亚埃尺度空间调控Fe1-N4配位结构实现高效C-H键氧化过程

doi:10.1016/S1872-2067(26)65096-6

催化学报 ›› 2026, Vol. 87: 305-315.DOI: 10.1016/S1872-2067(26)65096-6

亚埃尺度空间调控Fe₁-N₄配位结构实现高效C-H键氧化过程

段江林^a^,¹, 邓鹏程^a^,¹, 熊惠峰^a^,¹, 杨娜^b^,^*(), 周雪灵^a, 王静雯^a, 张瑞^c, 冯丹^d, 杨级^e^,^*(), 覃勇^f^,^*(), 任煜京^a^,^g^,^*()

^a 西北工业大学生命科学与技术学院, 生物与催化交叉研究中心, 陕西西安 710072
^b 电子科技大学材料与能源学院, 四川成都 611731
^c 上海应用技术大学化工与能源技术学部, 上海 201418
^d 西北工业大学分析测试中心, 陕西西安 710072
^e 厦门大学化学化工学院, 福建厦门 361005
^f 青岛科技大学材料科学与工程学院, 山东青岛 266042
^g 西北工业大学深圳研究院, 广东深圳 518057

收稿日期:2025-11-30 接受日期:2026-01-12 出版日期:2026-08-18 发布日期:2026-06-24
通讯作者: ^*电子信箱: yna@uestc.edu.cn (杨娜),
chem.yang@xmu.edu.cn (杨级),
qinyong@qust.edu.cn (覃勇),
作者简介:¹共同第一作者.
基金资助:
国家自然科学基金(22303031);国家自然科学基金(22472131);国家自然科学基金(22202075);国家自然科学基金(22402164);国家自然科学基金(22002118);国家重点研发项目(2023YFA1506603);四川省自然科学基金青年项目(2024NSFSC1103);广东省基础与应用基础研究基金(2024A1515012109);中央引导地方科技发展专项(2025ZY-XCZXZS-26)

Subangstrom spatial regulation of Fe₁-N₄ coordination structure for remarkably efficient C‒H bond oxidation

Jianglin Duan^a^,¹, Pengcheng Deng^a^,¹, Huifeng Xiong^a^,¹, Na Yang^b^,^*(), Xueling Zhou^a, Jingwen Wang^a, Rui Zhang^c, Dan Feng^d, Ji Yang^e^,^*(), Yong Qin^f^,^*(), Yujing Ren^a^,^g^,^*()

^a Interdisciplinary Research Center of Biology & Catalysis, School of Life Science and Technology, Northwestern Polytechnical University, Xi’an 710072, Shaanxi, China
^b School of Materials and Energy, University of Electronic Science and Technology of China, Chengdu 611731, Sichuan, China
^c Faculty of Chemical Engineering and Energy Technology, Shanghai Institute of Technology, Shanghai 201418, China
^d Analytical & Testing Center, Northwestern Polytechnical University, Xi’an 710072, Shaanxi, China
^e College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, Fujian, China
^f College of Materials Science and Engineering, Qingdao University of Science and Technology, Qingdao 266042, Shandong, China
^g Shenzhen Research Institute of Northwestern Polytechnical University, Shenzhen 518057, Guangdong, China

Received:2025-11-30 Accepted:2026-01-12 Online:2026-08-18 Published:2026-06-24
Contact: qinyong@qust.edu.cn (Y. Qin),
About author:¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22303031);National Natural Science Foundation of China(22472131);National Natural Science Foundation of China(22202075);National Natural Science Foundation of China(22402164);National Natural Science Foundation of China(22002118);National Key R&D Program of China(2023YFA1506603);Youth Science Foundation Project of Sichuan Province(2024NSFSC1103);Guangdong Basic and Applied Basic Research Foundation(2024A1515012109);Central Guidance for Local Scientific and Technological Development(2025ZY-XCZXZS-26)

摘要/Abstract

摘要：

催化活性中心的精准调控是提升多相催化性能的重要途径. 传统纳米催化剂通常通过调节晶面、台阶位、缺陷和低配位原子等结构来影响反应活性和选择性. 然而, 这类催化剂往往同时存在多种活性位点, 结构较为复杂, 难以建立明确的构效关系, 因此也限制了催化剂的理性设计. 单原子催化剂的出现, 为构建原子级均一活性中心提供了理想的平台, 从而能更清楚地研究金属配位结构、电子状态与催化性能之间的联系. 然而, 即便在典型的M₁-N-C体系中, 难以实现配位环境的精准均一调控. 传统制备方法中的高温处理过程通常会带来配位环境不均一、活性金属团聚以及N/C/O混合配位等问题.此外, 相比配位数、配体类型和自旋态这些已被广泛研究的结构因子, 金属‒配体键长这一结构参数对电子结构与反应动力学的影响, 却少有研究.

本文提出了一种面向单原子活性中心的亚埃尺度调控策略: 在结构完全均一的Fe₁-N₄单原子催化体系中, 我们实现了Fe-N键长的精确、连续调节, 并系统研究了这种微小几何变化对C‒H键氧化反应的影响. 通过构建了一个仅以Fe‒N键长为为变化因素的模型体系, 使Fe‒N配位键在2.03到1.93 Å的范围内实现连续压缩, 调控精度达到亚埃级. 多种表征结果一致表明, 在整个调控过程中Fe单原子始终保持一致的Fe₁-N₄配位结构和稳定的低自旋状态, 有效排除了配位数变化、自旋态转变及结构不均一性对催化性能的干扰. 催化评价结果显示, 仅0.1 Å的Fe‒N键压缩就可使C‒H键氧化速率提高近23倍, 说明单原子活性中心对极其微小的结构变化非常敏感. 理论计算进一步表明: 随着Fe‒N键缩短, Fe中心3d轨道电子密度增加, 电子更容易在金属中心积累. 这种电子富集显著增强了Fe对过氧基团的活化能力, 降低了反应能垒, 从而加快了反应过程.

综上, 本研究在结构完全均一的单原子催化体系中实现了亚埃尺度金属‒配体键长的调控, 并建立了Fe‒N键长、Fe电子结构与反应动力学之间可量化的构效关系. 该工作将多相催化中“精准化学”的调控范式从纳米-原子尺度进一步推进至亚埃尺度, 为非贵金属催化剂的理性设计提供了新的理念与方法.

关键词: 单原子催化剂, 亚埃尺度空间调控, C?H键氧化, Fe₁-N₄, 构效关系

Abstract:

Structural regulation of heterogeneous active centers has been widely explored at the nano- and atomic-level, yet achieving subangstrom precision remains highly challenging. Here, we demonstrate subangstrom spatial regulation of the Fe‒N bond within a fully uniform Fe₁-N₄ coordination structure. Strikingly, a 0.1 Å bond compression led to nearly a 23-fold enhancement in C‒H bond oxidation. Advanced characterizations confirmed the uniform low-spin Fe₁-N₄ configuration, with the Fe‒N bond distance gradually decreasing from 2.03 to 1.93 Å during pyrolysis. This subtle structural modification originates from the concerted effect of temperature- and curvature-induced distortion on the curved carbon surface, as further supported by theoretical simulations. The Fe‒N bond distance was found to govern the electronic structure of the Fe center, where compressed coordination promotes electron accumulation. This structural modulation directly results in the high capability for peroxide group activation on Fe₁ single atoms, which affords outstanding C‒H bond oxidation, comparable to supported noble metal catalysts. This study provides the experimental demonstration of structural regulation at subangstrom scale, extending the concept of “precise chemistry” in catalyst design from the nano- and atomic- to the subangstrom scale.

Key words: Single-atom catalyst, Subangstrom spatial regulation, C?H bond oxidation, Fe₁-N₄, Structure-performance relationship

段江林, 邓鹏程, 熊惠峰, 杨娜, 周雪灵, 王静雯, 张瑞, 冯丹, 杨级, 覃勇, 任煜京. 亚埃尺度空间调控Fe₁-N₄配位结构实现高效C-H键氧化过程[J]. 催化学报, 2026, 87: 305-315.

Jianglin Duan, Pengcheng Deng, Huifeng Xiong, Na Yang, Xueling Zhou, Jingwen Wang, Rui Zhang, Dan Feng, Ji Yang, Yong Qin, Yujing Ren. Subangstrom spatial regulation of Fe₁-N₄ coordination structure for remarkably efficient C‒H bond oxidation[J]. Chinese Journal of Catalysis, 2026, 87: 305-315.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65096-6

https://www.cjcatal.com/CN/Y2026/V87/I8/305

图/表 7

Fig. 1. Synthesis and structural characterizations of Fe1-N4/ND catalysts. (a) Schematic illustration of the catalyst synthesis including impregnation and thermal treatment. (b) XRD patterns of all Fe1-N4/ND catalysts with ND as reference. AC-HAADF-STEM images of Fe1-N4/ND-200 (c), Fe1-N4/ND-400 (d) and Fe1-N4/ND-600 (e) catalysts.

Fig. 2. Spectroscopic characterizations of Fe1-N4/ND catalysts. (a) 57Fe Mössbauer spectra. (b) The k3-weighted FT-EXAFS spectra of Fe1-N4/ND catalysts with Fe foil, Fe2O3 and FePc as comparison. (c) Corresponding EXAFS fitting curves in R space.

Table 1 The best-fitted EXAFS results of Fe1-N4/ND-T.

Sample	Shell	CN	R (Å)	σ² (10² Å²)	ΔE₀ (eV)	R-factor (%)
Fe Foil	Fe-Fe	12.0	2.54	—	—	—
Fe-Pc	Fe-N	4.0	1.98	—	—	—
Fe₁-N₄/ND-RT	Fe-N	3.8	2.03	0.6	‒2.4	0.4
Fe₁-N₄/ND-200	Fe-N	4.1	2.02	0.6	‒2.9	0.3
Fe₁-N₄/ND-400	Fe-N	4.0	1.96	0.8	‒7.5	0.2
Fe₁-N₄/ND-600	Fe-N	4.0	1.93	0.8	‒7.5	0.2

Fig. 3. Compression mechanism. (a) The radial distribution functions of corresponding Fe?N bond length at different temperatures during AIMD simulations of Fe1-N4 on curved graphene surface. (b) Schematic illustration for the compression of Fe?N bond on the curved graphene surface. (c) The theoretical and experimental compression ratio of different size carbon nanotubes. The structure of Fe1-N4 site on six, eight and fourteen of six-membered rings forming carbon nanotubes.

Fig. 4. Electronic structure confirmation. (a) The PDOS results of Fe-3d orbit for Fe1-N4/ND-600, Fe1-N4/ND-400 and Fe1-N4/ND-200 samples. XANES spectra (b) and corresponding average oxidation state (c) of Fe1-N4/ND-T samples.

Fig. 5. Catalytic performance evaluation results. Catalytic oxidation of TMB (a) and ethylbenzene (b) on Fe1-N4/ND-T catalysts. (c) Substrate scope for catalytic oxidations on Fe1-N4/ND-600 catalyst.

Fig. 6. The structure-activity relationship. (a) The adsorption energy (ΔE) of H2O2/OH on Fe1-N4/ND-T catalysts. (b-d) 3D (top view) and 2D (bottom view) charge density differences after OH adsorption on various Fe1-N4 models, herein, for the 3D view, charge accumulation and depletion are signified by yellow and blue isosurfaces; for the 2D view, charge accumulation and depletion are signified by red and blue areas. (e) The calculated Gibbs free energy diagram of H2O2 activation on Fe1-N4/ND-T catalysts. (f) The correlation between the activity of Fe1-N4/ND-T, the average oxidation state of Fe1 species, and compression ratio of Fe?N bond. The pentagon and circle represent TOF determined from catalytic oxidation of TMB and solvent-free C?H bond oxidation of ethylbenzene, and the star represents the average oxidation state of Fe1 species determined from XANES characterization.

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亚埃尺度空间调控Fe₁-N₄配位结构实现高效C-H键氧化过程

Subangstrom spatial regulation of Fe₁-N₄ coordination structure for remarkably efficient C‒H bond oxidation

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