Ti3C2Tx–Fe3O4–carbon nanotube composites were prepared for electrochemical energy storage in the negative electrodes of supercapacitors. The electrodes show a remarkably high areal capacitance of 6.59 F cm−2 in a neutral Na2SO4 electrolyte, which was obtained by the development of advanced nanofabrication strategies and due to the synergistic effect of the individual components. Enhanced capacitance was achieved using the in-situ synthesis method for the Fe3O4 nanoparticles. The superparamagnetic behavior of the Fe3O4 nanoparticles facilitated the fabrication of electrodes with a reduced binder content. Good mixing of the components was achieved using a celestine blue co-dispersant, which adsorbed on the inorganic components and carbon nanotubes and facilitated their co-dispersion and mixing. The capacitive behavior was optimized by the variation of the electrode composition and mass loading in a range of 30–45 mg cm−2. An asymmetric device was proposed and fabricated, which contained a Ti3C2Tx–Fe3O4–carbon nanotube negative electrode and a polypyrrole–carbon nanotube positive electrode for operation in an Na2SO4 electrolyte. The asymmetric supercapacitor device demonstrated high areal capacitance and excellent power-density characteristics in an enlarged voltage window of 1.6 V. This investigation opens a new avenue for the synthesis and design of MXene-based asymmetric supercapacitors for future energy storage devices.
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