Design and application of active sites in g-C3N4-based photocatalysts

doi:10.1016/j.jmst.2020.03.033

Abstract

Abstract:

With the development in photocatalysis field, photocatalysts have received increasing attention due to their important role in environmental pollution and energy crisis. As a nonmetallic photocatalyst, graphitic carbon nitride (g-C₃N₄) has been widely recognized because of its excellent optical properties, low cost, and environment friendliness. In the g-C₃N₄ intrinsic frameworks, carbon atom tends to be the reducing active site, while nitrogen atom tends to be the oxidizing active site and reducing active site according to the difference of electronegativity. However, the quantity and quality of these active sites are affected by many factors, including C-N covalent bonds, surface properties, etc. Active sites play an important role in photocatalysis; however, this role is not detailed in most reports. In this review, we proposed the following possible mechanisms of active sites in improving the photocatalytic activity of traditional g-C₃N₄ based on its intrinsic: morphology regulation, carrier migration, surface active treatment, and substrate adsorption. The following factors affecting the active sites of g-C₃N₄, including basal engineering and hybrid engineering, were also investigated. The roles of these active sites in improving the photocatalytic activity of g-C₃N₄-based photocatalytic materials, including morphology regulation, surface treatment, heteroatom doping, and interfacial interaction, were also expounded. Current challenges and future development of g-C₃N₄-based photocatalysts that are rich in active surface sites were also discussed. This review provides an in-depth understanding of g-C₃N₄-based photocatalysts.

Key words: Graphitic carbon nitride, Active sites, Photocatalyst, Solar fuels

Yang Li, Xin Li, Huaiwu Zhang, Jiajie Fan, Quanjun Xiang. Design and application of active sites in g-C₃N₄-based photocatalysts[J]. J. Mater. Sci. Technol., 2020, 56: 69-88.

Figures/Tables 22

Fig. 1. Distribution of reduction and oxidation active sites in the g-C3N4 frameworks at the molecular level.

Fig. 2. Schematic illustration of the factors affecting the quantity and quality of active sites on g-C3N4. Two main factors influence the active sites of g-C3N4: basal engineering, including morphology regulation and surface treatment; and hybrid engineering, including heteroatom doping and hybridization.

Fig. 3. Schematic illustration of the factors affecting the quantity and quality of active sites over g-C3N4 by basal engineering. The effect of basal engineering on the active site of g-C3N4 is mainly reflected in morphology control and surface treatment during the modification of precursors and traditional g-C3N4.

Fig. 4. TEM images of (a-c) the sample obtained from the precursor calcined at 500℃ (DCN-550) and (d-f) the sample obtained from the precursor calcined at 500℃ (DCN-600) samples; (g) Schematic illustration for the synthetic process of nanocage-like carbon nitride; (h) Schematic diagram of the possible photocatalytic H2 mechanism for nanocage-like structured g-C3N4 [74].

Fig. 5. (a) The molecular structures of g-C3N4 (CN0) and the modified g-C3N4 (CNx); Dependence of the H2 production rate on the content of (b) carbon and (c) nitrogen atoms, (d) C/N atomic ratio and (e) oxygen atoms [75].

Fig. 6. SEM images of (a) Melamine-derived PCN (CNB) samples, (b) Porous oxygen-rich PCN nanosheets (CNPS-O) samples and (c) -NH2 groups on the PCN nanosheets (CNPS-NH2) samples; (d and e) TEM images; (f) AFM image and (g) EDS elemental mapping images of CNPS-NH2 samples; (h) Schematic illustration of the preparation process of CNPS-NH2 samples [87].

Fig. 7. SEM images of (a) CN-0 (g-C3N4 nanosheets), (b) CN-1 (g-C3N4 nanosheets were prepared via plasma treatment in H2 atmosphere at 500℃), (c) CN-2 (g-C3N4 nanosheets were prepared via plasma treatment in H2 atmosphere at room temperature); TEM images of (d) CN-0, (e) CN-1, (f) CN-2; (g) Photocatalytic H2 evolution mechanism diagram of hydrogenated g-C3N4, hydrogenated g-C3N4 with hydrophilic group C-N-H, defect state, and exfoliated morphology obtained after g-C3N4 nanosheet treatment with hydrogen plasma at room temperature. Hydrophilic groups C-N-H enhanced the adsorption capacity of g-C3N4 for water molecules [92].

Fig. 8. SEM images of the as-obtained (a, b) LiCl-CN-4 h samples and the cross section (c) of the hollow tubes; TEM images of (d, e) the synthesized products and the high-resolution TEM image (f) of the hexagonal structures on the sample surface; (g) XPS spectra of LiCl-CN-4 h before and after Pb(II) adsorption; (h) Pb L3-edge EXAFS spectra for samples after Pb(II) treatment [105].

Fig. 9. (a) Illustration of the synthesis of IrO2/GCN; (b) XRD patterns of 40-IG (IrO2/GCN containing 40 wt.% IrO2), IrO2 NPs, and GCN; (c) TEM image of 40-IG. (d, e) HRTEM of 40-IG. (f) The corresponding FFT patterns of (e) [121].

Table 1 A brief summary of improved the active sites of g-C3N4.

Improvement strategy	Photocatalysts	Preparation methods	Active sites	Application	Photocatalytic activity	Refs.
Increase specific surface area	g-C₃N₄ nanorods	Supramolecular assembly	Edges, nitrogen defects	Photocatalytic H₂ production	118.5 μmol h^-1 6.8%@420 nm	[40]
Increase specific surface area	g-C₃N₄ nanosheets	Thermal treatment	Edges, defective sites	Photocatalytic H₂ production	1233.5 μmol h^-1 g^-1	[53]
Increase specific surface area	g-C₃N₄ microspheres	Hard template	Edges	Photocatalytic H₂ production	5785 μmol h^-1 g^-1	[127]
Surface activity treatment	Soluble g-C₃N₄ nanosheets	Hydrothermal treatment	Edges, hydrophilic groups	Photocatalytic H₂ production	17.98 μmol h^-1	[72]
Surface activity treatment	g-C₃N₄ nanosheets	Molecular assembly	Edges, cyano groups, adsorption sites	Photocatalytic benzaldehyde degradation	-	[73]
Surface activity treatment	g-C₃N₄ nanosheets	Plasma treatment	Edges, hydrophilic groups	Photocatalytic H₂ production	1230 μmol h^-1 g^-1 7.3%@420 nm	[48]
Heteroatoms doping	Crystallized LiCl-intercalated g-C₃N₄	Molten salts method	Edges, Cl and Li atoms, adsorption sites	Photocatalytic heavy metal removal	-	[50]
Heteroatoms doping	S-doped g-C₃N₄	Supramolecular assembly	Edges, S atoms, adsorption sites	Photocatalytic heavy metal removal	-	[79]
Interfacial interaction	Graphene-supported 1D nano-arrays of crystalline g-C₃N₄	Molten salts method	Edges, heterojunction, adsorption sites	Photocatalytic CO₂ reduction	12.63 μmol h^-1 g^-1 0.254%@420 nm (The total quantum yield of CO₂ conversion)	[57]
Interfacial interaction	ZnFe₂O₄/ g-C₃N₄	Thermal treatment	Edges, heterojunction	Photocatalytic H₂ production	200.77 μmol h^-1 g^-1	[85]

Fig. 10. Possible mechanisms of active sites in improving the photocatalytic activity of g-C3N4. Morphology regulation and surface activity treatment can directly increase the number of active sites by exposing additional edges and introducing active substances. Carrier migration and substrate adsorption can indirectly increase the number of active sites in the photocatalysis by increasing the concentration of carriers and substrates.

Fig. 11. (a) The formation process of the g-C3N4 nanotubes; (b) Photocatalytic hydrogen evolution with 10 vol% triethanolamine aqueous solution, 3 wt.% Pt as a co-catalyst and 0.015 g photocatalysts under visible light irradiation; (c) wavelength dependence of external quantum efficiency for g-C3N4 nanotubes [77].

Fig. 12. (a) SEM image of the few-layer C3N4, (b) TEM image of the few-layer C3N4, (c) Magnified TEM image of the few-layer C3N4. (d, e) AFM image and corresponding height profiles along the white line in d of the few-layer C3N4. (f) XRD patterns of bulk C3N4, microtube C3N4 and few-layer C3N4; (g) Charge transfer and separation mechanism of few-layer and bulk C3N4 under visible light irradiation [165].

Fig. 13. (a) Schematic of the synthesis of nanosheet-assembled hierarchical flower-like g-C3N4 (CMN); (b) Mechanism diagram of CMN for the photoreduction of CO2. Compared with g-C3N4, the CMN exhibited improved photoreduction capability for CO2 due to its high specific surface area and enhanced adsorption capacity for CO2 [32].

Fig. 14. (a) Graphical illustration for the synthesis of soluble g-C3N4 (SCN) nanosheets by a first hydrothermal delamination and its following vacuum freezing-drying technology and the microstructure formation of the soluble g-C3N4 (SCN) nanosheets; (b, c) Typical TEM and (d, e) AFM images of soluble g-C3N4 (SCN) nanosheets; (f) The photocatalytic H2-production activities of various samples: (f: a) SCN, (f: b) bulk g-C3N4, (f: c) SCN/g-C3N4 (0.1 wt.%), (f: d) SCN/g-C3N4 (0.3 wt.%), (f: e) SCN/g-C3N4 (0.5 wt.%), (f: f) SCN/g-C3N4 (0.8 wt.%), (f: g) SCN/g-C3N4 (1 wt.%), (f: h) SCN/g-C3N4 (5 wt.%) and (f: I) SCN/g-C3N4 (10 wt.%); (g) Photocatalytic cycling test of typical (g: b) g-C3N4 and (g: d) SCN/g-C3N4 (0.3 wt.%) photocatalysts [169].

Fig. 15. (a) Proposed formation process of cyano group introduction sample; (b) Proposed reaction mechanism for benzylamine oxidation. Reaction conditions: benzylamine (0.2 mmol), acetonitrile (2 mL), catalyst (10 mg), O2 (1 atm), 60 °C, LED light; The optimized structures and the corresponding bond lengths of (c) pure (g-C3N4)-Pb(II) and (d-i) (S-g-C3N4)-Pb(II) complexes [54,170].

Fig. 16. (a) Effect of w/w% Fe dopant on the performance of the g-C3N4 (gCN). Conditions: pH = natural (3-4), [Catalyst] =0.1 g L-1, [Peroxymonosulfate (PMS)] = 0.4 g L-1 and [Acid orange 7 (AO7)] = 8.5 mg L-1; (b) Proposed mechanism of PMS activation by g-C3N4 with 2.5 w/w% Fe3+ dopant (gCN-Fe3) for AO7 removal [176].

Fig. 17. (a-d) Optimized atomic configurations of oxygen intermediates (OO* and *OOH) adsorbed on NiCo2S4@N-GN (a, b) and NiCo2S4@g-C3N4 (c, d); (e) Calculated d-band positions of metallic Ni and Co sites and (f) free energy diagram of ORR and OER processes on bare NiCo2S4, NiCo2S4@NGN, and NiCo2S4@g-C3N4 [194].

Fig. 18. Adsorption and activation of NO molecules. Optimized geometric structure of NO molecules adsorption on g-C3N4 (CN) and (BiO)2CO3 nanospheres decorated g-C3N4 hybrid heterostructure (CN-BOC) (a), gray, brown, purple and red and pink spheres stand for C, N, Bi and O atoms, respectively; all lengths are given in ?; Eads stand for the adsorption energy of adsorption molecule; in situ DRIFTS spectra on CN (b) and CN-BOC (c) samples during NO adsorption processes; Adsorption and activation of O2 molecules. DMPO spin-trapping ESR spectra (O·2-) of CN and CN-BOC-4 samples (d); optimized geometric structure of the adsorption of O2 molecules on CN and CN-BOC (e), gray, brown, purple and red and pink spheres stand for C, N, Bi and O atoms, respectively; all lengths are given in ?; Eads stand for the adsorption energy of adsorption molecule [196].

Fig. 19. TEM images of (a, b) ZFO-50 (ZnFe2O4-modified g-C3N4 photocatalysts, where 50 represents the volume of ZnFe2O4 solution), (c) ZFO-100 (ZnFe2O4-modified g-C3N4 photocatalysts, where 100 represents the volume of ZnFe2O4 solution) and (d) ZFO-200 (ZnFe2O4-modified g-C3N4 photocatalysts, where 200 represents the volume of ZnFe2O4 solution) photocatalysts; Inset of (c) is a magnified image of the area in the white square; (e) Schematic of the band structure and charge transfer process in ZnFe2O4/g-C3N4 for photocatalytic hydrogen generation [206].

Fig. 20. (a) Eleven adsorption sites in tri-s-triazine-based g-C3N4 [130]; (b) Optimized adsorption configurations of H2, N2, H2O, CO, CO2 and CH4 on g-C3N4 [212].

Fig. 21. Brief summary of the application of g-C3N4-based photocatalytic materials rich in active sites in the field of photocatalysis. For practical applications, the following four main strategies can be applied to improve the photocatalytic activity of g-C3N4-based photocatalytic materials through active site enhancement: morphology regulation, surface treatment, heteroatom doping, and interfacial interaction.

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Design and application of active sites in g-C₃N₄-based photocatalysts

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