靶向构筑高性能单原子铂基氢析出反应电催化剂

doi:10.1016/S1872-2067(24)60199-3

催化学报 ›› 2025, Vol. 69: 259-270.DOI: 10.1016/S1872-2067(24)60199-3

靶向构筑高性能单原子铂基氢析出反应电催化剂

刘京^a^,^b^,¹^,^*(), 马贤迪^c^,¹, 卢政汉^b^,¹, 申东元^b, 赵阿雅^d, 韩晸宇^d, 龙剑平^a, 周震^c^,^e^,^f, 焦梦改^c^,^*(), 李国承^g^,^*(), 赵恩爱^b^,^*()

^a成都理工大学材料与化学化工学院, 四川成都 610059, 中国
^b韩国科学技术院材料科学与工程系, 大田, 韩国
^c郑州大学化工学院, 新能源科学与工程交叉研究中心, 河南郑州 450001, 中国
^d浦项科技大学化学工程系, 浦项, 韩国
^e南开大学材料科学与工程学院, 新能源材料化学研究所, 新能源转化与存储交叉科学中心, 先进能源材料化学教育部重点实验室, 天津 300350, 中国
^f龙门实验室, 河南洛阳 471023, 中国
^g浦项科技大学浦项加速器实验室, 浦项, 韩国

收稿日期:2024-10-31 接受日期:2024-11-13 出版日期:2025-02-18 发布日期:2025-02-10
通讯作者: *电子信箱: jingliu@cdut.edu.cn (刘京), mgjiao@zzu.edu.cn (焦梦改), lks3006@postech.ac.kr (李国承), eacho@kaist.ac.kr (赵恩爱).
作者简介:第一联系人：
¹共同第一作者.
基金资助:
韩国政府国家研究基金会(NRF-2019M3D1A1079306);韩国政府国家研究基金会(NRF-2021R1A2C1011415);四川省自然科学基金(2023NSFSC1079);河南省高等学校重点研究项目(24A530009);龙门实验室前沿探索项目(LMQYTSKT021)

Targeted construction of high-performance single-atom platinum-based electrocatalysts for hydrogen evolution reaction

Jing Liu^a^,^b^,¹^,^*(), Xiandi Ma^c^,¹, Jeonghan Roh^b^,¹, Dongwon Shin^b, Ara Cho^d, Jeong Woo Han^d, Jianping Long^a, Zhen Zhou^c^,^e^,^f, Menggai Jiao^c^,^*(), Kug-Seung Lee^g^,^*(), EunAe Cho^b^,^*()

^aCollege of Materials and Chemistry & Chemical Engineering, Chengdu University of Technology, Chengdu 610059, Sichuan, China
^bDepartment of Materials Science and Engineering, Korea Advanced Institute of Science and Technology, 291 Daehak-Ro, Yuseong-Gu, Daejeon 34141, Korea
^cInterdisciplinary Research Center for Sustainable Energy Science and Engineering (IRC4SE), School of Chemical Engineering, Zhengzhou University, Zhengzhou 450001, Henan, China
^dDepartment of Chemical Engineering, Pohang University of Science and Technology, Pohang, Gyeongbuk 37673, Korea
^eSchool of Materials Science and Engineering, Institute of New Energy Material Chemistry, Renewable Energy Conversion and Storage Center, Key Laboratory of Advanced Energy Materials Chemistry (Ministry of Education), Nankai University, Tianjin 300350, China
^fLongmen Laboratory, Luoyang 471023, Henan, China
^gBeamline Division, Pohang Accelerator Laboratory, Pohang University of Science and Technology, Pohang, Gyeongbuk 37673, Korea

Received:2024-10-31 Accepted:2024-11-13 Online:2025-02-18 Published:2025-02-10
Contact: *E-mail: jingliu@cdut.edu.cn (J. Liu), mgjiao@zzu.edu.cn (M. Jiao), lks3006@postech.ac.kr (K.-S. Lee), eacho@kaist.ac.kr (E. Cho).
About author:First author contact:
¹Contributed equally to this work.
Supported by:
National Research Foundation of Korea (NRF) grant funded by Korea Government (MSIT)(NRF-2019M3D1A1079306);National Research Foundation of Korea (NRF) grant funded by Korea Government (MSIT)(NRF-2021R1A2C1011415);Sichuan Natural Science Foundation(2023NSFSC1079);Key Research Projects of Higher Education Institutions of Henan Province(24A530009);Frontier Exploration Projects of Longmen Laboratory(LMQYTSKT021)

摘要/Abstract

摘要：

因具有高能量密度和零排放等优点, 氢能被认为是传统化石能源的最佳替代品. 质子交换膜水电解(PEMWE)是实现可持续环保制氢的一种有效策略. 其中, 析氢反应(HER)是电解水制氢的关键半反应. 贵金属铂(Pt)因具有适当的氢结合能, 被认为是酸性条件下电催化HER的首选材料. 而开发高性能的单原子Pt基HER电催化剂(Pt SAC)可以大幅度提高Pt的利用率, 进而降低催化剂的成本. 已有研究证实, 通过调控配位环境可以使Pt SAC在三电极系统中表现出与商业Pt/C相当的电催化HER活性. 然而, 有关将Pt SAC用作阴极材料构筑酸性电解槽并获得高性能水电解的报道较少. 因此, 探索一种简便易行的合成策略, 靶向构建在PEMWE实际应用中具有优异HER性能的Pt SAC是本文的主要研究思路.

本文首先以氮掺杂的活性炭黑珍珠2000为载体(NBP), 通过低温水热还原反应, 制备含几个金属原子的钌原子簇前驱体材料(Ru_xNBP). 随后以K₂PtCl₄为Pt源, 通过碳缺陷辅助还原的静电置换反应制备了Ru_xNBP负载的Pt SAC (Pt₁/Ru_xNBP). X射线衍射、高角环形暗场扫描透射电镜、X射线光电子能谱及X射线吸收谱结果表明, Pt₁/Ru_xNBP催化剂中的金属原子均匀分散. 其中, Pt主要以孤立的单原子形成分散存在, 且与吡啶氮基碳缺陷及两个Cl原子配位, 而Ru主要以含两个原子的Ru₂单元分散存在. 作为控制实验, 分别以NBP和BP为载体, 以K₂PtCl₄为Pt源, 通过碳缺陷辅助还原的静电置换反应制备了与Pt₁/Ru_xNBP目标Pt含量相同的Pt SAC (Pt₁/NBP和Pt₁/BP); 分别以NBP和Ru_xNBP为载体, 以Pt(acac)₂为Pt源通过热水反应制备了与Pt₁/Ru_xNBP目标Pt含量相同的Pt SAC (Pt/NBP和Pt/Ru_xNBP). 电化学测试上述Pt SAC在酸性条件下电催化HER活性的结果表明, 催化剂Pt₁/BP和Pt/NBP对电催化HER几乎没有活性; 而Pt₁/Ru_xNBP则展现出较好的电催化HER活性, 其在10 mA cm^‒2时的过电位(η₁₀)仅为11 mV, 远小于催化剂Ru_xNBP (228 mV), Pt₁/NBP (143 mV)和Pt/Ru_xNBP (271 mV)的η₁₀值, 甚至优于商业Pt/C (13 mV). 催化剂Pt₁/Ru_xNBP在20 mV过电位时的质量活性为4.818 A mg_PGM^‒1, 是商业Pt/C的5.7倍. 此外, Pt₁/Ru_xNBP也表现出较低的塔菲尔斜率(25 mV dec^‒1)以及较好的稳定性. 进一步研究催化剂在酸性电解槽中的性能发现, 基于Pt₁/Ru_xNBP为阴极材料组装的质子交换膜电解槽在1.0 A cm^‒2电流密度时的电压比基于商业Pt/C的电解槽低20 mV, 且其在3.0 A cm^‒2电流密度时的电压为1.807 V, 接近于美国能源部2026年目标 (1.8 V). 理论计算结果表明, 催化剂Pt₁/Ru_xNBP中与Ru₂单元相临近的单原子Pt为主要的HER活性位点, 且是Pt-Cl键和临近的Ru₂协同调控单原子Pt的5d结构, 提高了催化剂Pt₁/Ru_xNBP电催化HER的性能.

综上, 本文结合低温水热还原和静电置换反应, 在温和条件下实现了高性能Pt SAC的制备, 探究了其在酸性条件下的电催化HER性能, 阐明了反应机制, 为研究利用不同的前驱体和杂原子掺杂的碳材料制备金属原子级分散的HER电催化剂提供了参考.

关键词: 铂, 单原子电催化剂, 钌团簇, 析氢反应, 密度泛函理论

Abstract:

Exploring platinum single-atom electrocatalysts (SACs) is of great significance for effectively catalyzing the hydrogen evolution reaction in order to maximize the utilization of metal atoms. Herein, ruthenium clusters with several atoms (Ru_x) supported on nitrogen-doped, cost-efficient Black Pearls 2000 (Ru_xNBP), were synthesized as initial materials via a simple hydrothermal method. Then, [PtCl₄]^2‒ ion was reductively deposited on Ru_xNBP to obtain a Pt SAC (Pt₁/Ru_xNBP). Electrochemical measurements demonstrate the excellent HER performance of Pt₁/Ru_xNBP with a 5.7-fold increase in mass activity compared to the commercial Pt/C at 20 mV. Moreover, the cell voltage of the proton exchange membrane electrolyzer with Pt₁/Ru_xNBP is 20 mV lower compared to that with commercial Pt/C at 1.0 A cm^‒2. Physical characterization and density functional theory calculations revealed that the preserved Pt-Cl bond of [PtCl₄]^2‒ and the Ru_xNBP support co-regulate the 5dstate of isolated Pt atoms and enhance the catalytic HER capacity of Pt₁/Ru_xNBP.

Key words: Platinum, Single-atom eletrocatalyst, Ruthenium cluster, Hydrogen evolution reaction, Density functional theory

刘京, 马贤迪, 卢政汉, 申东元, 赵阿雅, 韩晸宇, 龙剑平, 周震, 焦梦改, 李国承, 赵恩爱. 靶向构筑高性能单原子铂基氢析出反应电催化剂[J]. 催化学报, 2025, 69: 259-270.

Jing Liu, Xiandi Ma, Jeonghan Roh, Dongwon Shin, Ara Cho, Jeong Woo Han, Jianping Long, Zhen Zhou, Menggai Jiao, Kug-Seung Lee, EunAe Cho. Targeted construction of high-performance single-atom platinum-based electrocatalysts for hydrogen evolution reaction[J]. Chinese Journal of Catalysis, 2025, 69: 259-270.

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图/表 6

Fig. 1. Flow chart of the sample preparation method.

Fig. 2. HAADF-STEM images of Pt1/RuxNBP with low (a) and high (b) magnification. (c) The corresponding intensity profile of Pt1/RuxNBP marked with yellow box in Fig. 1(b). (d) Elemental mapping of Pt1/RuxNBP.

Fig. 3. (a) XPS survey of Pt1/BP, Pt1/NBP, Pt/NBP, Pt/RuxNBP, and Pt1/RuxNBP. (b) High-resolution XPS spectra of N 1s for Pt1/RuxNBP. (c) The proportion (at.%) of NPd, NIm, M-N, NAm, and NPy in NBP, RuxNBP, Pt/NBP, Pt/RuxNBP, Pt1/RuxNBP, and Pt1/NBP, respectively. (d) High-resolution XPS spectra of Cl 2p for Pt1/BP, Pt/NBP, Pt1/NBP, Pt/RuxNBP, Pt1/RuxNBP, and Commercial K2PtCl4. (e) High-resolution XPS spectra of Ru 3p for RuxNBP, Pt/RuxNBP, and Pt1/RuxNBP. (f) High-resolution XPS spectra of Pt 4f for Pt(acac)2, Pt/NBP, Pt/RuxNBP, K2PtCl4, Pt1/BP, Pt1/NBP, and Pt1/RuxNBP.

Fig. 4. The Ru K-edge XANES (a) and k2-weighted FT EXAFS spectra (b) of Ru foil, Rux/NBP, Pt/RuxNBP, Pt1/RuxNBP, and RuO2. The Pt L3-edge XANES (c) and k2-weighted FT EXAFS spectra (d) of Pt foil, Pt/NBP, Pt/RuxNBP, Pt1/NBP, Pt1/RuxNBP, and PtO2.

Fig. 5. Electrochemical characterization of different catalysts. (a) The polarization curves for RuxNBP, Pt/NBP, Pt/RuxNBP, Pt1/BP, Pt1/NBP, Pt1/RuxNBP and the commercial Pt/C in 0.1 mol L?1 HClO4 solution with a scan rate of 1 mV s?1 and rotation speed of 2500 r min?1. (b) The HER mass activity of the corresponding electrocatalysts at an overpotential of 20 mV. (c) Tafel Plots of RuxNBP, Pt/NBP, Pt/RuxNBP, Pt1/BP, Pt1/NBP, Pt1/RuxNBP and the commercial Pt/C for HER. The polarization curves of Pt1/RuxNBP (d) and commercial Pt/C (e) at initial and after 10000 cycles. (f) Current-voltage relationships measured using 5 cm2 single electrolysis cell at 80 °C and atmospheric pressure of gases; cathodic catalyst: Pt1/RuxNBP (0.040 mgPt+Ru cm?2) and commercial Pt/C (0.031mgPt cm?2); anodic catalyst: commercial IrO2 (1 mgIrO2 cm?2); Nafion?-212 membrane.

Fig. 6. (a) The optimized configurations (top and side views) of two types of Pt1 sites in Pt1/RuxNBP, which include Pt1/RuxNBP-i with the Pt1 site positions near the Ru2 unit and Pt1/RuxNBP-ii with the Pt1 site locates far away from the Ru2 unit. The brown, blue, red, green, cyan, dark blue, and white spheres represent C, N, O, Cl, Pt, and Ru atoms, respectively. (b) The free energies diagram of the HER on the models involving Pt1-based active sites in the corresponding catalyst and Pt(111).

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靶向构筑高性能单原子铂基氢析出反应电催化剂

Targeted construction of high-performance single-atom platinum-based electrocatalysts for hydrogen evolution reaction

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