优化非晶-晶态异质结构协调钌锰氧化物的酸性水氧化活性和稳定性

doi:10.1016/S1872-2067(25)64850-9

催化学报 ›› 2026, Vol. 82: 61-73.DOI: 10.1016/S1872-2067(25)64850-9

优化非晶-晶态异质结构协调钌锰氧化物的酸性水氧化活性和稳定性

刘琳^a^,^b^,¹, 陈军^a^,^b^,¹, 李爱龙^c, 孔爽^d, 张莹^a, 乔亚飞^a^,^b, 张鹏飞^a, 李灿^a^,^b^,^*(), 韩洪宪^a^,^†()

^a中国科学院大连化学物理研究所, 大连洁净能源国家实验室, 催化基础国家重点实验室, 辽宁大连 116023
^b中国科学院大学, 北京 100049
^c中国科学技术大学, 精准智能化学全国重点实验室, 安徽合肥 230026
^d中国科学技术大学, 合肥微尺度物质科学国家研究中心, 安徽合肥 230026

收稿日期:2025-07-24 接受日期:2025-08-22 出版日期:2026-03-18 发布日期:2026-03-05
通讯作者: * 电子信箱: canli@dicp.ac.cn (李灿),hxhan@ybu.edu.cn (韩洪宪).
作者简介:¹共同第一作者.
^†延边大学理学院能源与资源催化实验室, 吉林延吉 133002
基金资助:
国家自然科学基金委人工光合成基础科学中心(22088102);国家重点研发计划专项(2025YFE0107800)

Harmonization of acidic OER activity and stability of ruthenium-manganese oxide by optimization of amorphous-crystalline heterostructure

Lin Liu^a^,^b^,¹, Jun Chen^a^,^b^,¹, Ailong Li^c, Shuang Kong^d, Ying Zhang^a, Yafei Qiao^a^,^b, Pengfei Zhang^a, Can Li^a^,^b^,^*(), Hongxian Han^a^,^†()

^aState Key Laboratory of Catalysis, Dalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China
^bUniversity of Chinese Academy of Sciences, Beijing 100049, China
^cState Key Laboratory of Precision and Intelligent Chemistry, University of Science and Technology of China, Hefei 230026, Anhui, China
^dHefei National Research Center for Physical Sciences at the Microscale, University of Science and Technology of China, Hefei 230026, Anhui, China

Received:2025-07-24 Accepted:2025-08-22 Online:2026-03-18 Published:2026-03-05
Contact: * E-mail: canli@dicp.ac.cn (C. Li),hxhan@ybu.edu.cn (H. Han).
About author:¹ Contributed to this work equally.
^†Present address: Laboratory of Catalysis for Energy and Resources, College of Sciences, Yanbian University, Yanji 133002, Jilin, China
Supported by:
National Natural Science Foundation of China(22088102);Key Special Project of the National Key R&D Program(2025YFE0107800)

摘要/Abstract

摘要：

利用可再生能源如太阳能、风能等与电解水制氢系统耦合, 可以规模化生产绿氢, 实现可再生能源的转化、储存和利用. 其中质子交换膜(PEM)电解水技术具有可以在大电流密度下生产高纯度氢、系统快速响应可以很好地与间歇性的可再生能源相匹配等优点, 受到广泛关注. 目前在工业化PEM电解水中, 能够稳定地进行水氧化的阳极电催化剂主要依赖稀缺、昂贵的贵金属铱, 这极大地限制了PEM电解水技术的大规模应用. 因此开发高活性和稳定的非铱基析氧反应(OER)电催化剂对大规模应用PEM电解水技术耦合可再生能源制氢至关重要. 钌基OER催化剂因其高活性和相对较低的成本, 在替代铱基OER催化剂方面展现出巨大的潜力. 然而, 优化钌基OER催化剂在酸性环境中的活性和稳定性仍然是一项具有挑战性的任务.

本文通过掺杂和相工程结合策略, 制备出一种钌锰氧化物催化剂. X射线衍射、拉曼光谱、高角度环形暗场扫描透射电子显微镜以及X射线吸收精细结构等表征结果表明, 钌锰氧化物是一种非晶相和晶相混合结构催化剂, 其中的晶相类似金红石相氧化钌结构; 锰在原子水平上均匀分布在整个催化剂中, 通过控制后处理温度可以对催化剂的结晶度进行调控, 使其结构实现从非晶态到非晶态-晶态以及结晶态转变. 本研究中的非晶态催化剂具有高OER活性但酸稳定性差, 而晶态催化剂具有增强的酸稳定性但是OER活性相对较差. 优化的具有非晶-晶态结构的催化剂(Ru₃Mn₁O_x-250), 能够实现OER活性和稳定性的协调. 该催化剂在10 mA/cm²下的过电位仅为211 mV, 可以在保持OER活性的同时在酸性电解质中保持稳定运行至少1000 h. 当该催化剂用作PEM电解槽阳极材料时, 可以在1.65 V (80 °C)下提供1 A/cm²的电流密度, 性能优于商用RuO₂催化剂(1.82 V). 大电流密度下的稳定性测试结果表明, 该催化剂可以在100 mA/cm²下保持稳定运行400 h, 甚至在1 A/cm²的工业电流密度下能够稳定运行100 h以上, 使其成为酸性条件下极具前景的OER电催化剂. 结合实验与理论计算结果表明, Mn主要以低价态形式原子级分散在整个非晶-晶相中, 形成不对称的Ru-O-Mn键, 导致Mn的八面体配位几何结构发生扭曲. 这种独特的微观结构导致: (1) 通过进一步降低活性位点的d带中心远离费米能级来增强OER活性, 削弱氧中间体的吸附, 加速速率决定步的*OOH中间体的形成; (2)通过增加*RuO(OH)₂形成的能量势垒来提高催化剂的稳定性, *RuO(OH)₂是催化剂在OER过程中形成RuO₄^-导致钌位点溶解的关键中间体.

综上可见, 非晶态-晶态异质结构设计策略是实现钌基催化剂活性-稳定性权衡的有效方法, 为开发在酸性电解质中稳定的高效OER催化剂提供了一种新方法.

关键词: 钌锰氧化物, 非晶-晶态结构, 析氧反应, 酸性电解质, 质子交换膜电解水

Abstract:

Ru-based oxygen evolution reaction (OER) catalysts exhibit considerable promise for the replacement of Ir-based catalysts due to their high activity and relatively low cost. However, optimization of activity and stability of Ru-based OER catalysts in acidic environment is still a challenging task. Here, we present an optimized amorphous-rutile crystalline heterostructure Ru₃Mn₁O_x-250 catalyst could achieve OER activity with an overpotential of only 211 mV at 10 mA/cm² while maintaining stable operation for at least 1000 h in acidic electrolyte. When the catalyst was used as an anode material in a proton exchange membrane (PEM) electrolyzer, it could deliver an industrial current of 1 A/cm² at 1.65 V (80 °C), outperforming the commercial RuO₂ catalyst (1.82 V). The catalyst can even maintain stable operation at 1 A/cm² for 100 h, showcasing its high OER activity and stability. The experimental and theoretical studies revealed that Mn is atomically dispersed throughout the amorphous-crystalline phases mainly in form of low valence state Mn, forming asymmetric Ru-O-Mn bonds which leads to distorted Oh coordination geometry of Mn with Ru. Such unique microstructure leads to: (1) enhancement of OER activity by reduction of the d band center further away from the Fermi level, weakening the adsorption of oxygen intermediates and accelerating the rate-determining *OOH intermediate formation; (2) enhancement of the catalyst stability by increasing the energy barrier of *RuO(OH)₂ formation, which is the key intermediate for the catalyst dissolution via RuO₄^- formation. This work demonstrates that an amorphous-crystalline heterostructure design strategy is an effective way to overcome the activity-stability trade-off, offering a new approach for the development of efficient OER catalysts stable in acidic electrolyte.

Key words: Ruthenium-manganese oxide, Amorphous-crystalline structure, Oxygen evolution reaction, Acidic electrolyte, Proton exchange membrane water, electrolysis

刘琳, 陈军, 李爱龙, 孔爽, 张莹, 乔亚飞, 张鹏飞, 李灿, 韩洪宪. 优化非晶-晶态异质结构协调钌锰氧化物的酸性水氧化活性和稳定性[J]. 催化学报, 2026, 82: 61-73.

Lin Liu, Jun Chen, Ailong Li, Shuang Kong, Ying Zhang, Yafei Qiao, Pengfei Zhang, Can Li, Hongxian Han. Harmonization of acidic OER activity and stability of ruthenium-manganese oxide by optimization of amorphous-crystalline heterostructure[J]. Chinese Journal of Catalysis, 2026, 82: 61-73.

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Fig. 1. XRD patterns (a) and Raman spectra (b) of Ru3Mn1Ox-150, Ru3Mn1Ox-250, Ru3Mn1Ox-350, and Ru3Mn1Ox-450. HR-TEM images of Ru3Mn1Ox-150 (c), Ru3Mn1Ox-250 (d), Ru3Mn1Ox-350 (e), and Ru3Mn1Ox-450 (f). The inset shows the corresponding selected electron diffraction patterns. (g) HAADF-STEM image of Ru3Mn1Ox-250. (h) EDS elemental mapping images of Ru3Mn1Ox-250. (i) HAADF-STEM image of Ru3Mn1Ox-450.

Fig. 2. Ru 3p (a), O 1s (b) XPS spectra of Ru3Mn1Ox-150, Ru3Mn1Ox-250 and Ru3Mn1Ox-450 catalysts. (c) Normalized Mn K-edge XANES spectra. (d) Normalized Ru K-edge XANES spectra. Inset: enlarged XANES spectra. (e) R-space of Mn K-edge EXAFS spectra. (f) R-space of Ru K-edge EXAFS spectra. Wavelet transform of RuO2 (g), Ru3Mn1Ox-250 (h), and Ru3Mn1Ox-450 (i).

Fig. 3. (a) LSV curves of Ru3Mn1Ox-150, Ru3Mn1Ox-250, Ru3Mn1Ox-350, Ru3Mn1Ox-450, and RuO2. (b) Overpotentials at current density of 10 mA/cm2, and current density at potential of 1.5 V (vs. RHE). (c) Tafel slopes. (d) Nyquist plots at potential of 1.25 V vs. SCE, the inset shows the equivalent circuit model used for impedance fitting. (e) Cdl values estimated through linear fitting of the scan rates. (f) Specific activity (normalized by ECSA). (g) Chronopotentiometry curves at 10 mA/cm2 in 1 mol/L H2SO4. (h) The concentrations of dissolved Ru and Mn in the electrolyte after 12 h of electrolysis at a current density of 10 mA/cm2. (i) Chronopotentiometry test of Ru3Mn1Ox-250 at 10 mA/cm2 in 0.1 mol/L HClO4.

Fig. 4. (a) pH-independence of OER activities of Ru3Mn1Ox-250. DEMS tests of 36O2, 34O2, and 32O2 signals for Ru3Mn1Ox-250 in H218O aqueous sulfuric acid electrolyte (b) and 18O labelled Ru3Mn1Ox-250 in H216O aqueous sulfuric acid electrolyte during LSV measurement at 0.7-1.4 V (vs. Ag/AgCl) (c). (d) Theoretical calculation models of RuO2, c-Ru0.75Mn0.25O2-x, and a/c-Ru0.75Mn0.25O2-x. (e) DOS of Ru d orbital for a/c-Ru0.75Mn0.25O2-x, c-Ru0.75Mn0.25O2-x, and RuO2. Reaction free energy of the acidic OER on RuO2 (f), c-Ru0.75Mn0.25O2-x (g), and a/c-Ru0.75Mn0.25O2-x (h).

Fig. 5. (a) Model of the dissolution process on a/c-Ru0.75Mn0.25O2-x. (b) Free energy profile for the dissolution process on RuO2, a-Ru0.75Mn0.25O2-x, c-Ru0.75Mn0.25O2-x, a/c-Ru0.75Mn0.25O2-x. (c) Schematic diagram of a PEM electrolyzer. (d) I-V curves of the PEM electrolyzer obtained at 80 °C. (e) V-t curve of the PEM electrolyzer for Ru3Mn1Ox-250, operating at 100 mA?cm-2, room temperature, and ambient pressure. (f) V-t curve of the PEM electrolyzer assembled with Ru3Mn1Ox-250 catalyst, operating at 1 A cm-2, 60 °C and ambient pressure.

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优化非晶-晶态异质结构协调钌锰氧化物的酸性水氧化活性和稳定性

Harmonization of acidic OER activity and stability of ruthenium-manganese oxide by optimization of amorphous-crystalline heterostructure

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