氧空位协同S型NiFe2O4-x/NiS异质结调控过氧单硫酸盐活化增强类光芬顿反应

doi:10.1016/S1872-2067(25)64841-8

催化学报 ›› 2025, Vol. 79: 186-204.DOI: 10.1016/S1872-2067(25)64841-8

氧空位协同S型NiFe₂O_4-_x/NiS异质结调控过氧单硫酸盐活化增强类光芬顿反应

王艳^a, 严晓蕊^a, 孙泽洋^a, 刘进军^a, 王义文^a, 胡陈超^a, 邓伊琳^b, 谢萌^c^,^*(), 谢吉民^d^,^*(), 张伟^b, 徐远国^a^,^*()

^a江苏大学化学化工学院, 江苏镇江212013
^b江苏大学能源研究院, 江苏镇江212013
^c江苏大学药学院, 江苏镇江212013
^d江苏江科石墨烯研究院有限公司, 江苏镇江212000

收稿日期:2025-06-03 接受日期:2025-08-13 出版日期:2025-12-05 发布日期:2025-10-27
通讯作者: 谢萌,谢吉民,徐远国
基金资助:
2024年度镇江市科技计划(产业前瞻与性关键技术(GJ2024012);2024年度镇江市科技计划(产业前瞻与性关键技术(GY2024027);江苏省自然科学基金(BK20221295);国家自然科学基金(22076068);国家自然科学基金(21777063)

Synergistic catalysis of oxygen vacancy and S-scheme heterojunction in NiFe₂O_4‒_x/NiS regulates peroxymonosulfate activation for enhanced photo-Fenton-like reaction

Yan Wang^a, Xiaorui Yan^a, Zeyang Sun^a, Jinjun Liu^a, Yiwen Wang^a, Chenchao Hu^a, Yilin Deng^b, Meng Xie^c^,^*(), Jimin Xie^d^,^*(), Wei Zhang^b, Yuanguo Xu^a^,^*()

^aSchool of Chemistry and Chemical Engineering, Jiangsu University, Zhenjiang 212013, Jiangsu, China
^bInstitute for Energy Research, Jiangsu University, Zhenjiang 212013, Jiangsu, China
^cSchool of Pharmacy, Jiangsu University, Zhenjiang 212013, Jiangsu, China
^dJiangsu Jiangke Graphene Research Institute Co., Ltd., Zhenjiang 212000, Jiangsu, China

Received:2025-06-03 Accepted:2025-08-13 Online:2025-12-05 Published:2025-10-27
Contact: Meng Xie, Jimin Xie, Yuanguo Xu
Supported by:
Fundamental Research and Development Plan of Zhenjiang City in 2024(Common Key Technologies)(GJ2024012);Fundamental Research and Development Plan of Zhenjiang City in 2024(Common Key Technologies)(GY2024027);Jiangsu Provincial Natural Science Foundation(BK20221295);National Natural Science Foundation of China(22076068);National Natural Science Foundation of China(21777063)

摘要/Abstract

摘要：

基于过氧单硫酸盐(PMS)的水净化高级氧化工艺易受到缓慢的激活速率阻碍, 这主要是由于传质过程的复杂性以及电子转移效率的限制所致. 通过类光芬顿氧化工艺, 借助光催化剂激活PMS来产生高活性氧物种(ROS), 已被证明是一种清洁且有效的处理技术, 能够高效去除水体环境中持久性有机污染物. 通过构建S型异质结可以有效促进电荷载流子的传输, 有利于提高PMS的激活效率. 此外, 空位的引入对催化剂内部的电子结构的调控具有关键作用, 可进一步提高PMS的吸附效率. 因此, 通过构建氧空位和异质协同调控PMS活化对于水体中有机污染物的降解至关重要, 但仍然是一个巨大的挑战.
本文创新性的设计了一种由乙二醇(EG)辅助构建氧空位(V_O)修饰的S型NiFe₂O_4-_x/NiS异质结的策略, 通过光激发PMS有效去除吡虫啉(IMD)有机污染物, 实现了99%的PMS分解效率. 原位辐照开尔文探针原子力显微镜及电子自旋共振表征证实了NiFe₂O_4-_x/NiS异质结中S型电荷转移机制的形成, 为IMD的氧化提供了丰富的活性位点和独特的电荷转移路径. 在低剂量PMS条件下(0.1 g/L), S型NiFe₂O_4-_x/NiS异质结在类光芬顿反应体系中表现出显著增强的降解速率(0.15 min^-1), 该速率是单组分NiS催化剂的19倍(0.0077 min^-1). 密度泛函理论计算证实, NiFe₂O_4-_x/NiS中V_O协同异质结能有效促进PMS的吸附, 并降低电子转移的能量障碍. 此外, 通过一系列的原位表征和实验证据相结合发现, S型异质结促进的电荷转移过程极大地加快了PMS的活化, 并提高其利用效率, 从而增强其在IMD氧化反应中的反应活性; 为NiFe₂O_4-_x/NiS通过光激发的PMS活化机制提供了机理上的见解, 表明IMD在NiFe₂O_4‒_x/NiS/Vis/PMS系统中的降解主要由自由基驱动和非自由基辅助的氧化过程共同驱动, 揭示了反应过程中涉及PMS还原和氧化过程的双重途径活化机制; 并提出了NiFe₂O_4-_x/NiS异质结中基于S型电荷转移通道增强PMS活化的路径: (1)富电子S^2-和Ni⁰物质协同PMS显著加速了Ni²⁺/Ni³⁺和Fe²⁺/Fe³⁺的氧化还原循环; (2)来自富电子V_O位点的光生电子转移极大的促进活性位点到PMS的电子穿梭, 有利于PMS和O₂的活化以产生自由基. 此外, 连续流反应器和生态毒性实验表明, 光激发NiFe₂O_4-_x/NiS协同激活PMS的新型氧化系统在去除有机污染物方面具有稳定性及对有机污染物的解毒能力, 突显了其在可持续水净化领域具有良好的应用潜力.
综上, 本文为设计用于非均相类光芬顿系统的催化剂提供了重要见解, 拓展了NiS材料在水净化方面的潜在应用; 强调了空位工程协同S型异质结在开发用于调控PMS活化的高效催化剂方面的潜力, 为实现有机污染物废水的经济高效处理提供了一种极具前景的解决方案.

关键词: S型异质结, 氧空位, 类光芬顿, 过氧单硫酸盐活化, 污染物降解

Abstract:

The regulation of peroxymonosulfate (PMS) activation by constructing oxygen vacancy and heterogeneous interface catalytic is crucial towards the oxidation of refractory pollutants still remains a major hurdle. This work demonstrates a strategy to constructed ethylene glycol (EG) well-coupled S-scheme heterojunction of NiFe₂O_4‒_x/NiS with oxygen vacancy (V_O)-modified to efficiently achieve pollutant removal by activating PMS through photoexcitation, a 99% PMS decomposition efficiency is achieved. Photoassisted Kelvin probe force microscopy and in-situ electron spin resonance verify the establishment of a charge-transfer pathway consistent in NiFe₂O_4-_x/NiS with an S-scheme heterojunction, which dramatically provides abundant active sites and distinct charge transport pathway for organic pollutant oxidation. The S-scheme NiFe₂O_4-_x/NiS heterojunction in the photo-Fenton-like system exhibited significantly enhanced degradation rate (0.15 min^-1) at a low PMS dosage of 0.1 g/L, which is 19 times greater than that of the pristine NiS (0.0077 min^-1). Density functional theory calculations confirmed that V_O in NiFe₂O_4-_x/NiS efficiently promoted PMS adsorption and lowered the energy barrier for electron transfer. Moreover, in-situ experiments and experimental evidence offer mechanistic insights into the PMS activation through photoexcitation, unraveling a dual-pathway activation mechanism involving reduction and oxidation processes over NiFe₂O_4-_x/NiS during the reaction. This work emphasizes the potential of vacancy engineering synergistic S-scheme heterojunction in developing efficient catalysts for regulating PMS activation, providing a promising solution the cost-effective and efficient treatment of organic wastewater.

Key words: S-scheme heterojunction, Oxygen vacancy, Photo-Fenton-like, Peroxymonosulfate activation, Pollution degradation

王艳, 严晓蕊, 孙泽洋, 刘进军, 王义文, 胡陈超, 邓伊琳, 谢萌, 谢吉民, 张伟, 徐远国. 氧空位协同S型NiFe₂O_4-_x/NiS异质结调控过氧单硫酸盐活化增强类光芬顿反应[J]. 催化学报, 2025, 79: 186-204.

Yan Wang, Xiaorui Yan, Zeyang Sun, Jinjun Liu, Yiwen Wang, Chenchao Hu, Yilin Deng, Meng Xie, Jimin Xie, Wei Zhang, Yuanguo Xu. Synergistic catalysis of oxygen vacancy and S-scheme heterojunction in NiFe₂O_4‒_x/NiS regulates peroxymonosulfate activation for enhanced photo-Fenton-like reaction[J]. Chinese Journal of Catalysis, 2025, 79: 186-204.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64841-8

https://www.cjcatal.com/CN/Y2025/V79/I12/186

图/表 9

Fig. 1. Schematic description the preparation procedure of the NiFe2O4-x/NiS (a), NiFe2O4-x (b), NiS (c), NiFe2O4-x /NiS (d) SEM images, SEM-coupled element mapping of NiFe2O4-x/NiS (scale bar: 2 μm), Ni: blue, S: yellow, O: green, Fe: red (e). TEM (f) and HRTEM images (g) of NiFe2O4-x/NiS. EPR spectra (h).

Fig. 2. XRD patterns (a), XPS survey spectra (b), Ni 2p (c), S 2p (d), Fe 2p (e), and O 1s (f) XPS spectra.

Fig. 3. UV-vis DRS spectra (a), Mott-Schottky plots (b) of NiS (left) and NiFe2O4?x (right). (c) UPS spectra of NiS (left) and NiFe2O4?x (right). (d) Schematic energy-level diagram, DMPO-?OH (e), DMPO-O2?-. (f) ESR spectra over NiS, NiFe2O4?x and NiFe2O4?x/NiS under visible-light irradiation.

Fig. 4. AFM topographic images of NiFe2O4-x/NiS (a), line-scanning surface potential curve in dark condition (b) and visible-light irradiation (c). TRPL spectra (d), SPV spectra (e), transient photocurrent responses (f), Nyquist plots (g), the S-scheme-mediated charge transfer (h) of NiFe2O4-x/NiS heterojunction.

Fig. 5. Degradation curves by the NiS, NiFe2O4-x, and NiFe2O4-x/NiS (a) and corresponding first-order kinetic rate constants (b). IMD degradation with different NiFe2O4-x/NiS systems (c) and corresponding kinetic rate constants (d). (e) Removal of multiple pollutants in NiFe2O4-x/NiS/Vis/PMS system. (f) IMD degradation performance over NiFe2O4/NiS with different VO concentrations. (g) The decomposition efficiency of PMS under different systems. (h) EPR spectra of NiFe2O4-x/NiS before and after photo-Fenton-like reaction. (i) Comparison of specific rate constant activity (kN, min-1 g-2) among the heterogeneous PMS-AOPs materials. Experimental conditions: [IMD]0 = 10 mg/L, [Catalyst] = 0.2 g/L, [PMS]0 = 0.1 g/L, initial pH= 7.0. [PMS]0 = 0.1 g/L, initial pH= 7.0, 30 °C, light intensity 38.2 mW/cm2.

Fig. 6. O2?- (a) and ?OH/SO4?- (b) captured by DMPO. 1O2 captured by TEMP ESR spectra (c), ROSs-quenching experiments (d), corresponding first-order kinetic rate constants (e) (insert: degree of contribution of the degradation path way), the EPR spectra (f) for ROSs, both with and without IMD, in NiFe2O4-x/NiS/Vis/PMS system, OCP curves with injection of PMS and IMD (g), and injection of IMD and PMS (h). Chronoamperometry curves with injection of PMS and IMD (i), and injection of IMD and PMS (j). (k) In-situ Raman spectra.

Fig. 7. Comparison of Ni 2p (a), Fe 2p (b), S 2p (c) and O 1s (d) XPS spectra before and after reaction over NiFe2O4-x/NiS/Vis/PMS system. (e) PMS adsorption energy. (f) Baer charge transfer to PMS. (g) O-O bond and O-H bond length of different PMS adsorption catalytic models. (h) ROSs generation during PMS activation over NiFe2O4-x/NiS. (i) Proposed enhancement catalytic mechanism of NiFe2O4-x/NiS/Vis/PMS system.

Fig. 8. Effects of catalyst dosage (a), PMS concentration (b), pH values (c), coexisting anions (d), different water matrices and HA concentrations (e). (f) Cyclic degradation of IMD. (g) The degradation efficiency of complex organic pollutants, involving ATZ, OFX, TC and IMD, [Catalyst] = 0.4 g/L, [PMS]0 =0.2 g/L, [Pollutants]0 = 1 ppm, initial pH = 7. (h) Continuous operation test for IMD degradation in the flow-through system (inset: the actual device image), reaction parameters: [PMS]0 =0.1 g, [Catalyst] = 0.2 g, [IMD]0 = 10 ppm, flow rate = 3 mL/min, initial pH = 7.

Fig. 9. (a) The possible pathways for IMD degradation over NiFe2O4-x/NiS/Vis/PMS. Estimation acute and chronic toxicity on fish, daphnid, and green algae using ECOSAR (h), toxicity analysis using T.E.S.T software (b-d). Photographs pine willow plants after different treatments (e), relative viability of LX-2 cells using a CCK-8 assay (f), living/dead LX-2 cells stained with Calcein-AM/PI (g).

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氧空位协同S型NiFe₂O_4-_x/NiS异质结调控过氧单硫酸盐活化增强类光芬顿反应

Synergistic catalysis of oxygen vacancy and S-scheme heterojunction in NiFe₂O_4‒_x/NiS regulates peroxymonosulfate activation for enhanced photo-Fenton-like reaction

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