构建S型g-C3N4/BiOBr异质结以增强光催化合成过氧化氢性能

doi:10.1016/S1872-2067(24)60277-9

催化学报 ›› 2025, Vol. 72: 118-129.DOI: 10.1016/S1872-2067(24)60277-9

构建S型g-C₃N₄/BiOBr异质结以增强光催化合成过氧化氢性能

曹腾飞^a, 徐全龙^b, 张军^c, 王升高^a, 狄廷敏^a^,^*(), 邓泉荣^a^,^*()

^a武汉工程大学材料科学与工程学院, 湖北省等离子化学与新材料重点实验室, 湖北武汉 430205
^b温州大学化学与材料工程学院, 浙江温州 325027
^c武汉工程大学化工与制药学院, 新型反应器和绿色化学工艺湖北省重点实验室, 湖北武汉 430205

收稿日期:2024-12-09 接受日期:2025-01-21 出版日期:2025-05-18 发布日期:2025-05-20
通讯作者: *电子信箱: ditingmin19@wit.edu.cn (狄廷敏),dqrwit@163.com (邓泉荣).
基金资助:
国家自然科学基金(22005228);武汉工程大学校内科学基金项目(K202069);武汉工程大学校内科学基金项目(K202224)

S-scheme g-C₃N₄/BiOBr heterojunction for efficient photocatalytic H₂O₂ production

Tengfei Cao^a, Quanlong Xu^b, Jun Zhang^c, Shenggao Wang^a, Tingmin Di^a^,^*(), Quanrong Deng^a^,^*()

^aHubei Key Laboratory of Plasma Chemistry and Advanced Materials, School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan 430205, Hubei, China
^bCollege of Chemistry and Materials Engineering, Wenzhou University, Wenzhou 325027, Zhejiang, China
^cKey Laboratory of Green Chemical Process of Ministry of Education, Key Laboratory of Novel Reactor and Green Chemical Technology of Hubei Province, School of Chemical Engineering and Pharmacy, Wuhan Institute of Technology, Wuhan 430205, Hubei, China

Received:2024-12-09 Accepted:2025-01-21 Online:2025-05-18 Published:2025-05-20
Contact: *E-mail: ditingmin19@wit.edu.cn (T. Di), dqrwit@163.com (Q. Deng).
Supported by:
National Natural Science Foundation of China(22005228);Scientific Research Foundation of Wuhan Institute of Technology(K202069);Scientific Research Foundation of Wuhan Institute of Technology(K202224)

摘要/Abstract

摘要：

过氧化氢是一种清洁、多功能且环境友好的氧化剂, 广泛应用于消毒、纺织、有机合成及环境修复等领域. 目前, 工业上主要采用蒽醌法制备过氧化氢, 该方法涉及复杂的加氢和氧化反应过程, 不仅需要大量的能量输入, 还会产生大量废水和废气, 对环境造成显著影响, 这与其作为清洁氧化剂的属性相矛盾. 相比之下, 人工光合作用技术通过利用地球上丰富的水资源和太阳能, 以半导体为催化剂催化生成过氧化氢, 展现出高效、温和且环保的优势. 对于单一组分的半导体光催化剂而言, 其氧化还原能力与高光利用率之间存在着不可调和的矛盾, 严重制约了效率的大幅提升及其实际应用. 因此, 通过耦合还原型半导体与氧化型半导体以构建S型异质结光催化剂, 被广泛认为是当前提升过氧化产率最为合理且高效的技术途径. 基于此, 本文的主要研究思路为: 通过将还原型半导体g-C₃N₄与氧化型半导体BiOBr进行有效耦合, 构建S型异质结体系, 并充分利用二者之间的协同效应以及S型异质结中电荷的有效分离与迁移特性, 从而实现高效过氧化氢的生成.

本文首先通过在具有嵌套结构的双坩埚中对尿素进行热聚合成功制备出超薄g-C₃N₄纳米片. 随后,为构建紧密的异质界面, 利用共沉淀的方法, 将BiOBr纳米片原位生长于g-C₃N₄纳米片的外表面, 成功构建了2D/2D S型g-C₃N₄/BiOBr异质结光催化剂. 所获得的复合材料表现出优异的光催化过氧化氢生成性能, 优化后的BCN₄异质结达到过氧化氢产率峰值(392 μmol L^-1 h^-1), 分别约为原始BiOBr和g-C₃N₄的8.7倍和2.1倍. 此外, 研究中还发现BiOBr表现出对过氧化氢强的降解能力, 但当与g-C₃N₄耦合后, 对过氧化氢的降解被显著抑制. 总体而言, g-C₃N₄/BiOBr异质结的构建大幅提高了BiOBr和g-C₃N₄光催化产过氧化氢活性, 这主要归因于S型异质结的形成有利于电荷的空间分离, 并保持体系中光生载流子的超强氧化还原能力, 这一点已通过时间分辨光致发光光谱、光电流测试和电子顺磁共振表征得到了验证. 此外, 通过原位辐照X射线光电子能谱和密度泛函理论计算, 系统地证实了g-C₃N₄和BiOBr之间界面内建电场诱导的S型电荷转移机制. 通过自由基捕获实验发现, g-C₃N₄/BiOBr S型异质结光催化产过氧化氢主要是通过两步单电子氧还原路径. 通过模拟复合材料和纯g-C₃N₄两步单电子氧还原过程各阶段的吉布斯自由能发现, 引入BiOBr形成后, g-C₃N₄在产过氧化氢过程中的能量势垒被显著降低, 为过氧化氢的形成反应提供了动力学优势.

综上, 本工作中g-C₃N₄和BiOBr催化剂之间构建的S型异质结弥补了各自的不足, 实现了高效的生产过氧化氢, 并利用一系列表征手段证明了S型电荷分离和迁移机制. 这项研究为S型异质结光催化剂的系统设计和构建提供了参考, 同时也为光催化材料高效催化生成过氧化氢提供了新思路.

关键词: S型异质结, BiOBr, g-C₃N₄, 光催化, 过氧化氢生成

Abstract:

The establishment of S-scheme heterojunctions has arisen as a promising strategy for the advancement of efficient photocatalytic systems with superior charge separation and redox ability, specifically for H₂O₂ production. In this investigation, an innovative 2D/2D g-C₃N₄/BiOBr S-scheme heterojunction was meticulously engineered through an in situ growth methodology. The synthetic composites exhibit boosted H₂O₂ production activity, achieving a peak generation rate of 392 μmol L^-1 h^-1, approximately 8.7-fold and 2.1-fold increase over the pristine BiOBr and g-C₃N₄, respectively. Such a superior activity should be attributed to the highly efficient charge separation and migration mechanisms, along with the sustained robust redox capability of S-scheme heterostructure, which are verified by time-resolved photoluminescence spectroscopy, photocurrent test and electron paramagnetic resonance measurements. Furthermore, the interfacial electric field induced S-scheme charge transfer mechanism between g-C₃N₄ and BiOBr is systematically certificated by in situ irradiated X-ray photoelectron spectroscopy and density functional theory calculation. This research offers a comprehensive protocol for the systematic development and construction of highly efficient S-scheme heterojunction photocatalysts, specifically tailored for enhanced H₂O₂ production.

Key words: S-scheme heterojunction, BiOBr, g-C₃N₄, Photocatalysis, H₂O₂ production

曹腾飞, 徐全龙, 张军, 王升高, 狄廷敏, 邓泉荣. 构建S型g-C₃N₄/BiOBr异质结以增强光催化合成过氧化氢性能[J]. 催化学报, 2025, 72: 118-129.

Tengfei Cao, Quanlong Xu, Jun Zhang, Shenggao Wang, Tingmin Di, Quanrong Deng. S-scheme g-C₃N₄/BiOBr heterojunction for efficient photocatalytic H₂O₂ production[J]. Chinese Journal of Catalysis, 2025, 72: 118-129.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60277-9

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图/表 13

Fig. 1. XRD patterns (a) and FTIR spectra (b) of the BiOBr, g-C3N4, and BCNX samples.

Fig. 2. FESEM images of g-C3N4 (a,d), BiOBr (b,e), and BCN4 (c,f) samples.

Fig. 3. TEM (a) and high-resolution TEM (b) images of sample BCN4.

Fig. 4. The UV-vis DRS of the g-C3N4, BiOBr and BCN4 samples.

Fig. 5. N2 sorption isotherms and the corresponding pore size distribution curves (inset) of g-C3N4, BCN4 and BiOBr samples.

Table 1 ABET, PV and APS data of g-C3N4, BCN4 and BiOBr samples.

Sample	A_BET (m² g^-1)	PV (cm³ g^-1)	APS (nm)
g-C₃N₄	96	0.51	21.2
BCN4	82	0.32	15.8
BiOBr	15	0.07	15.5

Fig. 6. XPS survey spectra (a), high-resolution XPS spectra of C 1s (b), N 1s (c), Bi 4f (d), O 1s (e), and Br 3d (f) of g-C3N4, BCN4 and BiOBr samples.

Fig. 7. (a) Time courses of photocatalytic H2O2 production over the obtained photocatalysts under 300 W Xe lamp irradiation. (b) Comparison of H2O2 yields over samples g-C3N4, BCNX and BiOBr for 1 h illumination. (c) Recycling tests for photocatalytic H2O2 production on g-C3N4, BCN4 and BiOBr samples. (d) Photocatalytic degradation of H2O2 under illumination and oxygen-free condition.

Fig. 8. TRPL spectra of the g-C3N4, BCN4 and BiOBr samples, the inset table presents the summarized fitting parameters and results.

Fig. 9. (a) I-T curves and (b) EIS of g-C3N4, BCN4 and BiOBr samples.

Fig. 10. (a) Active species quenching experiments. (b) Band structures of g-C3N4 and BiOBr. EPR spectra of DMPO-?O2- in methanol (c) and DMPO-?OH in aqueous dispersions (d) of BiOBr, g-C3N4 and BCN4 samples.

Fig. 11. Electrostatic potential of g-C3N4 (001) surface (a) and BiOBr (001) surface (b). (c) Gibbs free energy differences (ΔG) for each stage in the two-step single-electron ORR process over g-C3N4 and BiOBr/g-C3N4 composite. Top view (d) and side view (e,f) of the charge density difference of BiOBr/g-C3N4 with an isosurface of 2 × 10-3 e ?-3. (g) Planar-averaged electron density difference Δρ(z) for BiOBr/g-C3N4. The yellow and cyan regions respectively represent the accumulation and depletion of charge.

Fig. 12. (a) The band structures of individual BiOBr and g-C3N4. (b) The formation of IEF at the g-C3N4/BiOBr interface. (c) Charge migration pathway over g-C3N4/BiOBr heterojunction in the photocatalytic H2O2 production process.

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构建S型g-C₃N₄/BiOBr异质结以增强光催化合成过氧化氢性能

S-scheme g-C₃N₄/BiOBr heterojunction for efficient photocatalytic H₂O₂ production

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