Z-scheme heterojunction Zn3(OH)2(V2O7)(H2O)2/V-Zn(O,S) for enhanced visible-light photocatalytic N2 fixation via synergistic heterovalent vanadium states and oxygen vacancy defects

doi:10.1016/S1872-2067(25)64716-4

Abstract

Abstract:

Herein, we established a Zn₃(OH)₂(V₂O₇)(H₂O)₂/V-Zn(O,S) Z-scheme heterojunction (labeled ZnVO/V-Zn(O,S) with a heterovalent V⁴⁺/V⁵⁺ states and oxygen vacancies in both phases via a one-step in-situ hydrolysis method. The NaBH₄ regulated the ZnVO/V-Zn(O,S)-3 with rich Vo and suitable n(V⁴⁺)/n(V⁵⁺) ratio achieved an excellent photocatalytic nitrogen fixation activity of 301.7 μmol/(g•h) and apparent quantum efficiency of 1.148% at 420 nm without any sacrificial agent, which is 11 times than that of V-Zn(O,S). The Vo acts as the active site to trap and activate N₂ molecules and to trap and activate H₂O to produce the H for N₂ molecules photocatalytic reduction. The rich Vo defects can also reduce the competitive adsorption of H₂O and N₂ molecules on the surface active site of the catalyst. The heterovalent vanadium states act as the photogenerated electrons, quickly hopping between V⁴⁺ and V⁵⁺ to transfer for the photocatalytic N₂ reduction reaction. Additionally, the Z-scheme heterojunction effectively minimizes photogenerated carrier recombination. These synergistic effects collectively boost the photocatalytic nitrogen fixation activity. This study provides a practical method for designing Z-scheme heterojunctions for efficient photocatalytic N₂ fixation under mild conditions.

Key words: Zn₃(OH)₂(V₂O₇)(H₂O)₂, Z-scheme heterojunction, Heterovalent valence states, Oxygen vacancy, Photocatalytic N₂ fixation

Pengkun Zhang, Qinhan Wu, Haoyu Wang, Dong-Hau Kuo, Yujie Lai, Dongfang Lu, Jiqing Li, Jinguo Lin, Zhanhui Yuan, Xiaoyun Chen. Z-scheme heterojunction Zn₃(OH)₂(V₂O₇)(H₂O)₂/V-Zn(O,S) for enhanced visible-light photocatalytic N₂ fixation via synergistic heterovalent vanadium states and oxygen vacancy defects[J]. Chinese Journal of Catalysis, 2025, 74: 279-293.

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Figures/Tables 7

Fig. 1. FE-SEM images of ZnVO (a), V-Zn(O,S) (b), and ZnVO/V-Zn(O,S)-1(c), 2(d), 3(e), and 4(f). TEM (g) and HR-TEM (h) images of ZnVO/V-Zn(O,S)-3. Selection region for elements mapping (i) and TEM-EDX element-mapping images of ZnVO/V-Zn(O,S)-3 (j-m). N2 adsorption-desorption isotherm (n) and the pore size distribution curves (o) of ZnVO, V-Zn(O,S), and ZnVO/V-Zn(O,S)-3 catalysts.

Fig. 2. XRD patterns of ZnVO and ZnVO/V-Zn(O,S) (a), and ZnVO, ZnVO/V-Zn(O,S)-3, Zn(O,S), and V-Zn(O,S) (b). (c) Survey spectra of ZnVO, ZnVO/V-Zn(O,S)-3, and V-Zn(O,S). High-resolution Zn 2p (d), V 2p (e), and O 1s (f) XPS, and EPR spectra (g) of ZnVO, ZnVO/V-Zn(O,S)-3, and V-Zn(O,S). (h) S 2p XPS spectra of ZnVO, ZnVO/V-Zn(O,S)-3, and V-Zn(O,S).

Fig. 3. (a) UV-vis spectra of ZnVO, Zn(O,S), V-Zn(O,S), and ZnVO/V-Zn(O,S). (b) Mott-Schottky curves of ZnVO, V-Zn(O,S), and ZnVO/V-Zn(O,S)-3 conducted at 500, 1000, and 2000 Hz. UPS (c) and VB-XPS (d) spectra of ZnVO, V-Zn(O,S), and ZnVO/V-Zn(O,S)-3.

Fig. 4. PL (a), TRPL (b), TPC (c), EIS (d), CV (e) spectra at a scan rate of 100 mV/s, CV spectra at a scan rate of 10 mV/s (f), CV spectra under slower scan rates (g), the J vs. scan rate plot for calculating ECSA (h), LSV (i), and the Tafel plots (j) of ZnVO, V-Zn(O,S), and ZnVO/V-Zn(O,S) catalysts.

Fig. 5. (a) Photocatalytic N2 fixation over ZnVO, V-Zn(O,S), and ZnVO/V-Zn(O,S) catalysts. (b) ZnVO/V-Zn(O,S)-3 catalyst photocatalytic reduction under N2 and Ar atmospheres in a water solution. (c) Photocatalytic reductions of the ZnVO/V-Zn(O,S)-3 catalyst in acetonitrile and silver nitrate aqueous solutions. (d) 1H-NMR (400 MHz) spectra for the solutions after photocatalytic N2 fixation under the 14N2 or 15N2 atmosphere with ZnVOS as a photocatalyst. (e) Photocatalytic N2 fixation cycling tests for ZnVO/V-Zn(O,S)-3 catalyst. Zn 2p (f), V 2p (g), O 1s (h), and S 2p (i) XPS spectra after the cycling reaction. (j) XRD spectra of ZnVO/V-Zn(O,S)-3 before and after reaction. (k) The CV curves of ZnVO/V-Zn(O,S)-3 before and after 100 cycling tests under 50 mV/s. (l) The long-term stability of the chronopotential test of the ZnVO/V-Zn(O,S)-3 catalyst electrode.

Fig. 6. DMPO-?OH (a) and DMPO-?O2- (b)generated by ZnVO, V-Zn(O,S), and ZnVO/V-Zn(O,S)-3 catalysts. Type-II (c) and Z-scheme (d) heterojunction band diagrams proposed for the ZnVO/V-Zn(O,S)-3 photocatalyst. (e) The band alignment and charge transfer pathway of ZnVO before and after contact with V-Zn(O,S) in darkness and under light exposure. (f) In suit XPS spectrum of S 2p under light irradiation. DMPO-?OH (g) and DMPO-?O2- (h) generated by ZnVO, V-Zn(O,S), and ZnVO/V-Zn(O,S)-3 catalysts under different durations.

Fig. 7. Schematic diagram of photocatalytic N2 reduction process with the ZnVO/V-Zn(O,S)-3 catalyst in water under visible light.

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Z-scheme heterojunction Zn₃(OH)₂(V₂O₇)(H₂O)₂/V-Zn(O,S) for enhanced visible-light photocatalytic N₂ fixation via synergistic heterovalent vanadium states and oxygen vacancy defects

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