MXenes and composite belonging to the family of 2D material offer promising applications in the field of energy storage owing to their unique structure, metallic conductivity, and surface tunability. Herein, we have reported a simple approach for the synthesis of pristine Mo₂TIC₂T_x and Ni-intercalated Mo₂TiC₂T_x free-standing film. The prepared films were characterized using X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) for the electrochemical measurements. A binder-free, flexible, and chemically stable structure of synthesized Ni-Mo₂TiC₂T_x films shows a high gravimetric capacitance of 682 F g⁻¹, compared to the pristine Mo₂TiC₂T_x free-standing film which exhibited a gravimetric capacitance of 310 F g⁻¹ at 5 mV s⁻¹. Synthesized Ni-Mo₂TiC₂T_x electrode exhibited an energy density of 59.77 W h kg⁻¹ and power density of 0.4 kW kg⁻¹ along with long-term cyclic ability and stability of over 5000 cycles which makes it a good candidate material for energy storage devices.