One-pot hydrothermal synthesis and characterization of 2D MoS ₂ -based heterostructure for enhanced hydrogen evolution reaction

The MoS2 and MXene-based heterostructures were synthesized by a facile one-pot hydrothermal technique and characterized by PXRD, XPS, FE-SEM HRTEM, SAED EDX and electrochemical measurements, viz., LSV, EIS measurement and chronoamperometry. The structural-morphological results of the synthesized materials confirm that ultrathin petal-like MoS₂ nanosheets (d₀₀₂ ≈ 0.61 nm) uniformly coat d-MXene layers (d₀₀₄ ≈ 0.50 nm), evidencing the successful formation of heterostructure. XPS spectra identified Mo4+, Ti3+/Ti4+ and surface groups such as -OH and Ti-O, suggesting strong interfacial bonding and possible TiO2 domain contribution. The EDX analysis confirms the coexistence of Ti, C, Mo and S elements in the 2D heterostructure. Electrochemical measurements demonstrated enhanced HER-activity, with ≈10%–25% improvement in acidic and ≈35%–72% in alkaline medium compared to prior reports, which was attributed to a reduced overpotential, lower Tafel slope and minimized charge transfer resistance. The synergistic effects between MoS₂ and d-MXene components underpin the catalytic enhancement, offering a promising strategy for next-generation electrocatalysts.