AbstractIn the present study, we are able to synthesize flakes of the 3R‐polytypes of MoS2 and WS2 from sodium molybdate and sodium tungstate in the presence of H2S gas by solid‐state reaction. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy, X‐ray photoelectron spectroscopy (XPS), and X‐ray diffraction are utilized to characterize the morphology, structure, and chemical composition of the 3R‐MoS2 and 3R‐WS2 flakes. The electrocatalytic and photocatalytic activities of 3R‐MoS2 and 3R‐WS2 flakes have been measured in hydrogen evolution reactions.
