Synergistic catalysis of oxygen vacancy and S-scheme heterojunction in NiFe2O4‒x/NiS regulates peroxymonosulfate activation for enhanced photo-Fenton-like reaction

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

Abstract

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

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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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(25)64841-8

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

Figures/Tables 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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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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