Two-dimensional MXenes attract great interest due to their unique physical and chemical properties. Ti₃C₂T_x MXene is synthesized by ultrasonic assisted etching. The resulted microstructures are characterized and compared with those Ti₃C₂T_x samples synthesized via magnetically stirring etching, by X-ray diffractom-eter, N₂ adsorption and desorption, scanning electron microscope(SEM) and transmission electron microscope(TEM). The results demonstrate that ultrasonic assisted etching can further reduce the lamellar thickness of Ti₃C₂T_x and increase the atomic layer spacing, comparing with the method of magnetically stirring etching. A gradual dissolution is observed in the same Al atomic layers during etching. The particles with several tens of nanometers in size are frequently formed in contact with the surface of Ti₃C₂T_x. These nano-particles are determined to be hexagonal AlF₃ with space group of R3ˉ. A gradual change from crystalline form to amorphous structure is also detected for hexagonal AlF₃ with prolonged etching time.