In this paper, the effects of etching temperature and concentrations of hydrochloric acid (HCl) on the exfoliating process and the electrochemical performance of LIBs were systematically explored. The transformation from Ti3AlC2 to Ti3C2 was analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and Raman spectra. The suitable conditions of preparing Ti3C2 MXene though HCl and lithium fluoride (LiF) were obtained. Besides, the in-situ oxidation conditions of Ti3C2 during the etching process were studied. The TiO2/Ti3C2 was beneficial to improve the specific capacity from 125[Formula: see text]mAh[Formula: see text]g[Formula: see text] to 150[Formula: see text]mAh[Formula: see text]g[Formula: see text] at 1 C.