Electrochemical Investigation of Supercritical Fluid Synthesized Novel Heterostructure MXene/MoS₂/PANI

We report a supercritical fluid (SCF)-assisted synthesis of a tightly integrated MXene/MoS₂/PANI ternary heterostructure for high-performance supercapacitor applications. The SCF route enables rapid nucleation, controlled crystallization, and intimate interfacial coupling between Ti₃C₂T_x MXene and MoS₂ nanosheets, followed by uniform in situ polymerization of polyaniline (PANI) to construct a hierarchical conductive network. This rationally engineered architecture synergistically combines electric double-layer capacitance and pseudocapacitance while minimizing charge-transfer resistance and enhancing ion transport kinetics. The optimized composite delivers a high specific capacitance of ∼325 F g⁻¹ along with excellent cycling durability over 10,000 cycles, exhibiting progressive capacitance activation attributed to improved electrolyte accessibility and interfacial conductivity. The study introduces a time-efficient and structurally controlled strategy for fabricating MXene-based ternary heterostructures and establishes a scalable pathway toward advanced hybrid electrode materials for next-generation energy storage systems.