碳辅助金属配合物热解法制备高含量Fe-N4单原子催化剂用于氧还原反应

doi:10.1016/S1872-2067(20)63689-0

催化学报 ›› 2021, Vol. 42 ›› Issue (5): 753-761.DOI: 10.1016/S1872-2067(20)63689-0

碳辅助金属配合物热解法制备高含量Fe-N₄单原子催化剂用于氧还原反应

蒋军生^a, 韦何磊^a, 谭爱东^a, 司锐^b, 张伟德^a, 余宇翔^a^,^*()

^a华南理工大学化学与化工学院, 广东广州510641
^b中国科学院上海应用研究所, 上海同步辐射光源, 上海201204

收稿日期:2020-04-19 接受日期:2020-04-19 出版日期:2021-05-18 发布日期:2021-01-29
通讯作者: 余宇翔
基金资助:
广东省自然科学基金(2018A0303130101)

Fabricating high-loading Fe-N₄ single-atom catalysts for oxygen reduction reaction by carbon-assisted pyrolysis of metal complexes

Jun-Sheng Jiang^a, He-Lei Wei^a, Ai-Dong Tan^a, Rui Si^b, Wei-De Zhang^a, Yu-Xiang Yu^a^,^*()

^aSchool of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou 510641, Guangdong, China
^bShanghai Synchrotron Radiation Facility, Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201204, China

Received:2020-04-19 Accepted:2020-04-19 Online:2021-05-18 Published:2021-01-29
Contact: Yu-Xiang Yu
About author:^* E-mail: yuyx@scut.edu.cn
Supported by:
Natural Science Foundation of Guangdong province, China(2018A0303130101)

摘要/Abstract

摘要：

单原子催化剂凭借其超高的原子利用率及在某些反应中表现出的出色催化效果, 被认为是最有前途的电催化剂之一, 引起了研究人员的极大热情和兴趣. 制备高金属含量的单原子催化剂是基础研究和实际应用的前提和关键. 然而, 由于原子表面自由能随着尺寸的减小而急剧增加, 在制备和催化过程中, 单原子催化剂的金属原子很容易聚集成团簇甚至颗粒, 因此如何制备高负载量的单原子催化剂仍然是一个不小的挑战. 在众多单原子催化剂中, 非贵金属中铁基单原子被认为是燃料电池中的Pt催化剂的有效替代品. 在燃料电池的核心反应-电化学氧还原反应中, Fe-N_x被证明是铁单原子催化剂中的主要活性中心. 因此, 为了获得更好的氧还原性能, 提高铁单原子催化剂中Fe-N_x的含量就显得非常关键. 前期已报道了一些关于制备高Fe含量的铁单原子催化剂材料的策略, 例如空间限域策略和配位合成策略. 其中卟啉和葡萄糖作为配位剂, 双氰胺和三聚氰胺可热解成氮掺杂碳材料以捕获金属原子, 形成M-N_x. 同时, 具有高比表面积的富氧碳载体可以通过掺杂氮来作为固定金属原子的位点.

我们开发了一种简单直接的方法, 通过碳辅助金属配合物热解法制备高金属含量的Fe-N₄单原子催化剂, 即在最佳碳化温度800 °C、三聚氰胺存在下对氮掺杂多孔碳辅助分散铁邻苯二胺配合物进行热解. 在该方法中, 氮掺杂多孔碳是一种具有丰富氮缺陷, 高表面积(1267 m²·g^-1)和良好分散性的多孔生物质碳材料. 邻苯二胺作为含两个氨基的二齿配体, 可以很容易地与过渡金属配位, 形成稳定的平面四配位络合物. 此外, 由于在高温条件下过渡金属的催化作用, 邻苯二胺也被用作氮掺杂碳的前体. 因此, 氮掺杂多孔碳和邻苯二胺是合成高金属含量铁单原子催化剂的关键前驱体. 通过X射线光电子能谱, 大角度环形暗场扫描透射电子显微镜和X射线吸收精细结构光谱表征, 发现所制备的铁单原子催化剂中铁原子以单个原子的形式锚固在碳载体上, 并与碳基质的四个掺杂氮原子配位, 得到Fe-N₄的构型. 通过调节Fe前驱体量, 铁单原子催化剂中Fe的最高负载量达到7.5 wt%, 在目前已经报道的铁单原子催化剂中排第四.

电化学氧还原测试表明, 在0.10 M KOH溶液中, 随着铁含量的增加, 铁单原子催化剂的氧还原性能逐渐提高. 其中250Fe-SA/NPC-800样品表现出最高起始电位0.97 V和最正的半波电位0.85 V, 可与市售的40% Pt/C催化剂相媲美. 和已报道的铁单原子催化剂相比, 由于我们制得的催化剂的比表面积较低, 只有247 m²·g^-1, 所以制约了催化剂的性能. 在混合动力学势域中, 根据Koutecky-Levich方程计算得出的电子转移数约为3.6, 表明250Fe-SA/NPC-800主要催化四电子转移过程, 这可以归因于以Fe-N₄活性中心降低了四电子过程中关键中间体的形成能垒及过程的自由能变化. 此外, 250Fe-SA/NPC-800展现了较高的电化学稳定性. 连续工作6 h后, 250Fe-SA/NPC-800保留了超过87%的电流密度, 而Pt/C表现出明显的衰减, 仅保留了49%.

关键词: Fe-N₄单原子催化剂, 氧还原反应, 高含量, 配位效应, 四电子转移过程

Abstract:

Iron-based single-atom catalysts with nitrogen-doped carbon as support (Fe-SA/NPC) are considered effective alternatives to replace Pt-group metals for scalable application in fuel cells. However, synthesizing high-loading Fe-SA catalysts by a simple procedure remains challenging. Herein, we report a high-loading (7.5 wt%) Fe-SA/NPC catalyst prepared by carbon-assisted pyrolysis of metal complexes. Both the nitrogen-doped porous carbon (NPC) support with high specific surface area and ο-phenylenediamine (o-PD) play key roles role in the preparation of high-loading Fe-SA/NPC catalysts. The results of X-ray photoelectron spectroscopy, high-angle annular dark-field scanning transmission electron microscopy, and X-ray absorption fine structure spectroscopy experiments show that the Fe atoms are anchored on the carbon carriers in a single-atom site configuration and coordinated with four of the doped nitrogen atoms of the carbon substrates (Fe-N₄). The activities of the Fe-SA/NPC catalysts in the oxygen reduction reaction increased with increasing iron loading. The optimized 250Fe-SA/NPC-800 catalyst exhibited an onset potential 0.97 V of and a half-wave potential of 0.85 V. Our study provides a simple approach for the large-scale synthesis of high-loading single-atom catalysts.

Key words: Fe-N₄ single-atom catalysts, Oxygen reduction reaction, High-loading, Coordinated effect, Four-electron transfer process

蒋军生, 韦何磊, 谭爱东, 司锐, 张伟德, 余宇翔. 碳辅助金属配合物热解法制备高含量Fe-N₄单原子催化剂用于氧还原反应[J]. 催化学报, 2021, 42(5): 753-761.

Jun-Sheng Jiang, He-Lei Wei, Ai-Dong Tan, Rui Si, Wei-De Zhang, Yu-Xiang Yu. Fabricating high-loading Fe-N₄ single-atom catalysts for oxygen reduction reaction by carbon-assisted pyrolysis of metal complexes[J]. Chinese Journal of Catalysis, 2021, 42(5): 753-761.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(20)63689-0

https://www.cjcatal.com/CN/Y2021/V42/I5/753

图/表 11

Scheme 1. Schematic illustration of the formation of xFe-SA/NPC-T samples; yellow and blue-grey balls represent melamine and the Fe-o-PD complex, respectively.

Fig. 1. XRD patterns (A) and Raman spectra (B) of NPC, xFe-SA/NPC-800, and 375Fe-NP/NPC-800 samples.

Fig. 2. Morphology characterization of 250Fe-SA/NPC-800 sample. (A) SEM image; (B) TEM image; (C) High-resolution AC-HAADF-STEM image; (D) Low-resolution AC-HAADF-STEM image with corresponding EDX mapping.

Fig. 3. XPS spectra of 250Fe-SA/NPC-800. (A) XPS survey spectrum; (B) High-resolution C 1s spectrum; (C) High-resolution N 1s spectrum; (D) High-resolution Fe 2p spectrum.

Fig. 4. XAFS profiles of 250Fe-SA/NPC-800 catalyst. (A) Fe K-edge XANES profiles of 250Fe-SA/NPC-800 catalyst and reference samples; (B) Corresponding EXAFS fitting curves in R-space, with the inset showing a schematic model.

Fig. 5. ORR performance. (A) RDE polarization curves of the samples; (B) Onset and half-wave potentials of the samples (a = NPC, b = 100Fe-SA/NPC-800, c: 175Fe-SA/NPC-800, d: 250Fe-SA/NPC-800, e: 375Fe-NP/NPC-800); (C) LSV polarization curves of 250Fe-SA/NPC-800 with different rotation speeds (400-2025 rpm); (D) K-L plots of 250Fe-SA/NPC-800.

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碳辅助金属配合物热解法制备高含量Fe-N₄单原子催化剂用于氧还原反应

Fabricating high-loading Fe-N₄ single-atom catalysts for oxygen reduction reaction by carbon-assisted pyrolysis of metal complexes

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