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Plasmonic metallic Bi-modified defective Bi4Ti3O12 nanosheets with upward migrating electrons for efficient photocatalytic NO removal and NO2 inhibition
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Wenjie Hea, b, Lin Jinga, Wendong Zhangc, Xing'an Dongb, d, Yan Zoub, Xin Liua, Xin Lva, Peng Chenc, Jiazhen Liaoa, Xiao Zhangc, Rong Xiaoc, Yuechang Weie
Chinese Chemical Letters | 2026, 37(2) : 111357
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Chinese Chemical Letters | 2026, 37(2): 111357
• Communication •
Plasmonic metallic Bi-modified defective Bi4Ti3O12 nanosheets with upward migrating electrons for efficient photocatalytic NO removal and NO2 inhibition
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Wenjie Hea, b, Lin Jinga, Wendong Zhangc, Xing'an Dongb, d, Yan Zoub, Xin Liua, Xin Lva, Peng Chenc, Jiazhen Liaoa, Xiao Zhangc, Rong Xiaoc, Yuechang Weie
Affiliations
  • aChongqing Polytechnic University of Electronic Technology, Chongqing 401331, China
  • bEngineering Research Center for Waste Oil Recovery Technology and Equipment, Ministry of Education, Chongqing Technology and Business University, Chongqing 400067, China
  • cChongqing Key Laboratory of Green Synthesis and Application, College of Chemistry, Chongqing Normal University, Chongqing 401331, China
  • dCollege of Physics and Electronic Engineering, Chongqing Normal University, Chongqing 401331, China
  • eState Key Laboratory of Heavy Oil Processing, Key Laboratory of Optical Detection Technology for Oil and Gas, China University of Petroleum, Beijing 102249, China
About Author:

CRediT authorship contribution statement

Wenjie He: Writing – original draft, Methodology, Funding acquisition, Formal analysis, Data curation, Conceptualization.

Lin Jing: Writing – review & editing, Investigation, Data curation.

Wendong Zhang: Methodology.

Xing'an Dong: Funding acquisition, Formal analysis, Data curation.

Yan Zou: Data curation.

Xin Liu: Formal analysis.

Xin Lv: Formal analysis.

Peng Chen: Methodology, Formal analysis.

Jiazhen Liao: Methodology, Funding acquisition.

Xiao Zhang: Investigation.

Rong Xiao: Investigation.

Yuechang Wei: Writing – review & editing, Methodology, Conceptualization.

Published: 2026-02-15 doi: 10.1016/j.cclet.2025.111357
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The limited redox capability of photocatalysts often leads to harmful NO2 byproduct formation during photocatalytic NO oxidation. Herein, Bi4Ti3O12 nanosheets modified with plasmonic metallic bismuth and abundant oxygen vacancies were synthesized via an in-situ reduction method. The optimized catalyst (BTOR2, with a molar ratio of 40% NaBH4 to Bi4Ti3O12) achieved a maximum NO removal efficiency of 62.3%, significantly higher than pristine Bi4Ti3O12 (40.5%) while minimizing NO2 production. The results reveal that the synergistic effects of Bi's plasmonic resonance and oxygen vacancies enhanced visible light absorption and charge separation. The density functional theory (DFT) analysis showed electrons can transfer from Bi4Ti3O12 to Bi, promoting O2 activation to •O2- radicals. In-situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) confirmed that light-induced H2O adsorption was strengthened, improving •OH radical generation. These radicals promoted the selective conversion of activated NO- to NO3-, rather than NO2. This work provides valuable insights for advancing research into efficient photocatalysts for air pollution control.

Plasmonic metallic bismuth  /  Oxygen vacancy  /  Bi4Ti3O12  /  NO2 inhibition  /  Photocatalysis mechanism
Wenjie He, Lin Jing, Wendong Zhang, Xing'an Dong, Yan Zou, Xin Liu, Xin Lv, Peng Chen, Jiazhen Liao, Xiao Zhang, Rong Xiao, Yuechang Wei. Plasmonic metallic Bi-modified defective Bi4Ti3O12 nanosheets with upward migrating electrons for efficient photocatalytic NO removal and NO2 inhibition[J]. Chinese Chemical Letters, 2026 , 37 (2) : 111357 - . DOI: 10.1016/j.cclet.2025.111357
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Over the past half-century, photocatalysis has been widely applied to environmental control [1-3], including antibiotic degradation [4], VOCs removal [5], and Cr(VI)-containing wastewater purification [6]. The performance of photocatalytic reactions depends on factors such as light absorption, electron-hole separation, active radical generation, and surface oxidation capacity. To enhance photocatalytic performance, the photoelectric properties of materials must be adjusted, typically by introducing heteroatoms or composites to disrupt the material's charge balance, thereby improving light absorption, charge separation, and carrier migration [7-10].
The efficient generation of surface-active radicals is essential for pollutant degradation, which requires rapid light response and carrier transfer to the catalyst surface. Researchers have optimized material properties through ion doping, metal loading, and defect construction to improve performance [11-14]. For low-concentration atmospheric NO purification, low-energy consumption photocatalysis is an ideal choice [15]. However, in continuous flow reactors, the catalyst's deep oxidation capacity is limited, and surface deactivation caused by by-products affects NO degradation efficiency [16, 17]. Additionally, the by-product NO2, is more toxic than NO, so its suppression in photocatalysis process is crucial for effective NO purification. Bi4Ti3O12 is an Aurivillius-type layered compound with a high oxidation potential due to the hybridization of Bi 6s and O 2p orbitals, making it a suitable catalyst for NO degradation [18-22]. Modification of Bi4Ti3O12 with plasmonic metallic bismuth, can improve light absorption and electron mobility [23-25]. Meanwhile, defect sites are often constructed on the surface/interface of materials to decrease the band gap [26-29], and oxygen vacancies (OVs) are the most common defect sites usually constructed for oxide semiconductor modification, which can play the electrons enrichment center for boosting the generation of active radicals [30-33].
In this work, we developed Bi4Ti3O12 nanosheets modified with plasmonic metallic bismuth and oxygen vacancies by in-situ reduction. This modification significantly enhanced the photoelectric properties of the material. The optimized catalyst, BTOR2, demonstrated superior performance in removing ppb-level NO and suppressing NO2 generation compared to unmodified Bi4Ti3O12. Mechanisms for active radical generation and deep oxidation were elucidated through electron spin resonance (ESR) and in-situ DRIFTS analyses. This study offers insights into enhancing radical generation and pollutant purification via photocatalysis.
Phase analysis is shown in Fig. 1a, the X-ray diffraction (XRD) patterns of Bi4Ti3O12 (BTO) and Bi-modified defective Bi4Ti3O12 nanosheets (BTORX, X = 1, 2, 3 refer to NaBH4/Bi4Ti3O12 molar ratios of 20%, 40%, and 60%, respectively) display typical diffraction peaks at 2θ = 23.3°, 30.1°, 32.8°, 39.7°, 47.3°, and 57.2°, corresponding to orthorhombic Bi4Ti3O12 (JCPDS No. 35-0795). After reduction treatment, a new peak at 2θ = 37.2°, attributed to hexagonal metallic Bi (JCPDS No. 44-1246), appears in BTOR1, BTOR2, and BTOR3, confirming the successful introduction of metallic Bi. The electron paramagnetic resonance (EPR) analysis was used to quantify oxygen vacancies (OVs) in BTO and BTOR2. Under dark conditions, a Lorentzian line with g = 2.003 was observed (Fig. 1b), indicating OVs exist in as-synthesized catalysts [34]. BTOR2 exhibited a stronger magnetic signal than BTO, reflecting higher OVs density due to NaBH4 reduction. OVs can create defect levels, promoting electron transfer between valence and conduction bands, aiding radical species generation [35]. Under 10-min light irradiation, BTOR2 showed a stronger increase in magnetic signal than BTO, indicating higher carrier mobility of BTOR2 under light. All materials exhibited thin sheet-like morphologies (~50 nm thickness, Fig. S1 in Supporting information) with intact structures after reduction (Figs. 2a-e, and h). At 10 nm resolution, BTOR2 showed a heterostructure with metallic Bi clusters (~5 nm, marked in yellow) distributed on Bi4Ti3O12 nanosheets (Fig. 2i), while BTO displayed a uniform structure (Fig. 2f). Lattice fringes with spacings of 2.7248 Å and 0.9277 Å correspond to the (200) facet of orthorhombic Bi4Ti3O12 and the (2110) facet of hexagonal Bi, respectively (Figs. 2g and j). These results confirm the successful synthesis of metallic Bi-modified defective Bi4Ti3O12 nanosheets.
X-ray photoelectron spectroscopy (XPS) analysis was conducted to study the surface composition of BTO and BTORX (X = 1, 2, 3). The XPS survey spectra (Fig. S2a in Supporting information) show Bi, Ti, O, and C elements, confirming the purity of materials. High-resolution spectra for Bi, Ti, and O are shown in Figs. S2b-d (Supporting information). Peaks at 164.4 eV and 159.1 eV correspond to Bi3+ (Bi 4f5/2, 4f7/2). Metallic Bi peaks were undetected, possibly due to surface oxidation in air. Peaks at 466.2 eV, 464.0 eV, and 458.1 eV correspond to Bi 4d3/2 (Bi3+) [36], Ti 2p1/2 (Ti4+), and Ti 2p3/2 (Ti4+), respectively. The O 1s spectrum shows lattice oxygen peaks (530.3 eV, 529.8 eV) assigned to Ti-O and Bi-O bonds, and a 532.8 eV peak for adsorbed oxygen (O-H or H2O). These results confirm the chemical composition of the materials.
The photocatalytic NO purification performance of BTO and BTORX (X = 1, 2, 3) was evaluated by the removal of ppb-level NO and the increment of NO2 under light irradiation in a continuous flow reactor. CNO/C0 represents the variation of NO concentration. As shown in Fig. 3a, all materials responded to light and decreased the concentration of the NO within 5 min. The NO removal rates after 30 min for BTO, BTOR1, BTOR2, and BTOR3 were 40.5%, 46.5%, 62.3%, and 53.1%, respectively. The modified Bi4Ti3O12 materials outperformed the original Bi4Ti3O12, and BTOR2 achieving the highest NO removal efficiency of 62.3% (For comparison, see Table S1 in Supporting information). The NO2 increments after 5 min of illumination were 195, 20, 10, and 405 ppb for BTO, BTOR1, BTOR2, and BTOR3, respectively (Fig. 3b). The release of toxic NO2 by BTO and BTOR3 poses health risks, limiting their practical application. The formation of NO2 is effectively inhibited and NO purification is improved for BTOR2, it indicates that the surface oxidation properties of Bi4Ti3O12 are optimized by metallic Bi and oxygen vacancies. Stability tests showed that BTOR2 has application potential, and its performance remained stable after five cycles (Fig. S3 in Supporting information).
The efficiency of light absorption and electron-hole pair separation are key factors in photocatalytic performance. The UV-vis DRS spectra (Fig. S4a in Supporting information) show that as the reducing agent amount increased, the light absorption edges of BTORX (X = 1, 2, 3) catalysts occurred red-shifted, and the visible light response also increased. It is due to the localized surface plasmon resonance (LSPR) effect of metallic Bi, and the increased absorption confirms more plasmonic metallic Bi presence in modified Bi4Ti3O12. According to the evaluated band gaps (Fig. S4b) and empirical equations (Eqs. S1 and S2 in Supporting information), the ECB and EVB edges of Bi4Ti3O12 are calculated to be 0.32 V and 2.74 V, respectively (Supporting information). Figs. S4c and d (Supporting information) show the Bi-O and Bi-Bi bonds in different perspectives (View-1 and View-2 in Supporting information), the electron localized function of Bi/Bi4Ti3O12-OVs demonstrates strong interaction (marked in red) between Bi4Ti3O12 and metallic Bi, aiding the transfer of carriers. The charge carrier lifetime is 2.36 ns for BTOR2, longer than the 1.83 ns for BTO (Fig. 3c), indicating better charge mobility. Fig. 3d shows fast photocurrent rise and decay during light-dark cycles, with BTOR2 achieving a higher current than BTO, indicating efficient charge separation and rapid electron migration. The heterojunction between metallic Bi and Bi4Ti3O12 effectively separates e−/h+ pairs and promotes carrier transfer.
The process of photocatalytic active radical generation over Bi/Bi4Ti3O12-OVs is illustrated in Fig. 3e. Electron-hole pairs generated in Bi4Ti3O12 under light illumination. The EVB of Bi4Ti3O12 (2.74 V) is more positive than the redox potential of OH−/•OH (1.99 V), enabling the generation of •OH radicals from adsorbed H2O/OH− by holes. The DFT calculation results of charge density difference (Fig. 3f) and Bader charge (Fig. 3g) are analyzed. The quantification and visualization results demonstrate that electrons could transfer between Bi4Ti3O12 and metallic Bi. The free electrons of metallic Bi (Fermi level is -0.17 V) transfer to the conduction band (ECB = 0.32 V) of Bi4Ti3O12. Meanwhile, the free electrons of Bi4Ti3O12 also can jump to metallic Bi by light stimulation in theory. Importantly, the free electrons could be further transited to a more negative energy level than the redox potential of O2/•O2− (-0.33 V) through the light-induced LSPR effect. Thus, the adsorbed O2 could be oxidized to •O2− radicals or H2O2 species (O2 + 2e− + 2H+ → H2O2), and the H2O2 species could be further transformed into •OH radicals. In summary, •OH and •O2− radicals are the primary active species responsible for NO oxidation.
ESR analyses were performed on Bi4Ti3O12 and BTOR2 to trace active radical species. The results (Figs. 4a and b) show no signal in the dark. Under light, both BTO and BTOR2 exhibit six characteristic peaks of DMPO-•O2-, with BTOR2 showing stronger intensities (Fig. 4a). Additionally, four characteristic peaks with a 1:2:2:1 intensity ratio were assigned to the DMPO-•OH adduct, with BTOR2 displaying stronger signals than BTO again (Fig. 4b). The results indicate that metallic Bi and oxygen vacancies enhance the production of •O2- and •OH radicals.
Based on the described mechanism and experimental findings, the improved photocatalytic efficiency of Bi/Bi4Ti3O12-OVs composites is attributed to the combined influence of metallic Bi and oxygen vacancies. The photosensitive electrons of Bi4Ti3O12 will gather on the metallic Bi and migrate upward, thus the LSPR effect of metallic Bi can enhance the surface oxidation performance of the material.
An in-situ DRIFTS experiment was conducted at a gas flow rate of 25 mL/min (CNO = 50 ppm) to study the photocatalytic NO oxidation mechanism on Bi/Bi4Ti3O12-OVs. Fig. 4c shows the time-dependent infrared characteristic peak evolution under light. The baseline represents the background after subtracting the initial material surface peak under the helium atmosphere. After the adsorption and desorption equilibrium was reached on the surface of BTOR2, a series of characteristic peaks appeared (Table S2 in Supporting information). The broad peak at 3047 cm-1 is assigned to adsorbed H2O (O-H stretching vibration) [37], and peaks at 1476 cm-1, 1646 cm-1, and 1553 cm-1 correspond to NO and NO2 molecules [38, 39]. The NO molecule is activated into NO- (detected at 1386 m-1) after electron transfer [40, 41]. Under light irradiation, the H2O peak shifts to 3104 cm-1, indicating enhanced adsorption strength and contributing to •OH radical generation. The NO3- peak at 1264 cm-1 [42] confirms the deep photocatalytic oxidation of NO to NO3-. Fig. 4d shows the heat map of peak changes with light exposure time. After illumination, NO and NO2 accumulate slightly, while NO- intensity increases from 0.89 to 1.12, indicating the activation of NO to NO- and subsequent oxidation to NO3-. The intensity of NO3- increased from 0.32 to 0.52, confirming successful purification of NO/NO2.
In summary, this work presents a unique plasmonic metallic Bi-modified defective Bi4Ti3O12 nanosheets catalyst. The LSPR effect of metallic Bi and the abundant oxygen defects in the as-synthesized Bi/Bi4Ti3O12-OVs materials lead to enhanced visible light absorption and improved photogenerated carrier migration compared to the original Bi4Ti3O12. DFT calculations of the electron local function reveal a strong interaction between the surface metallic Bi and the Bi4Ti3O12 substrate, facilitating the transfer of photogenerated carriers. Moreover, the quantitative Bader charge and visualize charge density difference analysis results further demonstrate that free electrons can migrate from Bi4Ti3O12 to metallic Bi, with subsequent jump to higher energy level beyond the Eredox of O2/•O2-, promoting conversion of O2 to •O2- radicals. The in-situ DRIFTS analysis demonstrates that the Bi/Bi4Ti3O12-OVs can respond to light rapidly for the adsorption strength enhancement of H2O molecules, which benefits the generation of •O2- radicals. The key intermediate species, NO-, was further traced, and its highly reducing state leads it to be oxidized to NO3- more readily than NO. The results show that the optimized metallic Bi-modified defective Bi4Ti3O12 nanosheets catalysts exhibit excellent photocatalytic performance (62.3%) while minimizing toxic NO2 formation for stable deep NO oxidation. This study offers significant insights that can enhance research on effective photocatalysts for controlling air pollution.
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Year 2026 volume 37 Issue 2
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Article Info
doi: 10.1016/j.cclet.2025.111357
  • Receive Date：2024-12-24
  • Online Date：2026-10-29
  • Published：2026-02-15
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History
  • Received：2024-12-24
  • Revised：2025-03-22
  • Accepted：2025-05-20
Affiliations
    aChongqing Polytechnic University of Electronic Technology, Chongqing 401331, China
    bEngineering Research Center for Waste Oil Recovery Technology and Equipment, Ministry of Education, Chongqing Technology and Business University, Chongqing 400067, China
    cChongqing Key Laboratory of Green Synthesis and Application, College of Chemistry, Chongqing Normal University, Chongqing 401331, China
    dCollege of Physics and Electronic Engineering, Chongqing Normal University, Chongqing 401331, China
    eState Key Laboratory of Heavy Oil Processing, Key Laboratory of Optical Detection Technology for Oil and Gas, China University of Petroleum, Beijing 102249, China

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(Y. Wei)
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表12种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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