The effect of the method of preparation of Re-Mo-containing catalysts based on a ZSM-5 zeolite on their physicochemical properties, activity and stability in the course of non-oxidative conversion of methane into aromatic hydrocarbons was studied. The structure and morphology of resulted catalysts were investigated using X-ray structural analysis and high-resolution Z-contrast imaging in scanning transmission electron microscopy (HAADF-STEM). It was found out that catalysts prepared by solid-phase synthesis using nanoscale Mo and Re powders exhibit the highest activity and stability in the course of methane dehydroaromatization.