S/B/K共掺杂调控氮化碳电子结构用于高效光催化合成H2O2

doi:10.6023/A26040135

摘要/Abstract

基于石墨相氮化碳(g-C₃N₄)光催化氧气(O₂)还原合成过氧化氢(H₂O₂)具有重要的基础研究价值和实际应用价值. 针对g-C₃N₄电子结构对称性高、光生载流子复合严重、O₂活化能力弱及光催化合成H₂O₂效率低的核心瓶颈, 本工作提出了一种多元素共掺杂协同缺陷工程调控电子结构的改性策略, 通过两步煅烧结合离子热处理, 成功制备了S/B/K三元共掺杂的g-C₃N₄催化剂(KBSCN). 该策略同步实现了富电子S、缺电子B和K在g-C₃N₄骨架内的均匀掺杂, 以及氰基(−C≡N)和氮空位(N_v)的原位引入. 系统开展了结构表征、光电性能测试与光催化性能评价, 并结合密度泛函理论(DFT)计算, 揭示了多元素掺杂对g-C₃N₄电子结构与反应动力学的协同调控机制. 研究结果表明, S/B/K三元共掺杂可有效打破g-C₃N₄的对称结构, 拓宽可见光响应范围. 光催化O₂还原合成H₂O₂性能评价结果表明, 在可见光照射下, KBSCN催化剂上的H₂O₂生成速率高达8132 μmol•g⁻¹•h⁻¹, 为未改性g-C₃N₄(CN)生成速率的185倍. 机理研究表明, S/B/K三元共掺杂通过诱导最高占据分子轨道(HOMO)与最低未占据分子轨道(LUMO)的空间分离, 极大促进了光生载流子的分离与迁移. 此外, 结合自由基捕获实验、原位电子顺磁共振(EPR)、原位漫反射傅里叶变换红外(in situ DRIFT)表征与Bader电荷电子转移分析, S/B/K三元共掺杂可促进光催化O₂还原反应(ORR)采取以超氧自由基(•O₂⁻)为中间体的间接两电子还原路径, 从动力学上显著提升2e⁻-ORR的反应速率. 本工作通过对g-C₃N₄的电子结构与表面反应动力学的调控实现了可见光驱动下高效合成H₂O₂, 为低成本、高性能光催化合成H₂O₂催化剂的设计提供了新的思路.

关键词: 光催化, H₂O₂, g-C₃N₄, 多元素共掺杂, 协同效应

Efficient photocatalytic reduction of O₂ to H₂O₂ over graphitic carbon nitride (g-C₃N₄) is of significant practical value. To overcome the intrinsic drawbacks of g-C₃N₄ including high electronic structure symmetry, severe photogenerated carrier recombination, weak O₂ activation ability, and low photocatalytic H₂O₂ synthesis efficiency, herein a regulation strategy of electronic structure via multi-element co-doping coupled with defect engineering was proposed. A S/B/K ternary co-doped g-C₃N₄ catalyst (denoted as KBSCN) was fabricated by a facile two-step calcination followed by ionothermal treatment. This strategy enabled the simultaneous homogeneous incorporation of electron-rich S and electron-deficient B into the g-C₃N₄ framework, intercalation of K, as well as the introduction of cyano groups (−C≡N) and nitrogen vacancies (N_v). The structural and photoelectrochemical properties of KBSCN were systematically characterized, and its photocatalytic performance in photocatalytic reduction of O₂ to H₂O₂ was evaluated. Combined with density functional theory (DFT) calculations, the synergistic regulation mechanism of multi-element doping on the electronic structure and reaction kinetics of KBSCN was elucidated. S/B/K ternary co-doping can effectively break the inherent symmetric structure and broaden the visible light response range of g-C₃N₄. In photocatalytic reduction of O₂, under visible light irradiation, KBSCN exhibited a H₂O₂ production rate of 8132 μmol•g⁻¹•h⁻¹, which was 185 times that of pristine g-C₃N₄. Mechanistic studies indicate that S/B/K co-doping greatly promotes the separation and migration of photogenerated carriers by inducing the spatial separation of the highest occupied molecular orbital (HOMO) and the lowest unoccupied molecular orbital (LUMO). Moreover, by combining radical scavenging experiments, in situ electron paramagnetic resonance (EPR), in situ diffuse reflectance infrared Fourier transform (in situ DRIFT) spectroscopy characterizations and Bader charge analysis for electron transfer, it is revealed that S/B/K co-doping drives the photocatalytic O₂ reduction reaction (ORR) to proceed via an indirect two-electron reduction pathway with superoxide radicals (•O₂⁻) as the intermediate, thus significantly boosting the reaction kinetics of the 2e⁻-ORR process. This work provides a new avenue for the design of g-C₃N₄-based catalysts for efficient visible light-driven H₂O₂ synthesis via synergistic regulation of electronic structure and surface reaction kinetics.

Key words: photocatalysis, H₂O₂, g-C₃N₄, multi-element co-doping, synergistic effect

引用此文

冯丹宁, 封波, 万坤, 谢颂海, 裴燕, 乔明华, 宗保宁. S/B/K共掺杂调控氮化碳电子结构用于高效光催化合成H₂O₂[J]. 化学学报, 2026, 84(7): 1140-1152.

Danning Feng, Bo Feng, Kun Wan, Songhai Xie, Yan Pei, Minghua Qiao, Baoning Zong. Electronic Structure Engineering of g-C₃N₄ via S/B/K Co-Doping for Efficient Photocatalytic H₂O₂ Synthesis[J]. Acta Chimica Sinica, 2026, 84(7): 1140-1152.

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图/表 8

图1. (a) KBSCN制备过程示意图; (b) CN和(c) KBSCN的SEM图像; (d) CN的TEM图像; (e) KBSCN的HRTEM图像; (f) KBSCN的EDS元素分布图

Figure 1. (a) Schematic illustration of the preparation process of KBSCN, SEM images of (b) CN and (c) KBSCN, TEM image of (d) CN, and HRTEM image (e) and (f) EDS mapping images of KBSCN

图2. CN和KxCN的(a) XRD谱和(b) FTIR谱

Figure 2. (a) XRD patterns and (b) FTIR spectra of CN and KxCN

图3. CN和KBSCN的13C MAS NMR谱

Figure 3. 13C MAS NMR spectra of CN and KBSCN

图4. CN和KxCN的(a) XPS全谱、(b) C 1s谱和(c) N 1s谱; (d) KSCN和KBSCN的S 2p谱; (e) KBCN和KBSCN的B 1s谱; (f) KxCN的K 2p谱

Figure 4. (a) Survey XPS spectra, (b) C 1s spectra, and (c) N 1s spectra of CN and KxCN. (d) S 2p spectra of KSCN and KBSCN. (e) B 1s spectra of KBCN and KBSCN. (f) K 2p spectra of KxCN

图5. CN和KxCN上(a) H2O2的生成浓度随时间的变化和(b)光催化O2还原合成H2O2生成速率的比较; (c)不同气氛(O2、air、N2)下KBSCN上光催化O2还原合成H2O2的生成速率对比; (d) KBSCN与已报道的氮化碳基催化剂的H2O2生成速率对比; (e)不同入射光波长(400、420、450和500 nm)下获得的AQY与KBSCN的紫外−可见漫反射光谱的对比; (f) N2气氛下CN和KxCN对H2O2 (c0=5 mmol•L−1)的光催化分解性能; (g)光催化O2还原生成H2O2过程中CN和KxCN对应的kf与kd; (h) KBSCN在光催化O2还原合成H2O2反应中的循环套用稳定性; 所有光催化性能数据均为3次独立重复实验的平均值, 图中误差棒代表3次平行实验的标准偏差

Figure 5. (a) Time-dependent production of H2O2 and (b) comparison of the H2O2 production rate in photocatalytic O2 reduction over CN and KxCN. (c) H2O2 production rate over KBSCN in different atmospheres (O2, air, or N2). (d) Comparison of the H2O2 production rate between KBSCN and reported carbon nitride-based catalysts. (e) AQY obtained at different incident light wavelengths (400, 420, 450, and 500 nm) versus UV-vis DRS of KBSCN. (f) Photocatalytic decomposition of H2O2 (c0=5 mmol•L−1) over CN and KxCN under N2 atmosphere. (g) kf and kd for H2O2 production over CN and KxCN in photocatalytic reduction of O2 to H2O2. (h) Recyclability of KBSCN in photocatalytic O2 reduction to H2O2. All photocatalytic performance data are presented as the average of three independent replicate experiments, and the error bars in the figures represent the standard deviation of three parallel experiments

图6. CN和KxCN的(a) UV-vis DRS光谱和(b)能带结构及H2O2生成对应的氧化还原电位; (c) CN和KxCN的PL光谱; (d) CN和KBSCN的TRPL光谱; CN和KxCN的(e)瞬态光电流响应和(f) Nyquist图(插图为拟合EIS所采用的等效电路)

Figure 6. (a) UV-vis DRS spectra and (b) energy band structure and redox potential for photocatalytic production of H2O2 of CN and KxCN. (c) PL spectra of CN and KxCN. (d) TRPL spectra of CN and KBSCN. (e) Photocurrent response curves and (f) EIS Nyquist plots of CN and KxCN (the inset represents the equivalent circuit for fitting EIS)

图7. (a)不同捕获剂对KBSCN上H2O2生成速率的影响(所有光催化性能数据均为3次独立重复实验的平均值, 图中误差棒代表3次平行实验的标准偏差); (b)黑暗和光照条件下CN和KBSCN的DMPO-•O2− EPR谱; (c)在O2饱和的0.1 mol•L−1 KOH溶液(pH=13)中, 以1600 r•min−1的转速测试CN和KBSCN的LSV曲线; (d)由LSV测试结果计算得到CN和KBSCN的H2O2选择性和电子转移数; (e)不同光照时间间隔下KBSCN上的in situ DRIFT谱(测试条件: 可见光照射, O2-水蒸汽气氛)

Figure 7. (a) H2O2 production rate in the presence of different scavengers over KBSCN (All photocatalytic performance data are presented as the average of three independent replicate experiments, and the error bars in the figure represent the standard deviation of three parallel experiments). (b) EPR signals of DMPO-•O2− generated on CN and KBSCN under dark or visible light irradiation situation. (c) The LSV curves of CN and KBSCN measured at 1600 r•min−1 in O2-saturated 0.1 mol•L−1 KOH solution (pH=13); (d) Selectivity of H2O2 production and electron transfer number derived from LSV test. (e) In situ DRIFT spectra detected on KBSCN upon visible light irradiation at different time intervals (Experimental conditions: visible light irradiation and O2-water vapor atmosphere)

图8. (a) CN和KxCN的LUMO和HOMO分布图; (b) CN和KxCN上的O2吸附能; (c) CN和KBSCN活性位点上O2的差分电荷密度(黄色与青色区域分别代表电子富集与电子缺失); (d) CN和KxCN上光催化ORR的自由能变化曲线(插图为KBSCN表面发生的ORR过程); 粉色、棕色、灰色、红色、黄色、绿色、紫色分别代表氢、碳、氮、氧、硫、硼、钾原子

Figure 8. (a) LUMO and HOMO distributions for CN and KxCN. (b) Adsorption energy of O2 on CN and KxCN. (c) Differential charge density of O2 on the active site of CN and KBSCN (The yellow and the cyan regions represent electron accumulation and depletion, respectively). (d) Free energy profiles for photocatalytic ORR over CN and KxCN (The insets show the ORR process occurring on KBSCN). The pink, brown, gray, red, yellow, green, and purple colors represent hydrogen, carbon, nitrogen, oxygen, sulfur, boron, and potassium, respectively

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S/B/K共掺杂调控氮化碳电子结构用于高效光催化合成H₂O₂

Electronic Structure Engineering of g-C₃N₄ via S/B/K Co-Doping for Efficient Photocatalytic H₂O₂ Synthesis

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