Facile preparation of Ti₃C₂T_x sheets by selectively etching in a H₂SO₄/H₂O₂ mixture

MXenes and MXene-based composite materials have potential applications in a wide range of areas due to their unique physical and chemical characteristics. At present, it is still a major challenge to develop a simple, safe, and efficient route to prepare MXenes without using fluorinated etchants. Herein, we design a facile method to prepare Ti₃C₂T_x MXene sheets by selectively etching Ti₃AlC₂ powders in an aqueous diluted H₂SO₄ solution with H₂O₂ as an oxidant. In a system of H₂SO₄ and H₂O₂, an aqueous H₂SO₄ solution with a concentration of 6 mol/L is a strongly acidic medium with no volatility, and 30% H₂O₂ acts as a strong green oxidizer without harmful by-products. The experimental process is safe and convenient to conduct in a beaker under a water bath of 40°C. The etching process can be completed in 1 h under the air atmosphere conditions. The experimental results confirmed that the etched Ti₃AlC₂ powders can be successfully separated into Ti₃C₂T_x nanosheets under ultrasound treatment without using any intercalation agent. The relevant etching mechanism is may be attributed to the synergy effect of H₂SO₄ and H₂O₂, which triggers sequential selective etching of Al layers from the Ti₃AlC₂ phase. It may provide a new green way to prepare MXene-based materials without using toxic HF or HF-containing etchants.