溶解-再生长法构建Fe-Dy氧化物调控镍-有机框架电子结构的高性能水分解电催化剂

doi:10.1016/S1872-2067(20)63606-3

催化学报 ›› 2020, Vol. 41 ›› Issue (11): 1745-1753.DOI: 10.1016/S1872-2067(20)63606-3

溶解-再生长法构建Fe-Dy氧化物调控镍-有机框架电子结构的高性能水分解电催化剂

万梓霞^a, 何秋婷^a, 陈菊丹^a, 泰勒·伊西姆扬^c, 王宝^b, 杨秀林^a

a 广西师范大学化学与药学学院广西低碳能源材料重点实验室, 广西桂林 541004, 中国;
b 中国科学院过程工程研究所生化工程国家重点实验室, 北京 100190, 中国;
c 阿卜杜拉国王科技大学的沙特阿拉伯基础工业公司, 图瓦勒 23955-6900, 沙特阿拉伯

收稿日期:2020-02-26 修回日期:2020-03-31 出版日期:2020-11-18 发布日期:2020-08-15
通讯作者: 杨秀林, 王宝, 泰勒·伊西姆扬
基金资助:
国家自然科学基金（21965005）；广西自然科学基金（2018GXNSFAA294077）；广西高层次人才工程项目（F-KA18015，2018ZD004）；广西研究生教育创新计划（XYCSZ2019056，YCBZ2019031）.

Dissolution-regrowth of hierarchical Fe-Dy oxide modulates the electronic structure of nickel-organic frameworks as highly active and stable water splitting electrocatalysts

Zixia Wan^a, Qiuting He^a, Jundan Chen^a, Tayirjan Taylor Isimjan^c, Bao Wang^b, Xiulin Yang^a

a Guangxi Key Laboratory of Low Carbon Energy Materials, School of Chemistry and Pharmaceutical Sciences, Guangxi Normal University, Guilin 541004, Guangxi, China;
b State Key Laboratory of Biochemical Engineering, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100190, China;
c Saudi Arabia Basic Industries Corporation(SABIC) at King Abdullah University of Science and Technology(KAUST), Thuwal 23955-6900, Saudi Arabia

Received:2020-02-26 Revised:2020-03-31 Online:2020-11-18 Published:2020-08-15
Supported by:
This work was supported by the National Natural Science Foundation of China (21965005), Natural Science Foundation of Guangxi Province (2018GXNSFAA294077), Project of High-Level Talents of Guangxi (F-KA18015, 2018ZD004), and Innovation Project of Guangxi Graduate Education (XYCSZ2019056, YCBZ2019031).

摘要/Abstract

摘要： 世界经济的快速发展加剧了能源消耗，迫切需要探索替代的可持续能源，以减少对化石燃料的依赖.电化学水分解制氢由于具有较高的能量密度，是一种很有应用前景的可再生、环境友好的能源，也被认为是最有潜力的储能和转化方法之一.为了实现高效和经济的水电解，必须制备高活性、低成本和合适的析氧反应（OER）电催化剂.OER是水分解的半反应，由于具有四电子-质子耦合的转移过程，OER反应具有更高的超电势.因此，它决定了整个水分解系统的整体效率.虽然某些贵金属及其氧化物（IrO₂或RuO₂）具有较高的OER活性和较低的过电位，但这些材料的稀缺性和高成本严重限制了它们的大规模应用.相反，过渡金属及其衍生物，例如钴、镍和铁，由于价格低廉且地壳中含量丰富，因此是理想的电催化剂材料.通常，有两个主要途径可制备高活性OER电催化剂.一种方法是赋予结构优势，例如较大的比表面积、合理的孔径和丰富的活性位点；二是调节反应部位的电子结构，增强电化学活性.金属有机框架（MOF）的发展为水分解用非贵金属催化剂的设计提供了新的机会和平台，因为MOF的天然多孔结构可以促进基质或产物扩散并显著加速电荷转移.同时，MOF大的比表面积可均匀地暴露其活性位点，这为制备高性能OER电催化剂提供了良好的模板或前体.然而，目前报道的大多数MOF系统仍然存在一些重大问题，包括导电性差和结构上隐藏的金属中心，这严重阻碍了它们在电化学过程中的直接利用.此外，一些研究表明Dy和Ni自旋是铁磁耦合的，它可以增加铁的磁性并改变过渡金属基催化剂表面的粗糙度，但是相对较少的工作集中在其OER应用上.
本文成功地在碳布上通过简单的两步水热法制备了三维结构的铁镝氧化物原位调控的MOF-Ni阵列（FeDy@MOF-Ni/CC）.电化学研究表明，优化的FeDy@MOF-Ni/CC催化剂仅需251mV的低过电位即可达到10mA cm^-2，并具有52.1mV dec^-1的小Tafel斜率.另外，在1.0M KOH中连续测试80 h后，稳定性仅下降了5.5%.此外，在全水分解系统中仅需1.57V的电池电压即可达到10mA cm^-2，远远优于大多数先前报道的催化剂.研究认为，独特的3D菱形结构以及Fe-Dy-Ni物种的耦合协同作用赋予了其出色的催化性能.
本文采用红外光谱（FTIR）、拉曼光谱、热重分析（TGA）、比表面积测试和X射线光电子能谱（XPS）等表征手段研究了不同催化材料性能变化的原因.采用FTIR研究了相关材料的表面官能团，揭示出FeDy@MOF-Ni具有Fe@MOF-Ni和Dy@MOF-Ni典型的特征峰.此外，FeDy@MOF-Ni的拉曼光谱由Dy@MOF-Ni和Fe@MOF-Ni整合构成.同时，不同催化剂的TGA显示出不同的质量变化.这种明显的差异证明了两步水热法将Dy和Fe物种成功地掺杂到MOF-Ni中.比表面积测试结果表明，FeDy@MOF-Ni材料具有III型等温线特征，孔隙尺寸在30-50nm范围内，与MOF-Ni前驱体显著不同，进一步说明MOF-Ni的解离和FeDy@MOF-Ni的成功制备.采用XPS进一步表征了Fe-Dy氧化物的掺杂对催化剂组成和表面化学态的影响，发现FeDy@MOF-Ni具有最低的Ni²⁺/Ni³⁺和Fe²⁺/Fe³⁺比值和Dy结合能负移，表明不同物种之间存在较强的电子相互作用.

关键词: 金属有机框架, 氧化镝, 协同效应, 析氧反应, 水分解

Abstract: As the kinetically sluggish oxygen evolution reaction (OER) is considered to be a bottleneck in overall water splitting, it is necessary to develop a highly active and stable electrocatalyst to overcome this issue. Herein, we successfully fabricated a three-dimensional iron-dysprosium oxide co-regulated in-situ formed MOF-Ni arrays on carbon cloth (FeDy@MOF-Ni/CC) through a facile two-step hydrothermal method. Electrochemical studies demonstrate that the designed FeDy@MOF-Ni/CC catalyst requires an overpotential of only 251 mV to reach 10 mA cm^-2 with a small Tafel slope of 52.1 mV dec^-1. Additionally, the stability declined by only 5.5% after 80 h of continuous testing in 1.0 M KOH. Furthermore, a cell voltage of only 1.57 V in the overall water splitting system is sufficient to achieve 10 mA cm^-2; this value is far better than that of most previously reported catalysts. The excellent catalytic performance originates from the unique 3D rhombus-like structure, as well as coupling synergies of Fe-Dy-Ni species. The combination of lanthanide and transition metal species in the synthesis strategy may open entirely new possibilities with promising potential in the design of highly active OER electrocatalysts.

Key words: Metal-organic frameworks, Dysprosium oxide, Synergistic effect, Oxygen evolution, Water splitting

万梓霞, 何秋婷, 陈菊丹, 泰勒·伊西姆扬, 王宝, 杨秀林. 溶解-再生长法构建Fe-Dy氧化物调控镍-有机框架电子结构的高性能水分解电催化剂[J]. 催化学报, 2020, 41(11): 1745-1753.

Zixia Wan, Qiuting He, Jundan Chen, Tayirjan Taylor Isimjan, Bao Wang, Xiulin Yang. Dissolution-regrowth of hierarchical Fe-Dy oxide modulates the electronic structure of nickel-organic frameworks as highly active and stable water splitting electrocatalysts[J]. Chinese Journal of Catalysis, 2020, 41(11): 1745-1753.

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溶解-再生长法构建Fe-Dy氧化物调控镍-有机框架电子结构的高性能水分解电催化剂

Dissolution-regrowth of hierarchical Fe-Dy oxide modulates the electronic structure of nickel-organic frameworks as highly active and stable water splitting electrocatalysts

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