Sn电子调节器增强Fe位点电催化CO2还原性能

doi:10.1016/S1872-2067(24)60269-X

催化学报 ›› 2025, Vol. 72: 222-229.DOI: 10.1016/S1872-2067(24)60269-X

Sn电子调节器增强Fe位点电催化CO₂还原性能

胡呈弘^,¹, 张悦^,¹, 张仪, 黄沁彤, 沈葵, 陈立宇^*(), 李映伟^*()

华南理工大学化学化工学院, 广东省燃料电池技术重点实验室, 广东广州 510640

收稿日期:2024-11-30 接受日期:2025-01-14 出版日期:2025-05-18 发布日期:2025-05-20
通讯作者: *电子信箱: liyuchen@scut.edu.cn (陈立宇),liyw@scut.edu.cn (李映伟).
作者简介:¹共同第一作者.
基金资助:
国家自然科学基金(22138003);国家自然科学基金(22378136);国家自然科学基金(22422806);国家自然科学基金(22108083);国家自然科学基金(21825802);广东省珠江人才计划(2021QN02C847);广东省珠江人才计划(2021ZT09Z109);广东省自然科学基金(2024A1515011196);广东省自然科学基金(2023A1515010312);广东省自然科学基金(2023B1515040005);中央高校基本科研业务费(2024ZYGXZR011);广州市科技计划(2025A04J5244);制浆造纸工程国家重点实验室(2022C04);制浆造纸工程国家重点实验室(2022ZD05);制浆造纸工程国家重点实验室(2023PY06);制浆造纸工程国家重点实验室(2024ZD09);TCL青年学者项目

Single-atomic Fe sites modulated by Sn regulator for enhanced electrochemical CO₂ reduction

Chenghong Hu^,¹, Yue Zhang^,¹, Yi Zhang, Qintong Huang, Kui Shen, Liyu Chen^*(), Yingwei Li^*()

Guangdong Provincial Key Laboratory of Fuel Cell Technology, School of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou 510640, Guangdong, China

Received:2024-11-30 Accepted:2025-01-14 Online:2025-05-18 Published:2025-05-20
Contact: *E-mail: liyuchen@scut.edu.cn (L. Chen), liyw@scut.edu.cn (Y. Li).
About author:¹ Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22138003);National Natural Science Foundation of China(22378136);National Natural Science Foundation of China(22422806);National Natural Science Foundation of China(22108083);National Natural Science Foundation of China(21825802);Guangdong Pearl River Talents Program(2021QN02C847);Guangdong Pearl River Talents Program(2021ZT09Z109);Natural Science Foundation of Guangdong Province(2024A1515011196);Natural Science Foundation of Guangdong Province(2023A1515010312);Natural Science Foundation of Guangdong Province(2023B1515040005);Fundamental Research Funds for the Central Universities(2024ZYGXZR011);Science and Technology Program of Guangzhou(2025A04J5244);State Key Laboratory of Pulp and Paper Engineering(2022C04);State Key Laboratory of Pulp and Paper Engineering(2022ZD05);State Key Laboratory of Pulp and Paper Engineering(2023PY06);State Key Laboratory of Pulp and Paper Engineering(2024ZD09);TCL Young Talent Program

摘要/Abstract

摘要：

由可再生能源驱动的电催化二氧化碳还原反应(CO₂RR)可利用温室气体CO₂来制备高附加值产品. CO₂RR制CO选择性高, 且产物易于从电解质中分离, 具有良好的工业应用前景. 目前, CO₂RR制备CO的高活性催化剂主要为Au, Pd和Ag等贵金属材料, 限制了其商业化应用. 过渡金属基单原子催化剂(SACs)具有高原子利用率、可调的配位环境和精确的活性位点, 在CO₂RR中具有巨大潜力. 其中, Fe基SACs表现出类似贵金属的电子性质, 具有较高的CO₂RR制CO效率, 有望成为贵金属催化剂的替代材料. 然而, 在CO₂制CO过程中, Fe位点与*CO吸附较强, 不利于*CO的脱附, 导致Fe基SACs的CO₂RR活性仍无法媲美贵金属. 前期报道通过引入S和P等杂原子或过渡金属位点来调控Fe的电子结构, 降低*CO结合强度, 但这些调节剂对H也具有较强亲和力, 易诱发析氢副反应, 降低了CO₂RR的法拉第效率. 因此, 开发有效的策略来提高Fe基SACs的本征活性和选择性仍然是一个挑战.

本文构建了一种N掺杂碳负载的主族Sn和过渡金属Fe组成的双原子催化剂(Fe-Sn/NC), 利用析氢惰性的Sn位点调控活性中心Fe的电子结构, 以提高CO₂RR制CO性能. 首先, 采用浸渍法将Fe³⁺和Sn⁴⁺离子吸附于ZIF-8内. 随后, 在惰性气体中进行高温煅烧, 得到Fe-Sn/NC催化剂. 透射电镜结果证实Fe-Sn/NC中Fe和Sn以原子形式分散在NC基底上, 不存在团聚的金属颗粒. X射线光电子能谱和X射线吸收谱结果表明, Fe和Sn分别与三个N原子相连, 并形成了Fe-Sn键. Sn位点向Fe转移电子, 形成富电荷的Fe中心. 差分电荷图显示Sn位点的引入有效打破了FeN₄位点的电荷对称性, 态密度图表明Sn可以调节Fe位点的d带中心, 使其远离费米能级. 自由能垒计算结果表明, 上述电子调控机制有效地削弱了*CO在Fe位点上的吸附, 降低了CO₂向CO转化的反应能垒. 将Fe-Sn/NC在CO₂饱和的0.1 mol L⁻¹ KHCO₃溶液中进行性能测试, 结果表明, 在−0.5 V (相对于可逆氢电极)下的CO法拉第效率(FE_CO)达到98.6%, 并在−0.4到−0.9 V的宽电位范围内FE_CO保持在90%以上. Fe-Sn/NC在−0.9 V的转化频率值为1.5 × 10⁴ h⁻¹, 远高于Fe/NC材料. 此外, 为降低CO₂RR体系的能耗, 采用肼氧化反应(HzOR)替代热力学不利的阳极析氧反应(OER), 并利用Fe-Sn/NC作为正极和负极组建了CO₂RR//HzOR电解系统. 结果表明, 与传统CO₂RR//OER系统相比, CO₂RR//HzOR系统在5 mA cm⁻²时的电池电压降低了0.64 V, 理论上节省了38%的能量.

综上, 本工作提出了利用主族元素调节器调控Fe单原子电子结构的新思路, 通过弱化*CO在Fe位点上的吸附, 提升Fe单原子的CO₂RR性能, 揭示了主族金属调节器增强Fe基SAC性能的作用规律, 为具有成本效益的非贵金属基催化剂的设计和开发提供了新思路.

关键词: 单原子催化剂, 电催化CO₂还原, 电子结构调控, 双原子对, 主族金属

Abstract:

Single-atom Fe catalysts show significant promise in the electrocatalytic reduction of CO₂ (CO₂RR), while their performance remains inferior to that of precious metal catalysts due to the overly strong binding of *CO intermediates. Although the introduction of heteroatoms or transition metal sites can modulate the binding strength of *CO on Fe sites, these regulators often induce competitive hydrogen evolution reaction (HER) with reduced Faraday efficiency (FE). In this work, we employ HER-inert Sn as a regulator to tune the electronic structure of Fe, weakening *CO adsorption and enhancing CO₂RR performance. Diatomic Fe-Sn pairs supported on N-doped carbon (Fe-Sn/NC) were synthesized, achieving FE for CO exceeding 90% over a broad potential range from −0.4 to −0.9 V versus the reversible hydrogen electrode. Fe-Sn/NC shows a high turnover frequency of 1.5 × 10⁴ h⁻¹, much higher than that of Fe/NC. Characterization results and theoretical calculations demonstrate that bonding Sn site to Fe generates electron-rich Fe centers, effectively reducing the adsorption strength of *CO without triggering HER. Additionally, Fe-Sn/NC exhibits exceptional activity in hydrazine oxidation performance (HzOR). The HzOR-assisted CO₂RR system using Fe-Sn/NC as electrodes reduces energy consumption by 38% compared with the conventional CO₂RR coupled oxygen evolution reaction system.

Key words: Atomically dispersed catalyst, Electrochemical CO₂ reduction, Electronic modification, Diatomic pairs, Main-group element

胡呈弘, 张悦, 张仪, 黄沁彤, 沈葵, 陈立宇, 李映伟. Sn电子调节器增强Fe位点电催化CO₂还原性能[J]. 催化学报, 2025, 72: 222-229.

Chenghong Hu, Yue Zhang, Yi Zhang, Qintong Huang, Kui Shen, Liyu Chen, Yingwei Li. Single-atomic Fe sites modulated by Sn regulator for enhanced electrochemical CO₂ reduction[J]. Chinese Journal of Catalysis, 2025, 72: 222-229.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60269-X

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图/表 5

Fig. 1. (a) Schematic representation of the fabrication of Fe-Sn/NC. (b) SEM image of Fe-Sn/ZIF-8. SEM (c) and TEM (d) images of Fe-Sn/NC. (e) Aberration-corrected HAADF-STEM image of Fe-Sn/NC. (f) Line-scanning intensity profiles obtained from regions 1 and 2 highlighted in (e). (g) HAADF-STEM image and corresponding EDS element mappings of Fe-Sn/NC.

Fig. 2. High-resolution XPS spectra of Fe 2p for Fe/NC and Fe-Sn/NC (a), Sn 3d for Sn/NC and Fe-Sn/NC (b), and N 1s for Fe-Sn/NC (c). XANES spectra (d) and FT- EXAFS spectra (e) of the Fe K-edge for Fe foil, FePc, Fe2O3, FeO, and Fe-Sn/NC. (f) FT-EXAFS fitting of Fe K-edge for Fe-Sn/NC with the proposed structural model inset (Grey: C, blue: N, wine red: Fe, cyan: Sn). XANES spectra (g) and FT-EXAFS spectra (h) of the Sn K-edge for Sn foil, SnO2, and Fe-Sn/NC. (i) FT-EXAFS fitting curves of Sn K-edge for Fe-Sn/NC.

Fig. 3. Electrochemical tests in CO2-saturated 0.1 mol L-1 KHCO3 aqueous solution. LSV curves (a), FECO (b), jCO (c), TOF (d), and Tafel slope (e) of Fe-Sn/NC, Fe/NC, Sn/NC, and NC. (f) Stability test of Fe-Sn/NC at ?0.5 V (vs. RHE).

Fig. 4. (a) Free energy diagrams for CO2RR over various catalyst models. (b) Limiting potential differences for CO2RR and HER on various active moieties. The charge density difference of Fe/NC (c) and Fe-Sn/NC (d) models (yellow and cyan represent electron accumulation and depletion, respectively). Projected DOS for Fe/NC (e) and Fe-Sn/NC (f) with *CO adsorption.

Fig. 5. (a) CV curve of Fe-Sn/NC in 1 mol L-1 KOH with 0.1 mol L-1 N2H4. (b) Schematic diagram of CO2RR//HzOR electrolyzer. (c) Polarization curves for CO2RR//HzOR and CO2RR//OER systems. (d) Chronoamperometry measurement of Fe-Sn/NC as both anode and cathode at ?1.0 V, and the corresponding FEco.

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Sn电子调节器增强Fe位点电催化CO₂还原性能

Single-atomic Fe sites modulated by Sn regulator for enhanced electrochemical CO₂ reduction

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