碱-氰基双调控的g-C3N4/BiOCl S-型异质结用于纯水中高效可见光驱动H2O2光合成

doi:10.1016/S1872-2067(25)64893-5

催化学报 ›› 2026, Vol. 83: 143-161.DOI: 10.1016/S1872-2067(25)64893-5

碱-氰基双调控的g-C₃N₄/BiOCl S-型异质结用于纯水中高效可见光驱动H₂O₂光合成

廖紫怡, 蒋岚^*(), 杨扬, 王霖, 杨为佑, 侯慧林^*()

宁波工程学院, 微纳材料与器件创新研究院, 浙江宁波 315211

收稿日期:2025-08-01 接受日期:2025-09-02 出版日期:2026-04-18 发布日期:2026-03-04
通讯作者: * 电子信箱: jlan22@126.com (蒋岚), houhuilin86@163.com (侯慧林).
基金资助:
浙江省自然科学基金(LY23E020002);国家自然科学基金(52272085);国家自然科学基金(52372063);宁波市青年科技创新领军人才基金(2023QL031);“十四五”省级研究生教育改革项目(ZX2023000006)

Alkali-cyano dual-tailored g-C₃N₄/BiOCl S-scheme heterojunctions for highly efficient visible-light-driven H₂O₂ photosynthesis in pure water

Ziyi Liao, Lan Jiang^*(), Yang Yang, Lin Wang, Weiyou Yang, Huilin Hou^*()

Institute of Micro/Nano Materials and Devices, Ningbo University of Technology, Ningbo 315211, Zhejiang, China

Received:2025-08-01 Accepted:2025-09-02 Online:2026-04-18 Published:2026-03-04
Contact: * E-mail: jlan22@126.com (L. Jiang), houhuilin86@163.com (H. Hou).
Supported by:
Zhejiang Provincial Natural Science Foundation of China(LY23E020002);National Natural Science Foundation of China(52272085);National Natural Science Foundation of China(52372063);Ningbo Youth Science and Technology Innovation Leading Talents Project(2023QL031);"14th Five-Year Plan" Provincial-Level Graduate Education Reform Project(ZX2023000006)

摘要/Abstract

摘要：

过氧化氢(H₂O₂)作为一种重要的绿色氧化剂, 在化工、环境治理和能源转化等领域具有广泛应用. 当前工业化的蒽醌氧化法存在能耗高、污染大等问题, 亟需开发环境友好、可持续的制备新途径. 光催化合成H₂O₂由于能够直接利用太阳能驱动反应, 被认为是实现绿色制备的理想策略. 然而, 单一半导体光催化剂普遍存在可见光利用率低、光生载流子分离效率不足、反应选择性有限等问题. 石墨相氮化碳(g-C₃N₄)因其合成简便、能带结构适宜、环境稳定性好而备受关注, 但其光生电子-空穴对易复合、可见光吸收范围有限, 严重制约了其在H₂O₂光合成中的应用. 因此, 构筑新型异质结体系并通过能带结构调控提升光生载流子的分离效率与选择性, 对于实现高效H₂O₂光合成具有重要科学意义和应用价值.
本研究通过离子掺杂与官能团修饰相结合的策略, 对g-C₃N₄进行碱金属Na⁺/K⁺协同调控与氰基引入改性, 制备了具有优化能带结构和表面化学环境的CN-NH-NaK材料. 进一步与超薄BiOCl纳米片复合, 构筑了新型S型异质结(CN-NH-NaK/BiOCl). 该双调控策略一方面通过Na⁺/K⁺的引入有效调节电子结构和带隙分布; 另一方面, 氰基的存在增强了电子离域效应并改善了表面活性位点分布. 复合所得的CN-NH-NaK/BiOCl不仅展现出更强的可见光吸收能力, 而且显著促进了光生电子-空穴对的分离与传输. 在可见光(λ ≥ 400 nm)照射下, CN-NH-NaK/BiOCl的H₂O₂生成速率高达33.15 mmol·g^-1·h^-1, 相较于原始g-C₃N₄和BiOCl分别提高了118倍和83倍, 性能远超目前报道的各类g-C₃N₄和BiOCl基光催化剂. 值得注意的是, 即使在不含任何牺牲剂或电子供体的纯水体系中, 该异质结仍能保持5.18 mmol·g^-1·h^-1的H₂O₂生成速率, 优于大多数已报道的同类催化剂. 机理研究表明, 该异质结遵循S型电荷转移机制: 光生电子从BiOCl的导带迁移至g-C₃N₄的价带, 与其空穴发生复合, 从而保留了g-C₃N₄的高还原能力与BiOCl的高氧化能力. 这一机制不仅实现了光生载流子的高效分离, 而且选择性促进了2e^-氧还原反应(ORR), H₂O₂选择性高达94.06%. 与此同时, 光生空穴驱动的水氧化过程进一步保证了电子-空穴的有效利用. 此外, CN-NH-NaK/BiOCl表现出优异的光稳定性与循环使用性能. 在长期反应过程中, 催化剂的结构和性能几乎没有衰减, 表现出良好的耐久性. 进一步的应用研究表明, 该光催化剂还能够有效降解四环素盐酸盐等典型抗生素污染物, 展现了在环境修复领域的潜在应用价值. 综合来看, 本研究提出的碱-氰基双调控与S型异质结构筑策略为光催化H₂O₂合成提供了新的思路, 同时为环境净化与绿色能源转化开辟了新的可能.
综上, 本工作不仅实现了在纯水体系中高效、可见光驱动的H₂O₂光合成, 还为构建新型S型异质结光催化剂提供了可推广的策略. 未来, 该体系在太阳能利用、环境修复和清洁能源转化等领域具有广阔的应用前景. 本研究为实现绿色可持续发展的H₂O₂制备提供了重要参考.

关键词: S型异质结, H₂O₂光合成, g-C₃N₄, BiOCl

Abstract:

Efficient and sustainable photocatalytic hydrogen peroxide (H₂O₂) synthesis is crucial due to its role as an eco-friendly oxidant and the limitations of conventional industrial methods. Graphitic carbon nitride (g-C₃N₄) is a promising photocatalyst but suffers from inefficient charge separation and limited visible light absorption. This study introduces a dual-modified g-C₃N₄, incorporating Na⁺/K⁺ ions and cyano groups, coupled with ultrathin BiOCl nanosheets to form an S-scheme heterojunction (CN-NH-NaK/BiOCl). The modification enhances the electronic structure, visible light absorption, and charge separation. The CN-NH-NaK/BiOCl photocatalyst achieved an outstanding H₂O₂ production rate of 33.15 mmol·g^‒1·h^‒1 under visible light (λ ≥ 400 nm), outperforming pristine g-C₃N₄ (118-fold) and BiOCl (83-fold), and surpassing all previously reported g-C₃N₄- and BiOCl-based photocatalysts. Even in pure water, the production rate reached 5.18 mmol·g^‒1·h^‒1, exceeding that of most previously reported catalysts. Comprehensive characterization revealed an efficient S-scheme charge transfer mechanism, enabling selective 2e^‒ oxygen reduction reaction (94.06% selectivity) and water oxidation. The heterojunction demonstrated excellent stability, reusability, and enhanced degradation of tetracycline hydrochloride. This work provides a promising strategy for advanced S-scheme photocatalysts in sustainable H₂O₂ production and environmental remediation.

Key words: S-scheme heterojunction, H₂O₂ photosynthesis, g-C₃N₄, BiOCl

廖紫怡, 蒋岚, 杨扬, 王霖, 杨为佑, 侯慧林. 碱-氰基双调控的g-C₃N₄/BiOCl S-型异质结用于纯水中高效可见光驱动H₂O₂光合成[J]. 催化学报, 2026, 83: 143-161.

Ziyi Liao, Lan Jiang, Yang Yang, Lin Wang, Weiyou Yang, Huilin Hou. Alkali-cyano dual-tailored g-C₃N₄/BiOCl S-scheme heterojunctions for highly efficient visible-light-driven H₂O₂ photosynthesis in pure water[J]. Chinese Journal of Catalysis, 2026, 83: 143-161.

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图/表 9

Fig. 1. (a) Schematic diagram of the preparation process for CN-NH-NaK/BiOCl. SEM (b), TEM (c), and HRTEM (d) images of CN-NH-NaK/BiOCl. XRD patterns (e), FT-IR spectra (f), and N2 adsorption-desorption isotherms (g) of the as-prepared photocatalysts.

Fig. 2. (a) XPS survey spectra of the as-prepared photocatalysts. High-resolution XPS spectra of C 1s (b), N 1s (c), Bi 4f (d), O 1s (e), and Cl 2p (f).

Fig. 3. UV-vis DRS (a) and the corresponding Tauc plots (b) of BiOCl and CN-NH-NaK. VB-XPS spectra of BiOCl (c) and CN-NH-NaK (d). UPS spectra of BiOCl (e) and CN-NH-NaK (f). Work functions of BiOCl (g) and CN-NH-NaK (h) calculated based on the DFT theory.

Fig. 4. (a-e) Quasi-in-situ XPS spectra of CN-NH-NaK/BiOCl catalysts under dark and light illumination conditions. (f) Schematic diagram of the electron-transfer process between CN-NH-NaK and BiOCl. (g-i) Schematic diagram of the S-scheme heterojunction formed by BiOCl and CN-NH-NaK.

Fig. 5. (a) Photocatalytic H2O2 production by the photocatalyst in the presence of isopropanol as a sacrificial agent. (b) Comparison of H2O2 production rates among different photocatalysts. (c) Wavelength-dependent H2O2 evolution rate and the corresponding AQY values. (d) Cyclic stability of H2O2 generation over the CN-NH-NaK/BiOCl photocatalyst. (e) Photocatalytic decomposition of H2O2 by the photocatalyst. (f) Comparison of the H2O2 production rate (Kp) and decomposition rate (Kd). (g) Photocatalytic H2O2 production over CN-NH-NaK/BiOCl photocatalysts tested under different light condition. (h) Photocatalytic H2O2 production by the photocatalyst in pure water. (i) Comparison of H2O2 production rates in pure water among different photocatalysts. (j) Comparison of the photocatalytic H2O2 performance of the CN-NH-NaK/BiOCl photocatalyst with that of other reported photocatalysts.

Fig. 6. KPFM of BiOCl (a), CN-NH-NaK (b), and CN-NH-NaK/BiOCl (c); EIS Nyquist plots (d) and photocurrent responses (e) of as-prepared photocatalysts. (f,g) PL spectra and TRPL spectra of the as-prepared photocatalysts. (h-k) Proposed structural models for BCN, CN-NH-NaK, BiOCl, and CN-NH-NaK/BiOCl.

Fig. 7. EPR trapping experiments under dark (a) and light (b) conditions of BCN, BiOCl, CN-NH-NaK and CN-NH-NaK/BiOCl, respectively. H2O2 selectivity as a function of the applied potential (c) and the calculated average number of transferred electrons (n) (d) of the catalyst.

Fig. 8. (a,b) In-situ infrared spectroscopy monitoring of the photocatalytic H2O2 production process on CN-NH-NaK/BiOCl. (c) Optimized adsorption configurations for CN-NH-NaK, BiOCl and CN-NH-NaK/BiOCl. (d) Comparison of the Gibbs free energy changes for each step of the photocatalytic 2-electron ORR. (e-g) Charge density differences between the adsorbed *OOH intermediate and each sample. (h) Proposed mechanism of photocatalytic H2O2 production on CN-NH-NaK/BiOCl in pure water.

Fig. 9. (a) Degradation activity of different synthesized samples for the coupled photocatalytic production of hydrogen peroxide for the degradation of TH. (b) The corresponding first-order kinetic curves. (c) Comparison of corresponding degradation rates. (d) Photocatalytic coupled hydrogen peroxide production degradation of TH by CN-NH-NaK/BiOCl compared with the experiment of photocatalytic degradation of TH alone. (e) The corresponding first-order kinetic curves. (f) Comparison of corresponding degradation rates.

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碱-氰基双调控的g-C₃N₄/BiOCl S-型异质结用于纯水中高效可见光驱动H₂O₂光合成

Alkali-cyano dual-tailored g-C₃N₄/BiOCl S-scheme heterojunctions for highly efficient visible-light-driven H₂O₂ photosynthesis in pure water

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