In this study, a simple hydrothermal method has been developedto prepare Ti3C2Tx from Ti3AlC2 as a high-performance electrodematerial for supercapacitors. This method is environmentallyfriendly and has a low level of danger. The morphology andstructure of the Ti3C2Tx can be controlled by hydrothermalreaction time, temperature and NH4F amounts. The preparedTi3C2Tx was characterized by X-ray diffraction, field emissionscanning electron microscopy, Raman spectroscopy, X-rayphotoelectron spectroscopy and Brunauer-Emmet-Teller. Theresults show that the prepared Ti3C2Tx is terminated by O, OH,and F groups. The electrochemical properties of the Ti3C2Txsample exhibit specific capacitance up to 141 Fcm−3 in 3 MKOH aqueous electrolyte, and even after 1000 cycles, nosignificant degradation of the volumetric capacitance wasobserved. These results indicate that the Ti3C2Tx materialprepared by this hydrothermal method can be used in highperformance supercapacitors.