Multispectral solar-driven detoxification by S-scheme Ag2S/Co1-xS@Co9S8@C nanocatalyst of emerging persistent organic pollutant-levofloxacin

doi:10.1016/S1872-2067(26)65179-0

Abstract

Abstract:

Strategic regulation of photogenerated carriers along with efficient utilization of full solar spectrum is a crucial approach in photocatalytic reactions. In this aspect, creating S-scheme heterojunction efficiently promotes the spatial segregation of photogenerated charge carriers for participation in photoreactions. Herein, Ag₂S/Co_1-_xS@Co₉S₈@C (A-CCC) S-scheme heterojunction nanocatalysts was synthesized, demonstrating outstanding photocatalytic degradation efficiency under simulated solar light irradiation ranging from ultraviolet to near-infrared owing to strong interfacial electric field. Morphological and structural analyses via scanning electron microscopy, high-resolution transmission electron microscopy, X-ray diffraction, Raman, and in-situ-X-ray photoelectron spectroscopy confirmed the retention of the Co-ZIF-67-derived octahedral morphology with uniform Ag₂S nanoparticle distribution and formation of distinct Co_1-_xS and Co₉S₈ phases embedded in a carbon matrix. Ultraviolet photoelectron spectroscopy and band gap measurements elucidated an S-scheme heterojunction configuration driven by an internal electric field, promoting interfacial charge. A steady-state THz time-domain spectroscopy in transmission mode and multi-exponential time resolved photoluminescence spectra fitting and calculated amplitude-weighted and intensity-weighted lifetimes (~2.38 ns) demonstrated significant interfacial charge separation within the 5A-CCC. The 5 wt% Ag₂S-CCC (5A-CCC) nanocatalysts endows exceptional photocatalytic activity for environmentally persistent antibiotic levofloxacin (LCN) degrading about 99.7% with an apparent rate constant of 0.0326 min^-1 in 40 min reaction duration due to extended light absorption till near infra-red region for effective solar to thermal conversion (13.6%). Radical scavenging and reactive oxygen species probe studies revealed O₂^•- as the dominant active species, participated effectively in LCN degradation. For LCN degradation, fragmentation and intermediate products were observed using liquid chromatography-mass spectrometer. This study features a highly effective photocatalytic system and offers essential insights towards full-spectrum functioning nanocatalysts for environmental detoxification of persistent antibiotics.

Key words: Persistent organic pollutants, Levofloxacin, Full-solar spectrum, S-scheme heterojunction, Interfacial charge transfer

Sangeeta Adhikari, Sandip Mandal, Do-Heyoung Kim. Multispectral solar-driven detoxification by S-scheme Ag₂S/Co_1-xS@Co₉S₈@C nanocatalyst of emerging persistent organic pollutant-levofloxacin[J]. Chinese Journal of Catalysis, 2026, 89: 310-325.

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Figures/Tables 10

Fig. 1. (a) Schematic synthesis process of the A-CCC nanocatalysts. HRSEM images of Co1-xS@Co9S8@C (b) and 5% Ag2S/Co1-xS@Co9S8@C (c,d) nanocatalysts.

Fig. 2. TEM, HR-TEM, and elemental mapping of Co1-xS@Co9S8@C (a-c) and 5 wt% Ag2S/Co1-xS@Co9S8@C (d-f). (g) XRD patterns of the synthesized nanocatalysts. Raman spectra (h) and FTIR spectra (i) of CCC, Ag2S, and 5A-CCC nanocatalysts.

Fig. 3. High-resolution XPS profiles of Co 2p (a), S 2p (b), and Ag 3d (c) in CCC, Ag2S, and 5A-CCC. (d) UV-vis spectra of the powdered nanocatalysts. (e) Tauc plots of Ag2S nanocatalysts. (f) PL spectra of the powdered nanocatalysts. (g) Photocurrent response of CCC, Ag2S, and 5A-CCC nanocatalyst electrodes with 10 s light on/o? intervals. (h) EIS spectra of CCC, Ag2S, and 5A-CCC nanocatalyst electrodes. (i) LSV spectra of CCC and 5A-CCC nanocatalyst electrodes.

Fig. 4. NIR thermal images of the CCC, Ag2S, and 5A-CCC nanocatalysts at different NIR illumination durations. CCC(a-e), Ag2S (f-j) and 5A-CCC (k-o). All images were captured by an infrared thermal imager

Fig. 5. (a,b) UPS spectra of CCC and Ag2S nanocatalyst. (c) Band structure configuration, IEF formation, and proposed S-scheme charge transfer mechanism at the 5A-CCC nanocatalyst heterojunction.

Fig. 6. Photocatalytic experiments under the irradiation of UV (a), Visible + NIR (b), NIR light (c), and full solar spectrum (simulated solar light) (d). (e) Degradation percentages under different light conditions. (f) Rate constants for CCC, Ag2S, and 5A-CCC nanocatalysts. (g) LCN degradation with varying 5A-CCC nanocatalysts amounts. (h) LCN degradation time vs. LCN concentration. (i) LCN degradation efficiency with effect of co-existing ions using 5A-CCC nanocatalysts under simulated solar light (error bars represent in Figs. 6(a)-(d) and 6(g)-(h), the standard deviation (SD ≤ ±2%) of three independent experiments under same conditions).

Table 1 Photodegradation efficiencies and kinetics for LCN over different nanocatalysts under simulated solar irradiation.

Catalyst	Adsorption (%)	Photooxidation efficiency (%)	k in 30 min (min^-1)	R²
LCN = 20 ppm, catalyst = 20 mg, and reaction time = 40 min
CCC	8	46.0	0.00377	0.99
Ag₂S	2	13.3	8.41E^-4	0.99
2A-CCC	15	66.0	0.0054	0.97
5A-CCC	17	99.7	0.0326	0.98
10A-CCC	16	73.0	0.0121	0.97

Fig. 7. (a) Cyclic photocatalytic LCN degradation by 5A-CCC nanocatalyst. Characterizations of spent 5A-CCC nanocatalyst after 7 consecutive cyclic experiments: (b) XRD pattern before and after catalysis action. High-resolution XPS of Co 2p (c), Ag 3d (d), and S 2p (e) from spent 5A-CCC nanocatalyst. (f) HRSEM micrograph of spent 5A-CCC nanocatalyst. (g) High-resolution TEM images of spent 5A-CCC nanocatalyst. (h) EDAX spectra obtained from HRTEM micrographs for spent 5A-CCC nanocatalyst after seven consecutives cycles.

Fig. 8. (a) Scavenger studies. (b) NBT concentration versus nanocatalyst. (c) PL spectra of 2HTA using CCC, Ag2S, and 5A-CCC nanocatalysts. (d) S-scheme charge transfer mechanism. (e) PRF comparison of the prepared nanocatalysts with reported catalysts from Table 2. (f) Radar plot includes catalyst concentration, pollutant concentration, degradation efficiency, reaction time, light source and PRF for nanocatalysts from Table 2 (A: CoWO4/Bi4O5I2; B: CaTiO3@Ag@ZnO; C: Bi2MoO6-SOVs/ZnCdS; D: Bi5O7I/Bi2O2CO3/Ag2CO3; E: B doped BiVO4/Bi; and F: 5A-CCC). (g) Schematic representation of Photocatalytic-Photothermal synergy in 5A-CCC nanocatalyst. (error bars represent in Fig. 8(a), the standard deviation (SD ≤ ±2%) of three independent experiments under same conditions).

Table 2 PRF values of different nanocatalysts used in photocatalytic LCN degradation in a wastewater system.

Catalyst	Cat. conc. (g L^-1)	Pollutant conc. (mg L^-1)	Degradation efficiency (%)	Reaction time (adsorption + photocatalysis in min)	Light source	PRF (mg W^-1 min^-1 L^-1)	Ref.
CoWO₄/Bi₄O₅I₂	0.5	5	86.3	40	300 W Xe-lamp	0.0071	[71]
CaTiO₃@Ag@ZnO	1	10	90	100	55 W Xe-lamp	0.0163	[72]
Bi₂MoO₆-SOVs/ZnCdS	0.625	20	95.9	30	300 W Xe-lamp	0.0106	[73]
Bi₅O₇I/Bi₂O₂CO₃/Ag₂CO₃	0.5	10	86.9	60	300 W Xe-lamp	0.0048	[74]
B doped BiVO₄/Bi	0.2	30	61.09	70	300 W Xe-lamp	0.00290	[75]
5A-CCC	1	20	99.7	40	150 W Xe-lamp	0.016	This work

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Multispectral solar-driven detoxification by S-scheme Ag₂S/Co_1-xS@Co₉S₈@C nanocatalyst of emerging persistent organic pollutant-levofloxacin

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