Green and Controllable Preparation of Graphene/MoS ₂ Nanocomposites with Different Morphologies

ABSTRACT A novel preparation method based on a hydroxyl radical generation apparatus was developed for the continuous production of graphene/MoS 2 composites. By using different electrolytes—NaCl, CTAB, SDS, SDBS, and Na 2 SO 4 —composites with distinct and controllable morphologies were obtained. XRD analysis confirmed the successful exfoliation of MoS 2 and graphite and the formation of stable composites, while SEM and TEM revealed morphology variations depending on the electrolyte. XPS measurements showed that the CTAB‐prepared sample contained a rarely observed C–Mo bond. Electrical conductivity tests and linear sweep voltammetry (LSV) indicated that the CTAB‐prepared composite achieved a 2330% increase in conductivity and a substantially reduced HER overpotential (η 10 ≈ −0.63 V vs. RHE) compared to bulk MoS 2 . This study demonstrates a green, efficient, and scalable route for producing graphene/MoS 2 composites with tunable morphology, significantly enhanced electrical conductivity, and improved electrocatalytic performance. The approach also holds promise for the large‐scale fabrication of high‐performance graphene/MoS 2 ‐based materials for conductive and electrocatalytic applications.