错位堆叠限域和微孔缺陷固定协同生长高密度原子级FeII-N4氧还原活性位点

doi:10.1016/S1872-2067(21)63992-X

催化学报 ›› 2022, Vol. 43 ›› Issue (7): 1870-1878.DOI: 10.1016/S1872-2067(21)63992-X

错位堆叠限域和微孔缺陷固定协同生长高密度原子级Fe^II-N₄氧还原活性位点

陈梦慧^a^,^†, 陈永婷^b^,^†, 杨智力^a, 罗进^b, 蔡佳琳^a, 容忠言^a, 张久俊^a, 陈胜利^b^,^#(), 张世明^a^,^*()

^a上海大学理学院, 可持续能源研究院, 上海200244
^b武汉大学化学与分子科学学院, 湖北省化学电源材料与技术重点实验室, 湖北武汉430072

收稿日期:2021-10-29 接受日期:2021-12-02 出版日期:2022-07-18 发布日期:2022-05-20
通讯作者: 陈胜利,张世明
作者简介:第一联系人：
^†共同第一作者.
基金资助:
国家自然科学基金(21606149);国家自然科学基金(21832004);国家自然科学基金(22002110);上海市青年科技启明星计划(18QB1404400)

Synergy of staggered stacking confinement and microporous defect fixation for high-density atomic Fe^II-N₄ oxygen reduction active sites

Menghui Chen^a^,^†, Yongting Chen^b^,^†, Zhili Yang^a, Jin Luo^b, Jialin Cai^a, Joey Chung-Yen Jung^a, Jiujun Zhang^a, Shengli Chen^b^,^#(), Shiming Zhang^a^,^*()

^aInstitute for Sustainable Energy, College of Sciences, Shanghai University, Shanghai 200444, China
^bHubei Key Laboratory of Electrochemical Power Sources, College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, Hubei, China

Received:2021-10-29 Accepted:2021-12-02 Online:2022-07-18 Published:2022-05-20
Contact: Shengli Chen, Shiming Zhang
About author:First author contact:
^†Contributed to this work equally.
Supported by:
National Natural Science Foundation of China(21606149);National Natural Science Foundation of China(21832004);National Natural Science Foundation of China(22002110);Shanghai Rising-Star Program(18QB1404400)

摘要/Abstract

摘要：

聚合物电解质膜燃料电池(PEMFCs)具有高能量密度、高功率密度以及零排放等优点, 被认为是一种高效、实用的发电装置. 然而, PEMFCs阴极氧还原反应(ORR)的动力学缓慢, 需要使用大量的铂(Pt)催化剂, 其成本高、资源有限, 因此, 开发用于ORR的高性能、低成本的非贵金属催化剂(NPMCs)尤为重要. 在NPMCs中, 过渡金属(Fe, Co, Ni, Cu, Zn, Mn等)-氮-碳复合材料, 尤其是Fe-N_x-C, 被认为是一类非常有前景的代Pt催化剂. 但此类催化剂存在催化活性低、电化学稳定性差等问题. 为了获得高性能的NPMCs, 催化剂创新性的设计和合成受到高度关注.

研究表明, 在惰性气氛下高温热解含Fe、N和C的化学物质是制备Fe-N_x-C催化剂的有效途径. 在高温热解过程中, 形成的吡啶-N可进一步键合Fe原子形成Fe-N₄物种, Fe-N₄已被证实是高ORR活性的催化位点. 然而, 高温热解制备Fe-N_x-C催化剂时, 有两个主要问题制约催化剂性能的提高: 一方面, 原子Fe可以转化为聚集形态的Fe基纳米颗粒, 其催化ORR能力较差甚至无效; 另一方面, 含N物种的基团容易分解, 会导致Fe-N₄等活性位点的大量流失. 因此, 提出防止Fe原子聚集和活性位点流失的新策略备受期待.

本文提出了一种错位堆叠限域和微孔缺陷固定的协同调控策略. 通过热解酞菁铁(FePc)、酞菁(Pc)和锌(Zn)盐的混合物, 成功制备了高ORR性能的Fe-N_x-C催化剂. 该催化剂具有分级多孔的薄层碳纳米片结构, 其中含Fe物种全部为Fe-N₄活性位点即100%的“Fe-N₄活性位点/总Fe物种”比率. 相比之下, 单独热解FePc生成的催化剂中, “Fe-N₄活性位点/总Fe物种”比率仅为5.9%, 且形成的无定型碳样品中嵌有Fe基纳米颗粒. 实验表征和密度泛函理论计算表明, Pc作为大环化合物, 通过与FePc分子π-π作用形成的错位堆叠可以限域Fe原子, 防止其脱出聚集成Fe基纳米颗粒. Zn盐作为造孔剂, 通过Zn挥发诱导产生的微孔缺陷可以固定Fe^II-N₄活性位点. 错位堆叠限域和微孔缺陷固定协同产生了高密度的原子级Fe^II-N₄活性位点, 从而提高了催化剂的ORR活性. 优化的Fe^II-N₄-C电催化剂在碱性介质中展现出了优于商用Pt/C催化剂的半波电势、甲醇耐受性和电化学稳定性. 综上, 本文提出的调控策略对发展高性能NPMCs具有重要的启示意义.

关键词: 氧还原反应, 协同策略, 错位堆叠限域, 微孔缺陷固定, Fe^II-N₄

Abstract:

The development of high-performance nonprecious metal catalysts (NPMCs) to supersede Pt-based catalysts for the oxygen reduction reaction (ORR) in polymer electrolyte membrane fuel cells is highly desirable but remains challenging. In this paper, we present a pyrolysis strategy for spatial confinement and active-site fixation using iron phthalocyanine (FePc), phthalocyanine (Pc) and Zn salts as precursors. In the obtained carbon-based NPMC with a hierarchically porous nanostructure of thin-layered carbon nanosheets, nearly 100% of the total Fe species are Fe^II-N₄ active sites. In contrast, pyrolyzing FePc alone forms Fe-based nanoparticles embedded in amorphous carbon with only 5.9% Fe^II-N₄ active sites. Both experimental characterization and density functional theory calculations reveal that spatial confinement through the staggered π-π stacking of Pc macrocycles effectively prevents the demetallation of Fe atoms and the formation of Fe-based nanoparticles via aggregation. Furthermore, Zn-induced microporous defects allow the fixation of Fe^II-N₄ active sites. The synergistic effect of staggered stacking confinement and microporous defect fixation results in a high density of atomic Fe^II-N₄ active sites that can enhance the ORR. The optimal Fe^II-N₄-C electrocatalyst outperforms a commercial Pt/C catalyst in terms of half-wave potential, methanol tolerance, and long-term stability in alkaline media. This modulation strategy can greatly advance efforts to develop high-performance NPMCs.

Key words: Oxygen reduction reaction, Synergy strategy, Staggered stacking confinement, Microporous defects fixation, Fe^II-N₄

陈梦慧, 陈永婷, 杨智力, 罗进, 蔡佳琳, 容忠言, 张久俊, 陈胜利, 张世明. 错位堆叠限域和微孔缺陷固定协同生长高密度原子级Fe^II-N₄氧还原活性位点[J]. 催化学报, 2022, 43(7): 1870-1878.

Menghui Chen, Yongting Chen, Zhili Yang, Jin Luo, Jialin Cai, Joey Chung-Yen Jung, Jiujun Zhang, Shengli Chen, Shiming Zhang. Synergy of staggered stacking confinement and microporous defect fixation for high-density atomic Fe^II-N₄ oxygen reduction active sites[J]. Chinese Journal of Catalysis, 2022, 43(7): 1870-1878.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(21)63992-X

https://www.cjcatal.com/CN/Y2022/V43/I7/1870

图/表 8

Scheme 1. Schematic illustration of the preparation procedure for the Fe-Nx-C catalyst (c-(FePc+Pc+ZnCl2)).

Fig. 1. SEM (a), TEM (b), AC-HAADF-STEM (c) and corresponding elemental mapping of C (red), N (peacock blue), and Fe (yellow), and high-resolution AC-HAADF-STEM images (d) of the c-(FePc+Pc+ZnCl2) catalyst. Note that the white dots indicated by yellow circles in (d) are Fe atoms.

Fig. 2. DFT calculations. (a) Possible structures of MPc combined with Pc. (b) binding energies of Fe and average Fe-N bond length. (c) HOMO and LUMO isosurfaces for the calculated FePc molecule and FePc+Pc configuration.

Fig. 3. XRD patterns (a), pore-size distributions and N2 adsorption-desorption isotherms (inset) (b), XPS survey spectra (c) and deconvoluted N1s spectra (d) for the c-FePc, c-(FePc+Pc) and c-(FePc+Pc+ZnCl2) catalysts.

Table 1 Surface N species contents ((at%)) in various catalysts, as determined by XPS analysis.

Sample	Total N	Pyridinic N	Metal-N_x	Pyrrolic N	Graphitic N	Oxidized N
c-FePc	2.82	0.21	0.13	0.56	1.33	0.59
c-(FePc+Pc)	3.06	0.30	0.17	0.57	1.50	0.52
c-(FePc+Pc+ZnCl₂)	3.14	0.37	0.25	0.61	1.68	0.23

Fig. 4. 57Fe Mo?ssbauer spectra of c-FePc (a) and c-(FePc+Pc+ZnCl2) (b) catalysts.

Table 2 Mo?ssbauer parameters for the fitted components and their assignments for c-FePc and c-(FePc+Pc+ZnCl2).

Catalyst	Component	IS (mm s^-1)	QS (mm s^-1)	HF (T)	Real Area (%)	Assignment
c-FePc	Singlet 1	0.05	—	—	8.7	γ-Fe
	Doublet 1	0.26	3.52	—	2.6	Fe^IIN₄/C, medium spin
	Doublet 2	0.51	0.43	—	3.3	Fe^IIN₄/C, low spin
	Sextet 1	0.46	-0.12	49.692	9.3	Fe₃O₄
	Sextet 2	0.59	-0.32	45.319	2.3	Fe₃O₄
	Sextet 3	0.13	-0.05	33.061	7.0	α-Fe
	Sextet 4	0.34	-0.02	20.414	66.8	Fe₃C
c-(FePc+Pc+ZnCl₂)	Doublet 1	0.42	3.32	—	32.9	Fe^IIN₄/C, medium spin
	Doublet 2	0.35	0.89	—	52.3	Fe^IIN₄/C, low spin
	Doublet 3	0.52	1.93	—	14.9	Fe^IIN₂₊₂/C, high spin

Fig. 5. CV curves (a), ORR polarization curves (b) and half-wave potential (E1/2) and kinetic current density (jk) (c) at 0.9 V (vs. RHE) for c-FePc, c-(FePc+Pc), c-(FePc+Pc+ZnCl2) and Pt/C. Electron transfer number (n) and H2O2 yield (d), methanol tolerance (e) and durability test (f) at 0.70 V (vs. RHE) for c-(FePc+Pc+ZnCl2) and 20 wt% Pt/C.

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错位堆叠限域和微孔缺陷固定协同生长高密度原子级Fe^II-N₄氧还原活性位点

Synergy of staggered stacking confinement and microporous defect fixation for high-density atomic Fe^II-N₄ oxygen reduction active sites

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