TiO2-x@C/MoO2 Schottky junction: Rational design and efficient charge separation for promoted photocatalytic performance

doi:10.1016/S1872-2067(23)64488-2

Abstract

Abstract:

Limited solar light harvesting, sluggish charge transfer kinetics, and inferior affinity for adsorbed hydrogen species (H*) severely restrict the photocatalytic hydrogen generation activity of TiO₂ photocatalysts. Herein, we present a novel TiO_2-_x@C/MoO₂ Schottky junction prepared via a simple one-step in situ phase-transition-regulation strategy. Crucially, the abundant oxygen vacancies in TiO_2-_x@C/MoO₂narrow the bandgap and introduce defects to improve the photoresponse. The strongly bonded carbon layer not only serves as a fast charge-transport channel to improve the interlayer charge transfer efficiency but also protects oxygen vacancies from oxidation. Moreover, the Schottky barrier effectively impairs the recombination of electrons and holes and promotes the utilization of photogenerated electrons. Furthermore, the MoO₂ cocatalyst optimizes the Gibbs free energy for H₂ evolution. As a result of the favorable synergy, the resulting TiO_2-_x@C/MoO₂ presents a significantly enhanced photocatalytic H₂ production rate of 506 μmol g^-1 h^-1 compared to those of TiO_2-_x and TiO_2-_x@C (125.5- and 15.8-times larger, respectively). Moreover, outstanding stability over 27 h was achieved because of the protection provided by the surface carbon layer. This ingenious design and facile synthetic strategy offer exciting avenues for the design of strongly coupled Schottky junction photocatalysts for efficient solar-to-chemical conversions.

Key words: Oxygen vacancy, TiO₂, MoO₂, Carbon layer, H₂ evolution, Schottky junction

Xiu-Qing Qiao, Chen Li, Zizhao Wang, Dongfang Hou, Dong-Sheng Li. TiO_2-_x@C/MoO₂Schottky junction: Rational design and efficient charge separation for promoted photocatalytic performance[J]. Chinese Journal of Catalysis, 2023, 51: 66-79.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(23)64488-2

https://www.cjcatal.com/EN/Y2023/V51/I8/66

Figures/Tables 11

Fig. 1. Schematic of the preparation of TiO2-x@C/MoO2 Schottky junction.

Fig. 2. (a,b) XRD and partially enlarged patterns of all samples. Raman (c) and partially enlarged (d) spectra of MoO2, TiO2-x@C, and TCM-1 samples.

Fig. 3. TEM (a) and HRTEM (b) images of P25. TEM (c) and HRTEM (d) images of TiO2-x@C. (e) HAADF-STEM image, (e1) overlap and (e2)-(e4) element mapping of TiO2-x@C. (f-h) HRTEM image of TCM-1 sample and (i) inverse FFT pattern of HRTEM image. (j) HAADF-STEM image, (j1) overlap and (j2)-(j5) element mapping of TCM-1 sample.

Fig. 4. (a) EPR signals of P25, TiO2-x, TiO2-x@C, and TCM-1 samples. (b) XPS survey spectra of TiO2-x@C and TCM-1 samples. High-resolution XPS spectra of C 1s (c), Ti 2p (d), Mo 3d (e), and O 1s (f) of TiO2-x@C and TCM-1 photocatalysts.

Fig. 5. H2 production over time (a) and a comparison (b) of photocatalytic H2 generation rate of various photocatalysts. (c) Comparison of H2 evolution rates over TCM-1 and other reported photocatalysts. (d) Cyclic use of the TCM-1 photocatalyst. (e) XRD diffraction patterns of fresh and recycled TCM-1 photocatalyst.

Fig. 6. (a) UV-vis DRS spectra of all photocatalysts showing the Tauc plots used for the band gap determination of P25 and TiO2-x. (b) Mott-Schottky plots of TiO2-x. EIS Nyquist plots (c), PL spectra (d) of all samples. Photocurrent response (e) and time-resolved photoluminescence lifetime curves (f) of samples.

Fig. 7. (a) Atom-projected DOS for MoO2. (b) Gibbs free energy diagram. Electrostatic potentials for MoO2 (c) and TiO2-x (d).

Fig. 8. Schematic of the band structure and Fermi level of TCM sample (a) before contact and (b) after contact.

Fig. 9. (a) Photocatalytic degradation of TC under visible light, kinetics curves for TC degradation (b) and Cr(VI) reduction (c), and first-order reaction kinetics (d) over different photocatalysts. EPR spectra for ?OH (e) and ?O2- (f). (g) Comparison of the kinetic rate constants of previously reported photocatalysts.

Fig. 10. Proposed degradation pathways for TC by TCM sample under visible light irradiation.

Table 1 Toxicity of the TC/intermediates evaluated by T.E.S.T.

Target	LC50-96hr (mg L^‒1)	LD50 (mg Kg^‒1)	Bioaccumulation factor	Developmental toxicity	Mutagenic
C1	0.9	1524.04	0.71	0.86 Toxicant	0.60 Positive
C2	0.33	1363.25	1.65	0.90 Toxicant	0.64 Positive
C3	0.22	1197.10	N/A	0.91 Toxicant	0.35 Negative
C4	0.90	1052.15	0.95	0.82 Toxicant	0.63 Positive
C5	0.78	103.62	8.34	0.84 Toxicant	0.88 Positive
C6	1102.04	6270.10	2.43	0.51 Toxicant	0.01 Negative
C7	234.20	2970.28	7.68	0.50 Non-toxicant	‒0.01 Negative
C8	6.62	1529.48	0.36	0.85 Toxicant	0.66 Positive
C9	N/A	979.17	N/A	0.78 Toxicant	0.40 Negative
C10	0.27	437.29	0.17	0.87 Toxicant	0.63 Positive

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TiO_2-_x@C/MoO₂Schottky junction: Rational design and efficient charge separation for promoted photocatalytic performance

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