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Article

Bi2O2Se Nanosheets for Efficient Piezocatalytic H2O2 Production

by
Shun Li
1,
Xinbo Liu
1,
Xinyue Zhang
2,* and
Yong Liu
2,*
1
Institute of Quantum and Sustainable Technology (IQST), School of Chemistry and Chemical Engineering, Jiangsu University, Zhenjiang 212013, China
2
Foshan (Southern China) Institute for New Materials, Foshan 528200, China
*
Authors to whom correspondence should be addressed.
Catalysts 2025, 15(2), 157; https://doi.org/10.3390/catal15020157
Submission received: 5 December 2024 / Revised: 27 January 2025 / Accepted: 4 February 2025 / Published: 8 February 2025
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Abstract

Piezocatalysis is a promising technology for converting mechanical energy to chemical energy. Two-dimensional (2D) piezoelectric materials, with their large surface area, high charge mobility, and good flexibility, are among the most promising candidates in piezocatalysis. In this work, for the first time, we report Bi2O2Se nanosheets (NSs) with an average thickness of ~8 nm and a lateral size of ~160 nm for efficient piezocatalytic H2O2 production from water and oxygen under mechanical force induced by ultrasonication. The Bi2O2Se NSs achieved a high H2O2 production rate of 1033.8 μmol/g/h using ethanol as the sacrificial agent, significantly surpassing that of its bulk-sheet counterpart. Our results provide a novel potential 2D piezocatalytic material and offer valuable guidance for the design and development of high-efficiency H2O2 production driven by mechanical energy from water.

1. Introduction

Hydrogen peroxide (H2O2) is widely recognized for its advantages, such as its high oxidizing ability and environmental friendliness, making it valuable for applications in various areas, including disinfection, wastewater treatment, and green chemistry [1,2,3,4,5,6]. However, the primary production method of the anthraquinone process remains highly energy-intensive and environmentally detrimental due to its reliance on toxic solvents and complex, multi-step processes. As a result, there has been a growing interest in alternative, more sustainable pathways for H2O2 production. Notable green approaches include photocatalysis and electrocatalysis technologies [7,8,9,10,11,12,13,14,15,16,17,18,19]. Photocatalysis relies on the energy from light, while electrocatalysis utilizes electrical energy. Despite their promising promise, these methods are often hindered by the need for complex, expensive catalysts, which significantly limits their practical applications [20,21,22,23,24]. Therefore, developing cost-effective, scalable, and environmentally benign catalytic systems remains a critical goal for advancing H2O2 production in a more sustainable and efficient manner.
Piezocatalysis, using mechanical stress or pressure to drive catalytic reactions, is an emerging and promising approach to convert mechanical energy into chemical energy [25,26]. This method relies on piezoelectric materials, which generate electric charges when subjected to mechanical stress, to drive various chemical redox reactions (e.g., H2O2 production) [27,28,29,30,31,32,33,34,35,36]. Unlike the energy-intensive anthraquinone process, piezocatalysis operates under mild conditions and utilizes mechanical energy, such as water flow and ultrasonic vibration, to drive the reaction, making it a promising, attractive option for decentralized or on-demand H2O2 production [37,38]. Among all piezocatalytic materials, two-dimensional (2D) piezoelectrics are considered among the most promising candidates due to their ultrathin layered structure, high surface area, abundance of active sites, and piezoelectric response resulting from crystal noncentrosymmetry, such as 2D transition metal chalcogenides (TMCs) (e.g., MoS2 and ZnS) [39,40,41].
Bi2O2Se, as a novel 2D material, which belongs to the family of layered bismuth oxychalcogenides and features a distinctive anisotropic structure and tunable electronic properties, has garnered significant attention [42,43]. Due to its unique combination of an ultrathin layered structure, piezoelectric response, high charge mobility (>20,000 cm2/V·s) [44], and excellent chemical stability, 2D piezoelectric Bi2O2Se is a very promising potential piezocatalyst. Its intrinsic piezoelectricity arises from the lack of inversion symmetry in its crystal structure [45,46,47], which enables the generation of electric charges under mechanical stress—a key attribute for piezocatalytic applications. Herein, for the first time, we report 2D Bi2O2Se NSs as an efficient piezocatalyst for producing H2O2 from water and oxygen, driven by ultrasonic mechanical vibrations.

2. Results and Discussions

2.1. Morphology and Crystal Structure

X-ray diffraction (XRD) analysis was performed to investigate the crystal structure of the Bi2O2Se powder samples. As shown in Figure 1a, the diffraction peaks observed at 23.966°, 29.257°, 31.738°, 32.520°, 44.369°, 46.635°, 53.110°, and 57.636° correspond to the (101), (004), (103), (110), (114), (200), (211), and (213) crystal planes of tetragonal Bi2O2Se (JCPDS Card No. 25-1463), respectively, which align well with previously reported results [48]. Additionally, the bulk sheet crystals (BSs) display a pure tetragonal Bi2O2Se phase, which is consistent with the simulated patterns and NSs sample. This confirms that the synthesized Bi2O2Se material crystallizes without detectable impurity phases. The broader full width at half maximum (FWHM) observed for the nanosheets further validates the successful synthesis of a two-dimensional structure.
The scanning electron microscopy (SEM) image (Figure 1b) reveals that the powder sample exhibits a sheet-like morphology, with lateral dimensions up to several hundred nanometers and thicknesses of few nanometers. On the contrary, the BSs sample displays a thick-sheet morphology (Figure 1c). Energy-dispersive spectroscopy (EDS) mapping images (Figure 1d) of the NSs sample further demonstrate the homogeneous distribution of Bi, O, and Se elements. High-resolution transmission electron microscopy (HRTEM) was further employed to analyze the microstructure and crystallinity of the Bi2O2Se NSs (Figure 2). As shown in Figure 2b, the Bi2O2Se material has a 2D sheet-like structure, which is consistent with the SEM characterizations. Selected area electron diffraction (SAED) analysis (Figure 2c) confirmed the single crystalline nature of the Bi2O2Se NSs. The lattice fringes observed in Figure 3a reveal an interatomic spacing of 2.9 Å, corresponding to the (004) crystal plane of Bi2O2Se, in agreement with the XRD patterns and previously reported data [47,48]. Furthermore, the EDS mapping images in Figure 2d confirm the uniform distribution of elements within the Bi2O2Se NSs. Taking these results together, 2D Bi2O2Se ultrathin NSs were successfully synthesized.
The chemical states of elements (Bi, O, and Se) in the 2D Bi2O2Se NSs were characterized by X-ray photoelectron spectroscopy (XPS), as shown in Figure 3. All spectra were corrected using the C 1s peak at 284.4 eV as the reference. The peaks at ~159 eV and 164 eV correspond to the characteristic Bi 4f7/2 and Bi 4f5/2 peaks, respectively (Figure 3b). The peaks at ~529 eV and 531 eV are attributed to the O 1s signals from metal oxides (Figure 3c). The Se 3d peak appears at ~52.3 eV (Figure 3d), showing a slight shift compared to the standard peak, indicating strong interactions between Se and Bi. These XPS results further confirm the successful synthesis of Bi2O2Se.

2.2. Piezocatalytic Activity Performance

The piezocatalysis H2O2 production activity was tested under mechanical force provided by ultrasonic vibration. Figure 4a displays the produced H2O2 amount over different Bi2O2Se samples operating under ultrasonication (100 W and 45 kHz), using ethanol as the sacrificial agent. Among the samples, Bi2O2Se NSs demonstrated the highest H2O2 production yield, with a production rate of 1033.8 μmol/g/h, significantly surpassing the 803.1 μmol/g/h achieved by the Bi2O2Se BSs. Moreover, compared with previous catalysts (Table 1), Bi2O2Se NSs demonstrate comparable piezocatalytic performance, showing promising potential. This enhanced performance can be attributed to the ultrathin nature of Bi2O2Se NSs, which possess a greater number of surface-active sites and are more easily deformed under mechanical stress.
The effects of ultrasonic frequency on the piezocatalytic performance of Bi2O2Se NSs were further analyzed. As shown in Figure 4b, the Bi2O2Se NSs exhibited better H2O2 production performance at 35 kHz compared to 53 kHz, demonstrating that piezocatalytic efficiency is closely related to the resonance frequency of the Bi2O2Se nanomaterials. Furthermore, the stability of the Bi2O2Se NSs material was also tested. As shown in Figure 4c, after five cycles, the piezocatalytic performance almost remained unchanged, and the XRD pattern showed negligible changes in the crystalline phase before and after cycling catalytic tests (Figure 4d), confirming that the Bi2O2Se 2D piezoelectric materials exhibit excellent catalytic stability under piezocatalytic reaction conditions.

2.3. Mechanism Analysis

To further investigate the mechanism of piezocatalytic H2O2 production, the influence of reaction atmospheres and scavengers on piezocatalytic activity was investigated, as presented in Figure 5. Almost no H2O2 was produced under a N2 atmosphere, which is in sharp contrast with that under O2 and air. This suggests that the piezocatalytic synthesis of H2O2 follows an oxygen reduction reaction (ORR) pathway. The addition of hole scavenger EDTA-2Na resulted in an increased H2O2 yield, while the introduction of Ag⁺ inhibited the piezocatalytic activity, indicating that electrons play a dominant role. Additionally, with the addition of BQ, the H2O2 yield significantly decreased, suggesting that superoxide anion (•O2−) is an important intermediate in the generation of H2O2. Based on these results, we consider that the mechanism of piezocatalytic H2O2 production over Bi2O2Se is through an ORR involving a two-electron transfer process. The piezocatalytic H2O2 yield decreased without using ethanol. This is possibly because hydroxyl radicals (•OH) compete with O2 to gain electrons and form OH−. As a hydroxyl radical scavenger, ethanol consumed the •OH radicals in the system during the reaction, allowing more electrons to participate in the ORR, thus enhancing the H2O2 synthesis efficiency.
The piezo-electrochemical tests were conducted to further elucidate the charge transport characteristics of the Bi2O2Se piezoelectric materials. As shown in Figure 6a, at a voltage of 0.05 V, the transient piezo-electrochemical current density of the Bi2O2Se NSs was approximately twice that of the BSs. Additionally, as shown in Figure 6b, the Bi2O2Se NSs exhibited smaller impedance compared to that of BSs. These results indicate that the carrier recombination rate in the NSs is lower than that of BSs, allowing more carriers to migrate to the material’s surface and participate in catalytic reactions.
The band structure of the material is crucial in the piezocatalytic process. The Mott–Schottky plots (Figure 6c) were measured to calculate the band energy position of the Bi2O2Se NSs. According to the intercept of the Mott–Schottky plots, the flat band potential (Efb) was determined to be at −0.33 eV (vs. NHE) for SnSe NSs. As a result, the conduction band minimum (CBM) edge was estimated at −0.43 eV (~0.1 eV above the Efb). By combining the bandgap Eg (~1.76 eV) estimated from the UV–visible DRS spectra, the valence band maximum (VBM) was determined to be at 1.33 eV.
Based on the experimental results above, a possible mechanism for mechanically driven piezocatalytic H2O2 evolution over Bi2O2Se NSs is proposed. The band diagrams of the Bi2O2Se NSs are illustrated in Figure 6d. Based on the analysis of the material’s band structure and active radicals, the possible charge transfer processes in the piezocatalytic reaction system can be explained as follows. Under the external ultrasound, Bi2O2Se NSs undergo elastic deformation, generating a piezoelectric effect. This effect leads to the formation of a piezoelectric field within the material, promoting the separation of charge carriers on the two opposite sides of the Bi2O2Se NSs. Since the CBM of the material is more negative than the standard redox potential of the O2/•O2− couple, the electrons in the conduction band combine with dissolved O2 to generate superoxide anions (•O2−). These •O2− ions then further combine with electrons to produce H2O2. On the other hand, holes on the VBM will react with the sacrificial agent ethanol to facilitate the piezocatalytic reaction process. The overall reaction pathway follows an oxygen reduction reaction through a two-electron transfer mechanism.

3. Experimental Section

3.1. Synthesis of Bi2O2Se NSs

Bi2O2Se nanosheets were synthesized via a hydrothermal method [48]. The typical procedure is as follows (Scheme 1). First, 1.48 g of Bi(NO₃)₃·5H₂O (≥98%, Aladdin, Shanghai, China) is dissolved in 30 mL of deionized water and stirred for 30 min. Then, 1.39 g of sodium citrate (98%, Aladdin, China) is added, and the mixture is stirred for 30 min to obtain solution A. Separately, 2.664 g of PVP (AR, Aladdin, China) is dissolved in 30 mL of deionized water, followed by the sequential addition of 0.60 g of NaOH (≥98%, Aladdin, China) and 0.148 g of selenourea (98%, Merck, Darmstadt, Germany), with continuous stirring for 30 min to obtain solution B. The two solutions are mixed and stirred for 30 min and transferred to a Teflon-lined autoclave. The autoclave is placed in an oven and heated at 200 °C for 24 h. After the reaction, the product is washed with DI water and ethanol to remove impurities. Finally, the obtained product is vacuum-dried at 60 °C for 12 h to obtain the Bi2O2Se nanosheets. The bulk Bi2O2Se sheets (BSs) were purchased commercially.

3.2. Material Characterization

The crystal structure was analyzed by X-ray diffraction (XRD, Rigaku D/max-2550 VB, Rigaku Corporation, Akishima, Japan) using a Cu Kα radiation source (λ = 0.154 nm, 45 kV). The morphology and microstructure were investigated by both field emission scanning electron microscopy (FESEM, Zeiss Merlin, Carl Zeiss AG, Jena, Germany) and transmission electron microscopy (TEM, Talos F200i, Thermo Fisher Scientifi, Waltham, MA, USA). The surface electronic states of elements were characterized by X-ray photoelectron spectroscopy (XPS, ESCALAB 250 Xi, Thermo Fisher Scientifi, USA). The binding energy was calibrated with the C1s peak at 284.6 eV. The diffuse reflectance spectroscopy (DRS) was measured using a UV–vis-NIR spectrophotometer (Lambda 1050, PerkinElmer, Waltham, MA, USA) equipped with an integrating sphere.

3.3. Piezocatalytic Activity Tests

The piezocatalytic tests were conducted in a glass beaker containing 50 mL ethanol solution (10%), which was bubbled with O2 for 30 min prior to the reaction. In each test, 10 mg of the powder catalyst was added to the solution. Mechanical force was provided by an ultrasonic cleaner (Branson 2800, Branson Ultrasonics, Fremont, CA, USA). The reaction solution was kept at room temperature using a water-cooling system. At an interval of 30 min, 1 mL of the reaction solution was taken and filtrated. The concentration of H2O2 was determined using the classic Iodometric method [54]. Two solutions were prepared. Solution A consisted of 0.4 M potassium iodide, 0.06 M sodium hydroxide, and 0.1 mM ammonium molybdate, while Solution B was 0.1 M potassium hydrogen phthalate. For each measurement, 1 mL of the reaction solution was filtered and mixed with 0.5 mL solution A and 0.5 mL solution B. The resulting mixture was analyzed using a UV–vis spectrophotometer, measuring the characteristic absorption peak at 350 nm.

3.4. Piezo-Electrochemical Measurements

Piezo-electrochemical measurements were performed using an electrochemical workstation (CHI 760E, Shanghai Chenhua, Instrument Co., Ltd., Shanghai, China) in a standard three-electrode system with Bi2O2Se powder-coated conductive Cu as the working electrode, a Pt plate as the counter electrode, and Ag/AgCl as the reference electrode. A 0.1 M Na2SO4 deoxygenated solution (pH = 7 ± 0.2) was used as the electrolyte. The vibration was performed by 100 W ultrasonication excitation under a frequency of 45 kHz. The piezo-electrochemical current was measured at a potential of 0.05 V. The electrochemical impedance spectra (EIS) measurements were performed with a bias potential of −0.4 V. The Mott–Schottky plots were measured at −1.0 V, at frequencies of 500, 1000, and 1500 Hz, respectively.

4. Conclusions

We synthesized 2D Bi2O2Se nanosheets and investigated their piezocatalytic performance for H2O2 production under ultrasonic mechanical vibration. The results demonstrated that the morphology of the materials significantly impacts the piezocatalytic activity of Bi2O2Se, and the Bi2O2Se nanosheets achieved a high H2O2 production rate of 1033.8 μmol/g/h. The piezocatalytic H2O2 production activity was also dependent on the frequency of ultrasound and atmosphere. The free charge carriers generated under mechanical stress drive the ORR, leading to efficient H2O2 synthesis via a two-electron transfer pathway. This study demonstrates the promising application potential of Bi2O2Se nanomaterials in piezocatalysis, providing valuable insights for advancing the development of efficient 2D piezocatalysts. Prospectively, further advancements in scalable synthesis techniques for Bi2O2Se nanosheets and enhanced catalytic efficiency will pave the way for industrial applications.

Author Contributions

Conceptualization, S.L.; materials synthesis and catalytic tests, X.L.; writing—original draft preparation, X.Z. and S.L.; writing—review and editing, and supervision, Y.L.; funding acquisition, S.L and Y.L. All authors have read and agreed to the published version of the manuscript.

Funding

This work was supported by financial aid from the National Natural Science Foundation of China (Grant No. 22075126 and 52172187) and the Guangdong–Macao joint funding program for science and technology innovation (2022A0505020025).

Data Availability Statement

Data are contained within the article.

Conflicts of Interest

The authors declare no conflicts of interest.

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Catalysts 15 00157 g001
Figure 1. (a) XRD patterns of Bi2O2Se NSs and BCs. SEM images of (b) Bi2O2Se NSs and (c) BCs. (d) EDS mapping images of Bi2O2Se NSs.
Figure 1. (a) XRD patterns of Bi2O2Se NSs and BCs. SEM images of (b) Bi2O2Se NSs and (c) BCs. (d) EDS mapping images of Bi2O2Se NSs.
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Figure 2. (a) HRTEM image, (b) TEM image, (c) SAED patterns, and (d) EDS mapping images of Bi2O2Se NSs.
Figure 2. (a) HRTEM image, (b) TEM image, (c) SAED patterns, and (d) EDS mapping images of Bi2O2Se NSs.
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Figure 3. XPS spectra of Bi2O2Se NSs: (a) survey scan, (b) Bi 4f, (c) O 1s, and (d) Se 3d.
Figure 3. XPS spectra of Bi2O2Se NSs: (a) survey scan, (b) Bi 4f, (c) O 1s, and (d) Se 3d.
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Catalysts 15 00157 g004
Figure 4. (a) The yield of H2O2 over different Bi2O2Se samples under ultrasonic vibration. (b) The yield of H2O2 over Bi2O2Se NSs under different ultrasonication frequencies. (c) Cycling piezocatalytic experiments and (d) XRD patterns before and after tests.
Figure 4. (a) The yield of H2O2 over different Bi2O2Se samples under ultrasonic vibration. (b) The yield of H2O2 over Bi2O2Se NSs under different ultrasonication frequencies. (c) Cycling piezocatalytic experiments and (d) XRD patterns before and after tests.
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Figure 5. (a) Piezocatalytic tests of Bi2O2Se NSs under different atmospheres and sacrificial agents. (b) The corresponding reaction rates.
Figure 5. (a) Piezocatalytic tests of Bi2O2Se NSs under different atmospheres and sacrificial agents. (b) The corresponding reaction rates.
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Figure 6. (a) Transient piezo-electrochemical current and (b) impedance of different Bi2O2Se materials. (c) Mott–Schottky plots of Bi2O2Se NSs. (d) Energy band structure and piezocatalytic H2O2 production mechanism.
Figure 6. (a) Transient piezo-electrochemical current and (b) impedance of different Bi2O2Se materials. (c) Mott–Schottky plots of Bi2O2Se NSs. (d) Energy band structure and piezocatalytic H2O2 production mechanism.
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Scheme 1. Schematic of preparation process of 2D Bi2O2Se NSs.
Scheme 1. Schematic of preparation process of 2D Bi2O2Se NSs.
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Table 1. Comparison of piezocatalytic performance for H2O2 production with reported representative piezocatalysts.
Table 1. Comparison of piezocatalytic performance for H2O2 production with reported representative piezocatalysts.
CatalystsCatalytic ConditionsH2O2 Production Rate (μmol/g/h)Ref
g-C3N4ultrasonic vibration
45 kHz, 150 W		262[49]
MOC-AuNP/g-C3N4ultrasonic vibration
300 W		120.21[50]
porous CaCO3ultrasonic vibration
40 kHz, 210 W		331[51]
CdSultrasonic vibration
40 kHz		1460[52]
SrTiO3 nanorodsultrasonic vibration
40 kHz, 200 W		540[53]
Bi2O2Se NSsultrasonic vibration
45 kHz, 100 W		1033.8This work
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Li, S.; Liu, X.; Zhang, X.; Liu, Y. Bi2O2Se Nanosheets for Efficient Piezocatalytic H2O2 Production. Catalysts 2025, 15, 157. https://doi.org/10.3390/catal15020157

AMA Style

Li S, Liu X, Zhang X, Liu Y. Bi2O2Se Nanosheets for Efficient Piezocatalytic H2O2 Production. Catalysts. 2025; 15(2):157. https://doi.org/10.3390/catal15020157

Chicago/Turabian Style

Li, Shun, Xinbo Liu, Xinyue Zhang, and Yong Liu. 2025. "Bi2O2Se Nanosheets for Efficient Piezocatalytic H2O2 Production" Catalysts 15, no. 2: 157. https://doi.org/10.3390/catal15020157

APA Style

Li, S., Liu, X., Zhang, X., & Liu, Y. (2025). Bi2O2Se Nanosheets for Efficient Piezocatalytic H2O2 Production. Catalysts, 15(2), 157. https://doi.org/10.3390/catal15020157

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