金属硫化物前驱体的牺牲转化生成活性羟基氧化物催化剂以增强析氧反应

doi:10.1016/S1872-2067(25)64876-5

催化学报 ›› 2026, Vol. 82: 84-91.DOI: 10.1016/S1872-2067(25)64876-5

金属硫化物前驱体的牺牲转化生成活性羟基氧化物催化剂以增强析氧反应

孙欣然^a^,¹, 霍孟田^a^,¹, 孙健航^b, 梁宇^a, 秦愷池^a, 张浩杨^a, 邢子豪^a^,^*(), 常进法^a^,^*()

^a东北师范大学化学学院, 多酸与网格材料化学教育部重点实验室, 吉林长春 130024
^b中国刑事警察学院, 刑事科学技术学院(法庭科学学院), 辽宁沈阳 110854

收稿日期:2025-07-22 接受日期:2025-08-29 出版日期:2026-03-18 发布日期:2026-03-05
通讯作者: * 电子信箱: xingzh612@nenu.edu.cn (邢子豪),changjinfa@nenu.edu.cn (常进法).
作者简介:¹共同第一作者.
基金资助:
吉林省科技发展计划(20250102077JC);国家自然科学基金(22472023);国家自然科学基金(22572025);国家自然科学基金(22202037);中央高校基本科研业务费(2412024QD014);中央高校基本科研业务费(2412023QD019)

Sacrificial conversion of metal sulfide precursors into active oxyhydroxide catalysts for enhanced oxygen evolution reaction

Xinran Sun^a^,¹, Mengtian Huo^a^,¹, Jianhang Sun^b, Yu Liang^a, Kaichi Qin^a, Haoyang Zhang^a, Zihao Xing^a^,^*(), Jinfa Chang^a^,^*()

^aKey Laboratory of Polyoxometalate and Reticular Material Chemistry of Ministry of Education, Faculty of Chemistry, Northeast Normal University, Changchun 130024, Jilin, China
^bCollege of Criminal Science and Technology (College of Forensic Science), Criminal Investigation Police University of China, Shenyang 110854, Liaoning, China

Received:2025-07-22 Accepted:2025-08-29 Online:2026-03-18 Published:2026-03-05
Contact: * E-mail: xingzh612@nenu.edu.cn (Z. Xing),changjinfa@nenu.edu.cn (J. Chang).
About author:¹ Contributed equally to this work.
Supported by:
Science and Technology Development Plan Project of Jilin Province, China(20250102077JC);National Natural Science Foundation of China(22472023);National Natural Science Foundation of China(22572025);National Natural Science Foundation of China(22202037);Fundamental Research Funds for the Central Universities(2412024QD014);Fundamental Research Funds for the Central Universities(2412023QD019)

摘要/Abstract

摘要：

析氧反应(OER)因动力学缓慢, 成为制约电解水效率的瓶颈. 商用OER催化剂(如IrO₂, RuO₂)虽活性优异, 但地壳丰度低、成本高, 难以满足工业需求. 过渡金属硫化物(TMSs)作为OER的潜在催化剂, 具备可控的自旋态、丰富的金属-硫配位环境及可调的电子结构, 在非贵金属催化材料领域显示出明显潜力. 然而, TMSs在阳极条件下存在结构不稳定性, 易引发动态表面重构, 严重制约了TMSs催化剂的性能优化与应用. Ni, Co和Fe基硫化物在OER过程中常出现复杂的结构演化, 其活性相的形成机制以及在表面重构过程中真正的催化活性位点的鉴定, 仍需通过精准的材料设计和原位表征技术予以阐明.

本研究针对该关键挑战, 通过简单的一步气相沉积法制备了一种碱性OER预催化剂FeCoS₂/FeS₂. 为实现OER催化活性提升, 通过硫掺杂结合受控的电化学激活实现可控的表面重构. 具体包括: (1)制备立方自组装的FeCoS₂/FeS₂异质催化结构, Fe与Co之间存在电子转移, 降低界面电阻, 以实现异质界面引发的电子耦合与快速电子传输; (2)通过硫掺杂调控电子结构以及电化学激活步骤诱导受控的表面重构, 促使局部区域生成高度活性的金属(羟基)氧化物相; (3)结合原位光谱等表征方法对反应机理进行动态跟踪, 揭示FeCoS₂/FeS₂的催化提升机制, 分析异质界面的电子传输增强与表面重构过程中催化活性提升的内在关联. 结果表明, 制备的FeCoS₂/FeS₂催化剂表现出优异的OER性能, 在10 mA cm⁻²电流密度下, 经过1000次循环后, 过电位仅为287 mV. 在反应过程中, 该催化剂逐渐从硫主导转化为氧主导的高活性(氧)氢氧化物(Fe/Co-OOH), 从而显著提高了OER的催化活性. 通过反应前后的原位表征和结构研究, 发现金属硫化物的牺牲性质可以发挥作用, 验证了所提出设计策略的有效性, 并为设计高效且耐久的非贵金属OER催化剂提供了可行的路线.

综上, 本文为理解TMSs的表面重构提供了可行且系统的框架, 揭示了通过异质结构与电化学表面激活实现活性位点定向生成的潜在途径. 一方面, 明确了金属硫化物的牺牲性质可调控活性(氧)氢氧化物相的生成路径; 另一方面, 该策略有望扩展至Ni、Mn等其他过渡金属硫化物体系, 促进低成本高效OER催化剂的产业化应用, 并为实现更高耐久性与更低过电位的目标催化剂提供设计准则.

关键词: 表面重构, 过渡金属硫化物, 析氧反应, 异质结构, 电化学活化

Abstract:

Transition metal sulfides (TMSs) are promising electrocatalysts for the oxygen evolution reaction (OER) due to their tunable spin states, diverse metal-sulfur coordination environments, and controllable electronic structures. However, their structural instability under anodic conditions remains a critical challenge. In particular, the mechanisms governing active-phase formation and the identification of true catalytically active sites during surface reconstruction require further investigation. Herein, we report a cubic, self-assembled FeCoS₂/FeS₂ heterostructure catalysts. Through sulfur doping and electrochemical activation-induced surface reconstruction, the catalyst achieves 10 mA cm⁻² current density at an overpotential of only 287 mV in 1.0 mol L⁻¹ KOH after 1000 cycles. Experimental and in-situ spectroscopy analyses reveal that the heterogeneous interface enhances electron transfer, while dynamic reconstruction generates a highly active metal (oxy)hydroxide phase as the primary catalytically active species. This work provides mechanistic insights into the surface reconstruction of TMSs, and offers a viable strategy for designing efficient and durable non-noble metal electrocatalysts.

Key words: Surface reconstruction, Transition metal sulfides, Oxygen evolution reaction, Heterostructure, Electrochemical activation

孙欣然, 霍孟田, 孙健航, 梁宇, 秦愷池, 张浩杨, 邢子豪, 常进法. 金属硫化物前驱体的牺牲转化生成活性羟基氧化物催化剂以增强析氧反应[J]. 催化学报, 2026, 82: 84-91.

Xinran Sun, Mengtian Huo, Jianhang Sun, Yu Liang, Kaichi Qin, Haoyang Zhang, Zihao Xing, Jinfa Chang. Sacrificial conversion of metal sulfide precursors into active oxyhydroxide catalysts for enhanced oxygen evolution reaction[J]. Chinese Journal of Catalysis, 2026, 82: 84-91.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64876-5

https://www.cjcatal.com/CN/Y2026/V82/I3/84

图/表 4

Fig. 1. Synthesis and structural profiling of the FeCoS2/FeS2 catalyst. (a) Schematic illustration of the synthetic procedure for FeCoS2/FeS2. SEM (b) and TEM (c) micrographs of FeCo PBA. SEM (d) and TEM (e) micrographs of FeCoS2/FeS2. (f) HR-TEM image of FeCoS2/FeS2 with clearly resolved lattice fringes corresponding to the (131) plane of FeS2 and (101) plane of FeCoS2. (d) EDS elemental mapping images of the FeCoS2/FeS2.

Fig. 2. (a) The XRD pattern of FeCoS2/FeS2. (b) The XPS spectra of Fe 2p for FeCoS2/FeS2 and FeCo. (c) The XPS spectra of Co 2p for FeCoS2/FeS2 and FeCo. (d) The XPS spectra of S 2p for FeCoS2/FeS2 and FeCo. (e) EXAFS of Fe K-edge for the FeCoS2/FeS2, Fe2O3 and Fe foil. (f) EXAFS of Co K-edge for the FeCoS2/FeS2, CoO and Co foil.

Fig. 3. OER performance for FeCoS2/FeS2, FeCo and Commercial RuO2. (a) LSV curves. (b) Tafel plots. (c) Histograms of overpotential and Tafel slopes for FeCoS2/FeS2, FeCo and Commercial RuO2. EIS (d) and Cdl (e) of FeCoS2/FeS2, FeCo and Commercial RuO2. (f) Long-term stability tests for FeCoS2/FeS2 and Commercial RuO2 at 100 mA cm?2.

Fig. 4. LSV curves of (a) precatalyst (FeCoS2/FeS2) after CV activation in 1 mol L?1 KOH. 1000 CVs cycles were done in a 1.0?1.7 V range at 100 mV s?1. (b) EXAFS of Fe K-edge for the precatalyst (FeCoS2/FeS2) and reconstructed catalyst. (c) EXAFS of Co K-edge for the precatalyst (FeCoS2/FeS2) and reconstructed catalyst. (d) In-situ Raman spectra of pre-FeCoS2/FeS2 at 150?1000 cm?1 under OER conditions. Bode diagrams of precatalyst (FeCoS2/FeS2) (e) and precatalyst (FeCo) (f) at 1.455?1.600 V for in-situ EIS.

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金属硫化物前驱体的牺牲转化生成活性羟基氧化物催化剂以增强析氧反应

Sacrificial conversion of metal sulfide precursors into active oxyhydroxide catalysts for enhanced oxygen evolution reaction

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