A Ta3N5 photoanode with few deep-level defects derived from topologic transition of ammonium tantalum oxyfluoride for ultralow-bias photoelectrochemical water splitting

doi:10.1016/S1872-2067(24)60056-2

Abstract

Abstract:

An open challenge for developing solar-driven Ta₃N₅-based photoanodes with the ability to induce low-bias photoelectrochemical (PEC) water splitting is that their deep-level defects originated from low-valent tantalum cations (Ta³⁺) and nitrogen vacancies (V_N) seriously reduce the photovoltage and thus increase the bias for water splitting. Herein, we developed an effective topotactic transition synthesis route of producing few deep-level defects porous Ta₃N₅ film from the precursor film of ammonium tantalum oxyfluoride compound ((NH₄)₂Ta₂O₃F₆) pyramids on the Ta foil. The highly electronegative fluoride ions in (NH₄)₂Ta₂O₃F₆ could weaken the Ta-O bonds and the accompanied porous structure facilitates reactant diffusion, which favors the complete nitridation. Consequently, the resulting porous Ta₃N₅ film has very few deep-level defects, enabling an ultralow photocurrent onset potential at 0.2 V (vs. RHE) and a short-circuit photocurrent density (J_sc) of 3.28 mA cm^-2 after decorating oxygen evolution reaction (OER) cocatalysts under AM 1.5 G irradiation. Moreover, the J_sc can retain 85% of the initial value for a 5 h continuous stability test. By reducing the particle size of (NH₄)₂Ta₂O₃F₆ pyramid precursor, the deep-level defects could be further lowered in the Ta₃N₅ film, achieving the photoactivity for water oxidation at 0 V (vs. RHE) after modifying the OER co-catalyst.

Key words: (NH₄)₂Ta₂O₃F₆, Topologic transition, Less defective Ta₃N₅, Onset potential, Photoelectrochemical water splitting

Wei Xu, Chao Zhen, Huaze Zhu, Tingting Yao, Jianhang Qiu, Yan Liang, Shuo Bai, Chunlin Chen, Hui-Ming Cheng, Gang Liu. A Ta₃N₅ photoanode with few deep-level defects derived from topologic transition of ammonium tantalum oxyfluoride for ultralow-bias photoelectrochemical water splitting[J]. Chinese Journal of Catalysis, 2024, 61: 144-153.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(24)60056-2

https://www.cjcatal.com/EN/Y2024/V61/I6/144

Figures/Tables 4

Fig. 1. The synthesis and structures of Ta3N5 derived from (NH4)2Ta2O3F6. (a) Step 1. Preparation of pyramid-like (NH4)2Ta2O3F6 crystals on Ta foils by vapor-based solvothermal process. Step 2. Preparation of pyramid-like Ta3N5 crystals from (NH4)2Ta2O3F6 by one-step thermal-topotactic transition in an atmosphere of gaseous ammonia at 1000 °C for 6 h. (b,c) Low magnification SEM images of the films of (NH4)2Ta2O3F6 and porous Ta3N5. (d,e) High magnification SEM images of the films of (NH4)2Ta2O3F6 and porous Ta3N5. (f) TEM of a pyramid scraped from the (NH4)2Ta2O3F6 film. (g) TEM of a pyramid scraped from the porous Ta3N5. (h-j) Ta 4f, N 1s, F 1s XPS spectra of (NH4)2Ta2O3F6 and Ta3N5 films.

Fig. 2. Spectroscopic characterizations of Ta3N5 samples derived from different precursors. (a) Diffuse reflectance ultraviolet-visible absorption spectra. (b) Ta 4f XPS spectra. (c) Mott-Schottky plots. (d) Surface photovoltage spectra. (e) Transient photovoltage spectra. (f) Schematic diagrams of the photogenerated charge transfer process of Ta3N5 samples derived from (NH4)2Ta2O3F6 and Ta2O5 precursors.

Fig. 3. PEC performance of the few deep-level defect Ta3N5 photoanodes. (a) HAADF image of a single pyramid scraped from Ta3N5@Co(OH)2/NiCoFe-Bi film and EDS mapping images of O, Co, Fe elements. (b) J-V curves of Ta3N5, Ta3N5@Co(OH)2/NiCoFe-Bi photoanode tested in a 1 mol L?1 KOH aqueous solution (pH = 13.6). (c) Stability test at 1.23 V (vs. RHE). (d) IPCE curve of Ta3N5@Co(OH)2/NiCoFe-Bi and its estimated solar photocurrent based on the standard solar spectrum of AM 1.5 G. (e) Amount of oxygen evolved from Ta3N5@Co(OH)2/NiCoFe-Bi photoanode under an applied potential of 1.23 V vs. RHE and the corresponding Faradaic efficiency for O2 evolution. e- represents the number of electrons.

Fig. 4. The films of small-sized Ta3N5 pyramids with fewer deep-level defects. (a) SEM image of the film consisting of small-sized (NH4)2Ta2O3F6 pyramids. (b) Diffuse reflectance ultraviolet-visible absorption spectra of the Ta3N5 films produced from the films of small- and big-sized (NH4)2Ta2O3F6 pyramids, respectively. (c) LSV curves of the Ta3N5@Co(OH)2 photoanode of small-sized pyramids tested in a 1 mol L?1 KOH aqueous solution (pH = 13.6).

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A Ta₃N₅ photoanode with few deep-level defects derived from topologic transition of ammonium tantalum oxyfluoride for ultralow-bias photoelectrochemical water splitting

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