Peripheral NV-induced electron transfer to Fe1 single atoms for highly efficient O2 activation

doi:10.1016/S1872-2067(25)64651-1

Chinese Journal of Catalysis ›› 2025, Vol. 72: 187-198.DOI: 10.1016/S1872-2067(25)64651-1

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Peripheral N_V-induced electron transfer to Fe₁ single atoms for highly efficient O₂ activation

Fenli Liu^a^,¹, Man Yang^b^,¹, Jianglin Duan^a, Zhiyu Yin^a, Mingyang Shi^a, Fuqing Chen^a, Huifeng Xiong^a, Xin Liu^c, Wengang Liu^e, Qixing Xia^f, Shaodong Sun^b, Dan Feng^g, Haifeng Qi^d^,^*(), Yong Qin^e^,^h^,^*(), Yujing Ren^a^,ⁱ^,^*()

^aInterdisciplinary Research Center of Biology & Catalysis, School of Life Sciences, Northwestern Polytechnical University, Xi’an 710072, Shaanxi, China
^bSchool of Materials Science and Engineering, Xi’an University of Technology, Xi’an 710048, Shaanxi, China
^cSchool of Resources and Materials, Northeastern University at Qinhuangdao, Qinhuangdao 066004, Hebei, China
^dMax Planck-Cardiff Centre on the Fundamentals of Heterogeneous Catalysis FUNCAT, Translational Research Hub, Cardiff University, Maindy Road, Cardiff CF24 4HQ, UK.
^eCollege of Materials Science and Engineering, Qingdao University of Science and Technology, Qingdao 266042, Shandong, China
^fInstitute of Culture and Heritage, Northwestern Polytechnical University, Xi’an 710072, Shaanxi, China
^gAnalytical & Testing Center, Northwestern Polytechnical University, Xi’an 710072, Shaanxi, China
^hState Key Laboratory of Coal Conversion, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001, Shanxi, China
ⁱChongqing Innovation Center, Northwestern Polytechnical University, Chongqing 401135, China
^jShenzhen Research Institute of Northwestern Polytechnical University, Shenzhen 518057, Guangdong, China

Received:2024-12-11 Accepted:2025-03-01 Online:2025-05-18 Published:2025-05-20
Contact: *E-mail: qih11@cardiff.ac.uk (H. Qi), qinyong@qust.edu.cn (Y. Qin), renyj@nwpu.edu.cn (Y. Ren).
About author:¹ Contributed equally to this work.
Supported by:
National Key R&D Program of China(2023YFA1506603);National Natural Science Foundation of China(22472131);National Natural Science Foundation of China(22478316);National Natural Science Foundation of China(22208262);National Natural Science Foundation of China(52101272);National Natural Science Foundation of China(52271228);Natural Science Foundation of Chongqing China(CSTB2023NSCQ-MSX0165);Guangdong Basic and Applied Basic Research Foundation(2024A1515012109);Natural Science Foundation of Shandong Province(ZR2021YQ09);Taishan Scholars Project Special Funds(tsqn202312200);Foundation of State Key Laboratory of Coal Conversion(J24-25-903);Marie Skłodowska-Curie Actions Postdoctoral Fellowships(101107009-AtomCat4Fuel);UKRI(EP/Y029305/1)

Abstract

Abstract:

Catalytic oxidation plays a crucial role in chemical industry, in which the utilization of abundant and environmental-friendly oxygen (O₂) as oxidant aligns with sustainable development principles in green chemistry. However, the intrinsic inertness of ground-state O₂ molecule poses a long-standing challenge in developing an efficient non-noble metal-based catalyst. Herein, inspired by the electron transfer process in respiratory chain, we engineered long-range N_V to mediate Fe₁ center for O₂ activation in aerobic oxidation. Combined in/quasi-situ spectroscopic characterizations and control experiments suggest the Fe₁ site efficiently adsorbs O₂, and the N_V site facilitates electron delocalization to adjacent Fe₁, providing efficient transformation of O₂ to reactive oxygen species that boost oxidation reactions mildly. This Fe₁--N_V single-atom catalyst demonstrates outstanding catalytic performance in aerobic oxidations of alkanes, N-heterocycles, alcohols, and amines under relatively mild conditions. Our findings offer a new perspective for designing high-efficiency heterogeneous catalysts in aerobic oxidations, promising various potential applications.

Key words: Single-atom catalyst, Peripheral-nitrogen effect, Long-range N_V, Synergistic catalysis, Aerobic oxidation

Fenli Liu, Man Yang, Jianglin Duan, Zhiyu Yin, Mingyang Shi, Fuqing Chen, Huifeng Xiong, Xin Liu, Wengang Liu, Qixing Xia, Shaodong Sun, Dan Feng, Haifeng Qi, Yong Qin, Yujing Ren. Peripheral N_V-induced electron transfer to Fe₁ single atoms for highly efficient O₂ activation[J]. Chinese Journal of Catalysis, 2025, 72: 187-198.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(25)64651-1

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Figures/Tables 6

Fig. 1. Schematic diagram of flavin-dependent monooxygenase and Fe1--NV/CN single-atom catalyst for the transformation of O2 into ROS. (a) The NAD(P)H and reduced flavin with nitrogen-containing heterocycles serve as the excited electron supplier in O2 to ROS transformation on Fe1-N4-S1 active center. (b) The nitrogen vacancy on carbon nitride surface facilitates the electron delocalization to adjacent Fe1 single-atom site for O2 activation.

Fig. 2. Schematic illustration of catalyst preparation and characterizations for Fe1--NV/CN catalyst. (a) Schematic illustration for Fe1--NV/CN catalyst synthesis. (b) N2 adsorption-desorption isotherms on Fe1--NV/CN. (c) XRD pattern of Fe1--NV/CN and CN samples. SEM image (scale bar = 3 μm) (d), HAADF-STEM (scale bar = 200 nm) (e), EDS-mapping images (scale bar = 200 nm) (f), and AC-HAADF-STEM (scale bar = 2 nm) image (g) of Fe1--NV/CN catalyst.

Fig. 3. Structural characterization of Fe1--NV/CN catalyst. N 1s XPS spectra (a), ratio of different N species to C (b), and ESR spectra (c) for CN and Fe1--NV/CN samples. Fe K-edge XANES (d) and FT-EXAFS (e) spectra of Fe1--NV/CN and Fe1/CN samples. The intensities of Fe Foil, FeO and Fe2O3 references are respectively multiplied by 1/15, 1/2 and 1/5. WT-EXAFS spectra (f) and EXAFS fitting curve (g) of Fe1--NV/CN and Fe1/CN samples. (h) The structural illustration of Fe1--NV sites on CN surface.

Fig. 4. Catalytic aerobic oxidation of ethylbenzene on Fe1--NV/CN catalyst. (a) Catalytic performance of CN, Fe1--NV/CN and Fe1/CN samples in aerobic oxidation of ethylbenzene. The apparent activation energy of Fe1--NV/CN (b) and Fe1/CN (c). (d) The catalytic activity comparison between Fe1--NV/CN and reported metal-based catalysts in aerobic oxidation of ethylbenzene. (e) The catalytic stability test of Fe1--NV/CN.

Fig. 5. Substrate scope of catalytic aerobic oxidations on Fe1--NV/CN catalyst. (a) Oxidative dehydrogenation of heterocycles on Fe1--NV/CN catalyst. (b) Selective oxidation of amines towards imine synthesis on Fe1--NV/CN catalyst. (c) Selective oxidation of alcohol to aldehyde on Fe1--NV/CN catalyst. (d) Selective oxidative of C-H bond towards ketones synthesis on Fe1--NV/CN catalyst. Reaction conditions: a 0.5 mmol substrate, 20 mg catalyst, 2 mL H2O, 10 bar air, 100 °C, isolated yield; b 120 °C. c 0.5 mmol substrate, 20 mg catalyst, 2 mL toluene, 30 bar air, 100 °C, 24 h, GC yield; d 1 mL substrate, 50 mg catalyst, 40 bar air, 120 °C, GC yield; 60 bar air, 150 °C.

Fig. 6. In-situ spectral characterization of O2 activation on Fe1--NV/CN and Fe1/CN catalysts. The quasi-situ XANES (a) and FT-EXAFS (b) spectra of Fe1--NV/CN and Fe1/CN catalysts with the sequential introduction of O2 and ethylbenzene (the intensity of Fe Foil is multiplied by 1/8). (c) The quasi-situ 57Fe M?ssbauer spectrum of Fe1--NV/CN catalyst with the introduction of O2. (d) The ESR spectra of Fe1--NV/CN and Fe1/CN with the addition of O2.

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Peripheral N_V-induced electron transfer to Fe₁ single atoms for highly efficient O₂ activation

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