植入第二壳层对称硫配位调控铁单原子自旋态

doi:10.1016/S1872-2067(26)65184-4

催化学报 ›› 2026, Vol. 89: 453-463.DOI: 10.1016/S1872-2067(26)65184-4

植入第二壳层对称硫配位调控铁单原子自旋态

饶雪碧^a^,¹, 方慧玲^b^,¹, 孙嘉琳^a, 刘立群^a, 朱永康^a, 陈俊翔^b^,^*(), 张世明^a^,^*(), 刘彬^c^,^d^,^*()

^a上海大学理学院,可持续能源研究院,上海 200444
^b中国科学院福建物质结构研究所,结构化学国家重点实验室, 福建省氢能材料与技术重点实验室,福建福州 350002
^c香港城市大学材料科学与工程系,香港 999077
^d香港城市大学化学系,香港清洁能源研究院(HKICE)及超金刚石及先进薄膜研究中心(COSDAF),香港 999077

收稿日期:2026-02-09 接受日期:2026-04-07 出版日期:2026-10-18 发布日期:2026-09-01
通讯作者: *电子信箱: smzhang@shu.edu.cn (张世明),
cjxxjc729@fjirsm.ac.cn (陈俊翔),
bliu48@cityu.edu.hk (刘彬).
作者简介:
¹共同第一作者.
基金资助:
国家自然科学基金(22272105);国家自然科学基金(22572118);上海自然科学基金(23ZR1423900);香港城市大学启动基金(9020003);ITF-RTH-全球STEM教授职位(9446006);先进二氧化碳回收利用JC STEM实验室(9228005)

Regulating single-Fe-atom spin-state via implanting second-shell symmetrical sulfur coordination

Xuebi Rao^a^,¹, Huiling Fang^b^,¹, Jialin Sun^a, Liqun Liu^a, Yongkang Zhu^a, Junxiang Chen^b^,^*(), Shiming Zhang^a^,^*(), Bin Liu^c^,^d^,^*()

^aInstitute for Sustainable Energy, College of Sciences, Shanghai University, Shanghai 200444, China
^bState Key Laboratory of Structural Chemistry, and Fujian Provincial Key Laboratory of Materials and Techniques toward Hydrogen Energy, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002, Fujian, China
^cDepartment of Materials Science and Engineering, City University of Hong Kong, Hong Kong SAR 999077, China
^dDepartment of Chemistry, Hong Kong Institute of Clean Energy (HKICE) & Center of Super-Diamond and Advanced Films (COSDAF), City University of Hong Kong, Hong Kong SAR 999077, China

Received:2026-02-09 Accepted:2026-04-07 Online:2026-10-18 Published:2026-09-01
Contact: *E-mail:smzhang@shu.edu.cn(S. Zhang),cjxxjc729@fjirsm.ac.cn(J. Chen),bliu48@cityu.edu.hk(B. Liu).
About author:
¹ Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22272105);National Natural Science Foundation of China(22572118);Natural Science Foundation of Shanghai(23ZR1423900);City University of Hong Kong startup fund(9020003);ITF-RTH-Global STEM Professorship(9446006);JC STEM lab of Advanced CO2 Upcycling(9228005)

摘要/Abstract

摘要：

随着全球能源需求的持续增长, 开发高效、清洁的能量转换技术具有重要意义. 聚合物电解质膜燃料电池和金属-空气电池因其高能量密度、安全性和环境友好性而备受关注. 然而, 其阴极氧还原反应(ORR)动力学缓慢, 严重制约了实际应用. 尽管铂基催化剂具有优异的ORR性能, 但其高成本和资源稀缺性推动了非贵金属替代材料的发展. 近年来, 具有FeN₄活性中心的铁-氮-碳(Fe-N-C)催化剂因成本低廉, 氧还原反应(ORR)动力学性能优异, 是铂基催化剂极具潜力的替代材料. 然而, FeN₄位点对氧中间体的过强吸附仍限制了其性能提升. 因此, 如何精确调控FeN₄的配位环境, 尤其是通过外围杂原子掺杂调节其电子结构, 并深入阐明其ORR电催化机理, 仍是该领域的关键挑战. 合理设计FeN₄配位结构有望有效调控Fe与O之间的3d-2p轨道相互作用, 从而提升单原子铁催化剂的本征催化活性.

针对上述挑战, 本文提出了一种配位工程策略, 在FeN₄中心的第二配位壳层中对称地引入两个硫(S)原子, 构建FeN₄S₂活性中心. 该设计的核心创新在于通过第二壳层杂原子调控Fe中心的电子结构, 并通过自旋态调节优化氧中间体的吸附行为, 从而突破传统FeN₄催化剂的活性瓶颈. 球差校正透射电子显微镜和X-射线吸收精细结构结果表明, Fe, N, S共掺杂的碳骨架(Fe-N-S/CF)催化剂的活性中心为FeN₄S₂结构. ⁵⁷Fe Mössbauer谱图和零场冷却温度测试进一步揭示, 对称S掺杂有效调控了Fe 3d轨道的电子自旋极化, 使Fe中心从高自旋态转变为中自旋态. 这一自旋态转变源于d_z²-p, d_xz-p和d_yz-p轨道之间的协同相互作用, 是提升催化活性的根本原因. 电化学测试显示, 所制备的Fe-N-S/CF催化剂在碱性环境中表现出优异的ORR性能, 其起始电位高达1.048 V (vs. RHE), 半波电位为0.909 V (vs. RHE), 显著优于商业Pt/C催化剂; 在酸性条件下, 其活性亦明显超越以FeN₄为中心的Fe-N/CF体系. 此外, 基于FeN₄S₂空气电极构建的锌-空气电池展现出高达248.2 mW cm^-2的峰值功率密度及优异的充放电稳定性, 整体性能全面优于Pt/C对照体系. 密度泛函理论计算结果进一步证实, 对称的第二壳层S配位有效削弱了FeN₄中心的自旋极化, 进而优化了氧中间体(*O, *OH, *OOH)的吸附能. 在反应路径上, FeN₄的决速步骤为*O → *OH, 具有较高能垒; 而在FeN₄S₂体系中, 决速步骤转变为*O₂ → *OOH, 自由能垒显著降低. 原位拉曼光谱检测到FeN₄S₂表面*OOH中间体的富集, 与理论计算结果高度一致. 由此可见, 第二壳层S掺杂通过调控Fe自旋态, 有效削弱Fe-O键强度、优化反应路径, 从而显著提升单原子Fe位点的ORR催化活性.

综上, 本工作不仅提出了一种通过第二配位壳层杂原子调控金属中心自旋态的有效策略, 为高效非贵金属ORR催化剂的理性设计提供了新思路, 而且深化了对FeN₄基催化剂反应机理的认识. 未来, 可进一步拓展至其他杂原子掺杂或非对称配位结构对自旋态与电子结构的协同调控机制研究, 从而持续推动燃料电池及金属-空气电池等能量转换体系的性能提升与实际应用进程.

关键词: FeN₄活性位点, 硫掺杂, 第二配位壳层, 自旋态, 氧还原反应

Abstract:

Noble-metal-free iron-nitrogen-carbon (Fe-N-C) catalysts with well-defined FeN₄ active sites are promising alternatives to replace platinum (Pt) catalysts for oxygen reduction reaction (ORR). However, the precise design of the peripheral heteroatom-doped FeN₄ centers and the clarification of the underlying electrocatalytic ORR mechanism remain a significant challenge. Herein, we employ a coordination engineering strategy to implant two sulfur (S) atoms into the second coordination shell of the FeN₄ center (FeN₄S₂), which effectively modulates the Fe spin state via d_z²-p, d_xz-p, and d_yz-p interactions. The symmetrical S-doping in FeN₄S₂ can weaken the spin polarization of FeN₄ that induces a transition of single-Fe-atom from a high-spin to a medium-spin state, thereby optimizing the oxygen intermediates adsorption and transforming the ORR potential-determining step from *O → *OH over FeN₄ to *O₂ → *OOH over FeN₄S₂ with a lower free energy barrier, which greatly boosts the ORR performance in both alkaline and acidic media. The zinc-air battery with a FeN₄S₂ air electrode delivers a peak power density as high as 248.2 mW cm^-2 with exceptional charge-discharge stability, significantly outperforming the state-of-the-art Pt/C air electrode.

Key words: FeN₄ active sites, Sulfur-doping, Second coordination shell, Spin state, Oxygen reduction reaction

饶雪碧, 方慧玲, 孙嘉琳, 刘立群, 朱永康, 陈俊翔, 张世明, 刘彬. 植入第二壳层对称硫配位调控铁单原子自旋态[J]. 催化学报, 2026, 89: 453-463.

Xuebi Rao, Huiling Fang, Jialin Sun, Liqun Liu, Yongkang Zhu, Junxiang Chen, Shiming Zhang, Bin Liu. Regulating single-Fe-atom spin-state via implanting second-shell symmetrical sulfur coordination[J]. Chinese Journal of Catalysis, 2026, 89: 453-463.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65184-4

https://www.cjcatal.com/CN/Y2026/V89/I10/453

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Fig. 1. (a) Schematic illustration of the synthesis procedure. (b) TEM image of the Fe-N-S/CF catalyst and elemental mapping images showing distribution of C (blue), N (yellow), S (green), and Fe (red) elements. (c) Magnified AC-HAADF-STEM image of Fe-N-S/CF. (d) XRD patterns of N/CF, Fe-N/CF, and Fe-N-S/CF. (e) Raman spectra of Fe-N/CF and Fe-N-S/CF. (f) Pore size distribution of N/CF, Fe-N/CF, and Fe-N-S/CF.

Fig. 2. (a) N 1s XPS spectra of N/CF, Fe-N/CF, and Fe-N-S/CF. (b) Fe K-edge XANES spectra. (c) k3-weighted Fourier-transformed EXAFS spectra of Fe-N-S/CF and reference materials. (d) EXAFS fitting curves of Fe-N-S/CF in R-space and the corresponding fitting paths. (e) Wavelet transform of k3-weighted EXAFS spectrum for Fe-N-S/CF. (f) 57Fe M?ssbauer spectrum of Fe-N-S/CF. (g) χm-T plots and the μeff of Fe-N-S/CF and Fe-N/CF. (h) Schematic diagram showing spin-electron filled states of Fe2+ 3d orbital.

Fig. 3. Electrochemical performance. (a) LSV curves. (b) Comparison of E1/2 and jk at 0.85 V vs. RHE. (c) Comparison of E1/2 and jk at 0.85 V vs. RHE. (d) Tafel plots. (e) LSV curves of Fe-N-S/CF recorded at different rotation speeds (inset: K-L plots at the potential of 0.7, 0.8, and 0.85 V vs. RHE). (f) Electron transfer number (n) and H2O2 yields. (g) A radar chart comparing Eonset, E1/2, jk, Tafel slope, and n. (h) Amperometric i-t curves recorded at 0.7 V (vs. RHE) at a rotation speed of 1600 rpm. (i) LSV curves of Fe-N-S/CF before and after 15000 ADT cycles. Catalyst loading: 400 μg cm-2 for Fe-N-S/CF and 20 μg-Pt cm-2 for Pt/C, electrode rotation speed: 1600 rpm, electrolyte: 0.1 mol L-1 KOH solution.

Fig. 4. ZAB performance. (a) Schematic diagram of a typical ZAB device. (b) OCV curves (inset: the optical image of a Fe-N-S/CF ZAB). (c) Discharge polarization curves with peak power density indicated. (d) Discharge specific capacities at 10 mA cm-2. (e) Comparison of galvanostatic discharge curves at different current densities. (f) Galvanostatic discharge/charge cycling of ZABs evaluated at a current density of 5 mA cm-2.

Fig. 5. Reaction mechanism. (a) Free energy diagrams of ORR over FeN4, FeN4S2-2 at 1.23 V and FeN4, FeN4S2-1, FeN4S2-2, FeN4S2-3, FeN4S2-4 at 0 V. (b) The adsorption models of O2 and oxygen intermediates during the ORR process. PDOS of Fe 3d orbitals for FeN4 (c) and FeN4S2-2 (d). PCOHP analysis of the Fe-O bond formed after adsorption of *OH over FeN4 (e) and FeN4S2-2 (f). (g) In-situ Raman spectra recorded over Fe-N-S/CF at different potentials. Peak intensity at 1153 cm-1 (h) and 1532 cm-1 (i) versus applied potentials (vs. RHE).

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植入第二壳层对称硫配位调控铁单原子自旋态

Regulating single-Fe-atom spin-state via implanting second-shell symmetrical sulfur coordination

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