“…The catalyst activity was found to be influenced by several key factors, including the quantity of active sites in MoS 2 , the presence of sulfur vacancies, and the concentration of active components (Ni–Mo–S and Ni x S y ) within the catalyst. ,, As the hydrothermal treatment temperature increases, the lateral size, the number of stacked layers, and S/Mo atomic ratio of MoS 2 in the catalyst first decrease and then increase (Tables , , and ), reaching a minimum when the hydrothermal treatment temperature is 150 °C, i.e., in the following order: H-NiMo-150–400 < H-NiMo-120–400 < H-NiMo-180–400 < H-NiMo-90–400 < H-NiMo-200–400. The smaller lateral size of MoS 2 and the reduced number of stacked layers are more favorable for the exposed active sites. , Additionally, these factors promote the formation of a higher proportion of Ni–Mo–S and Ni x S y during the calcination process, thereby contributing to the improved activity of the catalyst. , At the same time, the smaller S/Mo ratio indicates the higher number of S vacancies in the catalyst, − which helps to improve the activity of the DBT reaction on the catalyst. Therefore, the order of activity of the DBT reaction on the catalyst is consistent with the results of XRD (Figure and Table ), TEM (Figure and Table ), ERP (Figure ), SEM-EDS (Table ), and XPS (Figure and Table ) characterization.…”