MOFs衍生的二氧化钛促进Ti-Fe2O3光阳极高效光电化学水氧化的多重效应

doi:10.1016/S1872-2067(24)60005-7

催化学报 ›› 2024, Vol. 61: 179-191.DOI: 10.1016/S1872-2067(24)60005-7

MOFs衍生的二氧化钛促进Ti-Fe₂O₃光阳极高效光电化学水氧化的多重效应

巴凯凯^a, 刘禹男^a, 张凯^a, 王平^b, 林艳红^a, 王德军^a, 李子亨^c, 谢腾峰^a^,^*()

^a吉林大学化学学院, 吉林长春 130012
^b吉林师范大学化学学院, 教育部环保材料制备与应用重点实验室, 吉林长春 130103
^c吉林大学物理学院, 先进电池物理与技术重点实验室, 吉林长春 130012

收稿日期:2023-12-20 接受日期:2024-03-11 出版日期:2024-06-18 发布日期:2024-06-20
通讯作者: * 电子信箱: xietf@jlu.edu.cn (谢腾峰).
基金资助:
国家自然科学基金(22172057);吉林省科技发展规划国际合作项目(20230402061GH)

Unveiling the multiple effects of MOF-derived TiO₂ on Ti-Fe₂O₃photoanodes for efficient and stable photoelectrochemical water oxidation

Kaikai Ba^a, Yuʼnan Liu^a, Kai Zhang^a, Ping Wang^b, Yanhong Lin^a, Dejun Wang^a, Ziheng Li^c, Tengfeng Xie^a^,^*()

^aCollege of Chemistry, Jilin University, Changchun 130012, Jilin, China
^bKey Laboratory of Preparation and Applications of Environmental Friendly Material of the Ministry of Education, College of Chemistry, Jilin Normal University, Changchun 130103, Jilin, China
^cKey Laboratory of Physics and Technology for Advanced Batteries, College of Physics, Jilin University, Changchun 130012, Jilin, China

Received:2023-12-20 Accepted:2024-03-11 Online:2024-06-18 Published:2024-06-20
Contact: * E-mail: xietf@jlu.edu.cn (T. Xie).
Supported by:
National Natural Science Foundation of China(22172057);International Cooperation Project of Jilin Scientific and Technological Development Program(20230402061GH)

摘要/Abstract

摘要：

光电化学(PEC)分解水是一种清洁可持续的获取氢燃料的方法, 其中产氧半反应(OER)是制约整个水分解过程效率的关键步骤. 因此, 光阳极的性能是决定太阳能到氢能转化效率的关键因素. 在各种水氧化光阳极材料中, 赤铁矿(α-Fe₂O₃)因具有良好的化学稳定性、合适的带隙(~2.1 eV)、无毒、储量丰富等优点而成为最有前途的光阳极材料之一. 然而, α-Fe₂O₃丰富的受体表面态和缓慢的水氧化动力学导致光生电荷复合严重, 限制了其在光电化学中的实际应用. 因此, 有必要对α-Fe₂O₃进行表面工程设计以提高水氧化效率.
本文提出了一种新方法, 以金属有机框架(Ti-MOFs)为模板, 在Ti-Fe₂O₃表面煅烧合成TiO₂层, 然后将富活性位点的ZIF-67加载在TiO₂/Ti-Fe₂O₃上作为助催化剂, 制备出具有较好光电化学性能的ZIF-67/TiO₂/Ti-Fe₂O₃复合光阳极. X射线衍射、高分辨透射电镜、X射线光电子能谱和拉曼光谱等表征结果证实成功合成了ZIF-67/TiO₂/Ti-Fe₂O₃. 同时, 氮气等温吸附脱附曲线和表面接触角测试结果表明, MOFs衍生的TiO₂为介孔材料. 采用表面光伏技术、光致发光光谱、飞秒-瞬态吸收光谱和电化学阻抗谱分析, 研究了光生电荷的分离和复合行为. 结果表明, MOFs衍生的TiO₂不仅可以作为钝化层有效抑制了表面复合, 还作为Ti-Fe₂O₃的电子阻挡层, 显著减少了电子向表面的流失, 从而大大提高了Ti-Fe₂O₃表面和体相的电荷分离效率. 进一步的累积电荷量测试、电化学阻抗谱和Bode图分析显示, 负载MOFs衍生TiO₂后, 可以明显促进光生空穴向电解质的注入, 其多孔结构也可以增加反应接触面积, 这有利于光生电荷在固液界面传输. 此外, 理论计算结果表明, Ti-Fe₂O₃水氧化速控步骤的能垒(ΔG = 3.38 eV)明显高于TiO₂ (ΔG = 1.67 eV), 说明OER更容易在TiO₂/Ti-Fe₂O₃表面发生, 这与其光电流密度结果一致. 为进一步提高反应活性和加快水氧化动力学, 负载助催化剂ZIF-67后, ZIF-67/TiO₂/Ti-Fe₂O₃复合光阳极实现了较好的光电化学性能, 其在1.23 V vs. RHE时光电流密度高达4.04 mA cm^-2, 是Ti-Fe₂O₃的9.3倍, 并且复合光阳极的入射光子电流转换效率和空穴注入效率分别达到93% (390 nm)和91%.
综上所述, 本研究通过MOFs衍生的TiO₂和ZIF-67助催化剂改性α-Fe₂O₃光阳极, 显著提升了其光电化学水氧化性能. 其中, MOFs衍生TiO₂不仅优化了电荷分离, 还促进了光生空穴的注入, 从而显著提高其光电化学水氧化性能. 本研究为构筑高性能的有机-无机杂化光阳极提供了新思路.

关键词: Ti-Fe₂O₃光阳极, 电荷分离, 多孔TiO₂, 多重效应, 水氧化

Abstract:

α-Fe₂O₃ is a promising photoanode that is limited by its high surface charge recombination and slow water oxidation kinetics. In this study, we synthesized a TiO₂ layer on Ti-Fe₂O₃ by annealing Ti-MOFs, followed by ZIF-67 as a co-catalyst, to fabricate a ZIF-67/TiO₂/Ti-Fe₂O₃ photoanode for photoelectrochemical (PEC) water splitting. The systematic experimental and theoretical results revealed that the improvement in performance was due to multiple effects of the MOF-derived TiO₂. This molecule not only passivates the acceptor surface states of Ti-Fe₂O₃, thereby reducing the number of surface recombination centers, but also acts as an electron barrier to promote charge separation in the Ti-Fe₂O₃ bulk. Moreover, MOF-derived TiO₂ can dramatically reduce the energy barrier for the OER of Ti-Fe₂O₃, thus promoting the conversion of the intermediate *OH into *O. The synergistic improvement in the bulk and surface properties effectively enhanced the water oxidation performance of Ti-Fe₂O₃. The ZIF-67/TiO₂/Ti-Fe₂O₃ photoanode exhibits a photocurrent density of up to 4.04 mA cm^‒2 at 1.23 V vs. RHE, which is 9.4 times as that of pure Ti-Fe₂O₃, and has long-term stability. Our work provides a feasible strategy for constructing efficient organic-inorganic hybrid photoelectrodes.

Key words: Ti-Fe₂O₃ photoanode, Charge separation, Porous TiO₂, Multiple effects, Water oxidation

巴凯凯, 刘禹男, 张凯, 王平, 林艳红, 王德军, 李子亨, 谢腾峰. MOFs衍生的二氧化钛促进Ti-Fe₂O₃光阳极高效光电化学水氧化的多重效应[J]. 催化学报, 2024, 61: 179-191.

Kaikai Ba, Yuʼnan Liu, Kai Zhang, Ping Wang, Yanhong Lin, Dejun Wang, Ziheng Li, Tengfeng Xie. Unveiling the multiple effects of MOF-derived TiO₂ on Ti-Fe₂O₃photoanodes for efficient and stable photoelectrochemical water oxidation[J]. Chinese Journal of Catalysis, 2024, 61: 179-191.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60005-7

https://www.cjcatal.com/CN/Y2024/V61/I6/179

图/表 12

Scheme 1. The preparation of the ZIF-67/TiO2/Ti-Fe2O3 photoanode.

Fig. 1. SEM images of Ti-Fe2O3 (a), Ti-MOF/Ti-Fe2O3 (b), TiO2/Ti-Fe2O3 (c), and ZIF-67/TiO2/Ti-Fe2O3 (d). TEM image (e), HRTEM image (f), and elemental mapping (g) of ZIF-67/TiO2/Ti-Fe2O3.

Fig. 2. XRD patterns (a), Raman spectra (b), and FTIR spectra (c) of ZIF-67/TiO2/Ti-Fe2O3, TiO2/Ti-Fe2O3, and Ti-Fe2O3. (d) N2 adsorption-desorption isotherms of MOF-derived TiO2. (e) Comparison of contact angles of TiO2/Ti-Fe2O3 and Ti-Fe2O3. (f) UV-vis absorption spectra.

Fig. 3. XPS spectra of ZIF-67/TiO2/Ti-Fe2O3: (a) survey; (b) Fe 2p; (c) Ti 2p; (d) O 1s; (e) Co 2p; (f) N 1s.

Fig. 4. LSV curves (the solid lines represent testing under illumination, while the dashed lines were run in the dark) (a), IPCE values (b), ABPE values (c) of Ti-Fe2O3, TiO2/Ti-Fe2O3, and ZIF-67/TiO2/Ti-Fe2O3, and stability test (d) of ZIF-67/TiO2/Ti-Fe2O3.

Table 1 Comparison of the photocurrent densities of Fe2O3-based photoanodes in the literature with our results at 1.23 V vs. RHE.

Photoanode	Photocurrent density (mA cm^-2)	Stability	Ref.
Ti:Fe₂O₃@CoFe-cMOFs	3.32	10 h stability ca. 95% of the original	[35]
CoPi/H₂TCPP/Ti-Fe₂O₃	1.84	2 h stability ca. 84% of the original	[36]
Fe_xNi_1‒_xOOH/B/Ti-Fe₂O₃	3.39	2 h stability ca. 93% of the original	[37]
Co-Sil/CTF/Gd-Fe₂O₃	2.74	5 h stability ca. 99% of the original	[38]
CoAl-LDH/F-Fe₂O₃	2.46	6 h stability ca. 90% of the original the original	[39]
Ti: Fe₂O₃@g-C₃N₄	3.38	5 h stability ca. 85% of the original	[40]
Ti-Fe₂O₃/CoFePi	2.15	3 h stability ca. 95% of the original	[41]
Co-Pi/CQDs/Fe₂O₃/TiO₂	3.00	3 h stability ca. 100% of the original	[42]
F:FeOOH/Zr:Fe₂O₃	2.11	2 h stability ca. 100% of the original	[43]
Fe₂O₃/FePO₄/FeOOH	2.00	1.3 h stability ca. 99% of the original	[44]
Fe₂O₃/Fe₂TiO₅/CoFe	1.25	24 h stability ca. 80% of the original	[45]
ZnFe₂O₄/Fe₂O₃	3.17	3 h stability ca. 86% of the original	[46]
NiFe(OH)_x/PSi/Ge-Fe₂O₃	4.57	65 h stability ca. 97% of the original	[47]
Ta:Fe₂O₃@CaFe₂O₄/FeNiO_x	2.70	50 h stability ca. 88% of the original	[48]
NiCoP/Fe₂O₃	3.80	4 h stability ca. 99% of the original	[49]
ZIF-67/TiO₂/Ti-Fe₂O₃	4.04	40 h stability ca. 90% of the original	this work

Fig. 5. TPV spectra (a) and the enlarged part (b) of peak 1 in the TPV spectra of Ti-Fe2O3, TiO2/Ti-Fe2O3, and ZIF-67/TiO2/Ti-Fe2O3. (c) Work function measurements of pure Ti-Fe2O3 and MOF-derived TiO2. (d) Open-circuit photovoltage (Voc) of Ti-Fe2O3, TiO2/Ti-Fe2O3, and ZIF-67/TiO2/Ti-Fe2O3. PL spectra (e) and PA spectra (f) of Ti-Fe2O3 and TiO2/Ti-Fe2O3.

Fig. 6. fs-TA spectra of Ti-Fe2O3 (a) and TiO2/Ti-Fe2O3 (b) excited at 400 nm. Transient absorption decays observed at 625 nm for Ti-Fe2O3 (c) and TiO2/Ti-Fe2O3 (d).

Fig. 7. Bode phase plots (a), bulk resistance of the photoanode (R1) (b), charge transfer resistance (c) at the solid-liquid interface (R2), charge transfer efficiency (ηCT) (d) of Ti-Fe2O3, TiO2/Ti-Fe2O3, and ZIF-67/TiO2/Ti-Fe2O3. CV curves (e) of ZIF-67/TiO2/Ti-Fe2O3, and measured capacitive currents plotted as a function of scan rates (f) for Ti-Fe2O3, TiO2/Ti-Fe2O3, and ZIF-67/TiO2/Ti-Fe2O3.

Fig. 8. J-t curves at 1.23 V vs. RHE under chopping light (a), accumulated charge density (b), ηinj (c), Nyquist plots (d) at 1.0 V vs. RHE, and enlarged Nyquist plots (e) of Ti-Fe2O3, TiO2/Ti-Fe2O3, and ZIF-67/TiO2/Ti-Fe2O3.

Fig. 9. Gibbs free energy changes during the OER for Ti-Fe2O3 and TiO2/Ti-Fe2O3.

Scheme 2. The charge transfer schematic mechanism diagram of Ti-Fe2O3 (a), TiO2/Ti-Fe2O3 (b), and ZIF-67/TiO2/Ti-Fe2O3 (c).

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MOFs衍生的二氧化钛促进Ti-Fe₂O₃光阳极高效光电化学水氧化的多重效应

Unveiling the multiple effects of MOF-derived TiO₂ on Ti-Fe₂O₃photoanodes for efficient and stable photoelectrochemical water oxidation

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