Two-dimensional Ti2CTx MXene nanosheets were prepared by the selective etching of Al layer from Ti2AlC MAX phase using HF treatment. The MXene sheets retained the hexagonal symmetry of the parent Ti2AlC MAX phase. Effect of the post-etch annealing ambient (Ar, N2, N2/H2 and Air) on the structure and electrochemical properties of the MXene nanosheets was investigated in detail. After annealing in Air, the MXene sheets exhibited variations in structure, morphology and electrochemical properties as compared to HF treated MAX phase. In contrast, samples annealed in Ar, N2 and N2/H2 ambient retained their original morphology. However, a significant improvement in the supercapacitor performance is observed upon heat treatment in Ar, N2 and N2/H2 ambients. When used in symmetric two-electrode configuration, the MXene sample annealed in N2/H2 atmosphere exhibited the best capacitive performance with specific capacitance value (51 F/g at 1A/g) and high rate performance (86%). This improvement in the electrochemical performance of annealed samples is attributed to highest carbon content, and lowest fluorine content on the surface of the sample upon annealing, while retaining the original 2D layered morphology, and providing maximum access of aqueous electrolyte to the electrodes.