将贵金属单原子限域于非晶态氢氧化镍中以增强碱性析氢反应

doi:10.1016/S1872-2067(26)65166-2

催化学报 ›› 2026, Vol. 90: 264-275.DOI: 10.1016/S1872-2067(26)65166-2

将贵金属单原子限域于非晶态氢氧化镍中以增强碱性析氢反应

杨光^a^,^b, 巩喜良^c, 孟泽硕^a^,^b, 侯爽^a^,^b, 杨明豪^a^,^b, 龚忠苗^a^,^b, 黄荣^b, 崔义^a^,^b^,^*()

^a 中国科学技术大学纳米技术与纳米仿生学院, 安徽合肥 230026, 中国
^b 中国科学院苏州纳米技术与纳米仿生研究所, 创新实验室, 纳米真空互联实验站, 江苏苏州 215123, 中国
^c 马里兰大学化学与生物化学系, 马里兰州学院公园市, 美国

收稿日期:2026-02-09 接受日期:2026-03-18 出版日期:2026-11-18 发布日期:2026-09-09
通讯作者: *电子信箱: ycui2015@sinano.ac.cn (崔义).
基金资助:
国家重点研发计划(2022YFA1503802);江苏省自然科学基金(BK20241821);国家自然科学基金(22172190);国家自然科学基金(22202232);中国科学院青年科学家基础研究项目(YSBR-022);中国科学院青年交叉团队项目(JCTD-2021-14)

Amorphous nickel hydroxide confined noble metal single atoms for enhanced alkaline hydrogen evolution reaction

Guang Yang^a^,^b, Xiliang Gong^c, Zeshuo Meng^a^,^b, Shuang Hou^a^,^b, Minghao Yang^a^,^b, Zhongmiao Gong^a^,^b, Rong Huang^b, Yi Cui^a^,^b^,^*()

^a School of Nano Technology and Nano Bionics, University of Science and Technology of China, Hefei 230026, Anhui, China
^b i-lab, Nano-X Vacuum Interconnected Workstation, Suzhou Institute of Nano-Tech and Nano-Bionics, Chinese Academy of Sciences, Suzhou 215123, Jiangsu, China
^c Department of Chemistry and Biochemistry, University of Maryland, College Park 20742, MD, United States

Received:2026-02-09 Accepted:2026-03-18 Online:2026-11-18 Published:2026-09-09
Contact: *E-mail:ycui2015@sinano.ac.cn(Y. Cui).
Supported by:
National Key R&D Program of China(2022YFA1503802);Natural Science Foundation of Jiangsu Province(BK20241821);National Natural Science Foundation of China(22172190);National Natural Science Foundation of China(22202232);CAS Project for Young Scientists in Basic Research(YSBR-022);Young Cross Team Project of CAS(JCTD-2021-14)

摘要/Abstract

摘要：

碱性水电解制氢是实现绿氢经济的关键技术, 开发高性能析氢反应(HER)电催化剂是该过程的核心. 单原子催化剂虽具有极高的原子利用率和可调的电子结构, 但在碱性介质中水解离动力学缓慢导致的本征活性不足; 以及孤立金属位点在长期运行下易团聚流失导致稳定性差的短板. 金属磷化物在碱性析氢条件下常发生表面重构, 形成具有较强水解离能力的氢氧化物层, 但其导电性较差, 往往导致催化剂失活. 而贵金属单原子虽具备优异的氢吸附自由能, 却缺乏有效的限域与稳定机制. 因此, 利用金属磷化物重构实现对单原子的有效限域和稳定, 并同时优化其局域反应微环境以增强碱性HER性能是本文的主要研究思路.

本研究提出了一种基于电化学重构策略构建非晶态氢氧化镍限域贵金属单原子的新型催化剂体系. 本文首先设计了钌单原子掺杂的磷化镍纳米片前驱体Ru-NiP_x, 并在电解水HER过程中诱导其表面重构, 成功获得具有非晶氢氧化镍限域层结构的Ru-NiP_x(OH)_y单原子催化剂. 球差校正扫描透射电镜和X-射线吸收谱表明, 重构后的Ru仍以单原子形式存在, 配位环境在单一Ru-Ni键的基础上引入了新的Ru-O键配位环境, 且平均氧化态升高. X-射线光电子能谱和飞行时间二次离子质谱深度剖析表明, 重构仅发生于表面层, 形成了非晶氢氧化镍限域层和限域其中的Ru单原子. 电化学性能测试显示, Ru-NiP_x(OH)_y单原子催化剂在10 mA/cm²电流密度下过电位仅为9 mV, Tafel斜率为31 mV/dec, 在100 mV过电位下质量活性高达10 A/mg, 并可稳定运行超过1000 h, 性能显著优于晶态氢氧化镍负载的Ru单原子催化剂(Ru-Ni(OH)₂). 将该策略拓展至Pt和Ir单原子体系同样观测到明显性能提升, 验证了其普适性. 进一步研究了重构过程的表面变化及HER的反应机制, 通过原位拉曼光谱和真空互联的X-射线光电子能谱观察到Ru-NiP_x表面重构过程的分步演化: 表面P位点优先溶出形成空位, 随后Ru与Ni先后重构, 最终形成非晶氢氧化镍层. 此外, 结合飞行时间二次离子质谱和原位电化学阻抗谱证实了非晶态的Ni(OH)₂层不仅具有优异的水解离能力, 还能作为质子传导层, 在Ru位点周围形成局域类酸环境, 从而显著增强HER动力学. 一系列表征说明重构后的非晶氢氧化镍层和Ru单原子之间存在强的协同作用, 共同实现了高活性和稳定性的碱性电解水析氢过程.

综上, 本工作通过重构驱动的限域效应和质子传导微环境构建, 成功将传统认知中导致催化剂失活的磷化物表面重构转化为构筑高性能单原子析氢催化剂的有效途径, 为设计和合成高活性、高稳定性的单原子电催化剂提供了新思路.

关键词: 碱性析氢反应, 单原子限域, 质子调控, 重构

Abstract:

The dynamic regulation of the local atomic environment under operational conditions represents a frontier in the development of single-atom catalysts (SACs) for the alkaline hydrogen evolution reaction (HER). Here, we report a strategy that harnesses in-situ electrochemical reconstruction to construct a functional confinement structure for single atoms. Using Ru-doped NiP_x as a precursor, we guide its surface under HER conditions to form an reconstructed amorphous Ni(OH)₂ layer which acts as a robust host to confine and stabilize Ru single atoms. The reconstructed Ru-NiP_x(OH)_y catalyst delivers an extremely low overpotential of 9 mV at 10 mA/cm² and maintains stable operation for over 1000 h. Comprehensive characterization—combining vacuum-interconnected X-ray photoelectron spectroscopy and in-situ Raman spectroscopy—reveals that this confining amorphous layer not only modulates the electronic structure of Ru but also accelerates water dissociation and proton transport, thereby generating a local acid-like environment around the active sites. This synergy between atomic confinement and microenvironment engineering profoundly optimizes the overall HER kinetics. Furthermore, similar improvements are observed when Pt or Ir single atoms are introduced, demonstrating the universality of this reconstruction-driven activation strategy. This work establishes a paradigm for activating SACs by programming reconstruction to build integrated architectures where confinement and tailored microenvironments cooperate to boost catalytic performance.

Key words: Alkaline hydrogen evolution reaction, Single-atom confinement, Proton regulation, Reconstruction

杨光, 巩喜良, 孟泽硕, 侯爽, 杨明豪, 龚忠苗, 黄荣, 崔义. 将贵金属单原子限域于非晶态氢氧化镍中以增强碱性析氢反应[J]. 催化学报, 2026, 90: 264-275.

Guang Yang, Xiliang Gong, Zeshuo Meng, Shuang Hou, Minghao Yang, Zhongmiao Gong, Rong Huang, Yi Cui. Amorphous nickel hydroxide confined noble metal single atoms for enhanced alkaline hydrogen evolution reaction[J]. Chinese Journal of Catalysis, 2026, 90: 264-275.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65166-2

https://www.cjcatal.com/CN/Y2026/V90/I11/264

图/表 5

Fig. 1. XRD patterns (a) and Raman spectra (b) of Ru-NiPx and NiPx. SEM image (c) and AFM image (d) of Ru-NiPx. (e) High-resolution STEM image of Ru-NiPx, where the bright spots circled in red represent Ru single atoms. (f) Three-dimensional Gaussian function-fitted atomic image of the region marked by the red box in (e). (g) STEM elemental mapping of P, O, Ni, and Ru.

Fig. 2. LSV curves of Ru-NiPx (a) and NiPx (b) after 1st and 10th HER cycles. Inset: Corresponding Tafel plots. (c) Chronopotentiometry curve of Ru-NiPx at 10 mA/cm2 for 100 h. Inset: Initial activation within 10 h. (d) Chronopotentiometry curve of NiPx at 10 mA/cm2 for 400 h.

Fig. 3. (a) Ru K-edge XANES spectra of Ru-NiPx, Ru-NiPx(OH)y, and references. Inset: Magnified pre-edge region. (b) Ru K-edge Fourier transform EXAFS spectra in R-space. (c) WT plots of Ru-NiPx and Ru-NiPx(OH)y. (d) TOF-SIMs 3D and 2D distribution maps of Ru-O fragments. (e) O 1s XPS spectra. (f) Ru 3p XPS spectra. (g) Ni 2p XPS spectra.

Fig. 4. (a) Schematic illustration of the in-situ Raman electrolytic cell. (b) Schematic illustration of a glovebox-electrochemical workstation and UHV-XPS chamber, connected via a vacuum transfer system. (c) In-situ Raman spectra under different applied potentials. (d) Quasi in-situ XPS spectra (recorded after emersion and transfer from the electrochemical cell under Ar protection) of the Ni 2p and Ru 3p regions for the electrode held at varying potentials. TOF-SIMs 3D (e) and 2D (f) distribution maps of H3O+ fragments.

Fig. 5. Polarization curves (a), Tafel slopes (b), Nyquist plots (c), and double-layer capacitance (d) comparisons of Ru-NiPx(OH)y and reference catalysts. (e,f) LSV curves and corresponding Tafel slopes normalized by ECSA. (g) Long-term durability test of Ru-NiPx(OH)y at 10 mA/cm2 in 1 mol/L KOH.

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将贵金属单原子限域于非晶态氢氧化镍中以增强碱性析氢反应

Amorphous nickel hydroxide confined noble metal single atoms for enhanced alkaline hydrogen evolution reaction

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