Pt原位还原诱导NiFe-MOF拓扑转变用于工业级电解海水制氢

doi:10.1016/S1872-2067(24)60271-8

催化学报 ›› 2025, Vol. 72: 211-221.DOI: 10.1016/S1872-2067(24)60271-8

Pt原位还原诱导NiFe-MOF拓扑转变用于工业级电解海水制氢

纳国豪^a^,¹, 郑红顺^a^,¹, 陈明鹏^a^,^*(), 孙华传^a, 吴阅文^a, 李德全^a, 陈赟^a, 赵勃然^a, 赵博^a, 周桐^a, 何天威^a, 张雨潇^a, 赵建红^a, 张裕敏^a, 张瑾^a, 刘锋^b, 崔浩^b, 柳清菊^a^,^*()

^a云南大学材料与能源学院, 云南省微纳材料与技术重点实验室, 国家级光电子能源材料国际联合研究中心, 云南昆明 650091
^b云南贵金属实验室有限公司, 云南昆明 650106

收稿日期:2024-12-03 接受日期:2025-02-03 出版日期:2025-05-18 发布日期:2025-05-20
通讯作者: *电子信箱: mpchen@ynu.edu.cn (陈明鹏),qjliu@ynu.edu.cn (柳清菊).
作者简介:¹ 共同第一作者.
基金资助:
国家重点研发计划(2022YFB3803600);国家自然科学基金(22368050);国家自然科学基金(22378346);云南省重点研发计划(202302AF080002);云南省基础研究计划项目(202401AU070229);云南省基础研究计划项目(202401AT070460);云南省教育厅科学研究基金项目(2024J0013);云南省教育厅科学研究基金项目(2024J0014);云南贵金属实验室科技计划项目(YPML-20240502008);云南贵金属实验室科技计划项目(YPML-2023050259);云南贵金属实验室科技计划项目(YPML-2023050260);云南省高校服务重点产业科技项目(FWCY-BSPY2024023);云南省教育厅科研基金支持项目及云南大学研究生科研创新基金支持项目(KC-24248426)

In-situ Pt reduction induced topological transformation of NiFe-MOF for industrial seawater splitting

Guohao Na^a^,¹, Hongshun Zheng^a^,¹, Mingpeng Chen^a^,^*(), Huachuan Sun^a, Yuewen Wu^a, Dequan Li^a, Yun Chen^a, Boran Zhao^a, Bo Zhao^a, Tong Zhou^a, Tianwei He^a, Yuxiao Zhang^a, Jianhong Zhao^a, Yumin Zhang^a, Jin Zhang^a, Feng Liu^b, Hao Cui^b, Qingju Liu^a^,^*()

^aYunnan Key Laboratory for Micro/Nano Materials & Technology, National Center for International Research on Photoelectric and Energy Materials, School of Materials and Energy, Yunnan University, Kunming 650091, Yunnan, China
^bYunnan Precious Metals Laboratory Co., Ltd., Kunming 650106, Yunnan, China

Received:2024-12-03 Accepted:2025-02-03 Online:2025-05-18 Published:2025-05-20
Contact: ^*E-mail: mpchen@ynu.edu.cn (M. Chen), qjliu@ynu.edu.cn (Q. Liu).
About author:¹ Contributed equally to this work.
Supported by:
National Key Research and Development Program of China(2022YFB3803600);National Natural Science Foundation of China(22368050);National Natural Science Foundation of China(22378346);Key Research and Development Program of Yunnan Province(202302AF080002);Yunnan Basic Applied Research Project(202401AU070229);Yunnan Basic Applied Research Project(202401AT070460);Scientific Research Fund Project of Yunnan Education Department(2024J0013);Scientific Research Fund Project of Yunnan Education Department(2024J0014);Scientific and Technological Project of Yunnan Precious Metals Laboratory(YPML-20240502008);Scientific and Technological Project of Yunnan Precious Metals Laboratory(YPML-2023050259);Scientific and Technological Project of Yunnan Precious Metals Laboratory(YPML-2023050260);Science and Technology Projects of Universities Serving Key Industries in Yunnan Province(FWCY-BSPY2024023);Yunnan Provincial Department of Education Scientific Research Fund-supported project and Yunnan University Graduate Research Innovation Fund-supported project(KC-24248426)

摘要/Abstract

摘要：

电解水制氢因气体纯度高、环保无污染、技术成熟, 近年来被视为实现“双碳”目标的关键技术之一. 在全球淡水资源紧缺的背景下,推动电解水制氢技术从淡水依赖型向海水利用型转型升级,已成为实现绿氢规模化生产的关键路径. 然而, 海水中的复杂成分会在电解过程中影响催化剂的活性及稳定性, 商用Pt/C催化剂无法满足实际应用需求. 因此, 灵活调控金属-载体相互作用从而增强催化剂性能和抗腐蚀能力至关重要, 不仅为突破海水电解制氢技术瓶颈提供有效解决方案, 还可为设计制备高效、稳定的析氢(HER)催化剂提供理论依据.

金属-有机框架(MOF)具有高比表面积和丰富活性位点,因此可用作理想的催化剂载体. 本文采用原位拓扑转变策略, 以一种典型镍铁MOF (NiFe-BDC, BDC:对苯二甲酸)作为催化剂载体, 将Pt量子点均匀沉积于其载体表面. 通过球差校正透射电子显微镜和X射线吸收光谱分析了拓扑转变后样品Pt/T-NiFe-BDC的结构组成以及催化剂中元素配位状态. NiFe-BDC载体发生相转变并生成了富含氧空位镍铁双氢氧化物, 同时Pt量子点中Pt-Pt键缩短, 从而增强了金属-载体相互作用, 优化了催化剂电子结构. 催化剂在碱性海水中展现出优异的HER催化性能, 在500和1000 mA cm^-²的大电流密度下, 催化剂仅需158和266 mV的超低过电位即可实现稳定析氢, 且连续运行500 h没有明显衰减. 将Pt/T-NiFe-BDC作为阴极、NiFe-BDC作为阳极组装的电解槽, 仅需1.89 V的槽压即可驱动1000 mA cm^-²的工业级电解水. 通过理论计算分析Pt/T-NiFe-BDC的电子结构和表面性质, 通过原位拉曼光谱解析界面水结构及其解离过程, 揭示了催化剂在HER过程中的可逆氢溢流机制. 催化剂载体表面氧空位能促进水分子的解离并使*H向Pt量子点溢流, 而Pt量子点提供了高效的*H吸附和结合位点, 使中间产物快速结合并脱附, 这一协同作用显著提升了催化剂HER动力学, 并增强了催化剂的稳定性和抗腐蚀能力.

综上所述, 本文通过Pt原位还原诱导NiFe-MOF拓扑转变, 设计制备了具有低过电位、强稳定性、强抗腐蚀性的Pt/T-NiFe-BDC催化剂用于高效HER, 并阐明了氧空位与Pt量子点协同触发的可逆氢溢流机制, 为实现工业规模电解海水提供了一种有效策略.

关键词: 电解海水, 析氢反应, 拓扑转变, 金属-载体相互作用, 可逆氢溢流

Abstract:

Metal-support interaction (MSI) is regarded as an indispensable manner to stabilize active metals and modulate catalytic activity, which shows great potentials in developing of efficient hydrogen evolution reaction (HER) electrode with high activity and strong robustness. Herein, this work presents a novel heterostructure with ultrafine platinum quantum dots (Pt QDs) on defective catalytic supports derived from metal-organic frameworks (MOFs). It is indicated substantial oxygen vacancies can be generated and Pt-Pt bonds can be optimized through topological transformation. The resulting Pt/T-NiFe-BDC (BDC: C₈H₆O₄) exhibits competitive HER activity in alkaline seawater, attaining ultralow overpotentials of 158 and 266 mV at 500 and 1000 mA cm^-2 with fast kinetics and outstanding stability. An asymmetric water electrolyzer using Pt/T-NiFe-BDC as a cathode only requires a voltage of 1.89 V to generate an industrial density of 1000 mA cm^-2 and shows no attenuation in 500-h continuous test at 500 mA cm^-2. Theoretical calculations and in-situ spectroscopic analysis reveal the reversible hydrogen spillover mechanism, in which oxygen vacancies facilitate the sluggish water dissociation and Pt QDs promote the H* combination. This study provides a new paradigm to engineer metal-supported catalysts for efficient and robust seawater splitting.

Key words: Seawater splitting, Hydrogen evolution reaction, Topological transformation, Metal support interaction, Reversible hydrogen spillover

纳国豪, 郑红顺, 陈明鹏, 孙华传, 吴阅文, 李德全, 陈赟, 赵勃然, 赵博, 周桐, 何天威, 张雨潇, 赵建红, 张裕敏, 张瑾, 刘锋, 崔浩, 柳清菊. Pt原位还原诱导NiFe-MOF拓扑转变用于工业级电解海水制氢[J]. 催化学报, 2025, 72: 211-221.

Guohao Na, Hongshun Zheng, Mingpeng Chen, Huachuan Sun, Yuewen Wu, Dequan Li, Yun Chen, Boran Zhao, Bo Zhao, Tong Zhou, Tianwei He, Yuxiao Zhang, Jianhong Zhao, Yumin Zhang, Jin Zhang, Feng Liu, Hao Cui, Qingju Liu. In-situ Pt reduction induced topological transformation of NiFe-MOF for industrial seawater splitting[J]. Chinese Journal of Catalysis, 2025, 72: 211-221.

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图/表 6

Fig. 1. Schematic illustration of the synthetic procedure of Pt/T-NiFe-BDC.

Fig. 2. (a) SEM image of NiFe-BDC. SEM (b), TEM (c), HAADF-STEM (d,e) images of Pt/T-NiFe-BDC. (f) Size distribution of Pt QDs. (g) EDS elemental mapping images of Pt, O, Fe, and Ni.

Fig. 3. (a) EPR spectra of NiFe-BDC, Pt/T-NiFe-BDC, Pt/NiFe-LDH and Pt/NiFe-BDC. High-resolution XPS spectra of O 1s (b), Fe 2p (c), Ni 2p (d). Pt L3-edge XANES spectra (e), R-space spectra (f), and k2-weighted wavelet transforms (WT) (g) of Pt/T-NiFe-BDC, Pt/NiFe-LDH, Pt foil, and PtO2.

Fig. 4. HER Performance. LSV curves (a), comprehensive comparisons of HER performance (b), and Tafel plots (c) of Pt/T-NiFe-BDC, Pt/NiFe-LDH, Pt/NiFe-BDC and Pt/C in 1 mol L-1 KOH. LSV curves (d) and Tafel plots (e) of the as-prepared catalysts in alkaline seawater. (f) Stability test at 500 mA cm-2. (g) Comparison of the overpotentials for HER in alkaline seawater.

Fig. 5. LSV curves (a) and comprehensive comparisons (b) of NiFe-BDC, NiFe-LDH, RuO2 and NF in 1 mol L-1 KOH for OER. (c) Polarization curves of NiFe-BDC and NiFe-LDH in alkaline water/seawater. Cell voltage curves (d) and long-term stability test (e) of Pt/T-NiFe-BDC||NiFe-BDC at 500 mA cm-2 in alkaline seawater. (f) Comparison of cell voltages between Pt/T-NiFe-BDC||NiFe-BDC and recently reported electrolyzer.

Fig. 6. (a) Top view of Pt/T-NiFe-BDC (atoms in orange, green, gray, red and white represent Fe, Ni, Pt, O and H, respectively). (b) The calculated PDOS of Pt QDs in Pt/T-NiFe-BDC and Pt-NiFe-LDH. (c) Relative energies of the HER process on Pt/T-NiFe-BDC-Ov, Pt/T-NiFe-BDC-PtQD and Pt/NiFe-LDH- PtQD in alkaline media. (d) Corresponding illustrations of the HER process on Pt/T-NiFe-BDC-OV in alkaline media. In-situ Raman spectra of Pt/T-NiFe-BDC (e) and Pt/NiFe-LDH (f). (g) The positions and ratios of ??3 peaks at various potentials.

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Pt原位还原诱导NiFe-MOF拓扑转变用于工业级电解海水制氢

In-situ Pt reduction induced topological transformation of NiFe-MOF for industrial seawater splitting

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[1]	冯超, 邵佳新, 吴汉洋, 杨恒攀, 蔚佳莹, 胡琪, 何传新. 超高过电位诱导NiS₂深度重构显著提高HER性能[J]. 催化学报, 2025, 72(5): 230-242.
[2]	马军, 徐冰, 曹硕, 李世艳, 储伟, Siglinda Perathoner, Gabriele Centi, 刘岳峰. 反应条件下Ni/Mo₂CT_x MXene催化剂结构演变调节CO₂还原性能[J]. 催化学报, 2025, 72(5): 243-253.
[3]	吴君, 刘立乾, 严鑫悦, 潘刚, 白家豪, 王成兵, 李福伟, 李永. 用于生物质基香草醛水相高选择性加氢脱氧的氮掺杂中空碳球负载Pd催化剂的微环境设计和构筑[J]. 催化学报, 2025, 71(4): 267-284.
[4]	段会梅, 李晓菲, 王传辉, 张丛筠, 余楷文, 陈磊, 张云尚, 纪嘉宾, 杨贤峰, 杨东江. Ir/TiO₂催化剂甲烷燃烧反应中TiO₂晶面依赖效应[J]. 催化学报, 2025, 70(3): 378-387.
[5]	李家欣, 吕燕, 吴雪岩, 郭新玉, 杨卓君, 郭继玺, 周天华, 贾殿赠. 分级结构NiO纳米管/纳米片表面限域生长Pt亚纳米团簇催化剂用于尿素辅助节能产氢[J]. 催化学报, 2025, 69(2): 203-218.
[6]	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(2): 259-270.
[7]	Athira Krishnan, K. Archana, A. S. Arsha, Amritha Viswam, M. S. Meera. 宽带隙半导体在电催化和光催化水分解绿色制氢中的潜在作用[J]. 催化学报, 2025, 68(1): 103-145.
[8]	郎程广, 许彦桐, 姚向东. 通过缺陷优化析氢反应电催化剂: 最新研究进展与展望[J]. 催化学报, 2024, 64(9): 4-31.
[9]	肖佳勇, 蒋超, 张辉, 邢卓, 邱明, 余颖. 具有亲水性的无定形棒状核壳结构NiMoP@CuNWs用于中性介质中高效析氢[J]. 催化学报, 2024, 63(8): 154-163.
[10]	黄子超, 杨婷惠, 张颖冰, 管超群, 桂文科, 况敏, 杨建平. 提高酸性CO₂电解的选择性:阳离子效应和催化剂创新[J]. 催化学报, 2024, 63(8): 61-80.
[11]	李志鹏, 刘晓斌, 于青平, 屈欣悦, 万均, 肖振宇, 迟京起, 王磊. 用于高电流密度析氢反应电催化剂的研究进展[J]. 催化学报, 2024, 63(8): 33-60.
[12]	陈晓, 杜云梅, 杨宇, 刘康, 赵晋灵, 夏晓丹, 王磊. 安培级电流密度下淬火优化CoPS纳米棒的晶型/非晶型比例以促进肼辅助的全水分解[J]. 催化学报, 2024, 62(7): 265-276.
[13]	赵万成, 马加朋, 田栋, 康宝涛, 夏方诠, 成婧, 吴亚军, 王梦遥, 武刚. 集成有CNTs和Ni-Ni(OH)₂异质结构的电解析氢自支撑薄膜催化剂[J]. 催化学报, 2024, 62(7): 287-295.
[14]	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(7): 156-165.
[15]	徐伟, 甄超, 朱华泽, 姚婷婷, 邱建航, 梁艳, 白朔, 陈春林, 成会明, 刘岗. 六氟钽酸氨拓扑转变制备低深能级缺陷Ta₃N₅光阳极实现超低偏压光电化学分解水[J]. 催化学报, 2024, 61(6): 144-153.