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S-scheme heterojunction of In 2 O 3 /H 1.5 CN/2Au was prepared by hydrothermal, acidizing and calcination methods. The two-dimensional thin layer H 1.5 CN avoided the aggregation of In 2 O 3 and completed the S-scheme charge transfer with In 2 O 3. Moreover, Au not only enhanced the visible light absorption capacity of composites but also provided more active sites for CO 2 reduction. [Display omitted] • S-scheme heterojunction of In 2 O 3 /H 1.5 CN/2Au achieve CO 2 photocatalytic conversion to CO and CH 4. • The enhanced photocatalytic activity results from effective interfacial charge migration and separation and increased active sites. • The LSPR effect of Au improves the utilization of visible light. The construction of S-scheme heterojunction is of great significance for the photocatalytic reduction of CO 2. Here, we prepared two-dimensional (2D) ultra-thin g-C 3 N 4 by acidifying the carbon nitride precursor, and used In 2 O 3 to construct a S-scheme heterojunction with 2D g-C 3 N 4 , and finally In 2 O 3 /H 1.5 CN was modified with Au nanoparticles. The physicochemical properties of the prepared materials were studied by SEM/TEM, XPS, DRS, PL and photochemical test. Meantime, the S-scheme charge transfer mechanism was demonstrated by UPS and ESR. As a result, on the one hand, S-scheme heterojunction accelerated the transfer of electrons on the CB of In 2 O 3 to the VB of g-C 3 N 4 , avoided the recombination of photon-generated carrier. On the other hand, Au, as an effective cocatalyst, promoted photoinduced electron transfer and provided more active sites for CO 2 reduction and the local surface plasmon resonance phenomenon caused by Au NPs enhanced the visible light absorption capacity of the composite material. Moreover, 2D thin layer of g-C 3 N 4 played a carrier effect to disperse In 2 O 3 cube. Therefore, In 2 O 3 /H 1.5 CN/2Au had stable CO 2 reduction products, and the yields of CO/CH 4 reached 141.24/77.05 μmol/g. [ABSTRACT FROM AUTHOR]

The 3D hierarchical structure of CdS/Ni-MOF inhibits the agglomeration of CdS, improve light harvesting, increase active surface area, reaction sites, promote charge transfer and separation, which greatly improves the efficiency of CO 2 conversion. However, when the CdS is overloaded and its hierarchical structure is destroyed, the heterostructure plays a major role in improving the performance. Based on the above results, we propose the preliminary mechanism of 20%-CdS/Ni-MOF photocatalytic reduction of CO 2. Firstly, under UV–Vis illumination, Ni-MOF and CdS are excited to produce electrons (e−) and holes (h+). Then, because of the tight interface contact, the e- excited by Ni-MOF could be transferred to CdS with more positive CB, and CdS as the active site could reduce CO 2 to CO more effectively. At the same time, the h+ in the VB of Ni-MOF and CdS participate in the oxidation reaction to produce O 2 and H 2 O 2 , which achieving the elimination of holes. Such charge separation and transfer of the electron-hole pairs facilitate enhanced photocatalytic activity. [Display omitted] • The 3D hierarchical heterostructure was synthesized by a simple strategy. • 20%-CdS/Ni-MOF showed excellent performance in the vapor–solid reaction system. • The hierarchical structure and heterostructure of CdS/Ni-MOF play a synergistic role. Fabricating the hierarchical heterostructure is efficient way for enhancing CO 2 conversion of semiconductor photocatalysts. Herein, a simple strategy has been employed to prepare several 3D hierarchical CdS/Ni-MOF heterostructure photocatalysts, and the selective photoreduction of CO 2 to CO under simulated sunlight in the gas–solid phase reactor. Among the prepared photocatalysts, 20%-CdS/Ni-MOF shows the best CO yield, which was 16 times and 7 times that of Ni-MOF and CdS, respectively. By controlling the morphology of the catalyst, we found that the significant improvement in photocatalytic activity can be ascribed to the synergistic effect of heterostructure in CdS/Ni-MOF and its unique hierarchical structure, which can improve the efficiency of charge transmission and provides abundant active sites, etc. Finally, the preliminary photocatalytic mechanism was discussed by in situ FTIR and liquid ultraviolet spectrophotometer. [ABSTRACT FROM AUTHOR]