碳点介导缺陷工程中的激子解离用于高效可见光驱动纯水全反应合成H2O2

doi:10.1016/S1872-2067(25)64865-0

催化学报 ›› 2026, Vol. 80: 174-188.DOI: 10.1016/S1872-2067(25)64865-0

碳点介导缺陷工程中的激子解离用于高效可见光驱动纯水全反应合成H₂O₂

孙开渠^a^,^b, 郭梓轩^b, 罗俊^a, 王雪颖^a, 秦浩源^b, 王立晶^c, 赵楠^a^,^*(), 卢昶雨^a^,^*(), 施伟龙^b^,^*()

^a河北地质大学水资源与环境学院, 河北省水资源可持续开发与利用重点实验室, 河北石家庄 050031
^b江苏科技大学材料科学与工程学院, 江苏镇江 212100
^c商丘师范学院化学化工学院, 河南商丘 476000

收稿日期:2025-06-17 接受日期:2025-09-04 出版日期:2026-01-18 发布日期:2026-01-05
通讯作者: 赵楠,卢昶雨,施伟龙
基金资助:
国家自然科学基金(22578190);中国博士后科学基金(2023M743178);中国石油化工行业太阳能电池电极材料重点实验室开放基金(2024A093);功能无机材料化学重点实验室开放课题(黑龙江大学);石家庄市驻冀高校基础研究项目优秀青年项目(241790627A);河北地质大学校内杰出青年项目(JQ202403);河北地质大学博士科研启动基金项目(BQ2024050);河北地质大学国家预研项目(KY2025QN21)

Carbon dots mediated excitons dissociation in defect engineering for high-efficient visible-light-driven overall H₂O₂ photosynthesis from pure water

Kaiqu Sun^a^,^b, Zixuan Guo^b, Jun Luo^a, Xueying Wang^a, Haoyuan Qin^b, Lijing Wang^c, Nan Zhao^a^,^*(), Changyu Lu^a^,^*(), Weilong Shi^b^,^*()

^aSchool of Water Resource and Environment, Hebei Province Key Laboratory of Sustained Utilization & Development of Water Recourse, Hebei GEO University, Shijiazhuang 050031, Hebei, China
^bSchool of Material Science and Engineering, Jiangsu University of Science and Technology, Zhenjiang 212100, Jiangsu, China
^cHenan Engineering Center of New Energy Battery Materials, College of Chemistry and Chemical Engineering, Shangqiu Normal University, Shangqiu 476000, Henan, China

Received:2025-06-17 Accepted:2025-09-04 Online:2026-01-18 Published:2026-01-05
Contact: Nan Zhao, Changyu Lu, Weilong Shi
Supported by:
National Natural Science Foundation of China(22578190);China Postdoctoral Science Foundation(2023M743178);Open Fund of the Key Laboratory of Solar Cell electrode Materials in China Petroleum and Chemical Industry(2024A093);Key Laboratory of Functional Inorganic Material Chemistry(Heilongjiang University);Excellent Youth Fund of Basic Research Project of Universities in Shijiazhuang(241790627A);Outstanding Youth Project of Hebei GEO University in 2024(JQ202403);PhD Research Startup Foundation of Hebei GEO University in 2024(BQ2024050);National Pre-research Funds of Hebei GEO University in 2025(KY2025QN21)

摘要/Abstract

摘要：

过氧化氢(H₂O₂)作为一种环保氧化剂, 在废水处理、医疗消毒和绿色化学合成等方面具有重要应用. 目前, H₂O₂的工业生产主要依赖于蒽醌工艺, 但该工艺的多步加氢-氧化循环存在高能耗和产生有毒副产物的局限性. 近年来, 只需要水、氧气和太阳能为原料的光催化合成技术被认为是一种由纯水合成H₂O₂的有效策略. 然而, 在没有牺牲剂的纯水体系中, 现有的光催化体系通常受到高激子结合能、载流子复合严重和竞争性反应途径的限制, 导致H₂O₂产率和选择性达不到实际要求. 目前的研究主要集中在提高光催化氧还原产H₂O₂途径, 对光催化水氧化产H₂O₂途径的开发利用比较有限. 如何促进激子解离, 使自由载流子能有效参与纯水中的双路径光催化反应, 从而实现H₂O₂的高效合成, 仍是当前亟待解决的难题.

针对上述挑战, 本文通过对催化剂各组分的多功能化设计, 采用水热法和煅烧法制备了负载碳点且富含S空位的ZnIn₂S₄催化剂(H-CDs/ZIS-Vs). 该催化剂能够高效解离激子、定向分离光生载流子, 同时提升对反应中间产物的吸附能力, 从而有效驱动氧还原与水氧化协同的双路径反应, 提高表面生成H₂O₂的反应选择性. 通过一系列理化性质表征测试证实了H-CDs/ZIS-Vs微米花中S空位的形成和碳点的成功引入. 光催化产H₂O₂测试表明, 在纯水中不额外通气时, H-CDs/ZIS-Vs表现出了较高的H₂O₂产率, 是初始ZnIn₂S₄(ZIS)的6倍. 理论计算和变温荧光结果清楚地表明, H-CDs和S空位的存在调节了ZnIn₂S₄的局部电荷密度, 显着降低了激子结合能并促进了激子解离的发生. 紫外-可见漫反射光谱和能带结构分析结果表明, H-CDs和S空位的引入拓宽了ZnIn₂S₄的可见光吸收范围, 并且其能带结构在热力学上能够同时满足驱动氧还原反应(ORR)和水氧化反应(WOR)的要求. 表面光电压和瞬态光电压光谱结果表明, S空位与H-CDs能分别作为电子和空穴的有效捕获位点, 显著抑制光生电子-空穴对的复合. 光电性能测试与时间分辨光致发光光谱结果均表明, H-CDs/ZIS-Vs中的光生载流子分离效率显著提高, 同时其对H₂O₂的生成选择性也更高. O₂程序升温脱附(O₂-TPD)曲线表明, H-CDs/ZIS-Vs具有更强的氧气吸附能力, 这有利于氧气参与光催化生成H₂O₂的反应. 同位素标记和捕获实验结果表明, 光催化氧还原反应与水氧化反应在H₂O₂的生成过程中均起着关键作用, 并且双电子反应路径被确定为主要贡献机制. 原位漫反射红外光谱结果表明, 在光催化产H₂O₂过程中检测到了*OH, *·O₂^‒, *OOH, *HOOH吸附态中间体的存在. 结合理论计算进一步证实, H-CDs/ZIS-Vs具有更适宜的微观结构, 能够有效吸附并转化双通道光催化生成H₂O₂过程中的各种中间产物.

综上, 本文通过硫空位和碳点的耦合促进了激子的解离并使自由载流子参与到光催化双通道产H₂O₂反应当中, 实现了H₂O₂的高效合成. 本研究详细阐明了激子解离与自由光生载流子参与H₂O₂合成的微观过程, 不仅为设计高效光催化剂提供了理论指导, 也为在复杂光催化反应中协同优化激子效应与界面工程开辟了新方向.

关键词: 光合作用, H₂O₂, 激子解离, 碳点, 缺陷工程

Abstract:

The pursuit of an efficient photocatalytic pathway for hydrogen peroxide (H₂O₂) synthesis from pure water without adding additional sacrifice agents poses a formidable research endeavor and remains a pivotal challenge. Herein, we demonstrate that incorporating hexaketocyclohexane-derived carbon dots (H-CDs) and S vacancies into ZnIn₂S₄ weakens the exciton effect, leading to the dissociation into free carriers that participate in the dual pathways of oxygen reduction reaction and water oxidation reaction, thereby achieving efficient photocatalytic H₂O₂ production with a high H₂O₂ yield of 17.8 mM/g/h under visible light in pure water. Experimental results combined with theoretical calculations clearly illustrate that the presence of H-CDs and S vacancies modulates the local charge density of ZnIn₂S₄, markedly diminishing the exciton binding energy and facilitating the occurrence of exciton dissociation. Moreover, S vacancies and H-CDs effectively capture free electrons and extract free holes, respectively, significantly inhibiting the recombination of photogenerated electron-hole pairs. By optimizing the electronic structure and optical properties of ZnIn₂S₄, they thermodynamically satisfy the conditions for oxygen reduction and water oxidation reactions. Additionally, the synergy between H-CDs and S vacancies in ZnIn₂S₄ enhances the adsorption of oxygen and intermediate products, increasing their participation in the reaction and facilitating the conversion to H₂O₂. This work offers novel insights into catalyst design from the perspective of excitons dissociation, and underscores the distinct roles that free charge carriers play in various pathways for photocatalytic H₂O₂ production.

Key words: Photosynthesis, H₂O₂, Exciton dissociation, Carbon dots, Defect engineering

孙开渠, 郭梓轩, 罗俊, 王雪颖, 秦浩源, 王立晶, 赵楠, 卢昶雨, 施伟龙. 碳点介导缺陷工程中的激子解离用于高效可见光驱动纯水全反应合成H₂O₂[J]. 催化学报, 2026, 80: 174-188.

Kaiqu Sun, Zixuan Guo, Jun Luo, Xueying Wang, Haoyuan Qin, Lijing Wang, Nan Zhao, Changyu Lu, Weilong Shi. Carbon dots mediated excitons dissociation in defect engineering for high-efficient visible-light-driven overall H₂O₂ photosynthesis from pure water[J]. Chinese Journal of Catalysis, 2026, 80: 174-188.

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https://www.cjcatal.com/CN/Y2026/V80/I1/174

图/表 8

Fig. 1. (a) Schematic illustration for the preparation process of H-CDs/ZIS-Vs photocatalyst. SEM (b), TEM (c), and HRTEM (d) images of H-CDs/ZIS-Vs-4. XRD patterns (e), high-resolution S 2p XPS spectra (f), and EPR spectra (g) of as-prepared samples.

Fig. 2. UV-vis DRS (a), band gap energies (inset shows VB-XPS spectra) (b) and the corresponding energy band structures (c) of ZIS, ZIS-Vs and H-CDs/ZIS-Vs-4. Concentration of photocatalytic H2O2 production curves (d) and photocatalytic H2O2 evolved rate (e) of various catalysts under visible light irradiation. (f) Repeated photocatalytic H2O2 production over H-CDs/ZIS-Vs-4 under visible light irradiation. (g) Photocatalytic H2O2 production of various catalysts under different conditions. (h) Summary of recently reported photocatalytic H2O2 production under visible light irradiation.

Fig. 3. (a) Charge density difference (CDD) calculation results of ZIS, ZIS-Vs and H-CDs/ZIS-Vs-4. Steady-state PL spectra with a function of temperature of ZIS (b), ZIS-Vs (c) and H-CDs/ZIS-Vs-4 (d). Low-temperature steady-state PH spectra (77 K) (e), and low-temperature time-resolved PH spectra (77 K) (f) of ZIS, ZIS-Vs and H-CDs/ZIS-Vs-4. (g) Illustration of the excitonic behaviors in H-CDs/ZIS-Vs.

Fig. 4. Steady-state SPV spectra (a) and TPV spectra (b) of ZIS, ZIS-Vs and H-CDs/ZIS-Vs-4. Maximum extraction rate (tmax) of charge (c), maximum charge extraction efficiency (A) (d), electron attenuation constants (τ) (e) of charge recombination process and the number of effective charges (Aeff) (f) for ZIS, ZIS-Vs and H-CDs/ZIS-Vs-4 based on TPV spectra.

Fig. 5. Pseudo-colored TAS spectra of ZIS (a), ZIS-Vs (d) and H-CDs/ZIS-Vs-4 (g). TAS spectra with different delay times of ZIS (b), ZIS-Vs (e) and H-CDs/ZIS-Vs-4 (h) under the pump excitation of 320 nm. Fitting curves of TAS decay dynamics of ZIS (c), ZIS-Vs (f) and H-CDs/ZIS-Vs-4 (i) at 553 nm.

Fig. 6. PL spectra (a), TRPL spectra (b), photocurrent response curves (c) and EIS Nyquist plots (d) of ZIS, ZIS-Vs and H-CDs/ZIS-Vs-4. (e) RRDE polarization curves at different rotation rates (ω = 600, 900, 1200 and 1600 rpm) over H-CDs/ZIS-Vs-4 sample. H2O2 selectivity (f) and the corresponding number of electron transfer (g) over ZIS, ZIS-Vs and H-CDs/ZIS-Vs-4. (h) TPD-O2 profiles of ZIS, ZIS-Vs and H-CDs/ZIS-Vs-4.

Fig. 7. (a) Theoretical calculation of adsorbed O2 environment charge density difference (CDD) for ZIS, ZIS-Vs and H-CDs/ZIS-Vs. (b) Adsorption energy of H+, O2, *O2 and *OOH of ZIS, ZIS-Vs and H-CDs/ZIS-Vs. Calculated free-energy diagrams of oxygen reduction (c) and water oxidation (d) processes linked to H2O2 production. (e) In-situ DRIFT spectra of H-CDs/ZIS-Vs-4 recorded during the photoreaction.

Fig. 8. Schematic illustration of the photocatalytic H2O2 production mechanism based on H-CDs/ZIS-Vs composite photocatalyst.

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碳点介导缺陷工程中的激子解离用于高效可见光驱动纯水全反应合成H₂O₂

Carbon dots mediated excitons dissociation in defect engineering for high-efficient visible-light-driven overall H₂O₂ photosynthesis from pure water

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