Controllable Synthesis\nof Porous 1T-MoS<sub>2</sub> with Large Surface Area via Continuous\nHydrothermal System

1T-phase MoS<sub>2</sub>, a versatile two-dimensional\ntransition-metal\ndichalcogenide, is typically synthesized using a one-pot hydrothermal\nmethod. However, inadequate control of the sulfurization, reduction,\nand crystallization processes in the autoclave leads to multilayer\n1T-MoS<sub>2</sub> with high crystallinity, a small surface area,\nand few defects. Considering the aforementioned issues, a two-stage\nmicroreactor continuous hydrothermal flow synthesis (CHFS) system\ncoupled with accurate control and rapid processing is used to prepare\n1T-MoS<sub>2</sub> with abundant voids and a large surface area under\n250 °C and 4.0–4.5 MPa. And density functional theory\ncalculations reveal that nitrogenous species, acting as reductants\nand electron donors, lower the energy of 1T-MoS<sub>2</sub> by intercalation\nand surface adsorption, facilitating its swift synthesis within the\npresulfurization stage for 10 min and reduction stage for 24 min.\nThe precisely controlled synthesis of porous 1T-MoS<sub>2</sub>, originating\nfrom prenucleation clusters, results in a large surface area of 201.5\nm<sup>2</sup>/g, concentrated mesopores of 2–5 nm, and a pore\nvolume of 0.58 cm<sup>3</sup>/g. Moreover, a significant transformation\nfrom the 1T to the 2H phase is prevented by rapid cooling downstream\nof the CHFS system.