Photogenerated carriers transfer and separation from the substance itself to produce spatial isolated electron-hole pairs is crucial for the utilization of composite photocatalysts in the field of photocatalytic hydrogen (H2) evolution. Herein, novel oxygen-doped porous graphitic carbon nitride (g-C3N4) micro-sheets decorated with Ag2MoO4 have been fabricated by a facile calcination method followed by in situ deposition strategy. The physicochemical properties of the obtained Ag2MoO4/OC3N4 composites were characterized via SEM, TEM, EDS, XRD, N2 adsorption-desorption, XPS, UV–vis DRS, PL, transient photocurrent response, and EIS, as well as DFT calculation. In addition, the effects of Ag2MoO4 content, type of scavengers, pH value of reaction solution and dosage of scavenger on photocatalytic H2 production were investigated. The results show that the modification of ammonium acetate thermal polymerization with urea could enhance the porosity of g-C3N4 and its specific surface area. The Ag2MoO4 nanoparticles are highly dispersed on the OC3N4 surface, reducing the charge transfer resistance at their interfaces. The OC3N4 photocatalyst achieves H2 yield of 8629.11 μmol/g over 2 h, which is about 1.46 times higher than that of C3N4. The H2 production amount over the optimal Ag2MoO4/OC3N4 composite photocatalyst (50 mg) is further enhanced to 16619 μmol/g, which is 1.93 and 180 times higher than that of OC3N4 and Ag2MoO4, respectively. The S-scheme charge transfer mechanism of Ag2MoO4/OC3N4 is proposed based on the DFT calculation. This work provides a facile and easy strategy to develop g–C3N4–based photocatalysts through adjusting chemical composition and photocatalytic properties.
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