Supercritical CO₂‐Assisted Reverse‐Micelle‐Induced Solution‐Phase Fabrication of Two‐Dimensional Metallic 1T‐MoS₂ and 1T‐WS₂

Abstract Metallic 1T phase molybdenum disulfide (MoS₂) and tungsten disulfide (WS₂) are both expected to exhibit promising catalytic activity, but they are highly unstable in nature. Exploring an efficient route to fabricate a high ratio of 1T‐MoS₂ and 1T‐WS₂ is highly desirable. Herein, for the first time, we report a two‐step process for synthesizing stable two‐dimensional (2D) metallic 1T phase MS₂ nanosheets in the reverse‐micelle‐induced emulsion microenvironment with the assistance of supercritical CO₂ (SC CO₂). TEM, Raman and XPS characterizations demonstrate that the as‐prepared MoS₂ nanosheets consist of 1T‐ and 2H‐phase, and the content of 1T phase is more than 90 %. The obtained 1T‐MoS₂ exhibits excellent stability and good activity for the hydrogen evolution reaction. A potential of ≈330 mV at a current density of 10 mA cm⁻² and a Tafel slope of 70 mV per decade were obtained for 1T‐MoS₂. TEM and UV/Vis spectrum characterizations also testify that we have obtained 1T‐WS₂. Thus this strategy utilizing a reverse‐micelle‐induced method for fabrication of 2D 1T‐MS₂ can widen the potential applications in photoelectrocatalysis and photoelectronic devices.