Hydrothermal-Assisted In Situ Intercalation Synthesis of Ti₃C₂T_x MXene in 6 Hours

Area of Science:

• Materials Science
• Nanotechnology
• Chemical Engineering

Background:

• Scalable and time-efficient synthesis of high-quality MXenes remains a challenge.
• Existing methods for Titanium Carbide (Ti3C2Tx) MXene production are often time-consuming and yield-limited.

Purpose of the Study:

• To develop a facile, high-yield, and time-efficient method for synthesizing Ti3C2Tx MXene.
• To achieve in situ intercalation and delamination of MXene sheets.

Main Methods:

• Utilized hydrothermal-assisted etching with a mild etchant system (HCl/LiF) and in situ intercalant (LiCl).
• Employed a closed hydrothermal autoclave for enhanced etchant reactivity and kinetics.
• Leveraged Li+ ions to weaken van der Waals forces for exfoliation.

Main Results:

• Achieved synthesis and delamination of Ti3C2Tx MXene in 6 hours at 90°C.
• Obtained a high yield of 74.2% ± 3.7% delaminated nanosheets with monolayer thickness (1-1.5 nm).
• Characterization confirmed successful Al etching, effective delamination, and surface terminations (-Cl, -F, -O) with high electrical conductivity (7500 S cm⁻¹).

Conclusions:

• The developed single-step methodology offers a scalable and efficient route for MXene synthesis.
• This advancement significantly reduces synthesis time compared to conventional protocols.
• The findings open new avenues for the commercial application of MXene materials.