Controllable Synthesis of Porous 1T-MoS₂ with Large Surface Area via Continuous Hydrothermal System

1T-phase MoS2, a versatile two-dimensional transition-metal dichalcogenide, is typically synthesized using a one-pot hydrothermal method. However, inadequate control of the sulfurization, reduction, and crystallization processes in the autoclave leads to multilayer 1T-MoS2 with high crystallinity, a small surface area, and few defects. Considering the aforementioned issues, a two-stage microreactor continuous hydrothermal flow synthesis (CHFS) system coupled with accurate control and rapid processing is used to prepare 1T-MoS2 with abundant voids and a large surface area under 250 °C and 4.0–4.5 MPa. And density functional theory calculations reveal that nitrogenous species, acting as reductants and electron donors, lower the energy of 1T-MoS2 by intercalation and surface adsorption, facilitating its swift synthesis within the presulfurization stage for 10 min and reduction stage for 24 min. The precisely controlled synthesis of porous 1T-MoS2, originating from prenucleation clusters, results in a large surface area of 201.5 m2/g, concentrated mesopores of 2–5 nm, and a pore volume of 0.58 cm3/g. Moreover, a significant transformation from the 1T to the 2H phase is prevented by rapid cooling downstream of the CHFS system.