光电催化分解水稳定性达100 h的亚稳相β-Fe2O3光阳极

doi:10.1016/S1872-2067(21)63822-6

催化学报 ›› 2021, Vol. 42 ›› Issue (11): 1992-1998.DOI: 10.1016/S1872-2067(21)63822-6

光电催化分解水稳定性达100 h的亚稳相β-Fe₂O₃光阳极

李洋^a, 张宁斯^a^,^#(), 刘昌昊^a, 张园明^a, 徐晓明^a, 王文静^a, 冯建勇^a, 李朝升^a^,^b^,^*(), 邹志刚^a^,^b

^a南京大学工程与应用科学学院, 固态微结构国家实验室, 高级微结构协同创新中心, 江苏南京210093
^b南京大学纳米技术江苏省重点实验室, 高级微结构协同创新中心, 江苏南京210093

收稿日期:2021-02-08 修回日期:2021-02-08 接受日期:2021-04-06 出版日期:2021-11-18 发布日期:2021-05-18
通讯作者: 张宁斯,李朝升
基金资助:
国家重点研发计划(2018YFA0209303);国家自然科学基金(22025202);国家自然科学基金(U1663228);国家自然科学基金(51972165)

Metastable-phase β-Fe₂O₃ photoanodes for solar water splitting with durability exceeding 100 h

Yang Li^a, Ningsi Zhang^a^,^#(), Changhao Liu^a, Yuanming Zhang^a, Xiaoming Xu^a, Wenjing Wang^a, Jianyong Feng^a, Zhaosheng Li^a^,^b^,^*(), Zhigang Zou^a^,^b

^aCollaborative Innovation Center of Advanced Microstructures, National Laboratory of Solid State Microstructures, College of Engineering and Applied Sciences, Nanjing University, Nanjing 210093, Jiangsu, China
^bJiangsu Key Laboratory for Nano Technology, Nanjing University, Nanjing 210093, Jiangsu, China

Received:2021-02-08 Revised:2021-02-08 Accepted:2021-04-06 Online:2021-11-18 Published:2021-05-18
Contact: Ningsi Zhang,Zhaosheng Li
About author:^#E-mail: zhangningsi@nju.edu.cn
^*Tel: +86-25-83686304-800; Fax: +86-25-83686632; E-mail: zsli@nju.edu.cn;
Zhaosheng Li was born in China in 1975. He received his PhD in condensed matter physics from the Institute of Solid State Physics, Chinese Academy of Sciences, China, in 2003. After a two-year postdoctoral fellowship at Nanjing University, he became a lecturer at this university. In 2006, he was promoted to Associate Professor of Materials Science and Engineering at Nanjing University. Since December 2011, he has become a full Professor of Materials Science and Engineering at the College of Engineering and Applied Sciences, Nanjing University. His current research interests include photoelectrochemistry and photocatalysis. He was appointed as the Associate Editor of Chin. J. Catal. in 2020.
Supported by:
National Key Research and Development Program of China(2018YFA0209303);National Natural Science Foundation of China(22025202);National Natural Science Foundation of China(U1663228);National Natural Science Foundation of China(51972165)

摘要/Abstract

摘要：

利用半导体光电催化分解水制氢是将太阳能转化为化学能的有效途径之一, 具有重要的科学意义和巨大的应用前景. 铁基半导体具有光谱响应范围广、绿色环保和价格低廉等优点, 是具应用前景的光阳极材料之一. 在铁基半导体中, α-Fe₂O₃光阳极的光电催化性能已经被广泛报道, 亚稳相氧化铁的光电催化性能尚未有深入研究. 本课题组曾经报道用于光电催化分解水的亚稳相β-Fe₂O₃颗粒组装膜光阳极[Natl. Sci. Rev., 2020, 7, 1059-1067]. β-Fe₂O₃光阳极的太阳能-氢能理论转化效率为20.9%, 优于α-Fe₂O₃光阳极. β-Fe₂O₃的热稳定性和在长时间光电催化反应过程中的光化学稳定性是决定其应用前景的核心问题.
本文报道了一种喷雾热裂解制备β-Fe₂O₃薄膜的方法. 该方法提高了β-Fe₂O₃的热稳定性, 从而提高了β-Fe₂O₃在长时间光电化学反应中的光电化学稳定性. 与电泳沉积方法制备的β-Fe₂O₃颗粒组装膜相比, 利用喷雾热裂解法制备的亚稳相β-Fe₂O₃薄膜的热稳定性得到显著增加. 物相表征结果表明, 经过相同的煅烧处理或者激光辐照后, 电泳沉积方法制备的β-Fe₂O₃颗粒组装膜发生了明显相变;而由喷雾热裂解制备的β-Fe₂O₃平板膜依旧保持稳定, 没有发生相变. β-Fe₂O₃薄膜与衬底之间存在较高的应力, 与颗粒组装膜相比, 平板膜在退火热处理与激光辐照下都表现出更好的稳定性. β-Fe₂O₃薄膜与衬底之间的应力增加了亚稳相β-Fe₂O₃的相变势垒, 提高了β-Fe₂O₃的相变温度.
通过引入Ti⁴⁺掺杂提高载流子浓度, 改善载流子传输, 使得β-Fe₂O₃光阳极的光电催化性能提升了3倍. 结果表明, β-Fe₂O₃光阳极薄膜具有良好的光化学稳定性, 其光电催化分解水性能在模拟太阳光条件下工作110 h后未出现明显的衰减.
本文提出了一种增加亚稳相β-Fe₂O₃热稳定性的方法, β-Fe₂O₃光阳极具有较好的光化学稳定性, 在光电催化方面具有较好的应用前景.

关键词: 亚稳相, 热裂解, β-Fe₂O₃光阳极, 钛掺杂, 稳定性, 光电催化分解水

Abstract:

Planar films of pure and Ti⁴⁺-doped β-Fe₂O₃ were prepared by a spray pyrolysis method. X-ray diffraction patterns and Raman spectra of the metastable β-Fe₂O₃ film showed that its thermal stability was significantly improved because of covalent bonds in the interfaces between the film and substrate, while only weak Van der Waals bonds existed at the interfaces within the particle-assembled β-Fe₂O₃film prepared by electrophoretic deposition. The as-prepared planar films were thus able to withstand higher annealing temperature and stronger laser irradiation power in comparison with the β-Fe₂O₃particle-assembly. Ti⁴⁺ doping was used to increase the concentration of carriers in the metastable β-Fe₂O₃ film. Compared with pure β-Fe₂O₃photoanodes, the highest saturated photocurrent for water splitting over the Ti⁴⁺-doped β-Fe₂O₃ photoanode was increased by a factor of approximately three. The β-Fe₂O₃photoanode exhibited photochemical stability for water splitting for a duration exceeding 100 h, which indicates its important potential application in solar energy conversion.

Key words: Metastable phase, Spray pyrolysis, β-Fe₂O₃ photoanode, Titanium doping, Stability, Photoelectrochemical water splitting

李洋, 张宁斯, 刘昌昊, 张园明, 徐晓明, 王文静, 冯建勇, 李朝升, 邹志刚. 光电催化分解水稳定性达100 h的亚稳相β-Fe₂O₃光阳极[J]. 催化学报, 2021, 42(11): 1992-1998.

Yang Li, Ningsi Zhang, Changhao Liu, Yuanming Zhang, Xiaoming Xu, Wenjing Wang, Jianyong Feng, Zhaosheng Li, Zhigang Zou. Metastable-phase β-Fe₂O₃ photoanodes for solar water splitting with durability exceeding 100 h[J]. Chinese Journal of Catalysis, 2021, 42(11): 1992-1998.

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图/表 7

Fig. 1. Raman spectra of the β-Fe2O3 films prepared by electrophoretic deposition (a) and spray pyrolysis (b) at 532 nm with different filters (Theoretical Raman spectra of β-Fe2O3 as a standard come from Ref. [28]).

Fig. 2. Sketches showing increase in phase transition barrier from the metastable to the mature phase caused by stress between the film and substrate (a), and interfaces between the film and substrate (b). Phase transition barrier: ΔG2 > ΔG1.

Fig. 3. Current-potential curves of the pure and Ti4+-doped β-Fe2O3 photoanodes measured in 1 M NaOH aqueous solution under AM 1.5 G (100 mW cm-2) illumination.

Fig. 4. (a) XRD patterns of 4% Ti4+-doped β-Fe2O3; (b) Raman scattering spectra of β-Fe2O3 photoanodes with different concentrations of titanium-ion doping.

Fig. 5. (a) Fe 2p XPS spectra of pure β-Fe2O3 and 4% Ti4+-doped β-Fe2O3; Ti 2p (b) and O 1s (c) XPS spectra of 4% Ti4+-doped β-Fe2O3; (d) Ti 2p XPS spectra of β-Fe2O3 doped at different concentrations.

Fig. 6. Mott-Schottky (a) and Nyquist plots (b) of β-Fe2O3 photoanodes.

Fig. 7. (a) Chronoamperometry (i-t) of 4% Ti4+-doped β-Fe2O3 photoanode measured at 1.5 V vs. RHE under the xenon illumination; (b) Raman scattering spectra of the 4% Ti4+-doped β-Fe2O3 photoanode before and after the PEC water splitting for 110 h.

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光电催化分解水稳定性达100 h的亚稳相β-Fe₂O₃光阳极

Metastable-phase β-Fe₂O₃ photoanodes for solar water splitting with durability exceeding 100 h

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