High-crystalline g-C3N4 photocatalysts: Synthesis, structure modulation, and H2-evolution application

doi:10.1016/S1872-2067(23)64491-2

Abstract

Abstract:

Graphitic carbon nitride (g-C₃N₄) has received extensive attention in the photocatalytic field because of its low cost, nontoxicity, suitable bandgap structure, and high physicochemical stability among diverse photocatalysts. However, traditional g-C₃N₄ materials prepared by the high-temperature calcination of various organic precursors generally exhibit poor crystallinity and possess numerous internal and surface defects, leading to the rapid recombination of photo-excited charges. Constructing a highly crystalline g-C₃N₄ photocatalyst, as opposed to the traditional poorly crystalline g-C₃N₄, effectively reduces internal and surface defects, facilitating efficient separation and rapid transfer of photoexcited charges. As a result, the photocatalytic performance is significantly enhanced. In this review, recent progress in highly crystalline g-C₃N₄ photocatalysts is summarized. The microstructural characteristics of highly crystalline g-C₃N₄ photocatalysts are discussed in detail. Synthetic methods for highly crystalline g-C₃N₄, such as the salt-assisted (multicomponent salt and single-component salt), template, two-step calcination method, microwave-assisted method, and others, are meticulously presented. Additionally, various modification strategies for highly crystalline g-C₃N₄, encompassing bandgap engineering, heterojunction construction, and co-catalyst modification, are presented. Subsequently, a detailed description of the photocatalytic H₂-evolution applications of highly crystalline g-C₃N₄ materials is given. Lastly, the paper concludes with a discussion on the outlook for highly crystalline g-C₃N₄ photocatalysts, aiming to offer novel insights into the design of highly efficient crystalline g-C₃N₄ photocatalysts.

Key words: Photocatalysis, High-crystalline g-C₃N₄, Synthesis, Modification, H₂ evolution

Binbin Zhao, Wei Zhong, Feng Chen, Ping Wang, Chuanbiao Bie, Huogen Yu. High-crystalline g-C₃N₄ photocatalysts: Synthesis, structure modulation, and H₂-evolution application[J]. Chinese Journal of Catalysis, 2023, 52: 127-143.

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Figures/Tables 14

Fig. 1. Brief description of crystalline g-C3N4.

Fig. 2. Schematic diagram for (a) the synthesis of g-C3N4 using various precursors and (b) the polymerization pathway of traditional poor-crystalline g-C3N4 by calcining the dicyandiamide precursor.

Fig. 3. Graphic illustration for the microstructures corresponding to charge separation and transfer of traditional poor-crystalline g-C3N4 (a) and high-crystalline g-C3N4 (b).

Fig. 4. (a) XRD patterns of traditional bulk g-C3N4 nanosheets (BCNNs), traditional crystalline g-C3N4 nanosheets (CCNNs), and g-C3N4 nanosheets with an in-plane highly ordered structure (PCNNs-IHO). (b) HRTEM image of PCNNs-IHO. (a,b) Reprinted with permission from Ref. [84]. Copyright 2021, John Wiley and Sons. (c) XRD patterns of CCN0 (1), CCN0.03 (2), CCN0.1 (3), and CCN0.2 (4). (d) TEM image of CCN0.1. Reprinted with permission from Ref. [85]. Copyright 2021, John Wiley and Sons.

Table 1 The synthesis of high-crystalline g-C3N4.

Photocatalyst	Precursor	Synthetic method	Synthetic temperature (°C)	Specific surface area (m² g^-1)	Ref.
g-CN1	melamine	salt-assisted method (KCl/LiCl)	550	125	[86]
NDCCN	urea	salt-assisted method (Na₂CO₃/Li₂CO₃)	550	—	[87]
KPCN	melamine	salt-assisted method (KBr)	580	10	[55]
PC-CN0.1	dicyandiamide	salt-assisted method (NaHCO₃)	550	15.34	[49]
HC-CN0.05	dicyandiamide	salt-assisted method (CH₃COONa)	550	13.6	[83]
CNRs	cyanamide	template method (anodic alumni oxide)	600	25	[88]
HcPCN	urea	template method (poly(dimethylsiloxane))	550	93.8	[89]
U350-670	urea	two-step calcination method	670	122.9	[90]
HP550	dicyandiamide	high pressure	550	6.2	[91]

Fig. 5. (a) XRD patterns and Gaussian fitting results of pure g-C3N4 (bulk g-CN) and (g-CN1). (b) XRD patterns of g-CN1 before and after photocatalytic H2-evolution tests. (c,d) HRTEM images of g-CN1. Reprinted with permission from Ref. [86]. Copyright 2016, American Chemical Society. PL (e) and time-resolved fluorescence decay spectra (f) of pure g-C3N4 (CN) and crystalline g-C3N4 (NDCCN). Reprinted with permission from Ref. [87]. Copyright 2019, Elsevier.

Fig. 6. (a) Schematic illustration of the synthesis of KPCN. (b) XRD patterns of PCN and KPCN. (c,d) HRTEM images of KPCN. Reprinted with permission from Ref. [55]. Copyright 2019, John Wiley and Sons.

Fig. 7. (a,b) XRD patterns of bulk g-C3N4 (1), PC-CN0 (2), PC-CN0.05 (3), PC-CN0.1 (4), and PC-CN0.2 (5). (c) TEM image of PC-CN0.1. Reprinted with permission from Ref. [49]. Copyright 2020, Elsevier. Graphic diagram for the synthesis of traditionally disordered g-C3N4 (d) and high-yield and crystalline g-C3N4 (e). Reprinted with permission from Ref. [83]. Copyright 2023, Elsevier.

Fig. 8. (a) Synthetic diagram for the synthesis of CNRs through AAO template strategy. (1) AAO template (gray) filled with cyanamide (white). (2) Heating. (3) Removal of template to obtain CNRs (yellow). Reprinted with permission from Ref. [88]. Copyright 2011, American Chemical Society. (b) HcPCN via soft-template-induced method. (c) XRD patterns of PCN and HcPCN, (d-f) HRTEM images of HcPCN (the scale bar is 2 nm). Reprinted with permission from Ref. [89]. Copyright 2021, Royal Society of Chemistry.

Fig. 9. (a) Graphic illustration of Ux-670. (b) Photographs of various samples. SEM (c), TEM (d) and HRTEM (e-g) images of U350-670. (h) XRD patterns of pure g-C3N4 (U550) and Ux-670. Reprinted with permission from Ref. [90]. Copyright 2022, Elsevier.

Fig. 10. (a) XRD patterns of pure g-C3N4 (CN550) and MCN1000-18. (b) HRTEM image of MCN1000-18. (c) XRD patterns of various g-C3N4 photocatalysts prepared using the microwave-assisted strategy with melamine (MM), cyanamide (MC), and thiourea (MT). Reprinted with permission from Ref. [103]. Copyright 2014, Royal Society of Chemistry. (d) XRD patterns of various samples. Steady-state PL spectra (e), TR-PL spectra (f), and transient photocurrent responses (g) of CN540 and CN16. Reprinted with permission from Ref. [104]. Copyright 2016, John Wiley and Sons.

Fig. 11. Schematic diagram for the synthesis of g-C3N4 under normal pressure (a) and high pressure (b). Reprinted with permission from Ref. [91]. Copyright 2018, Elsevier. Cs-corrected HRTEM (c) and the corresponding Fourier transformation images (d) of CCN. Reprinted with permission from Ref. [105]. Copyright 2019, John Wiley and Sons.

Fig. 12. (a) Synthetic illustration of S-CNNTs. (b) UV-vis spectra, and the corresponding Kubelka-Munk plots (inset). Reprinted with permission from Ref. [113]. Copyright 2022, Elsevier. (c) Graphical diagram for the synthesis of Zn-CCN. (d) Kubelka-Munk function spectra of various samples. Reprinted with permission from Ref. [114]. Copyright 2019, Elsevier. UV-vis spectra (e) and band gaps (f) calculated using the Kubelka-Munk (K-M) equation. Reprinted with permission from Ref. [116]. Copyright 2022, Elsevier.

Table 2 Photocatalytic H2-evolution activity of high-crystalline g-C3N4.

Photocatalyst	Photocatalyst amount/ Co-catalyst	Sacrificial agent	Light source	Activity (μmol g^-1 h^-1)	Quantum efficiency	Ref.
PC-CN0.1	50 mg/1.0 wt% Pt	10 vol% lactic acid	Four 3-W 420-nm LEDs	1010.0 (H₂)	1.56% (420 nm)	[49]
CPCN	50 mg/1.0 wt% Pt	10 vol% triethanolamine	300 W Xe lamp (λ ≥ 420 nm)	1356.0 (H₂)	11.4% (420 nm)	[56]
GCN-HC	50 mg/3.0 wt% Pt	10 vol% triethanolamine	300 W Xe lamp (λ > 420 nm)	339.4 (H₂)	3.8% (420 nm)	[72]
CCN0.1	50 mg/1.0 wt% Pt	10 vol% lactic acid	Four 3-W 420-nm lamp	758.8 (H₂)	1.17% (420 nm)	[85]
g-CN1	50 mg/3.0 wt% Pt	10 vol% triethanolamine	300 W Xe Lamp (λ > 420 nm)	1472.0 (H₂)	50.7% (405 nm)	[86]
CCN₅₅₀	50 mg/3.0 wt% Pt	10 vol% methanol	300W Xe lamp (λ > 420 nm)	660.0 (H₂)	6.8% (420 nm)	[92]
3DBC-C₃N₄-N	25 mg/3.0 wt% Pt	10 vol% triethanolamine	300 W Xe lamp (λ > 420 nm)	10600.0 (H₂)	26% (420 nm)	[93]
MC-CN	100 mg/3.0 wt% H₂PtCl₆	10 vol% triethanolamine	300 W Xe lamp (λ > 420 nm)	181.51 (H₂)	1.58% (420 nm)	[99]
HC-CN	100 mg/3.0 wt% Pt	10 vol% triethanolamine	300 W Xe Lamp (λ > 400 nm)	808.5 (H₂)	6.17% (420 nm)	[102]
HcPCN	20 mg/3.0 wt% Pt	10 vol% triethanolamine	300 W Xe lamp (λ ≥ 420 nm)	9520.0 (H₂)	11.0% (420 nm)	[89]
U350-670	10 mg/1.1 wt% Pt	10 vol% triethanolamine	300 W Xe lamp (λ > 420 nm)	14665.0 (H₂)	—	[90]
MCN_1000-18	10 mg/0.5 wt% Pt	15 vol% triethanolamine	300 W Xe lamp (λ > 420 nm)	2000.0 (H₂)	5.6% (420 nm)	[103]
HP550	50 mg/1.0 wt% Pt	10 vol% triethanolamine	350 W Xe lamp (λ > 420 nm)	772.40 (H₂)	1.6% (420 nm)	[91]
KCCN2	50 mg/3.0 wt% Pt	20 vol% triethanolamine	300 W Xe lamp (λ > 420 nm)	5238.0 (H₂)	25.7% (420 nm)	[107]
CCNNSs	50 mg/3.0 wt% Pt	10 vol% triethanolamine	300 W Xe lamp (AM 1.5G)	9577.6 (H₂)	9.01% (420 nm)	[144]
CC-CN6	50 mg/1.0 wt% Pt	10 vol% methanol	Four 3-W 420-nm LEDs	5906.0 (H₂)	12.61% (420 nm)	[145]
530 LOP-CN	30 mg/3.0 % Pt	10 vol% triethanolamine	300 W Xe lamp (λ ≥ 400 nm)	1790.0 (H₂)	3.3% (420 nm)	[146]
cMel-5	50 mg/3.0 wt% Pt	10 vol% triethanolamine	200 W Xe lamp (λ ≥ 420 nm)	6480.0 (H₂)	20.7% (420 nm)	[147]
CCNNSs	50 mg/3.0 wt% Pt	10 vol% methanol	Visible light (λ > 420 nm)	1060.0 (H₂)	8.57% (420 nm)	[148]
HCN-25 min	50 mg/0.2 wt% Pt	10 vol% triethanolamine	300 W Xe Lamp (λ > 420 nm)	1631.6 (H₂)	2.1 % (420 nm)	[149]
MTCN-6	40 mg/1.0 wt% Pt	20 vol% triethanolamine	300 W Xe lamp (λ > 420 nm)	1511.2 (H₂)	3.9% (420 nm)	[150]
PCN_mp-30	10 mg/0.5 wt% Pt	10 vol% triethanolamine	300 W Xe lamp (λ ≥ 420 nm)	6170.0 (H₂)	1.47% (420 nm)	[151]
15% ReS₂/CCN	20 mg/3.0 wt% H₂PtCl₆·6H₂O	10 vol% triethanolamine	300 W Xe lamp	3460.0 (H₂)	1.26% (420 nm)	[118]
HCN/Ti₃C₂ (HCNT20)	20 mg/1.0 wt% Pt	10 vol% triethanolamine	Four 3-W 420-nm LEDs	4225.0 (H₂)	14.6% (420 nm)	[152]
CCN/LaOCl-1.5	50 mg/0.5 wt% Pt/ 0.2 wt% CoO_X	—	300 W Xe lamp (λ > 300 nm)	1212.0 (H₂) 562.0 (O₂)	1.13% (400 nm)	[120]
g-C₃N₄-D2	20 mg/1.0 wt% Pt/ 3.0 wt% Co₃O₄	—	300 W Xe lamp (AM1.5G)	49.60 (H₂) 24.71 (O₂)	—	[123]

Table 2 Photocatalytic H2-evolution activity of high-crystalline g-C3N4.

Photocatalyst	Photocatalyst amount/ Co-catalyst	Sacrificial agent	Light source	Activity (μmol g^-1 h^-1)	Quantum efficiency	Ref.
PC-CN0.1	50 mg/1.0 wt% Pt	10 vol% lactic acid	Four 3-W 420-nm LEDs	1010.0 (H₂)	1.56% (420 nm)	[49]
CPCN	50 mg/1.0 wt% Pt	10 vol% triethanolamine	300 W Xe lamp (λ ≥ 420 nm)	1356.0 (H₂)	11.4% (420 nm)	[56]
GCN-HC	50 mg/3.0 wt% Pt	10 vol% triethanolamine	300 W Xe lamp (λ > 420 nm)	339.4 (H₂)	3.8% (420 nm)	[72]
CCN0.1	50 mg/1.0 wt% Pt	10 vol% lactic acid	Four 3-W 420-nm lamp	758.8 (H₂)	1.17% (420 nm)	[85]
g-CN1	50 mg/3.0 wt% Pt	10 vol% triethanolamine	300 W Xe Lamp (λ > 420 nm)	1472.0 (H₂)	50.7% (405 nm)	[86]
CCN₅₅₀	50 mg/3.0 wt% Pt	10 vol% methanol	300W Xe lamp (λ > 420 nm)	660.0 (H₂)	6.8% (420 nm)	[92]
3DBC-C₃N₄-N	25 mg/3.0 wt% Pt	10 vol% triethanolamine	300 W Xe lamp (λ > 420 nm)	10600.0 (H₂)	26% (420 nm)	[93]
MC-CN	100 mg/3.0 wt% H₂PtCl₆	10 vol% triethanolamine	300 W Xe lamp (λ > 420 nm)	181.51 (H₂)	1.58% (420 nm)	[99]
HC-CN	100 mg/3.0 wt% Pt	10 vol% triethanolamine	300 W Xe Lamp (λ > 400 nm)	808.5 (H₂)	6.17% (420 nm)	[102]
HcPCN	20 mg/3.0 wt% Pt	10 vol% triethanolamine	300 W Xe lamp (λ ≥ 420 nm)	9520.0 (H₂)	11.0% (420 nm)	[89]
U350-670	10 mg/1.1 wt% Pt	10 vol% triethanolamine	300 W Xe lamp (λ > 420 nm)	14665.0 (H₂)	—	[90]
MCN_1000-18	10 mg/0.5 wt% Pt	15 vol% triethanolamine	300 W Xe lamp (λ > 420 nm)	2000.0 (H₂)	5.6% (420 nm)	[103]
HP550	50 mg/1.0 wt% Pt	10 vol% triethanolamine	350 W Xe lamp (λ > 420 nm)	772.40 (H₂)	1.6% (420 nm)	[91]
KCCN2	50 mg/3.0 wt% Pt	20 vol% triethanolamine	300 W Xe lamp (λ > 420 nm)	5238.0 (H₂)	25.7% (420 nm)	[107]
CCNNSs	50 mg/3.0 wt% Pt	10 vol% triethanolamine	300 W Xe lamp (AM 1.5G)	9577.6 (H₂)	9.01% (420 nm)	[144]
CC-CN6	50 mg/1.0 wt% Pt	10 vol% methanol	Four 3-W 420-nm LEDs	5906.0 (H₂)	12.61% (420 nm)	[145]
530 LOP-CN	30 mg/3.0 % Pt	10 vol% triethanolamine	300 W Xe lamp (λ ≥ 400 nm)	1790.0 (H₂)	3.3% (420 nm)	[146]
cMel-5	50 mg/3.0 wt% Pt	10 vol% triethanolamine	200 W Xe lamp (λ ≥ 420 nm)	6480.0 (H₂)	20.7% (420 nm)	[147]
CCNNSs	50 mg/3.0 wt% Pt	10 vol% methanol	Visible light (λ > 420 nm)	1060.0 (H₂)	8.57% (420 nm)	[148]
HCN-25 min	50 mg/0.2 wt% Pt	10 vol% triethanolamine	300 W Xe Lamp (λ > 420 nm)	1631.6 (H₂)	2.1 % (420 nm)	[149]
MTCN-6	40 mg/1.0 wt% Pt	20 vol% triethanolamine	300 W Xe lamp (λ > 420 nm)	1511.2 (H₂)	3.9% (420 nm)	[150]
PCN_mp-30	10 mg/0.5 wt% Pt	10 vol% triethanolamine	300 W Xe lamp (λ ≥ 420 nm)	6170.0 (H₂)	1.47% (420 nm)	[151]
15% ReS₂/CCN	20 mg/3.0 wt% H₂PtCl₆·6H₂O	10 vol% triethanolamine	300 W Xe lamp	3460.0 (H₂)	1.26% (420 nm)	[118]
HCN/Ti₃C₂ (HCNT20)	20 mg/1.0 wt% Pt	10 vol% triethanolamine	Four 3-W 420-nm LEDs	4225.0 (H₂)	14.6% (420 nm)	[152]
CCN/LaOCl-1.5	50 mg/0.5 wt% Pt/ 0.2 wt% CoO_X	—	300 W Xe lamp (λ > 300 nm)	1212.0 (H₂) 562.0 (O₂)	1.13% (400 nm)	[120]
g-C₃N₄-D2	20 mg/1.0 wt% Pt/ 3.0 wt% Co₃O₄	—	300 W Xe lamp (AM1.5G)	49.60 (H₂) 24.71 (O₂)	—	[123]

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High-crystalline g-C₃N₄ photocatalysts: Synthesis, structure modulation, and H₂-evolution application

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