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The development of Ti 3 C 2 T x -based high performance electrode materials has been proposed to meet the practical requirements of supercapacitors. In this study, transition metal complexes decorated MXene Ti 3 C 2 T x hybrid electrode nanocomposites are fabricated by a facile polyvinylpyrrolidone (PVP)-assisted liquid impregnation strategy (abbreviated as PVP-M/akTi 3 C 2 T x (M = Mn or Ni)). The intercalated Ti 3 C 2 T x is observed to possess a distinct layered structure wrapped by cloud-like Mn/Ni complexes, which form a heterojunction to help the charge transfer of PVP-M/akTi 3 C 2 T x in aqueous electrolytes such as KOH, LiOH, Li 2 SO 4 and Na 2 SO 4. The electrochemical performance of pristine and modified MXene in the above electrolytes changes greatly, mainly due to the difference of electrolytes' ionic radius and conductivity. Typically, the PVP-Mn/akTi 3 C 2 T x and PVP-Ni/akTi 3 C 2 T x nanocomposites exhibit superior specific capacitances of 154.6 F g−1 and 167.65 F g−1 at 0.3 A g−1 current density in 1 M KOH electrolyte, respectively. Moreover, due to the complete progressive activation process of the electrode materials, the specific capacitance further increased by 25% and 56% after thousands of cycles, and finally kept at 95.70% and 96.21% of the maximum value respectively, indicating the superstability of these electrode materials. This study provides a new perspective to tailor the microstructures of Ti 3 C 2 T x electrode materials for energy applications. [ABSTRACT FROM AUTHOR]