Ti3AlC2 with HCl, (c) image of the purple filtrate from the acid washing process, (d) Al-Ti3AlC2 particles after acid washing using HCl, (e) higher magnification of (d).
MXenes are a family of two-dimensional (2D) transition metal carbides, nitrides, and carbonitrides with a general formula of M n+1 X n T x , in which two, three, or four atomic layers of a transition metal (M: Ti, Nb, V, Cr, Mo, Ta, etc.) are interleaved with layers of C and/or N (shown as X), and T x represents surface termination groups such as −OH, O, and −F. Here, we report the scalable synthesis and characterization of a MXene with five atomic layers of transition metals (Mo 4 VC 4 T x ), by synthesizing its Mo 4 VAlC 4 MAX phase precursor that contains no other MAX phase impurities. These phases display twinning at their central M layers which is not present in any other known MAX phases or MXenes. Transmission electron microscopy and X-ray diffraction were used to examine the structure of both phases. Energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, Raman spectroscopy, and highresolution scanning transmission electron microscopy with energy-dispersive X-ray spectroscopy were used to study the composition of these materials. Density functional theory calculations indicate that other five transition metal-layer MAX phases (M′ 4 M″AlC 4 ) may be possible, where M′ and M″ are two different transition metals. The predicted existence of additional Al-containing MAX phases suggests that more M 5 C 4 T x MXenes can be synthesized. Additionally, we characterized the optical, electronic, and thermal properties of Mo 4 VC 4 T x . This study demonstrates the existence of an additional subfamily of M 5 X 4 T x MXenes as well as a twinned structure, allowing for a wider range of 2D structures and compositions for more control over properties, which could lead to many different applications.
MXene/carbon composite electrodes with high loadings of MXene were prepared via electrospinning. These flexible and free-standing electrodes exhibit high areal capacitance relative to pure carbon nanofibers and MXene-coated fibers and textiles.
Noble metal (gold
or silver) nanoparticles or patterned films are
typically used as substrates for surface-enhanced Raman spectroscopy
(SERS). Two-dimensional (2D) carbides and nitrides (MXenes) exhibit
unique electronic and optical properties, including metallic conductivity
and plasmon resonance in the visible or near-infrared range, making
them promising candidates for a wide variety of applications. Herein,
we show that 2D titanium carbide, Ti3C2Tx, enhances Raman signal from organic dyes on a substrate and
in solution. As a proof of concept, MXene SERS substrates were manufactured
by spray-coating and used to detect several common dyes, with calculated
enhancement factors reaching ∼106. Titanium carbide
MXene demonstrates SERS effect in aqueous colloidal solutions, suggesting
the potential for biomedical or environmental applications, where
MXene can selectively enhance positively charged molecules.
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