一种高效稳定的高熵合金电催化剂用于析氢反应

doi:10.1016/S1872-2067(24)60067-7

催化学报 ›› 2024, Vol. 62: 156-165.DOI: 10.1016/S1872-2067(24)60067-7

一种高效稳定的高熵合金电催化剂用于析氢反应

赵贵^a^,^b^,^c^,¹, 路宽^d^,¹, 李玉楠^e, 卢发贵^a^,^b^,^c, 高朋^a^,^b^,^c, 南兵^e, 李丽娜^e, 张熠霄^a^,^b^,^c, 徐鹏涛^a^,^b^,^c^,^*(), 刘晰^a^,^b^,^c^,^*(), 陈立桅^a^,^b^,^c^,^*()

^a上海交通大学化学化工学院, 物质科学原位中心, 上海 200240
^b上海交通大学变革性分子前沿科学中心, 上海 200240
^c上海交通大学上海电化学能源器件工程技术研究中心, 上海 200240
^d中国科学院山西煤炭化学研究所, 煤转化国家重点实验室, 山西太原 030001
^e上海高等研究院上海同步辐射光源, 上海 201204

收稿日期:2024-01-05 接受日期:2024-05-27 出版日期:2024-07-18 发布日期:2024-07-10
通讯作者: *电子信箱: xupengtao@sjtu.edu.cn (徐鹏涛), liuxi@sjtu.edu.cn (刘晰), lwchen2018@sjtu.edu.cn (陈立桅).
作者简介:¹共同第一作者.
基金资助:
国家重点研发计划(2021YFA1500300);国家重点研发计划(2022YFA1500146);国家重点研发计划(2021YFB3800300);国家自然科学基金(22072090);国家自然科学基金(22272106);国家自然科学基金(21991153);国家自然科学基金(21991150);国家自然科学基金(22372099)

An efficient and stable high-entropy alloy electrocatalyst for hydrogen evolution reaction

Gui Zhao^a^,^b^,^c^,¹, Kuan Lu^d^,¹, Yunan Li^e, Fagui Lu^a^,^b^,^c, Peng Gao^a^,^b^,^c, Bing Nan^e, Lina Li^e, Yixiao Zhang^a^,^b^,^c, Pengtao Xu^a^,^b^,^c^,^*(), Xi Liu^a^,^b^,^c^,^*(), Liwei Chen^a^,^b^,^c^,^*()

^aSchool of Chemistry and Chemical Engineering, in-situ Center for Physical Sciences, Shanghai Jiao Tong University, Shanghai 200240, China
^bFrontiers Science Center for Transformative Molecules, Shanghai Jiao Tong University, Shanghai 200240, China
^cShanghai Electrochemical Energy Device Research Center (SEED), Shanghai Jiao Tong University, Shanghai 200240, China
^dState Key Laboratory of Coal Conversion, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001, Shanxi, China
^eShanghai Synchrotron Radiation Facility, Shanghai Advanced Research Institute, Shanghai 201204, China

Received:2024-01-05 Accepted:2024-05-27 Online:2024-07-18 Published:2024-07-10
Contact: *E-mail: xupengtao@sjtu.edu.cn (P. Xu), liuxi@sjtu.edu.cn (X. Liu), lwchen2018@sjtu.edu.cn (L. Chen).
About author:First author contact:
¹ Contributed equally to this work.
Supported by:
National Key R&D Program of China(2021YFA1500300);National Key R&D Program of China(2022YFA1500146);National Key R&D Program of China(2021YFB3800300);National Natural Science Foundation of China(22072090);National Natural Science Foundation of China(22272106);National Natural Science Foundation of China(21991153);National Natural Science Foundation of China(21991150);National Natural Science Foundation of China(22372099)

摘要/Abstract

摘要：

水分解是一种利用可再生能源驱动的绿色制氢方法, 零碳排放特性使其成为解决氢能源生产的重要途径. 在电化学水分解中, 制备高活性和稳定性的催化剂至关重要. 高熵合金(HEAs)由于独特的结构和性能使其成为理想的催化剂材料, 其多元成分和可调组成提供了丰富的表面活性位点和灵活的催化特性, 有望提高水分解的效率并降低成本. 然而, 简易高效地制备HEAs仍面临挑战, 且目前对HEA催化剂的结构-活性关系的了解存在不足. 因此, 探索一种简便有效的方法用以制备高性能HEAs催化剂, 并深入理解其在水分解反应中的作用机制和结构演变, 能够为未来绿色制氢技术的发展提供重要的科学基础和技术支持.

本文采用了电化学测量、Cu K-边和Pt L₃-边的原位同步辐射X射线吸收光谱(XAS)测试以及密度泛函理论(DFT)计算相结合的方法, 系统地研究了高熵合金电催化剂PtPdRhRuCu/C的析氢反应(HER)活性、反应机制以及结构演变规律. PtPdRhRuCu HEAs纳米颗粒由简便的一步溶剂热法制备, 直径约为6.7 ± 0.6 nm, 其合金结构和元素分布通过多种表征手段(扫描透射电子显微镜、X射线衍射和能量色散X射线光谱等)得到确认. XAS对Cu K-边和Pt L₃-边的分析结果显示, HEAs纳米颗粒表面的少量铜氧化物在HER过程中被还原至金属态. 扩展X射线吸收精细结构的拟合结果表明, HEAs在工况HER中保持了金属态和无序的原子排列, 没有新的分离相形成. 电化学测试结果表明, 得益于多金属活性位点, PtPdRhRuCu/C催化剂在酸性和碱性条件下均表现出较好的HER活性和耐久性. 在10 mA cm^‒2的电流密度下, 该催化剂在1 mol L^‒1 KOH中具有23.3 mV的极低过电位, 优于商业Pt/C催化剂(50.3 mV), 其质量活性是Pt/C的7.9倍, 达到3.0 A mg^‒1_Pt. PtPdRhRuCu的高熵效应显著提升了催化剂在HER中的长期稳定性, 在稳定性测试中, PtPdRhRuCu/C催化剂在10000次循环伏安测试后几乎无性能衰减, 而Pt/C的过电位增加了约24 mV. 在‒55 mV过电位下的30 h的HER测试中, PtPdRhRuCu/C保持95.7%的初始电流密度, 而Pt/C衰减了53.6%. 在酸性条件下, PtPdRhRuCu/C的循环稳定性和耐久性也优于Pt/C. DFT计算结果表明, PtPdRhRuCu/C较好的HER性能和稳定性归因于高熵合金的协同效应, 多金属成分提供了多样的活性位点, 优化了HER反应路径, 特别是在Volmer步骤中降低了水裂解的反应能垒. PtPdRhRuCu/C上的HER过程遵循Volmer-Tafel机理, 水分子优先吸附在Ru位点, 促进HO‒H键的解离, 解离出的质子迁移到Pt上, 而OH通过Ru和Rh的桥接作用而稳定, 最终在Cu上释放H₂.

综上, 本文展示了高熵合金在HER中较好的性能, 并通过详细的表征深入理解了其构-效关系. 研究成果为高熵合金催化剂的合理设计和应用提供理论支持, 为未来高效、耐久和低成本的绿色制氢技术提供重要的科学依据和技术支持.

关键词: 析氢反应, 高熵合金, 原位X射线吸收光谱, 一步溶剂热法, 低过电位

Abstract:

High-entropy alloy (HEA) catalysts exhibit enhanced hydrogen evolution reaction (HER) activity in water electrolysis, yet the understanding of their structure and active sites in reaction environments remains unclear. Here, we systematically investigated the HER activity and stability of PtPdRhRuCu/C through a combination of electrochemical measurements, in situ synchrotron radiation X-ray absorption spectroscopy (XAS) at the Cu K-edge and Pt L₃-edge, and density functional theory (DFT) calculations. Uniformly sized PtPdRhRuCu HEA nanoparticles were prepared via a facile one-step solvothermal method. In situ XAS results revealed that the HEA nanoparticles maintained metallic states and a disordered arrangement of the overall structure at hydrogen evolution potential, implying the absence of the separated phases. Relying on multi-metal active sites, PtPdRhRuCu/C demonstrated a remarkably low overpotential of 23.3 mV at 10 mA cm^-2 in alkaline HER, which is significantly lower than the overpotential observed in commercial Pt/C (50.3 mV), and achieving a mass activity 7.9 times that of Pt/C. DFT calculations show that the synergy of each metal site optimizes the dissociation energy barrier of water molecules. This study not only demonstrates the advancement of high-entropy alloys in electrocatalysis but also provides a comprehensive understanding of the structure-activity relationship of these unique catalysts through detailed characterizations. Our findings further contribute to the rational design and application of high-entropy alloy catalysts, specifically in HER.

Key words: Hydrogen evolution reaction, High-entropy alloy, In situ X-ray absorption spectroscopy, One-step solvothermal method, Lower overpotential

赵贵, 路宽, 李玉楠, 卢发贵, 高朋, 南兵, 李丽娜, 张熠霄, 徐鹏涛, 刘晰, 陈立桅. 一种高效稳定的高熵合金电催化剂用于析氢反应[J]. 催化学报, 2024, 62: 156-165.

Gui Zhao, Kuan Lu, Yunan Li, Fagui Lu, Peng Gao, Bing Nan, Lina Li, Yixiao Zhang, Pengtao Xu, Xi Liu, Liwei Chen. An efficient and stable high-entropy alloy electrocatalyst for hydrogen evolution reaction[J]. Chinese Journal of Catalysis, 2024, 62: 156-165.

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Fig. 1. STEM-ADF image (a) and STEM-BF image (b) of PtPdRhRuCu NPs. The size distribution of PtPdRhRuCu NPs and high-resolution (HR) BF images are presented in the insets of (a) and (b), respectively. (c) SEAD image of PtPdRhRuCu NPs. (d) XRD pattern of PtPdRhRuCu/C. (e) Elemental distribution of PtPdRhRuCu NPs.

Fig. 2. HER polarization curves (a), area activity (normalized to the electrode geometric surface area, at -0.07 V vs. RHE) and mass activity (normalized to Pt mass, at -0.07 V vs. RHE) (b), and Tafel slope (c) of PtPdRhRuCu/C, PtPdRhRu/C, PtPdRh/C, PtPd/C, and Pt/C in 1 mol L?1 KOH. The abscissa of (b) represents the number of metals contained in the five catalysts in (a). (d) HER polarization curves of PtPdRhRuCu/C and Pt/C before and after CV cycles in 1 mol L?1 KOH. (e) Chronoamperometry tests of PtPdRhRuCu/C and Pt/C at an overpotential of 55 mV in 1 mol L?1 KOH. (f) Chronoamperometry tests of PtPdRhRuCu/C and Pt/C at different overpotential with initial 80 mA cm-2 current densities in 0.5 mol L?1 H2SO4.

Fig. 3. In situ XANES (a,d) and EXAFS spectra (c,f) of Cu K-edge (a-c) and Pt L3-edge (d-f) at a series of applied potential under HER process. Details of the XANES spectra outlined by the black dashed in (a) and (d) are shown in (b) and (e), respectively.

Fig. 4. (a) Top and side views of the structural configuration of PtPdRhRuCu. (b) The structural configuration of stable adsorption species on PtPdRhRuCu during HER. From left to right: H2O, OH, H and H2, Red balls = O and White balls = H. (c) The PDOSs of the PtPdRhRuCu. (d) Energy pathways for alkaline HER on PtPdRhRuCu/C and Pt/C. (e) Calculated HER free-energy changes on PtPdRhRuCu/C and Pt/C. (f) Activation energy for water dissociation on PtPdRhRuCu/C and Pt/C.

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一种高效稳定的高熵合金电催化剂用于析氢反应

An efficient and stable high-entropy alloy electrocatalyst for hydrogen evolution reaction

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