酞菁镍分子结构的精确设计: 优化电子和空间效应用于CO2电还原

doi:10.1016/S1872-2067(23)64412-2

催化学报 ›› 2023, Vol. 48: 117-126.DOI: 10.1016/S1872-2067(23)64412-2

酞菁镍分子结构的精确设计: 优化电子和空间效应用于CO₂电还原

李静静^a^,¹, 张锋伟^a^,^*^,¹(), 詹新雨^b^,¹, 郭河芳^a, 张涵^a, 昝文艳^a^,^*(), 孙振宇^b^,^*(), 张献明^a^,^c^,^*()

^a山西大学晶态材料研究所, 分子科学研究所, 山西太原030006
^b北京化工大学有机无机复合材料国家重点实验室, 北京100029
^c太原理工大学化学学院, 新材料界面科学与工程教育部重点实验室, 山西太原030024

收稿日期:2022-10-31 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: fwzhang@sxu.edu.cn (张锋伟),zanwy@sxu.edu.cn (昝文艳),zhangxianming@tyut.edu.cn (张献明),sunzy@mail.buct.edu.cn (孙振宇).
作者简介:¹共同第一作者
基金资助:
国家自然科学基金(22272095);国家自然科学基金(21972010);山西省自然科学研究基金(20210302123434);山西省省筹资金资助回国留学人员科研项目(2022-003);煤转化国家重点实验室开放课题基金(J22-23-604)

Precise design of nickel phthalocyanine molecular structure: Optimizing electronic and spatial effects for remarkable electrocatalytic CO₂ reduction

Jingjing Li^a^,¹, Fengwei Zhang^a^,^*^,¹(), Xinyu Zhan^b^,¹, Hefang Guo^a, Han Zhang^a, Wen-Yan Zan^a^,^*(), Zhenyu Sun^b^,^*(), Xian-Ming Zhang^a^,^c^,^*()

^aInstitute of Crystalline Materials, Institute of Molecular Science, Shanxi University, Taiyuan 030006, Shanxi, China
^bState Key Laboratory of Organic-Inorganic Composites, Beijing University of Chemical Technology, Beijing 100029, China
^cCollege of Chemistry, Key Laboratory of Interface Science and Engineering in Advanced Material, Taiyuan University of Technology, Taiyuan 030024, Shanxi, China

Received:2022-10-31 Accepted:2023-02-01 Online:2023-05-18 Published:2023-04-20
Contact: * E-mail: fwzhang@sxu.edu.cn (F. Zhang),zanwy@sxu.edu.cn (W.-Y. Zan),zhangxianming@tyut.edu.cn (X.-M. Zhang),sunzy@mail.buct.edu.cn (Z. Sun).
About author:¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22272095);National Natural Science Foundation of China(21972010);Natural Science Research Foundation of Shanxi Province(20210302123434);Shanxi Scholarship Council of China(2022-003);Foundation of State Key Laboratory of Coal Conversion(J22-23-604)

摘要/Abstract

摘要：

大气中CO₂浓度的快速增加对气候变化和人类生存环境造成严重威胁, 亟需开发新的方法与技术来捕获CO₂并将其转化为高附加值产品. 传统的热催化技术通过选择性加氢和环加成等技术路线可将CO₂转化为低碳烷烃、醇类和碳酸二甲酯等化工品. 与之相比, 洁净的催化技术如CO₂电还原(CO₂RR)具有反应条件温和、操作简单、能量利用率高和产品类型可控等特点而备受关注. 将CO₂电还原为各种气体或液体产物是CO₂转化的理想策略, 具有广阔的应用前景. 然而, 实现CO₂的高效电还原需要克服以下瓶颈, 包括CO₂还原的电位过高、产物选择性差和竞争性析氢反应严重等问题. 为了在低过电位、高选择性、高稳定性和大电流密度下进行CO₂RR, 人们研究了不同类型的杂化纳米催化剂, 包括无金属碳材料, 金属/金属氧化物和金属硫化物电催化剂等. 最近研究人员报道了CoPc(NH₂)₄和CoPc(CN)₈分子催化剂并应用于CO₂RR, 但缺乏对取代基的位阻分布和电子推拉效应对CO₂RR性能影响的相关研究. 因此, 开发具有特定官能团取代基和明确结构的新型分子基催化剂, 进而深入研究其对CO₂RR的影响显得极为重要.
本文通过两步合成策略构建了一系列具有不同官能团和位置取代的酞菁镍(NiPc)分子衍生物(α-NO₂, α-NH₂, β-NO₂和β-NH₂). 将这些NiPc分子衍生物通过简单的机械混合固定在氧化碳纳米管(CNTs)表面, 得到分子级分散的电催化剂(MDEs). 深入探讨了NiPc基分子催化剂的几何效应和电子效应对CO₂RR催化性能的影响规律, 从根本上了解CO₂RR的活化路径、反应机理和构效关系. 结果表明, NiPc(α-NO₂)₄/CNTs催化剂对CO₂RR具有最佳的催化性能, 在相对可逆电压−1.0 V时电流密度为7.01 mA cm⁻²和FE_CO为99%, 在宽电势范围−0.7~−1.2 V, FE_CO超过91.1%, 与密度泛函理论计算结果一致, 表明NiPc(α-NO₂)₄/CNTs吸电子和邻位取代−NO₂是CO₂RR生产CO最合适的催化剂.
通过红外谱图证实了具有不同空间取代基团的NiPc衍生物的成功制备. 透射电镜结果表明, 碳纳米管载体具有均匀的管状结构. 球差电镜显示有大量的亮点, 说明金属Ni以单原子的形式存在, 结合同步辐射结果表明Ni的价态在0和+2之间, 进一步证明Ni物种是原子分散的, 并且与N原子配位. NiPc/CNTs的高分辨率N 1s XPS谱可以分峰为吡啶N(398.5 eV)和Ni−N(399.6 eV). 相比之下, NiPc(α-NO₂)₄/CNTs中的Ni−N(400.9eV)的结合能高于NiPc/CNTs, 而NiPc(α-NH₂)₄/CNTs中的Ni−N(399.4 eV)结合能低于NiPc/CNTs. NiPc/CNTs的Ni 2p XPS谱包括以872.3和854.9 eV为中心的两个峰, 分别对应于Ni 2p_1/2和Ni 2p_3/2. Ni 2p在NiPc(α-NO₂)₄/CNTs (Ni 2p_1/2 873.3 eV和Ni 2p_3/2 855.9 eV)中的结合能高于NiPc/CNTs. 结果表明, 吸电子的−NO₂基团从Ni−N₄活性位点得到电子, 从而使结合能转移到更高的位置. 反之, NiPc(α-NH₂)₄/CNTs (Ni 2p_1/2 872.2 eV和Ni 2p_3/2 854.1 eV)的结合能低于NiPc/CNTs的, 表明供电子基团使结合能向较低的位置移动. 此外, 通过Mulliken电荷分析, 计算了不同NiPc基分子催化剂中Ni原子与邻近原子之间的电荷转移, 与NiPc分子基团的推拉电子效应和外围取代基的空间位置密切相关. 电催化结果表明, NiPc(α-NO₂)₄/CNTs的FE_CO在-1.0 V时最大, 为99.0%, 这与计算结果α-NO₂取代的NiPc可以使*COOH形成的能垒最小, 显著提高了CO₂RR性能结果一致. 综上, 本研究在分子水平上为精准设计和制备具有较好的CO₂RR催化活性和选择性的电催化剂提供参考.

关键词: 二氧化碳还原, 精准设计, 电催化剂, 酞菁镍

Abstract:

The atomic dispersion offered by transition metal-nitrogen-carbon electrocatalysts (M-N-C) represents a promising system for efficient catalysis of the CO₂ reduction reaction (CO₂RR) to a CO product. However, accurate elucidation of the catalytic mechanism of M-N-C catalysts synthesized by pyrolysis is impeded by the ambiguity of the coordination environment of the MN_x active site. Herein, by combining theoretical and experimental methods, the influence of the electronic and geometric effects of the NiN₄ site in a group of nickel phthalocyanine (NiPc)-based molecular catalysts on the performance of CO₂RR are investigated. Density functional theory calculations indicate that only electron-withdrawing and ortho-nitro-substituted NiPc-based molecularly dispersed electrocatalysts can significantly enhance the NiN₄ active site for CO₂ activation. The lowest activation energy is required for forming the *COOH intermediate compared to other reference catalysts. Our modeling is in complete accordance with our experimental results, proving that the position of the substituent groups and push-pull electron effects simultaneously play crucial roles in CO₂RR catalyst performance.

Key words: CO₂ reduction reaction, Precise design, Electrocatalyst, Nickel phthalocyanine

李静静, 张锋伟, 詹新雨, 郭河芳, 张涵, 昝文艳, 孙振宇, 张献明. 酞菁镍分子结构的精确设计: 优化电子和空间效应用于CO₂电还原[J]. 催化学报, 2023, 48: 117-126.

Jingjing Li, Fengwei Zhang, Xinyu Zhan, Hefang Guo, Han Zhang, Wen-Yan Zan, Zhenyu Sun, Xian-Ming Zhang. Precise design of nickel phthalocyanine molecular structure: Optimizing electronic and spatial effects for remarkable electrocatalytic CO₂ reduction[J]. Chinese Journal of Catalysis, 2023, 48: 117-126.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(23)64412-2

https://www.cjcatal.com/CN/Y2023/V48/I5/117

图/表 5

Scheme 1. Schematic of the preparation route for NiPc-based molecularly dispersed electrocatalysts.

Fig. 1. TEM (a), HRTEM (b), HAADF-STEM (c) images, and EDS maps (d) of NiPc(α-NO2)4/CNTs. Ni K-edge XANES spectra (e) and Fourier transformed EXAFS spectra (f) of NiPc(α-NO2)4/CNTs, NiPc(α-NH2)4/CNTs, NiPc/CNTs, standard NiO, and Ni foil.

Fig. 2. High-resolution XPS spectra in N 1s region (a?c) and Ni 2p region (d?f) of NiPc/CNTs, NiPc(α-NO2)4/CNTs, and NiPc(α-NH2)4/CNTs MDEs.

Fig. 3. (a) Linear sweep voltammetry curves of NiPc(α-NO2)4/CNTs and reference catalysts. (b) FECO at different potentials on various catalysts. (c) Product selectivity comparison at ?1.0 V vs. RHE. (d) CO partial current density at various potentials. (e) Electrochemical impedance spectroscopy (EIS) curves with corresponding fitting profiles for NiPc-based MDEs. (f) TOF values of CO2 to CO over various NiPc-based MDEs at different potentials.

Fig. 4. (a) The reaction pathway and free energy diagrams of CO2RR to CO over NiPc-based MDEs. (b) The difference in CO2RR and HER limiting potentials. (c?e) Various DFT optimized intermediates along the CO2RR pathway by NiPc(α-NO2)4/CNTs.

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酞菁镍分子结构的精确设计: 优化电子和空间效应用于CO₂电还原

Precise design of nickel phthalocyanine molecular structure: Optimizing electronic and spatial effects for remarkable electrocatalytic CO₂ reduction

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