Two-dimensional (2D) MXenes sheet-like micro-structures have attracted attention as an effective electrochemical energy storage material due to their efficient electrolyte/cation interfacial charge transports inside the 2D sheets which results in ultrahigh rate capability and high volumetric capacitance. In this article, Ti3C2TxMXene is prepared by a combination of ball milling and chemical etching from Ti3AlC2powder. The effects of ball milling and etching duration on the physiochemical properties are also explored, as well as the electrochemical performance of as-prepared Ti3C2MXene. The electrochemical performances of 6 h mechanochemically treated and 12 h chemically etched MXene (BM-12H) exhibit an electric double layer capacitance behavior with an enhanced specific capacitance of 146.3 F g−1compared to 24 and 48 h treated samples. Moreover, 5000-cycle stability tested sample’s (BM-12H) charge/discharge show increased specific capacitance due to the termination of the -OH group, intercalation of K+ion and transformation to TiO2/Ti3C2hybrid structure in a 3 M KOH electrolyte. Interestingly, a symmetric supercapacitor (SSC) device fabricated in a 1 M LiPF6electrolyte in order to extend the voltage window up to 3 V shows a pseudocapacitance behavior due to Li on interaction/de-intercalation. In addition, the SSC shows an excellent energy and power density of 138.33 W h kg−1and 1500 W kg−1, respectively. The ball milling pre-treated MXene exhibited an excellent performance and stability due to the increased interlayer distance between the MXene sheets and intercalation and deintercalation of Li+ions.