静电纺丝法合成S型异质结CoTiO3/g-C3N4纳米纤维及其增强的可见光光催化活性研究

doi:10.1016/S1872-2067(23)64566-8

催化学报 ›› 2024, Vol. 59: 237-249.DOI: 10.1016/S1872-2067(23)64566-8

静电纺丝法合成S型异质结CoTiO₃/g-C₃N₄纳米纤维及其增强的可见光光催化活性研究

杨令坤^a, 李宗军^a, 王鑫^b^,^*(), 李铃铃^a^,^*(), 陈哲^a^,^*()

^a吉林化工学院材料科学与工程学院, 吉林吉林 132022
^b宁夏大学化学化工学院, 国家实验化学教学示范中心, 煤炭高效利用与绿色化工国家重点实验室, 宁夏银川 750021

收稿日期:2023-11-21 接受日期:2024-01-14 出版日期:2024-04-18 发布日期:2024-04-15
通讯作者: *电子信箱: chenzhe0809@foxmail.com (陈哲), lilingling2013@163.com (李铃铃), wangxin@nxu.edu.cn (王鑫).
基金资助:
国家自然科学基金(22278172);吉林省教育厅项目(YDZJ202201ZYTS591);吉林省教育厅项目(20210509049RQ);吉林省教育厅项目(JJKH20230287KJ);青年成长科技项目(20230508144RC);吉林市科技创新发展计划项目(20240103016)

Facile electrospinning synthesis of S-scheme heterojunction CoTiO₃/g-C₃N₄ nanofiber with enhanced visible light photocatalytic activity

Lingkun Yang^a, Zongjun Li^a, Xin Wang^b^,^*(), Lingling Li^a^,^*(), Zhe Chen^a^,^*()

^aSchool of Material Science and Technology, Jilin Institute of Chemical Technology, Jilin 132022, Jilin, China
^bState Key Laboratory of High-Efficiency Utilization of Coal and Green Chemical Engineering, National Demonstration Center for Experimental Chemistry Education, College of Chemistry and Chemical Engineering, Ningxia University, Yinchuan 750021, Ningxia, China

Received:2023-11-21 Accepted:2024-01-14 Online:2024-04-18 Published:2024-04-15
Contact: *E-mail: chenzhe0809@foxmail.com (Z. Chen), lilingling2013@163.com (L. Li), wangxin@nxu.edu.cn (X. Wang).
Supported by:
The National Natural Science Foundation of China(22278172);The Education Department Project of Jilin Province(YDZJ202201ZYTS591);The Education Department Project of Jilin Province(20210509049RQ);The Education Department Project of Jilin Province(JJKH20230287KJ);The Youth Growth Fund(20230508144RC);Jilin Science and Technology Innovation Development Program Project(20240103016)

摘要/Abstract

摘要：

随着社会的高速发展, 化石燃料的消耗量急剧上升, 这不仅导致了能源的短缺, 而且引发了二氧化碳(CO₂)及其他有害气体的过量排放, 造成环境污染. 利用太阳能将CO₂光催化转化为碳基燃料是解决上述问题的一种有效途径. 在众多半导体光催化材料中, 钙钛矿氧化物(CoTiO₃)由于具有独特的电子和晶体结构以及较好的稳定性而备受关注. 然而, 由于单一半导体光催化剂中光生电子-空穴对的复合率较高, 导致其催化还原CO₂的能力有限, 制约了其在可见光催化反应中的实际应用. 研究发现, 构建异质结是提高半导体光催化还原CO₂效率的重要策略之一, 因此寻找可与CoTiO₃能带结构很好匹配的半导体材料至关重要. 近年来, 有机聚合物g-C₃N₄因具有独特的层状结构、较好的热稳定性和化学稳定性, 对可见光响应性能良好而受到人们的关注. 本研究旨在构建g-C₃N₄与CoTiO₃的S型异质结, 以优化体系中光生载流子分离效率, 从而有效提升光催化性能.

本文首先采用静电纺丝法制备出CoTiO₃纳米纤维, 然后通过一步煅烧法构建CoTiO₃/g-C₃N₄ S型异质结光催化剂. X射线衍射仪、傅里叶红外光谱仪、扫描电镜和透射电镜结果证实成功制得了CoTiO₃/g-C₃N₄复合光催化剂. 在可见光照射下, 测试了不同CoTiO₃质量百分含量(0.5%, 1%, 1.5%, 2%和3%, 命名为0.5% CTO/CN, 1% CTO/CN, 1.5% CTO/CN, 2% CTO/CN和3%CTO/CN)的CoTiO₃/g-C₃N₄ S型异质结光催化剂对CO₂的还原能力(反应时间为4 h). 结果发现, 2% CTO/CN催化剂显示出最高的光催化性能, 其催化生成CO和CH₄的产率分别为46.5和0.825 mol g^-1 h^-1, 且生成CO的选择性为98.3%. 同时, 为了进一步验证光催化性能增强规律, 作为补充实验, 进行了盐酸四环素(TCH)、土霉素(OTC)和氧氟沙星(OFX)光催化降解实验. 结果表明, 2% CTO/CN表现出最高的光催化降解效率, 2% CTO/CN在光催化CO₂还原和抗生素降解方面均表现出较好的催化性能, 这归因于g-C₃N₄与CoTiO₃之间S型异质结的形成. 此外, 为了讨论光催化还原CO₂的选择性, 采用原位红外和理论计算得到中间体的活化过程及其吉布斯自由能, 并利用同位素标定实验进一步确认了光催化还原CO₂反应产物中碳源均来自于CO₂气氛.

经过稳态荧光、时间分辨荧光、瞬态光电流响应和电化学阻抗图谱测试进一步验证表明, 2% CTO/CN异质结的形成降低了光生电子-空穴对的复合率和界面电荷转移电阻, 为电荷转移提供了更好的路径, 从而提高了光催化性能. 为了深入探究S型异质结的反应机理, 通过原位X射线光电子能谱、原位电子顺磁共振和密度泛函理论计算研究了光照前后界面处电子流向. 具体来说, 在g-C₃N₄和CoTiO₃接触之前, g-C₃N₄的功函数小于CoTiO₃, 费米能级高于CoTiO₃; 当g-C₃N₄和CoTiO₃接触时, 电子会从g-C₃N₄转移到CoTiO₃, 直到它们的费米能级达到平衡. 此时, g-C₃N₄侧的界面电子耗尽, CoTiO₃侧的界面电子富集, 使g-C₃N₄的带边向上弯曲带正电, 而CoTiO₃的带边向下弯曲带负电. 从而, 在CTO/CN的界面处形成了内建电场(IEF), 阻碍电子从g-C₃N₄向CoTiO₃的持续流动. 光照时, 光子同时被CoTiO₃和g-C₃N₄吸收, 激发电子从价带跃迁至相应的导带. 随后, 在形成的IEF驱动下, CoTiO₃中的光生电子倾向于迁移到g-C₃N₄, 与g-C₃N₄中的光生空穴结合, 使得体系中还原性和氧化性更强的电子和空穴得以保留, 从而进一步提高光催化性能. 综上, S型电荷转移途径不仅促进了光生载流子的分离, 使得更多电子参与反应, 而且同时保留了还原性和氧化性较强光生电子和空穴, 因此, CTO/CN在光催化还原CO₂和降解抗生素方面表现出较好的性能. 本文为基于g-C₃N₄的S型异质结材料在CO₂光还原和抗生素降解领域的应用提供参考.

关键词: 静电纺丝, S型异质结, g-C₃N₄, 光催化降解, 光催化还原CO₂

Abstract:

Photocatalysts featuring S-scheme heterojunctions offer considerable potential for both the photocatalytic CO₂ conversion and the degradation of antibiotics, providing practical solutions for energy crises and environmental challenges. In this work, 1D/2D CoTiO₃/g-C₃N₄ (CTO/CN) S-scheme heterojunction is synthesized through electrospinning and calcination. The close interweaving of g-C₃N₄ nanosheets around CoTiO₃ nanofibers creates ample contact areas and active sites, resulting in exceptional photocatalytic CO production capability. The optimal mass ratio of CoTiO₃ to g-C₃N₄ is 2%, and the CO and CH₄ yields are 46.5 and 0.825 μmol g^-1 h^-1. Moreover, comparing with monomeric g-C₃N₄, this composite achieves a better CO yield with 43.5 times and displays an impressive product selectivity of 98.3% for CO₂-CO photoreduction. In addition, the 2% CTO/CN photocatalyst demonstrates outstanding photocatalytic degradation efficiency, with degradation rates of 95.88%, 95.53%, and 71.23% for tetracycline hydrochloride, oxytetracycline, and ofloxacin, respectively. These enhanced photocatalytic properties are attributed to the S-scheme system constructed by CoTiO₃ with g-C₃N₄, maintaining strong oxidation-reduction capabilities while efficiently segregating photogenerated charges, with the existence of S-scheme heterojunction confirmed through various analyses. Furthermore, in situ studies and ¹³C calibration experiments reveal that CO and CH₄ originate from the photocatalytic CO₂conversion, further highlighting the potential of this work in advancing CO₂ photoreduction. This study offers novel insights into designing effective S-scheme heterojunction photocatalysts for practical applications to address environmental and energy challenges.

Key words: Electrospinning, S-scheme, g-C₃N₄, Photocatalytic degradation, Photocatalytic CO₂ reduction

杨令坤, 李宗军, 王鑫, 李铃铃, 陈哲. 静电纺丝法合成S型异质结CoTiO₃/g-C₃N₄纳米纤维及其增强的可见光光催化活性研究[J]. 催化学报, 2024, 59: 237-249.

Lingkun Yang, Zongjun Li, Xin Wang, Lingling Li, Zhe Chen. Facile electrospinning synthesis of S-scheme heterojunction CoTiO₃/g-C₃N₄ nanofiber with enhanced visible light photocatalytic activity[J]. Chinese Journal of Catalysis, 2024, 59: 237-249.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(23)64566-8

https://www.cjcatal.com/CN/Y2024/V59/I4/237

图/表 15

Scheme 1. Schematic of the formation process for CTO/CN composites.

Fig. 1. XRD patterns (a) and FTIR spectra (b) of CoTiO3, g-C3N4, and 2% CTO/CN.

Fig. 2. SEM (a), TEM (b), and HRTEM (c) images and EDS spectra (d-i) of CTO/CN.

Fig. 3. (a) Full spectra of the prepared samples. High-resolution XPS spectra of C 1s (b), N 1s (C), Co 2p (d), Ti 2p (e), and O 1s (f).

Fig. 4. (a) N2 adsorption-desorption isotherms and (b) pore size distribution curves for g-C3N4, CoTiO3, and 2% CTO/CN.

Fig. 5. (a) CO and CH4 yields of as-prepared catalysts. (b) Cyclic CO2 photoreduction performance using 2% CTO/CN as the catalyst. (c) XRD pattern of 2% CTO/CN after photocatalytic cycling. (d) TEM image of 2% CTO/CN after cycling in photocatalytic reactions. (e) Photocatalytic degradation rates of TCH, OTC, and OFX antibiotics and their corresponding degradation kinetics (f) for the as-prepared samples.

Fig. 6. (a) In situ FTIR results of CO2 absorption and photocatalytic CO2 reduction on 2% CTO/CN under light of 420 nm. (b) GC-MS results of 13CO2 isotope calibration test.

Fig. 7. Gibbs free energy diagrams of CO2 photoreduction to CO/CH4 over CTO/CN.

Fig. 8. UV-Vis DRS (a), Tauc plot for bandgap (b), PL spectra (c), and TRPL decay curve (d) of g-C3N4, CoTiO3 and 2% CTO/CN.

Fig. 9. (a) EIS tests of as-prepared samples. (b) Transient photocurrent of the as-prepared samples. Mott-Schottky curve of (c) of g-C3N4 and (d) CoTiO3.

Fig. 10. Structure models of g-C3N4 (a) and CoTiO3 (d). Corresponding DOS of g-C3N4 (b) and CoTiO3 (e). Work function of g-C3N4 (c) and CoTiO3 (f).

Fig. 11. Planar-averaged charge density difference for (a) and (b) 2% CTO/CN as a function of position in the z-direction. A positive value indicates electron accumulation; a negative value indicates electron depletion.

Fig. 12. (a) Full spectra of prepared samples. In situ irradiation XPS spectra of C 1s (b), N 1s (c), Co 2p (d), Ti 2p (e), and O 1s (f).

Fig. 13. DMPO-?O2- (a) and DMPO-?OH (b) signal peaks of pure g-C3N4, CoTiO3, and 2% CTO/CN.

Fig. 14. Schematic of light-induced carrier transfer in the CTO/CN composite.

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静电纺丝法合成S型异质结CoTiO₃/g-C₃N₄纳米纤维及其增强的可见光光催化活性研究

Facile electrospinning synthesis of S-scheme heterojunction CoTiO₃/g-C₃N₄ nanofiber with enhanced visible light photocatalytic activity

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