<p>Titanium carbide (Ti₃C₂), a two-dimensional material known as MXene, is a promising electrode material for supercapacitors. Herein, MXene was synthesized by etching the Ti₃AlC₂ MAX phase, followed by intercalation with polyethyleneimine (PEI). Additionally, the precursor MoS₂ was injected into MXenes at an early stage. The MXene and MoS₂/MXene@PEI materials were characterized using X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and BET analysis techniques. Several techniques were employed to assess the electrochemical properties of MXene, MoS₂/MXene, and MoS₂/MXene@PEI heterostructures. Based on the results of the electrochemical experiments, it has been demonstrated that the MoS₂/MXene@PEI NCs electrodes have the potential to achieve a maximum specific capacitance of 632&#xa0;F g⁻¹. Additionally, the discharge current density of these electrodes is 1&#xa0;A g⁻¹. Additionally, MoS₂ has been demonstrated to reduce the charge transfer resistance of MoS₂/MXene@PEI, as indicated by the results of electrochemical impedance testing. The electrochemical performance of MoS₂/MXene@PEI NCs was remarkable, particularly in terms of reversibility, cycle stability, and rate performance. The research concludes that MoS₂/MXene@PEI is an excellent candidate for use as an electrode in supercapacitors.</p> Graphical Abstract <p></p>