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The atomically thin nanosheets of graphitic carbon nitride (g-C 3 N 4 ) with mesopores have been successfully exfoliated with supercritical CO 2 (scCO 2 ). The thickness of the assynthesized samples could be directly tailored by simply regulating the scCO 2 pressure. The obtained bilayer mesoporous g-C 3 N 4 nanosheets doped with monatomic Co through a microwaveassisted approach havve been employed as single-atom catalysts to enhance the photocatalytic hydrogen evolution performance. The as-prepared Co/P/CN-sc sample exhibited a boosted H 2 production performance due to its unique structural advantages by exposing more active sites and facilitating the separation of charge carriers. Based on X-ray photoelectron spectroscopy, steady-state and time-resolved photoluminescence spectroscopy, X-ray absorption fine structure measurement, and density functional theory (DFT) calculations, a possible mechanism has been proposed. The work shows a new perspective for designing an inexpensive photocatalyst with a unique structure through a facile and green approach for photocatalytic hydrogen evolution.

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A well-ordered hierarchically micromesoporous carbon has been successfully fabricated in a reverse microemulsion system via a heated evaporation-induced self-assembly (HISA) method. An additional heat accelerates the rate of the solvent evaporation for accomplishing the self-assembly process of the surfactant. Interestingly, it only takes about 7 min for the preparation of polymer by using this facile HISA. The tedious prepolymerization process between phenol and resorcinol can be saved by directly mixing them together in the system, and the subsequent thermal consolidation process at 100 °C for about 24 h in the usual method can also be eliminated. Meanwhile, evaporation-induced self-assembly (EISA) and hydrothermal (HT) approaches have also been employed to prepare the porous carbon in F127/MMA reverse microemulsion. Hierarchically porous carbon materials prepared by using reverse microemulsion as the electrode of supercapacitors exhibit an excellent performance in electrochemical application. Hierarchically porous organosilica materials and Si/C nanocomposites have also been prepared in the reverse microemulsion by utilizing HISA, which indicates the universality of this versatile approach. This general approach can provide a facile and sustainable route to construct the architecture of hierarchically porous materials for various applications.