阴阳离子对促进结晶氮化碳激子解离实现过氧化氢高效人工光合成

doi:10.1016/S1872-2067(25)64896-0

催化学报 ›› 2026, Vol. 82: 174-186.DOI: 10.1016/S1872-2067(25)64896-0

阴阳离子对促进结晶氮化碳激子解离实现过氧化氢高效人工光合成

李俊青^a^,^b^,¹, 何科林^a^,¹, 陶英^a, 陈超^a^,^*(), 谢林富^a, 马云飞^a, 王骏鹏^a, 许长文^a, 李杨^b^,^*(), 张启涛^a^,^*()

^a深圳大学微纳光电子学研究院, 教育部二维材料光电科技国际联合实验室, 广东深圳 518000
^b深圳大学射频异质异构集成全国重点实验室, 广东深圳 518000

收稿日期:2025-07-28 接受日期:2025-09-22 出版日期:2026-03-18 发布日期:2026-03-05
通讯作者: * 电子信箱: chenchao@szu.edu.cn (陈超),yang.li@szu.edu.cn (李杨),qitao-zhang@szu.edu.cn (张启涛).
作者简介:¹共同第一作者.
基金资助:
广东省重点领域研发计划(2023B0909010002);广东省基础与应用基础研究基金(2024A1515010976);深圳市科技计划(JCYJ20250604181535046);深圳市孔雀计划(20210802524B);中国博士后基金(GZC20241085);中国博士后基金(GZC20230562);中国博士后基金(GZC20230564);中国博士后基金(2024M760583);国家自然科学基金(22406161);国家自然科学基金(52402234);深圳市超常二维材料与信息技术重点实验室

Promoting exciton dissociation in crystalline carbon nitride via cation-anion synergy for hydrogen peroxide photosynthesis

Junqing Li^a^,^b^,¹, Kelin He^a^,¹, Ying Tao^a, Chao Chen^a^,^*(), Linfu Xie^a, Yunfei Ma^a, Junpeng Wang^a, Changwen Xu^a, Yang Li^b^,^*(), Qitao Zhang^a^,^*()

^aInternational Collaborative Laboratory of 2D Materials for Optoelectronics Science and Technology of Ministry of Education, Institute of Microscale Optoelectronics, Shenzhen University, Shenzhen 518000, Guangdong, China
^bState Key Laboratory of Radio Frequency Heterogeneous Integration, Shenzhen University, Shenzhen 518000, Guangdong, China

Received:2025-07-28 Accepted:2025-09-22 Online:2026-03-18 Published:2026-03-05
Contact: * E-mail: chenchao@szu.edu.cn (C. Chen),yang.li@szu.edu.cn (Y. Li),qitao-zhang@szu.edu.cn (Q. Zhang).
About author:¹ Contributed equally to this work.
Supported by:
Key-Area Research and Development Program of Guangdong Province(2023B0909010002);Guangdong Basic and Applied Basic Research Foundation(2024A1515010976);Shenzhen Science and Technology Program(JCYJ20250604181535046);Shenzhen Peacock Plan(20210802524B);Postdoctoral Research Foundation of China(GZC20241085);Postdoctoral Research Foundation of China(GZC20230562);Postdoctoral Research Foundation of China(GZC20230564);China Postdoctoral Science Foundation(2024M760583);National Natural Science Foundation of China(22406161);National Natural Science Foundation of China(52402234);Shenzhen Key Laboratory of 2D Metamaterials for Information Technology

摘要/Abstract

摘要：

过氧化氢(H₂O₂)是一种绿色氧化剂和能源载体, 广泛应用于纺织、食品加工、造纸、医疗、航空航天和废水处理等领域. 目前95%以上的H₂O₂依赖蒽醌法合成, 该工艺存在高能耗、有机废物排放量高及H₂O₂储运过程易泄漏等问题. 通过太阳能驱动光催化氧还原反应(ORR)实现人工光合成H₂O₂, 因低能耗、环境友好且可原位生产, 成为替代蒽醌法的理想路径. 聚合物氮化碳(PCN)作为经典的非金属有机光催化材料, 兼具高化学稳定性、环境相容性及低成本优势, 但PCN材料的低介电常数导致光生电子-空穴之间存在较强的库仑作用力, 导致激子解离效率低以及载流子转移速率慢、复合严重, 极大制约了其光催化活性的提升.

本文采用一步熔盐法合成了同时引入K离子和-C≡N基团的高结晶性PCN (M-KPCN), 通过阳离子和阴离子之间的强耦合作用强化了内建电场, 显著降低了光催化材料的激子结合能, 极大的提升了载流子分离和电荷传输效率. 变温荧光光谱测试结果直观表明, M-KPCN材料的激子结合能从传统的PCN的53.17 meV减至34.64 meV, 同时室温激子解离效率由11.9%提高到25%. Zeta电位测定结果表明, 阴阳离子对的相互作用有效增强了内建电场强度. 密度泛函理论计算结果表明, 激子解离效率提高的原因在于分子偶极矩的扩大(从原始PCN的1.17 D增大至16.38 D)和电荷密度的局域化分布. 飞秒瞬态吸收光谱表明, 离子对之间的相互作用可以有效地促进电子转移, 形成浅电子陷阱, 减少深层陷阱对电子的捕获, 从而增强材料的光催化活性. 与未改性的PCN相比, 在可见光光照条件下, M-KPCN材料的人工光合成H₂O₂的速率可达9.3 mmol g^-1 h^-1, 性能提升了46.6倍. 通过自由基捕获实验、电子顺磁共振和原位红外等表征手段确定了人工光合成H₂O₂是通过两步单电子ORR路径合成. 机理研究发现, M-KPCN材料可以显著增强光催化材料与O₂分子之间的作用, O₂在M-KPCN表面吸附能被显著降低至-1.012 eV, 电子转移数增加至0.899, 这表明催化剂表面因阴阳离子对耦合作用导致的局域电子富集显著增强对O₂的吸附和活化; 另一方面, 阴阳离子对相互作用强化的内建电场有效促进了激子解离, 二者的协同作用最终实现了H₂O₂的高效人工光合成. 此外, M-KPCN材料还可以实现多种芳香醇向芳香醛的高效选择性人工光合成, 底物转化率高达84%-93%且选择性大于99%.

综上, 本工作创新性的通过一步熔盐法在高结晶氮化碳材料中成功引入了阴阳离子对, 有效解决了PCN有机光催化材料的激子解离效率低、载流子复合快的本征缺陷, 实现了H₂O₂及多种芳香醛高附加值化学品的高效人工光合成, 阐明了反应机制, 为设计和发展更高效的人工光合成催化剂提供了新思路.

关键词: 聚合物氮化碳, 阴阳离子对, 熔盐法, 激子解离, 过氧化氢光合成

Abstract:

Enhancing the carrier separation efficiency and charge transport properties of polymeric carbon nitride (PCN) has been a major focus of research. Extensive interest has been directed toward its modification and functionalization. In this study, a molten-salt approach was employed to simultaneously introduce cationic (K⁺) and anionic (-C≡N) species, enabling the one-step synthesis of highly crystalline PCN with significantly improved carrier separation and charge transport efficiencies. Comprehensive experimental characterization and theoretical calculations reveal that the coupling interaction between the cations and anions substantially increased the localized charge distribution, thereby facilitating exciton dissociation. Moreover, the incorporation of -C≡N and K⁺ ion pairs enhanced the adsorption and activation of O₂, driving the two-electron oxygen reduction reaction (2e^- ORR) to produce H₂O₂, exhibiting a remarkable 46.6-fold increase over unmodified PCN. This work provided valuable insights into the critical role of cation-anion pairs in enhancing exciton dissociation, paving the cost-effective way for photocatalysts toward efficient solar energy conversion and high-value-added chemicals artificial photosynthesis.

Key words: Polymeric carbon nitride, Cation-anion ion pairs, Molten salt approach, Exciton dissociation, H₂O₂ photosynthesis

李俊青, 何科林, 陶英, 陈超, 谢林富, 马云飞, 王骏鹏, 许长文, 李杨, 张启涛. 阴阳离子对促进结晶氮化碳激子解离实现过氧化氢高效人工光合成[J]. 催化学报, 2026, 82: 174-186.

Junqing Li, Kelin He, Ying Tao, Chao Chen, Linfu Xie, Yunfei Ma, Junpeng Wang, Changwen Xu, Yang Li, Qitao Zhang. Promoting exciton dissociation in crystalline carbon nitride via cation-anion synergy for hydrogen peroxide photosynthesis[J]. Chinese Journal of Catalysis, 2026, 82: 174-186.

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https://www.cjcatal.com/CN/Y2026/V82/I3/174

图/表 6

Fig. 1. Synthesis processes and morphology of M-KPCN. (a) Schematic diagram of the synthesis procedures of M-KPCN. (b,c) HR-TEM images of the M-KPCN sample. HAADF-STEM image (d) and distribution of element mapping images (e,f) of M-KPCN sample.

Fig. 2. Structural characterization of M-KPCN. XRD patterns (a), FT-IR spectra (b), and ESR spectra (c) of U-PCN, M-PCN, U-KPCN and M-KPCN. C 1s (d) and N 1s (e) XPS spectra of U-PCN and M-KPCN. (f) Solid-state 13C MAS NMR spectra of original U-PCN and M-KPCN. UV-vis diffuse reflection spectra (g) and Tauc plot (h) of U-PCN, M-PCN, U-KPCN and M-KPCN. (i) Schematic illustration of band structures of U-PCN, M-PCN, U-KPCN and M-KPCN.

Fig. 3. Characterization of exciton dissociation and charge transport. (a) Transient photocurrent response under visible light illumination. EIS spectra (b), PL spectra (c), and Time-resolved PL spectra (d) of as-formed samples. Temperature-dependent PL spectra of M-PCN (e) and M-KPCN (f). Calculated charge density distribution of VBM and CBM in U-PCN (g,h) and M-KPCN (i,j). The charge difference density of O2 adsorbed on U-PCN (k) and M-KPCN (l). The yellow represents the electron accumulation area, and the light blue represents the electron dissipation area. The blue, gray, white, and red spheres represent N, C, H, and O atoms, respectively. (m) Quantitative charge transfer (ΔQ) from photocatalyst to adsorbed O2.

Fig. 4. 2D mapping fs-TA spectra of U-PCN (a) and M-KPCN (d). TA spectra of U-PCN (b) and M-KPCN (e). Corresponding TA kinetic traces of U-PCN (c) and M-KPCN (f). C 1s (g), N 1s (h), and K 2p (i) spectra of M-KPCN in dark and light.

Fig. 5. Photocatalytic performance of M-KPCN in the photosynthesis of H2O2 and high-value-added chemicals. (a) Photocatalytic H2O2 generation rates of as-prepared samples. (b) Photocatalytic H2O2 generation rates and associated AQY under photoirradiation (wavelengths of 365, 420, 450, 500, and 600 nm). (c) Repeated runs of photocatalytic H2O2 production over M-KPCN for 5 times under visible light irradiation (3 h for each cycle). Yield and conversion rate of benzyl alcohol (d), methylbenzyl alcohol (e), and 4-methoxybenzyl alcohol (f) using M-KPCN photocatalyst under visible light irradiation.

Fig. 6. Produced free radicals and proposed mechanism study. (a) Koutecky-Levich plots of U-PCN, M-PCN and M-KPCN measured by RDE. (b) Photocatalytic H2O2 generation by M-KPCN with the addition of AgNO3, BQ, and TBA sacrificial reagents. (c) Photocatalytic H2O2 generation by M-KPCN with different atmosphere conditions. In-situ EPR signals of ?O2- (d) and ?OOH (e) over M-KPCN in the presence of DMPO. (f) EPR signals of 1O2 was tested in the presence of TEMP. (h) Calculated Gibbs free energy variation during H2O2 production process for each intermediate species using U-PCN and M-KPCN.

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阴阳离子对促进结晶氮化碳激子解离实现过氧化氢高效人工光合成

Promoting exciton dissociation in crystalline carbon nitride via cation-anion synergy for hydrogen peroxide photosynthesis

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