具有高效析氧催化性能的铁基双元金属有机框架纳米棒研究

doi:10.1016/S1872-2067(20)63686-5

催化学报 ›› 2021, Vol. 42 ›› Issue (4): 637-647.DOI: 10.1016/S1872-2067(20)63686-5

具有高效析氧催化性能的铁基双元金属有机框架纳米棒研究

吴楚楚^a^,^b^,^c, 张晓明^a^,^b, 李焕巧^a^,^b, 夏章讯^a^,^b, 于陕升^d, 王素力^a^,^b^,^*(), 孙公权^a^,^b^,^#()

^a中国科学院大连化学物理研究所, 洁净能源国家实验室(筹)燃料电池研究部, 辽宁大连116023
^b中国科学院大连化学物理研究所, 醇类燃料电池及复合电能源研究中心, 辽宁大连116023
^c中国科学院大学, 北京100049
^d吉林大学材料科学系, 吉林长春130012

收稿日期:2020-05-17 接受日期:2020-06-23 出版日期:2021-04-18 发布日期:2021-01-22
通讯作者: 王素力,孙公权
基金资助:
中国科学院战略先导专项(XDA21090300);国家自然科学基金(91834301);大连化物所科研创新基金项目(DICP ZZBS201705)

Iron-based binary metal-organic framework nanorods as an efficient catalyst for the oxygen evolution reaction

Chuchu Wu^a^,^b^,^c, Xiaoming Zhang^a^,^b, Huanqiao Li^a^,^b, Zhangxun Xia^a^,^b, Shansheng Yu^d, Suli Wang^a^,^b^,^*(), Gongquan Sun^a^,^b^,^#()

^aDivision of Fuel Cells and Battery, Dalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China
^bKey Laboratory of Fuel Cells & Hybrid Power Sources, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China
^cUniversity of Chinese Academy of Sciences, Beijing 100049, China
^dDepartment of Materials Science, Jilin University, Changchun 130012, Jilin, China

Received:2020-05-17 Accepted:2020-06-23 Online:2021-04-18 Published:2021-01-22
Contact: Suli Wang,Gongquan Sun
About author:^#Tel/Fax: +86-411-84379063; E-mail: gqsun@dicp.ac.cn
^*Tel/Fax: +86-411-84762570; E-mail: suliwang@dicp.ac.cn;
Supported by:
Strategic Priority Research Program of the Chinese Academy of Sciences(XDA21090300);National Natural Science Foundation of China(91834301);DICP Grant(DICP ZZBS201705)

摘要/Abstract

摘要：

析氧反应(OER)是电解水制氢的关键步骤,β开发高效、稳定、廉价的OER电催化剂是目前该领域的研究热点.ββ碱性电解液中的OER电催化剂成分以Mn、Fe、Co、Ni等为主,β其中单一组分的Fe基化合物催化活性不高,β但碱性电解液中的痕量铁杂质极易掺入Ni、Co等非Fe基材料的结构中,β极大影响其OER催化性能,β即现有大部分非Fe基化合物无法回避Fe的影响.ββ为探究Fe基多金属电催化剂的活性规律,β本文以结构清晰、组分可控的Fe基金属有机框架材料为基底,β通过掺入Mn、Co、Ni等元素构建双元金属化合物Fe₂M-MIL-88B(M = Mn, Co, Ni),β并围绕上述Fe基双金属电催化剂的构效关系展开研究.ββ
扫描电镜、透射电镜、X射线衍射光谱、红外光谱等表征结果表明,β所制备的Fe基双金属材料均为具有MIL-88B构型的纳米棒,β其特征三核金属簇Fe₃O中的一个铁原子被第二元金属所替代,β从而形成相应的三核混合金属簇Fe₂MO.ββ上述Fe基双金属催化剂的析氧催化活性顺序为: Fe₂Ni > Fe₂Co > Fe₂Mn > Fe (0.1βM KOH电解液).ββ其中,βFe₂Ni-MIL-88B电催化剂在10βmA cm^-2析氧电流对应的过电位仅需307βmV,β明显低于OER基准电催化剂20 wt% Ir/C(376βmV).ββ
结合材料的元素组成、电化学活性比表面积(ECSA)及金属价态分析发现,β第二元金属的引入会在不同程度上降低Fe的价态,β其中Ni的影响程度最大,βCo次之,βMn的影响最小.ββ借助分子轨道理论对上述实验现象进行了解释.ββ处于低自旋态的Ni²⁺与邻近桥氧O^2-之间存在电子排斥作用,β因此部分电子将从Ni²⁺经O^2-转移至高自旋态的Fe³⁺,β从而在Ni²⁺和Fe³⁺之间形成了较强的电子耦合作用.ββCo²⁺具有和Ni²⁺相似的构型,β但影响稍小.ββ而Mn²⁺和Fe³⁺同为高自旋态,β对Fe³⁺的电子结构影响最小,β导致活性改善程度最低.ββ密度泛函理论计算得到的自旋态变化情况印证了上述推测.ββ该系列Fe基双金属材料的催化性能主要受金属活性位点的电子结构影响,βFe与邻近金属间形成的电子耦合作用修饰了金属活性位点的电子结构,β从而提高了材料的OER本征催化活性.

关键词: 析氧反应, 金属有机框架, 电催化, 电子耦合作用, 水氧化

Abstract:

First-row transition metal compounds have been widely explored as oxygen evolution reaction (OER) electrocatalysts due to their impressive performance in this application. However, the activity trends of these electrocatalysts remain elusive due to the effect of inevitable iron impurities in alkaline electrolytes on the OER; the inhomogeneous structure of iron-based (oxy)hydroxides further complicates this situation. Bimetallic metal-organic frameworks (MOFs) have the advantages of well-defined and uniform atomic structures and the tunable coordination environments, allowing the structure-activity relationships of bimetallic sites to be precisely explored. Therefore, we prepared a series of iron-based bimetallic MOFs (denoted as Fe₂M-MIL-88B, M = Mn, Co, or Ni) and systematically compared their electrocatalytic performance in the OER in this work. All the bimetallic MOFs exhibited higher OER activity than their monometallic iron-based counterpart, with their activity following the order FeNi > FeCo > FeMn. In an alkaline electrolyte, Fe₂Ni-MIL-88B showed the lowest overpotential to achieve a current density of 10 mA cm^-2 (307 mV) and the smallest Tafel slope (38 mV dec^-1). The experimental and calculated results demonstrated that iron and nickel exhibited the strongest coupling effect in the series, leading to modification of the electronic structure, which is crucial for tuning the electrocatalytic activity.

Key words: Oxygen evolution reaction, Metal-organic frameworks, Electrocatalysis, Electronic coupling effect, Water oxidation

吴楚楚, 张晓明, 李焕巧, 夏章讯, 于陕升, 王素力, 孙公权. 具有高效析氧催化性能的铁基双元金属有机框架纳米棒研究[J]. 催化学报, 2021, 42(4): 637-647.

Chuchu Wu, Xiaoming Zhang, Huanqiao Li, Zhangxun Xia, Shansheng Yu, Suli Wang, Gongquan Sun. Iron-based binary metal-organic framework nanorods as an efficient catalyst for the oxygen evolution reaction[J]. Chinese Journal of Catalysis, 2021, 42(4): 637-647.

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图/表 10

Scheme 1. Scheme of the preparation and structure of Fe2M-MIL-88B (Orange, blue, gray, red, and white spheres represent Fe, M, C, O, and H atoms, respectively).

Fig. 1. SEM and TEM images of Fe2Mn-MIL-88B (a,e), Fe-MIL-88B (b,f), Fe2Co-MIL-88B (c,g), and Fe2Ni-MIL-88B (d,h) (inset: distributions of the length of the samples). TEM images of Fe2Ni-MIL-88B (i) and the corresponding elemental mapping of oxygen (j), iron (k), and nickel (l), along with the corresponding EDX spectra (m) in the selected region.

Fig. 2. XRD patterns (a) and FT-IR spectra (b,c) of Fe2M-MIL-88B.

Fig. 3. OER polarization curves (a) and Tafel plots (b) calculated from the polarization curves of Fe2M-MIL-88B and 20% Ir/C in O2-saturated 0.1 M KOH; (c) EIS spectra of Fe2M-MIL-88B at an overpotential of 350 mV with an inset showing the equivalent circuit model (symbols: raw data; lines: linear fit results); (d) Chronoamperometry results of Fe2Ni-MIL-88B/CC and OER polarization curves before (dashed curve) and after (solid curve) the stability test (without iR-correction); (e) ECSA of Fe2M-MIL-88B calculated from LSV measurements performed in a non-faradaic region at different scan rates.

Table 1 Comparison of the electrocatalytic OER performance of Fe2M-MIL-88B with that of other reported MOF electrocatalysts tested in 0.1 M KOH on a GC-RDE.

Catalyst	Loading (mg cm^-2)	η (mV) @10 mA cm^-2	Tafel slope (mV dec^-1)	Ref.
Fe₂Ni-MIL-88B	0.191	307	38	This work
Fe₂Co-MIL-88B	0.191	348	47	This work
MAF-X27-OH	0.18	461	66	[28]
NiFe-MOF	0.3	406	—	[27]
Ti₃C₂T_x-CoBDC	0.208	410	48.2	[30]
Fe₃-Co₂	0.2	283	43	[29]
Fe:2D-Co-NS	0.2	282	59	[31]
FeCo-MNS-1.0	0.36	298	21.6	[65]
CTGU-10c2	0.14	240	58	[32]

Fig. 4. N2 adsorption-desorption isotherms (a) and pore size distributions (b) of Fe2M-MIL-88B.

Fig. 5. (a) LSV measurements of the catalysts in O2-purged 0.0316 M KOH (pH 12.57, ■), 0.1 M KOH (pH 13.12, ●), 0.316 M KOH (pH 13.54, ▲), and 1 M KOH (pH 13.98, ▼). OER current density at (b) 1.550 V vs. RHE and the indicated potential (c) after iR-correction at the investigated pH values.

Fig. 6. (a) XPS survey patterns of all the samples; (b) Mn 2p high-resolution spectrum of Fe2Mn-MIL-88B; (c) Fe 2p high-resolution spectra of all samples (Dashes: raw data. Gray line: fitting results); (d) Mn 3s high-resolution XPS spectrum of Fe2Mn-MIL-88B; (e) Co 2p and (f) Ni 2p high-resolution spectra of Fe2Co-MIL-88B and Fe2Ni-MIL-88B, respectively; (g) Fe3+ content calculated from the fitting results of Fe2M-MIL-88B.

Fig. 7. Schematic representation of the electronic coupling between Fe and Ni in Fe2Ni-MIL-88B.

Table 2 Energies of Fe2M-MIL-88B with varied Mulliken spin states.

Initial spin multiplicity		1	2	3
Fe₂Mn	Final spin	3.82×2, -3.45^Mn	-3.77, 1.52, 3.68^Mn	-3.80, 3.01, 3.28^Mn
Fe₂Mn	Energy (Ha)	-4887.845132	-4887.833044	-4887.818988
Fe	Final spin	3.83×2; 3.81	3.78, -3.82, 1.10	3.75, -3.80, 2.08
Fe	Energy (Ha)	-5000.539747	-5000.531345	-5000.533114
Fe₂Co	Final spin	1.72, -1.40, 0.69^Co	1.72, -1.37, 0.70^Co	1.87, -0.70, 0.82^Co
Fe₂Co	Energy (Ha)	-5119.585567	-5119.585562	-5119.582236
Fe₂Ni	Final spin	1.90, -1.86, 1.35^Ni	1.66, -2.13, 1.23^Ni	1.97, -1.67, 1.39^Ni
Fe₂Ni	Energy (Ha)	-5245.130615	-5245.129398	-5245.130189

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具有高效析氧催化性能的铁基双元金属有机框架纳米棒研究

Iron-based binary metal-organic framework nanorods as an efficient catalyst for the oxygen evolution reaction

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[1]	唐小龙, 李锋, 李方, 江燕斌, 余长林. 单原子催化剂在光催化和电催化合成过氧化氢中的研究进展[J]. 催化学报, 2023, 52(9): 79-98.
[2]	石靖, 郭煜华, 谢飞, 章名田, 张洪涛. 氧化还原活性配体的电子效应对钌催化水氧化反应的影响[J]. 催化学报, 2023, 52(9): 271-279.
[3]	张季, 俞爱民, 孙成华. 非金属掺杂石墨烯异核双原子催化剂氮还原特性研究[J]. 催化学报, 2023, 52(9): 263-270.
[4]	胡金念, 田玲婵, 王海燕, 孟洋, 梁锦霞, 朱纯, 李隽. MXene负载3d金属单原子高效氮还原电催化剂的理论筛选[J]. 催化学报, 2023, 52(9): 252-262.
[5]	洪岩, 王琦, 阚子旺, 张禹烁, 郭晶, 李思琦, 刘松, 李斌. 电化学氮还原氨反应催化剂的最新研究进展[J]. 催化学报, 2023, 52(9): 50-78.
[6]	刘勇, 赵晓丽, 隆昶, 王晓艳, 邓邦为, 李康璐, 孙艳娟, 董帆. 原位构筑动态Cu/Ce(OH)_x界面用于高活性、高选择性和高稳定性硝酸盐还原合成氨[J]. 催化学报, 2023, 52(9): 196-206.
[7]	高晖, 张恭, 程东方, 王永涛, 赵静, 李晓芝, 杜晓伟, 赵志坚, 王拓, 张鹏, 巩金龙. 构建Cu台阶位促进电催化CO₂还原制醇类化学品的研究[J]. 催化学报, 2023, 52(9): 187-195.
[8]	邹心仪, 顾均. 酸性条件下二氧化碳高效电还原策略[J]. 催化学报, 2023, 52(9): 14-31.
[9]	王潇涵, 田汉, 余旭, 陈立松, 崔香枝, 施剑林. 非晶相电催化剂在电解水领域的研究进展[J]. 催化学报, 2023, 51(8): 5-48.
[10]	阎菲, 张由子, 刘思碧, 邹睿卿, Jahan B Ghasemi, 李炫华. 供体-受体型卟啉基金属有机框架实现有效电荷分离高效光催化析氢[J]. 催化学报, 2023, 51(8): 124-134.
[11]	韩璟怡, 管景奇. 通过表面镧改性和体相锰掺杂协助钴尖晶石酸性下析氧[J]. 催化学报, 2023, 51(8): 1-4.
[12]	周波, 石建巧, 姜一民, 肖磊, 逯宇轩, 董帆, 陈晨, 王特华, 王双印, 邹雨芹. 强化脱氢动力学实现超低电池电压和大电流密度下抗坏血酸电氧化[J]. 催化学报, 2023, 50(7): 372-380.
[13]	李慧杰, 池漫洲, 辛兴, 王瑞杰, 刘天府, 吕红金, 杨国昱. 异金属取代的多金属氧酸盐@光响应型金属-有机框架用于高选择性光催化CO₂还原[J]. 催化学报, 2023, 50(7): 343-351.
[14]	王元男, 王立娜, 张可新, 徐靖尧, 武倩楠, 谢周兵, 安伟, 梁宵, 邹晓新. 钙钛矿氧化物在水裂解反应中的电催化研究[J]. 催化学报, 2023, 50(7): 109-125.
[15]	周纳, 王家志, 张宁, 王志, 王恒国, 黄岗, 鲍迪, 钟海霞, 张新波. 富含缺陷的Cu@CuTCNQ复合材料增强电催化硝酸盐还原成氨[J]. 催化学报, 2023, 50(7): 324-333.