氮掺杂多孔碳负载Fe纳米颗粒用于高性能电催化还原CO2与Zn-CO2电池

doi:10.1016/S1872-2067(23)64415-8

催化学报 ›› 2023, Vol. 48: 185-194.DOI: 10.1016/S1872-2067(23)64415-8

氮掺杂多孔碳负载Fe纳米颗粒用于高性能电催化还原CO₂与Zn-CO₂电池

杨文倩^a^,¹, 薛自前^b^,¹, 杨俊^a, 冼家慧^a, 刘庆林^a, 范雅楠^a, 郑凯^a, 廖锫钦^a, 苏徽^c, 刘庆华^c, 李光琴^a^,^*(), 苏成勇^a^,^*()

^a中山大学化学学院, 莱恩功能材料研究所, 光电材料与技术国家重点实验室, 教育部生物无机与合成化学实验室, 广东广州510006, 中国
^b京都大学综合细胞材料科学研究所, 京都大学高级研究所, 京都, 日本
^c中国科学技术大学国家同步辐射实验室, 安徽合肥230026, 中国

收稿日期:2022-11-29 接受日期:2023-02-01 出版日期:2023-05-18 发布日期:2023-04-20
通讯作者: * 电子信箱: liguangqin@mail.sysu.edu (李光琴), cncesscy@mail.sysu.edu.cn (苏成勇).
作者简介:第一联系人：
¹共同第一作者
基金资助:
国家重点研发计划(2021YFA1500401);广东省珠江人才计划引进创新团队(2017ZT07C069);广东省珠江人才计划本土创新团队(2017BT01C161);国家自然科学基金(22075321);国家自然科学基金(21821003);国家自然科学基金(21890380)

Fe nanoparticles embedded in N-doped porous carbon for enhanced electrocatalytic CO₂ reduction and Zn-CO₂ battery

Wenqian Yang^a^,¹, Ziqian Xue^b^,¹, Jun Yang^a, Jiahui Xian^a, Qinglin Liu^a, Yanan Fan^a, Kai Zheng^a, Peiqin Liao^a, Hui Su^c, Qinghua Liu^c, Guangqin Li^a^,^*(), Cheng-Yong Su^a^,^*()

^aState Key Laboratory of Optoelectronic Materials and Technologies, MOE Laboratory of Bioinorganic and Synthetic Chemistry, Lehn Institute of Functional Materials, School of Chemistry, Sun Yat-Sen University, Guangzhou 510006, Guangdong, China
^bInstitute for Integrated Cell-Material Sciences, Kyoto University, Institute for Advanced Study, Kyoto University, Yoshida, Ushinomiya-cho, Sakyo-ku, Kyoto 606-8501, Japan
^cNational Synchrotron Radiation Laboratory, University of Science and Technology of China, Hefei 230026, Anhui, China

Received:2022-11-29 Accepted:2023-02-01 Online:2023-05-18 Published:2023-04-20
Contact: * E-mail: liguangqin@mail.sysu.edu.cn (G. Li), cesscy@mail.sysu.edu.cn (C.-Y. Su).
About author:First author contact:
¹Contributed equally to this work.
Supported by:
National Key R&D Program of China(2021YFA1500401);Program for Guangdong Introducing Innovative and Entrepreneurial Teams(2017ZT07C069);Local Innovative and Research Teams Project of Guangdong Peal River Talents Program(2017BT01C161);National Natural Science Foundation of China(22075321);National Natural Science Foundation of China(21821003);National Natural Science Foundation of China(21890380)

摘要/Abstract

摘要：

电催化CO₂还原为CO因其技术与经济上的可行性而被认为是推进碳中和最有前景的反应之一. 然而, 水溶液中激烈的竞争性析氢反应阻碍生成单一高选择性产物. 目前, 贵金属纳米催化剂表现出较好的CO选择性, 但稀缺性和高成本限制了其进一步应用. Fe纳米颗粒(NPs)具有电催化活性, 且储量丰富成本低, 被认为是一种潜在可替代贵金属的电催化剂, 但Fe存在易氧化、团聚、稳定性差、吸附CO₂能力低等问题. 因此, 探索同时具有良好活性和稳定性的新型Fe NPs催化剂仍具有重要意义. 金属-有机骨架(MOFs)衍生物被认为是合成锚定和激活金属纳米颗粒的良好前驱体. 因此, 将Fe NPs固定在MOFs衍生物中为开发稳定、高活性的Fe NPs催化剂提供了可行的机会.
本文通过修饰MOFs前驱体的策略, 对IRMOF-3(Zn)进行少量含铁配体单羧酸二茂铁的取代, 结合一步热解碳化, 制备了Fe NPs负载在海绵状氮掺杂多孔碳的复合催化剂(Fe@NPC). 同时对配体为对苯二甲酸的MOF-5和配体为2-氨基-对苯二甲酸的IRMOF-3(Zn)进行热解碳化, 制备了对照样品多孔碳MOF-5-D和氮掺杂多孔碳IRMOF-3-D. 光电子能谱(XPS)和X射线吸收精细结构谱(XAFS)结果表明, 在Fe@NPC中含有大量的Fe-Fe键以及极少量的Fe-N/C键, 说明Fe主要以纳米颗粒形式存在, 少量Fe-N/C分布在Fe NPs表面, 在Fe NPs与氮掺杂碳基底间起到良好的连接作用. 此外, Fe@NPC具有较大的比表面积(1264 m² g^-1)和高于MOF-5-D与IRMOF-3-D的CO₂吸附能力(93.5 cm³ g^-1), 这种具有CO₂强吸附和丰富活性位点的多级孔结构为加速传质、加快CO₂转化奠定了良好的基础.
在H-cell与-0.6 V_RHE的条件下, IRMOF-3-D的最大CO法拉第效率(FE_CO)为65.3%, 是MOF-5-D(49.9%)的1.3倍, 说明氮掺杂在一定程度上促进了CO₂的电还原. 此外, Fe@NPC在-0.3 V_RHE到-1.0 V_RHE的宽电位化学区间均表现出较好的性能, 即最大的电流密度, 最低的起始电位以及92.1%的最高的FE_CO. 而且Fe@NPC在流动池中可以获得更高的FE_CO(96.4%), 同时能够在H-cell与流动池中均保持良好的稳定性. 由于*COOH高能垒, 它的产生被认为是高效电化学CO₂-CO转换的瓶颈. 进一步采用原位衰减全反射-傅里叶变换红外(ATR-IR)来实时监测中间体, 并深入探究Fe@NPC作用于CO₂还原过程的机理, 观测到中间体*COOH的逐渐形成和积累, 以及同一反应时间内*COOH在Fe@NPC上的更快动力学形成过程; 进一步说明Fe位点与氮掺杂多孔碳之间的协同作用显著提高了Fe@NPC的CO₂的捕获能力和传质能力并加速了CO生成的动力学.
本文以Fe@NPC为阴极组装了Zn-CO₂电池, 发现该电池具有良好的充电放电性能, 放电过程中可提供3.0 mW cm^-2的峰值功率密度, 同时表现出良好的稳定性(120个循环), 实现CO₂电还原与储能的良好结合, 并表现出高效的能量转换装置的良好应用潜力. 综上, 本文为设计用于高选择性的CO₂还原反应和能量转换器件的铁基催化剂提供了一种新方法.

关键词: Fe纳米颗粒, MOFs衍生物, 氮掺杂多孔碳, CO₂电催化, Zn-CO₂电池

Abstract:

The selective electrochemical reduction of CO₂ to CO is a promising solution for the design of carbon-neutral, sustainable processes. Achieving a highly selective single reduction product is still challenging because of the energetically favorable competing hydrogen evolution reaction. We report the fabrication of N-doped sponge-like porous graphitic carbon structures embedded with Fe nanoparticles (Fe@NPC) via the pre-modification of a metal-organic framework (IRMOF-3(Zn)) with carboxyferrocene, followed by pyrolysis. The as-prepared Fe@NPC exhibited a 96.4% CO Faradaic efficiency at -0.5 V_RHE and good stability. The exceptional CO₂ reduction performance is attributed to the unique structure of the composite catalyst, which provides abundant hierarchical pores that increase CO₂ adsorption and mass transfer, and active Fe sites that synergistically accelerate the kinetics of CO generation. The in situ attenuated total reflectance-Fourier transform infrared analysis provided proof of the improved ability of Fe@NPC to accumulate the crucial intermediate *COOH compared with other pyrolyzed porous carbons. Fe@NPC was used in a Zn-CO₂ battery that delivered a maximum power density of 3.0 mW cm^-2, evidencing its potential for application in energy-converting devices.

Key words: Fe nanoparticles, Metal organic frameworks, N-doped porous carbon, CO₂ electroreduction, Zn-CO₂ battery

杨文倩, 薛自前, 杨俊, 冼家慧, 刘庆林, 范雅楠, 郑凯, 廖锫钦, 苏徽, 刘庆华, 李光琴, 苏成勇. 氮掺杂多孔碳负载Fe纳米颗粒用于高性能电催化还原CO₂与Zn-CO₂电池[J]. 催化学报, 2023, 48: 185-194.

Wenqian Yang, Ziqian Xue, Jun Yang, Jiahui Xian, Qinglin Liu, Yanan Fan, Kai Zheng, Peiqin Liao, Hui Su, Qinghua Liu, Guangqin Li, Cheng-Yong Su. Fe nanoparticles embedded in N-doped porous carbon for enhanced electrocatalytic CO₂ reduction and Zn-CO₂ battery[J]. Chinese Journal of Catalysis, 2023, 48: 185-194.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(23)64415-8

https://www.cjcatal.com/CN/Y2023/V48/I5/185

图/表 5

Fig. 1. (a) Schematic representation of the Fe@NPC preparation. SEM (b), TEM (c), HRTEM (d) images over Fe@NPC.

Fig. 2. High-resolution XPS N 1s spectra (a) and EPR spectra (b) of Fe@NPC and control samples. (c) Fe K-edge XANES spectra. (d) FT-EXAFS spectra of R space of Fe@NPC, Fe2O3, and Fe foil.

Fig. 3. LSV tests (a), FEco (b), and JCO (c) for different catalysts in the H-cell. FEs (d) and partial current densities (e) of reduction products using Fe@NPC in a GDE cell. (f) Stability of Fe@NPC in the flow cell.

Fig. 4. In situ ATR-FTIR spectra (a) and color contour map (b) of Fe@NPC collected at -0.6 VRHE using CO2-saturated 0.5 mol L-1 KHCO3 as electrolyte. (c) Proposed pathway for CO2 electroreduction using Fe@NPC.

Fig. 5. (a) Schematic configuration of ZCB with Fe@NPC cathode. (b) Photograph of a LED (~2.2 V) powered by Fe@NPC. (c) Polarization plot and power density. (d) Galvano-static discharge curve and corresponding FECO. (e) Galvanostatic discharge-charge cycling plots for 120 cycles of Fe@NPC.

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氮掺杂多孔碳负载Fe纳米颗粒用于高性能电催化还原CO₂与Zn-CO₂电池

Fe nanoparticles embedded in N-doped porous carbon for enhanced electrocatalytic CO₂ reduction and Zn-CO₂ battery

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