Defect engineering of water-dispersible g-C3N4 photocatalysts by chemical oxidative etching of bulk g-C3N4 prepared in different calcination atmospheres

doi:10.1016/j.jmst.2021.07.013

Abstract

Abstract:

In this study, water-dispersible graphitic carbon nitride (g-C₃N₄) photocatalysts were successively prepared through the chemically oxidative etching of bulk g-C₃N₄ that was polymerized thermally in different calcination atmospheres such as air, CO₂, and N₂. The different calcination atmospheres directly influenced the physicochemical and optical properties of both bulk and water-dispersible g-C₃N₄, changing the photocatalytic degradation behavior of methylene blue (MB) and tetracycline hydrochloride (TC-HCl) for water-dispersible g-C₃N₄. The bubble-burst process in the thermal polymerization of thiourea produced defective edges containing C=O groups that preferred substituting the C-NH_x groups over bulk g-C₃N₄. In the oxygen-free N₂ atmosphere among the different calcination atmospheres, more C=O functional groups were generated on the defective edges of bulk g-C₃N₄, resulting in the highest N vacancy of the tri-s-triazine structure. During the successive chemical oxidation, S- or O-containing functional groups were introduced onto water-dispersible g-C₃N₄. The water-dispersible g-C₃N₄ photocatalyst from the oxygen-free N₂ atmosphere (NTw) contained the most O- and S- functional groups on the g-C₃N₄ surface. Consequently, NTw exhibited the highest photocatalytic activity in the MB and TC-HCl photodegradation because of its slowest recombination process, which was ascribed to the unique surface properties of NTw such as abundant functional groups on the defective edges and N-deficient property.

Key words: g-C₃N₄, Water-dispersible photocatalyst, Calcination atmosphere, Charge separation, Chemically oxidative etching, Defect edges

Thi Kim Anh Nguyen, Thanh-Truc Pham, Bolormaa Gendensuren, Eun-Suok Oh, Eun Woo Shin. Defect engineering of water-dispersible g-C₃N₄ photocatalysts by chemical oxidative etching of bulk g-C₃N₄ prepared in different calcination atmospheres[J]. J. Mater. Sci. Technol., 2022, 103: 232-243.

Figures/Tables 13

Scheme 1. Schematic illustration of the preparation of all the g-C3N4 materials in this study.

Fig. 1. TEM images of bulk and water-dispersible g-C3N4 photocatalysts.

Table 1 Textural data and band gaps of the prepared photocatalysts.

Sample	S_BET (m²/g) ^a	V (cm³/g) ^a	L (nm) ^a	Band gap (eV) ^b
ATb	25.0	0.203	18.3	2.40
CTb	17.9	0.121	26.5	2.35
NTb	11.4	0.130	45.9	2.46
fATw	70.1	0.455	14.5	2.60^c
fCTw	23.0	0.142	24.5	2.74^c
fNTw	24.0	0.248	40.0	2.52^c

Fig. 2. FTIR spectra (A) and XRD patterns (B) of bulk and freeze-dried water-dispersible g-C3N4 photocatalysts.

Fig. 3. XPS data of C 1s, N 1s, O 1s and S 2p for bulk and freeze-dried water-dispersible g-C3N4 photocatalysts.

Scheme 2. Schematic illustration of the bubble burst process over bulk g-C3N4, the chemical oxidative etching on water dispersible g-C3N4, and the corresponding morphologies.

Fig. 4. Atomic ratios of sulfur and oxygen to carbon for bulk and freeze-dried water-dispersible g-C3N4 photocatalysts. The values were calculated from the XPS data.

Fig. 5. UV-vis absorption spectra (A, B) and Tauc plots of E (eV) vs (αhν) (C, D) for bulk and water-dispersible g-C3N4 photocatalysts.

Fig. 6. PL emission spectra (A) of bulk g-C3N4 and water-dispersible g-C3N4 (inset) and EIS Nyquist plots (B) for bulk g-C3N4 and freeze-dried water-dispersible g-C3N4.

Fig. 7. Time-resolved fluorescence decay spectra in the ns time scale for bulk and water-dispersible g-C3N4 with excitation 400 nm (Inset table: the calculated average fluorescence lifetime (τav)).

Fig. 8. Kinetic data of MB adsorption in the dark (A) for the bulk and water-dispersible g-C3N4 photocatalysts and corresponding pseudo-second-order kinetic plots (B). Kinetic data of TC-HCl adsorption in the dark (C) for the bulk and water-dispersible g-C3N4 photocatalysts and corresponding pseudo-second-order kinetic plots (D).

Table 2 Kinetic data for adsorption and photocatalytic degradation of MB and TC-HCl for the prepared photocatalysts.

Sample	Adsorption kinetics						Photocatalytic kinetics
	MB			TC-HCl			MB		TC-HCl
	q_e (mg/g_cat)	k_ads (g/mg min)^{2 a}	r²	q_e (mg/g_cat)	k_ads (g/mg min)^{2 a}	r²	k_app × 10³ (min^-1) ^b	r²	k_app × 10³ (min^-1) ^b	r²
ATb	20.9	0.0469	0.9865	29.5	0.0333	0.9992	1.5	0.9774	6.6	0.9965
CTb	55.3	0.0169	0.9921	21.2	0.0458	0.9967	2.7	0.9992	2.1	0.9963
NTb	13.1	0.0734	0.9873	28.0	0.0361	0.9992	0.5	0.9689	2.1	0.9914
ATw	126.9	0.0074	0.9987	29.4	0.033	0.9975	14.4	0.9905	10.0	0.9977
CTw	101.2	0.0094	0.9986	33.1	0.0295	0.9974	18.7	0.9937	15.9	0.9991
NTw	184.0	0.0052	0.9989	27.0	0.0363	0.9982	25.3	0.9767	17.3	0.9992

Fig. 9. MB photodegradation results for bulk and water-dispersible g-C3N4 under visible-light irradiation (A) C/C0 vs. t and (B) ln(C/C0) vs. t. TC-HCl photodegradation results for bulk and water-dispersible g-C3N4 under visible-light irradiation (C) C/C0 vs. t and (D) ln(C/C0) vs. t.

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Defect engineering of water-dispersible g-C₃N₄ photocatalysts by chemical oxidative etching of bulk g-C₃N₄ prepared in different calcination atmospheres

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