两步焙烧法制备大比表面积和结晶性增强超薄g-C3N4纳米片及其高效光催化产H2O2

doi:10.3866/PKU.WHXB202406019

Abstract

Abstract:

The generation of hydrogen peroxide (H₂O₂) from water and oxygen redox reaction by photocatalysis has acquired increasing attention owing to its green and clean properties. Aiming at the low intrinsic photocatalytic activity of carbon nitride (g-C₃N₄), here, an ultrathin g-C₃N₄ nanosheet photocatalyst with a large surface area and enhanced crystallinity was fabricated by a two-step thermal polymerization technique. The calcination parameters showed a significant impact on the structural properties and catalytic performance of g-C₃N₄. The remarkable H₂O₂ yield (3177.0 µmol·g^-1·h^-1) of CN-T-1 (by two-step calcination, 1 ℃·min^-1 optimal heating rate) was 3.7 times that (858.6 µmol·g^-1·h^-1) of CN-O-1 (by one-step calcination, 1 ℃·min^-1 heating rate) and higher than those of pure g-C₃N₄ in literature. Most of the H₂O₂ yield for CN-T-1 remained after five cycles, showing good stability. The enhanced catalytic performance of CN-T-1 than CN-O-1 is owing to its larger specific surface area, enhanced crystallinity, higher oxygen adsorption ability and photogenerated carrier separation efficiency, longer lifetime of carriers, and slightly larger bandgap (3.07 eV, +0.26 eV bigger than CN-O-1) with more positive valence band position owing to ultrathin layers. The •O₂^- radicals were verified to be the primary active species. A two-step single electron ORR pathway (O₂ + e^- → •O₂^- → H₂O₂) was confirmed for H₂O₂ production over CN-T-1.

Key words: Photocatalytic, H₂O₂ production, g-C₃N₄ nanosheet, photocatalytic mechanism

Heng Chen, Longhui Nie, Kai Xu, Yiqiong Yang, Caihong Fang. Remarkable Photocatalytic H₂O₂ Production Efficiency over Ultrathin g-C₃N₄ Nanosheet with Large Surface Area and Enhanced Crystallinity by Two-Step Calcination[J]. Acta Phys. -Chim. Sin. 2024, 40(11), 2406019. doi: 10.3866/PKU.WHXB202406019

Figures/Tables 13

Fig 1

Fig 2

Fig 3

Table 1

Fig 4

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Fig 6

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Fig 9

Table 2

Contrast of catalytic performance for H2O2 production over the catalysts reported in the literature and this work in the presence of sacrificial agents."

Catalyst	Sacrificial agent	Catalyst dosage	Light source	H₂O₂ yield	Ref.
CN-T-1	ethanol	0.2 mg·mL⁻¹	150 W high-pressure sodium lamp	635.4 µmol·L⁻¹ (1 h) or 3177.0 µmol·g⁻¹·h⁻¹	This work
g-C₃N₄	ethanol	0.4 mg·mL⁻¹	300 W Xe lamp λ > 420 nm	30.59 µmol·L⁻¹ (1 h)	1
g-C₃N₄	glucose	0.25 mg·mL⁻¹	λ = 385 nm LED 80 mW cm⁻²	66 µmol·L⁻¹ (1 h)	15
CN	isopropyl alcohol	0.5 mg·mL⁻¹	300 W Xe lamp λ ≥ 420 nm	50.5 µmol·L⁻¹ (1 h)	17
CN-HP	isopropyl alcohol	0.5 mg·mL⁻¹	300 W Xe lamp λ > 420 nm	81.6 µmol·L⁻¹ (40 min)	27
m-CNNP	isopropyl alcohol	1 mg·mL⁻¹	400 nm ≤ λ ≤ 700 nm	43.07 µmol·L⁻¹ (4 h)	28
BCN	isopropyl alcohol	1 mg·mL⁻¹	300 W Xe lamp λ > 420 nm	223.76 µmol·g⁻¹·h⁻¹	29
CN	isopropyl alcohol	0.2 mg·mL⁻¹	300 W Xe lamp 76 mW cm⁻²	1520 µmol·g⁻¹·h⁻¹	31
CN	ethanol	0.6 mg·mL⁻¹	300 W Xe lamp	171.6 µmol·L⁻¹ (1.5 h)	33
CN	ethanol	0.4 mg·mL⁻¹	300 W Xe lamp λ > 370 nm	403 µmol·L⁻¹ (1 h)	37
CN	isopropyl alcohol	0.5 mg·mL⁻¹	300 W Xe lamp λ > 420 nm	54 µmol·g⁻¹·h⁻¹	38
CN	ethanol	1 mg·mL⁻¹	300 W Xe lamp λ > 420 nm	998 µmol·L⁻¹ (4 h)	39
Bulk CN	ethanol	1 mg·mL⁻¹	300 W Xe lamp λ > 420 nm	49.79 µmol·L⁻¹ (1 h)	48
CN	ethanol	1 mg·mL⁻¹	Blue LED light	83.76 µmol·L⁻¹ (1 h)	53
CN1	ethanol	1 mg·mL⁻¹	300 W Xe arc lamp λ > 420 nm	310 µmol·L⁻¹ (1 h)	56
CN2	ethanol	1 mg·mL⁻¹	300 W Xe arc lamp λ > 420 nm	470 µmol·L⁻¹ (1 h)	56
g-C₃N₄	isopropyl alcohol	1 mg·mL⁻¹	300 W Xe lamp	485 µmol·L⁻¹ (3 h)	58
CNNP	isopropyl alcohol	0.5 mg·mL⁻¹	400 nm ≤ λ ≤ 700 nm 43.2 mW cm⁻²	34 µmol·L⁻¹ (1 h)	62
g-C₃N₄	isopropyl alcohol	0.4 mg·mL⁻¹	300 W Xe arc lamp AM 1.5	99 µmol·g⁻¹·h⁻¹	67
g-C₃N₄	isopropyl alcohol	1 mg·mL⁻¹	300 W Xe lamp λ > 420 nm	22.21 µmol·L⁻¹ (1 h)	69
CN	isopropyl alcohol	1 mg·mL⁻¹	300 W Xe lamp λ > 420 nm	102 µmol·L⁻¹ (1 h)	75

Table 2

Fig 10

Fig 11

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Sample	S_BET/(m²·g⁻¹)	d/(nm)	V/(cm³·g⁻¹)
CN-O-1	22.8	17.7	0.13
CN-T-1	237.9	13.2	0.82
CN-T-5	218.7	11.9	0.61
CN-T-10	190.4	11.3	0.52

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Remarkable Photocatalytic H₂O₂ Production Efficiency over Ultrathin g-C₃N₄ Nanosheet with Large Surface Area and Enhanced Crystallinity by Two-Step Calcination

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Remarkable Photocatalytic H2O2 Production Efficiency over Ultrathin g-C3N4 Nanosheet with Large Surface Area and Enhanced Crystallinity by Two-Step Calcination

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Remarkable Photocatalytic H₂O₂ Production Efficiency over Ultrathin g-C₃N₄ Nanosheet with Large Surface Area and Enhanced Crystallinity by Two-Step Calcination