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Although preparation conditions are known to affect the morphology and catalytic performance of hydrothermally synthesized MoS2, the influence of pH remains unclear. Herein, unsupported MoS2 was prepared from ammonium tetrathiomolybdate (ATTM) by a hydrothermal reaction at various pH values under a reaction pressure of 2 MPa. The physical and chemical properties of the MoS2 samples were characterized, and the catalytic performance for CO methanation was examined. With increasing pH, the morphology of the MoS2 particles transformed from aggregates of irregular grain-like particles to flower-like particles through the agglomeration of fine mesoporous nanoflakes. Hydrothermal synthesis at a pH of 9.5 increased the MoS2 crystallinity by enhancing the stacking of the (0 0 2) lattice plane. The MoS2 samples prepared at pH 7.0 and 9.5 showed increased CO conversion during methanation, which was associated with a low concentration of Mo5+ species and the presence of surface sulfate species. Thus, a high pH during catalyst preparation may promote the complete decomposition of ATTM to MoS2 and the formation of sulfur vacancies, which can facilitate methanation.

Morphology and Catalytic Performance of MoS2 Hydrothermally Synthesized at Various pH Values