掺杂超薄聚合物氮化碳缺陷态能级的精准调控及其光催化性能增强研究

doi:10.1016/S1872-2067(26)65181-9

催化学报 ›› 2026, Vol. 90: 220-230.DOI: 10.1016/S1872-2067(26)65181-9

掺杂超薄聚合物氮化碳缺陷态能级的精准调控及其光催化性能增强研究

门程正^a, 黄淼婷^a, 苏通明^b, 廖思蔚^a, 石建英^a^,^*()

^a 中山大学化学学院, 功能材料莱恩研究所, 广东广州 510275
^b 广西大学化学化工学院, 广西南宁 530004

收稿日期:2026-04-25 接受日期:2026-06-25 出版日期:2026-11-18 发布日期:2026-09-09
通讯作者: *电子信箱: shijying@mail.sysu.edu.cn (石建英).
基金资助:
国家自然科学基金(22371314);国家自然科学基金(22075332);国家自然科学基金(22208065)

Fine-tuning the energy level of defect states in doped ultrathin carbon nitride polymer for enhanced photocatalytic performance

Chengzheng Men^a, Miaoting Huang^a, Tongming Su^b, Siwei Liao^a, Jianying Shi^a^,^*()

^a School of Chemistry, Lehn Institute of Functional Materials, Sun Yat-Sen University, Guangzhou 510275, Guangdong, China
^b School of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, Guangxi, China

Received:2026-04-25 Accepted:2026-06-25 Online:2026-11-18 Published:2026-09-09
Contact: *E-mail:shijying@mail.sysu.edu.cn(J. Shi).
Supported by:
National Natural Science Foundation of China(22371314);National Natural Science Foundation of China(22075332);National Natural Science Foundation of China(22208065)

摘要/Abstract

摘要：

石墨相氮化碳(CN)作为一种无金属聚合物半导体, 因其具有可见光响应、化学稳定性高且可规模化合成等优势, 被视为太阳能光催化分解水制氢和CO₂还原的理想候选材料. 然而, 本征CN存在光生载流子复合严重、导电性差及可见光捕获能力不足等瓶颈, 制约了其实际应用. 引入缺陷态或掺杂异质原子(如碳掺杂)被认为是拓展可见光吸收、调控能带结构的有效策略, 但缺陷态能级在带隙内的分布特征如何影响光生电子行为、光吸收与电荷分离的协同关系, 以及其与宏观光催化性能之间的定量关联, 迄今缺乏系统的实验阐明. 因此, 精准调控缺陷态能级分布并揭示其对光催化各基元步骤的影响机制, 对理性设计高性能CN基光催化剂具有重要的科学意义.

本文提出了一种通过芳香族二羧酸异构体(邻苯二甲酸、间苯二甲酸、对苯二甲酸)调控碳掺杂超薄氮化碳缺陷态能级分布的新策略. 以尿素为前驱体, 分别引入三种不同羧基取代位置的苯二甲酸, 经一步热聚合-原位剥离法制备了系列碳掺杂超薄多孔CN纳米片(PTCN, IPCN, PPCN). 系统表征表明, 不同异构体因空间位阻和几何构型差异, 导致CN骨架中碳掺杂浓度和七嗪环结构有序度显著不同: 邻位取代(PTCN)空间位阻最大, 碳掺杂量最低; 对位取代(PPCN)位阻最小, 碳掺杂量最高但结构无序度最大; 间位取代(IPCN)则实现了掺杂浓度与结构完整性的最佳平衡. 光谱与动力学研究揭示了三种材料截然不同的缺陷态能级特征: IPCN呈现窄分布的缺陷能级, 表现为无吸收拖尾的紫外-可见光谱和约530 nm处尖锐的光致发光(PL)发射峰; 而PPCN形成连续分布的多重缺陷能级, 导致可见光区呈现宽化吸收尾和宽化PL谱. 飞秒瞬态吸收光谱显示, 2-IPCN的激子湮灭(τ₂ = 15.2 ps)和缺陷态捕获(τ₃ = 316 ps)寿命显著长于2-PPCN和2-PTCN, 表明其电荷复合速率降低. 时间分辨PL和光电化学测试进一步证实, IPCN的局域化缺陷态提供了合适的热力学驱动力, 促进光生载流子空间分离并向催化活性位点高效迁移. 在可见光(λ ≥ 420 nm)下, 最优的2-IPCN样品表现出卓越的光催化活性: 产氢速率达4058 μmol g⁻¹ h⁻¹(为CN的7.7倍), CO₂还原产CO速率达526.3 μmol g⁻¹ h⁻¹(为CN的18.4倍), 且循环稳定性良好. 表观量子效率与吸收光谱高度吻合, 说明吸收光子可被高效利用. 密度泛函理论计算表明, 碳掺杂诱导最高占据分子轨道与最低未占分子轨道空间分离, 产生内建偶极场驱动载流子分离; 而IPCN的窄分布缺陷能级有效抑制了辐射复合, 同时加速了电子向Pt或Co(bpy)₃²⁺助催化剂活性位点的转移.

综上, 本文阐明了缺陷态能级分布对光吸收、电荷分离及表面反应协同调控的微观机制, 为聚合物光催化剂的理性设计提供了新的分子工程策略. 未来, 通过梯度/分级缺陷结构或二元异构体共掺杂进一步精细调控缺陷能级, 有望实现电导率、电荷分离与催化活性之间的协同优化, 推动CN基光催化材料在太阳能转化领域的实际应用.

关键词: 超薄氮化碳, 光催化, 缺陷能级, 缺陷工程

Abstract:

The mechanisms governing photo-induced electron behavior and its link to visible light responsiveness in graphitic carbon nitride (CN), particularly doped or defective variants, remain poorly understood. This study presents a strategy for band structure modulation in carbon-doped CN through isomeric modulation of benzene dicarboxylic acid dopant precursors. Ultraviolet-visible (UV-vis) absorption, photoluminescence (PL) spectroscopy, and density functional theory calculations were employed to determine the energy band structure, while time-resolved spectra probed carrier dynamics across different timescales. Isophthalic acid-doped carbon nitride (IPCN) exhibits a narrowly distributed defect energy level. This manifests in a tailless UV-vis absorption profile and a sharp PL emission peak in the visible region. In contrast, terephthalic acid-doped carbon nitride (PPCN) displays multiple, continuously distributed defect levels. This results in band-edge absorption overlapping with a broad visible spectrum and a broadened PL emission peak, arising from the superposition of band-edge transitions and low-energy absorption tails. The defect levels with continuous distribution in PPCN enhance electrical conductivity but also promotes charge recombination. Conversely, the defect states in IPCN provide a suitable thermodynamic driving force for carrier migration to catalytic active site, in addition to promote spatial charge carrier separation. Consequently, visible-light CO₂ reduction and H₂ evolution activities of carbon-doped CN are markedly enhanced. This work elucidates the synergistic balance between optical absorption efficiency and charge separation performance in doped CN, providing experimental validation for the rational design of CN-based photocatalysts with superior optical and catalytic properties.

Key words: Ultrathin carbon nitride, Photocatalysis, Defect levels, Defect engineering

门程正, 黄淼婷, 苏通明, 廖思蔚, 石建英. 掺杂超薄聚合物氮化碳缺陷态能级的精准调控及其光催化性能增强研究[J]. 催化学报, 2026, 90: 220-230.

Chengzheng Men, Miaoting Huang, Tongming Su, Siwei Liao, Jianying Shi. Fine-tuning the energy level of defect states in doped ultrathin carbon nitride polymer for enhanced photocatalytic performance[J]. Chinese Journal of Catalysis, 2026, 90: 220-230.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65181-9

https://www.cjcatal.com/CN/Y2026/V90/I11/220

图/表 8

Fig. 1. (a) Schematic illustration of the synthesis process of ultrathin porous CN nanosheets. The buff, yellow, and brown nanosheets represent PTCN, IPCN, and PPCN, respectively. TEM images of 2-PTCN (b,c), 2-IPCN (d,e), and 2-PPCN (f,g). (h) Wide-angle XRD patterns of CN, 2-PTCN, 2-IPCN and 2-PPCN.

Fig. 2. Solid-state 13C NMR (a) and high-resolution N 1s XPS (b) spectra of CN, 2-PTCN, 2-IPCN, and 2-PPCN. Magnified FT-IR (c) and Raman (d) spectra of CN, 2-PTCN, 2-IPCN, and 2-PPCN.

Fig. 3. Time course of photocatalytic H2 production (a) and photocatalytic H2 production rate (b) of CN, x-PTCN, x-IPCN, x-PPCN (x = 1, 2, 3). (c) Schematic diagram system model of the photocatalytic hydrogen production. Time course of photocatalytic CO2 reduction for gas generation (d) and CO and H2 production rate (e) of CN, 2-PTCN, 2-IPCN, 2-PPCN. (f) Schematic diagram system model of photocatalytic CO2 reduction. (g,h) Cyclic experiments of photocatalytic H2 production and CO2 reduction over the 2-IPCN photocatalyst.

Fig. 4. UV-vis spectra (inset: photographs showing the colors of the samples) and PL spectra (excitation wavelength: 340 nm) of CN, x-PTCN (a,d), x-IPCN (b,e), x-PPCN (c,f) (x = 1, 2, and 3).

Fig. 5. DFT-derived frontier orbital and electronic structure maps. HOMO (a,c,e) and LUMO (b,d,f) isosurfaces, band diagrams and corresponding DOS (g-i) for pristine CN and CN with carbon substituted at distinct pyridinic-nitrogen positions.

Fig. 6. Fs-TA spectra of 2-PTCN (a), 2-IPCN (b), and 2-PPCN (c) at different delay times under a 370 nm pump pulses. Kinetic curves at 660 nm for 2-PTCN (d), 2-IPCN (e), and 2-PPCN (f) samples with corresponding exponential fits. The time-resolved fluorescence decay spectra of CN, 2-PTCN, 2-IPCN, and 2-PPCN were presented as follows: excited at 340 nm and monitored at 460 nm (g), excited at 340 nm and monitored at 530 nm (h), and excited at 340 nm and monitored at 600 nm (i).

Fig. 7. Transient photocurrent response plots (a) and EIS, Nyquist plots (b) of CN, 2-PTCN, 2-IPCN, and 2-PPCN. (c) Schematic diagram of the proposed mechanism for the enhanced photocatalytic performance over 2-IPCN. The UV-vis wavelength-dependent AQY of 2-PTCN (d), 2-IPCN (e), and 2-PPCN (f).

Fig. 8. Comparison of photogenerated carrier migration and separation behaviors in carbon-doped carbon nitrides with localized versus delocalized electronic structures.

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掺杂超薄聚合物氮化碳缺陷态能级的精准调控及其光催化性能增强研究

Fine-tuning the energy level of defect states in doped ultrathin carbon nitride polymer for enhanced photocatalytic performance

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