Two–dimensional MXene synthesized from MAX phase ceramic has good electrical conductivity, promising to be used as electrodes. In this study, Nb4C3Tx (T = –OH, –F, or =O) MXene and low–entropy (Nb0.8Ti0.05V0.05Zr0.05Ta0.05)4C3Tx (T = –OH, –F, or =O) MXene were prepared by etching Nb4AlC3 and (Nb0.8Ti0.05V0.05Zr0.05Ta0.05)4AlC3 ceramics in the HF acid at 60 °C. By investigating the electrochemical properties of lithium batteries, it was found that the Nb4C3Tx and (Nb0.8Ti0.05V0.05Zr0.05Ta0.05)4C3Tx could provide the specific capacities of 163.7 mAh·g−1 and 130 mAh·g−1 after 50 cycles at a current density of 0.1 A·g−1, respectively, and maintain the coulombic efficiency close to 100%, good for the utilization of electrodes in lithium batteries.