Studying of 2D Titanium Carbide Structure by Raman Spectroscopy after Heat Treatment in Argon and Hydrogen Atmospheres

Abstract

Herein we show the effect of heat treatment of two dimensional layered titanium carbide structure (Ti 3 C 2 T x ), so called MXene. As prepared MXene has functional groups -OH, -F, -Cl. In order to remove the functional groups we heat treated the MXene in Ar (with 0.01% O 2 ) and H 2 (with 0.01% H 2 O) atmospheres. We discovered the significant decrease in the amount of functional groups (-F and -Cl) and increase in the -O content, which refers to the oxidation of the material. Also we determined the optimal regime for Raman spectroscopy in order to avoid any changes in the structure of the material. We revealed that titanium carbide changes its structure at 700 °C and 900 °C into two different titanium dioxide modifications like rutile and anatase in Ar (with 0.01% O 2 ) atmosphere. Also there are small changes occurred in Ti 3 C 2 Tx structure and formation of amorphous carbon after 700 °C treatment in H 2 (with 0.01% H 2 O) atmosphere and formation of TiO 2 (rutile) at 900 °C. Energydispersive X-ray spectroscopy (EDX) revealed the reduction of functional groups at 700 °C in both atmospheres and total disappearance of -F and -Cl and increasing the oxygen at 900 °C. The huge increase of oxygen by atomic percent, can be explained by the initial oxygen content in argon and hydrogen gases.

Investigation and Optimization of Mxene functionalized Mesoporous Titania Films as Efficient Photoelectrodes

“…More prominently, there is an intense peak at around 151 cm -1 . The high intensity of this peak could be related to the increased laser power, leading to the formation of oxidized Ti3C2 [54,69]. All these facts are well supported by various literature and signify successful synthesis of Ti3C2Tx.…”

Investigation and Optimization of Mxene Functionalized Mesoporous Titania Films as Efficient Photoelectrodes

“…More prominently, there was an intense peak at around 151 cm −1 . The high intensity of this peak could be due to the increased laser power, leading to the formation of oxidized Ti 3 C 2 [ 53 , 68 ]. These results are supported by various reports in the literature, and can be taken to signify the successful synthesis of Ti 3 C 2 T x .…”

Electronic and Optical Properties of 2D Transition Metal Carbides and Nitrides (MXenes)

“…Experimentally, MXenes' surface terminations are still poorly understood despite use of different characterization techniques for their analysis and monitoring including, X‐ray photoelectron spectroscopy (XPS), nuclear magnetic resonance spectroscopy (NMR), neutron scattering, X‐ray atomic pair distribution function (X‐ray PDF), scanning transmission electron microscopy (STEM), electron energy loss spectroscopy (EELS), Raman spectroscopy, and thermogravimetric analysis coupled with mass spectroscopy (TGA‐MS) . This is because MXenes surface is fairly complex and highly sensitive to the nature of transition metal on the surface, etching, delaminating, and storage conditions.…”

“…Although Raman spectroscopy has been extensively employed to study vibrational properties of MAX phases, there are only a few studies that reported Raman spectra of MXenes . It was shown that the frequencies and vibrational modes are strongly influenced by surface terminations .…”