具有非对称配位结构的硫族杂原子掺杂Ni-N-C单原子催化剂及其电化学二氧化碳还原性能

doi:10.1016/S1872-2067(24)60103-8

催化学报 ›› 2024, Vol. 64: 54-65.DOI: 10.1016/S1872-2067(24)60103-8

具有非对称配位结构的硫族杂原子掺杂Ni-N-C单原子催化剂及其电化学二氧化碳还原性能

王佳琳^a, 张凯妮^a, Ta Thi Thuy Nga^b, 王亦清^a, 石玉川^a, 魏代星^a, 董崇礼^b, 沈少华^a^,^*()

^a西安交通大学能源与动力工程学院, 陕西西安 710049
^b淡江大学物理系, 台湾新北 25137

收稿日期:2024-05-14 接受日期:2024-06-29 出版日期:2024-09-18 发布日期:2024-09-19
通讯作者: * 电子信箱: shshen_xjtu@mail.xjtu.edu.cn (沈少华).
基金资助:
国家自然科学基金(52225606);国家自然科学基金(52488201)

Chalcogen heteroatoms doped nickel-nitrogen-carbon single-atom catalysts with asymmetric coordination for efficient electrochemical CO₂ reduction

Jialin Wang^a, Kaini Zhang^a, Ta Thi Thuy Nga^b, Yiqing Wang^a, Yuchuan Shi^a, Daixing Wei^a, Chung-Li Dong^b, Shaohua Shen^a^,^*()

^aInternational Research Center for Renewable Energy, State Key Laboratory of Multiphase Flow in Power Engineering, Xi'an Jiaotong University, Xi'an 710049, Shaanxi, China
^bDepartment of Physics, Tamkang University, New Taipei City 25137, Taiwan, China

Received:2024-05-14 Accepted:2024-06-29 Online:2024-09-18 Published:2024-09-19
Contact: * E-mail: shshen_xjtu@mail.xjtu.edu.cn (S. Shen).
Supported by:
National Natural Science Foundation of China(52225606);National Natural Science Foundation of China(52488201)

摘要/Abstract

摘要：

电化学二氧化碳还原反应(eCO₂RR)作为一种能将CO₂转化为高附加值碳基燃料的清洁技术, 对于实现碳中和具有重要意义. 近年来, 过渡金属单原子催化剂(M-N-C SACs)因具备出色的稳定性、活性以及较高的原子利用效率, 已被广泛认为是用于eCO₂RR生产CO中极具潜力的催化剂之一. 其中, 具有饱和对称配位结构的Ni-N₄已被证实是eCO₂RR的活性中心. 然而, Ni-N₄-C SACs中心金属周围对称的几何结构和电子构型导致其在eCO₂RR过程中能垒较高. 同时, 其电催化活性也仍有待提升.

为了调控M-N-C SACs中心金属周围电子排布, 本文分别使用S粉、Se粉和Te粉作为杂原子源, 通过高温焙烧方法将硫族元素(如: S, Se和Te)引入对称的Ni-N₄-C构型中, 获得具有不对称配位环境和电子结构的Ni-X-N₃-C SACs (X: S, Se和Te). 球差电镜结果表明成功合成了Ni-X-N₃-C单原子催化剂, 同步辐射拟合结果证明了SACs中心Ni原子与三个邻近的N原子和一个杂原子(S, Se和Te)成键形成Ni-X-N₃-C配位结构. 此外, X射线光电子能谱结果表明, 随着杂原子(S, Se和Te)的掺杂, Ni 2p轨道结合能逐渐降低, 说明杂原子与金属Ni成键, 导致了中心金属Ni原子周围电荷分布明显变化. 配位原子电负性大小顺序依次为: N > S > Se > Te, 因此Ni 2p轨道的结合能大小趋势为: Ni-N₄-C > Ni-S-N₃-C > Ni-Se-N₃-C > Ni-Te-N₃-C. 同步辐射结果表明, 与具有标准平面4配位(Ni-N₄)的酞菁镍(NiPc)相比, Ni-X-N₃-C SACs (X代表S, Se和Te)中Ni的边前峰强度明显增大, 归因于杂原子的引入导致中心对称结构发生变化. 理论计算结果进一步揭示了杂原子的引入会改变中心金属周围的配位环境, 诱导电荷重分布, 使得Ni原子的d带中心位置更接近费米能级, 增强了*COOH中间体在催化剂表面的吸附强度, 从而提升了eCO₂RR中CO产物选择性. 特别是Se掺杂使得Ni原子的d带中心最接近费米能级, 从而显著降低了*COOH的形成能垒, 增强了eCO₂RR活性. Bader电荷计算结果表明, 与Ni-S和Ni-Te活性位相比, Ni-Se活性位周围具有最多的电荷, 有更强的电子亲和力, 有利于eCO₂RR过程中电子转移. 因此, Se掺杂的Ni-Se-N₃-C在‒0.70 V相对标准氢电极电压下实现了最高98%的CO选择性, 高于Ni-S-N₃-C和Ni-Te-N₃-C. 基于此, 以Ni-Se-N₃-C和Zn箔作为阴极和阳极材料组装的Zn-CO₂电池实现了1.82 mW cm^‒2的峰值功率密度, 并在2 mA cm^‒2电流密度下保持超过20 h的充放电稳定性.

综上所述, 本文通过一种简单通用的浸渍-焙烧-酸刻蚀的方法, 将杂原子(如:S, Se和Te)引入具有对称配位结构的Ni-N₄-C SAC中, 得到具有不对称配位的Ni-X-N₃-C (X代表S, Se和Te) SACs用于高效的eCO₂RR. 本文深入揭示了杂原子掺杂对SACs中心金属原子的配位环境和电子结构的影响作用, 为合理设计具有高活性和选择性的eCO₂RR催化剂提供参考.

关键词: 电化学二氧化碳还原, 硫族杂原子, 单原子催化剂, 不对称配位, CO生成

Abstract:

The electronic configuration of central metal atoms in single-atom catalysts (SACs) is pivotal in electrochemical CO₂ reduction reaction (eCO₂RR). Herein, chalcogen heteroatoms (e.g., S, Se, and Te) were incorporated into the symmetric nickel-nitrogen-carbon (Ni-N₄-C) configuration to obtain Ni-X-N₃-C (X: S, Se, and Te) SACs with asymmetric coordination presented for central Ni atoms. Among these obtained Ni-X-N₃-C (X: S, Se, and Te) SACs, Ni-Se-N₃-C exhibited superior eCO₂RR activity, with CO selectivity reaching ~98% at -0.70 V versus reversible hydrogen electrode (RHE). The Zn-CO₂ battery integrated with Ni-Se-N₃-C as cathode and Zn foil as anode achieved a peak power density of 1.82 mW cm^-2 and maintained remarkable rechargeable stability over 20 h. In-situ spectral investigations and theoretical calculations demonstrated that the chalcogen heteroatoms doped into the Ni-N₄-C configuration would break coordination symmetry and trigger charge redistribution, and then regulate the intermediate behaviors and thermodynamic reaction pathways for eCO₂RR. Especially, for Ni-Se-N₃-C, the introduced Se atoms could significantly raise the d-band center of central Ni atoms and thus remarkably lower the energy barrier for the rate-determining step of *COOH formation, contributing to the promising eCO₂RR performance for high selectivity CO production by competing with hydrogen evolution reaction.

Key words: Electrochemical CO₂ reduction reaction, Chalcogen heteroatoms, Single-atom catalysts, Asymmetric coordination, CO production

王佳琳, 张凯妮, Ta Thi Thuy Nga, 王亦清, 石玉川, 魏代星, 董崇礼, 沈少华. 具有非对称配位结构的硫族杂原子掺杂Ni-N-C单原子催化剂及其电化学二氧化碳还原性能[J]. 催化学报, 2024, 64: 54-65.

Jialin Wang, Kaini Zhang, Ta Thi Thuy Nga, Yiqing Wang, Yuchuan Shi, Daixing Wei, Chung-Li Dong, Shaohua Shen. Chalcogen heteroatoms doped nickel-nitrogen-carbon single-atom catalysts with asymmetric coordination for efficient electrochemical CO₂ reduction[J]. Chinese Journal of Catalysis, 2024, 64: 54-65.

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Fig. 1. Synthesis and morphology characterizations of Ni-N4-C and Ni-X-N3-C (X: S, Se, and Te) SACs. (a) Synthesis procedure of Ni-N4-C and Ni-X-N3-C (X: S, Se, and Te). TEM images of Ni-N4-C (b), Ni-S-N3-C (c), Ni-Se-N3-C (d), and Ni-Te-N3-C (e). HAADF-STEM images of Ni-N4-C (f), Ni-S-N3-C (g), Ni-Se-N3-C (h), and Ni-Te-N3-C (i), with transition-metal single atoms marked by red circles.

Fig. 2. Structural characterizations of Ni-N4-C and Ni-X-N3-C (X: S, Se, and Te) SACs. (a) High-resolution XPS Ni 2p spectra of Ni-N4-C, Ni-S-N3-C, Ni-Se-N3-C, and Ni-Te-N3-C. Ni K-edge XANES spectra (inset shows the fitted pre-edge region) (b), and Fourier-transformed k3-weighted EXAFS spectra of Ni-S-N3-C, Ni-Se-N3-C, Ni-Te-N3-C, and corresponding references (c). (d) Wavelet transformed EXAFS spectra of Ni foil, NiO, and Ni-Se-N3-C. FT-EXAFS fitting curves and (inset) corresponding structure model of Ni-S-N3-C (e), Ni-Se-N3-C (f), and Ni-Te-N3-C (g).

Fig. 3. eCO2RR performances and in-situ spectral characterizations of Ni-N4-C and Ni-X-N3-C (X: S, Se, and Te) SACs. CO Faradaic efficiencies (FEs) (a) and CO partial current densities (b) for Ni-N4-C, Ni-S-N3-C, Ni-Se-N3-C, and Ni-Te-N3-C at different applied potentials. (c) TOFs for CO production over Ni-N4-C, Ni-S-N3-C, Ni-Se-N3-C, and Ni-Te-N3-C. In-situ Raman spectra of Ni-S-N3-C (d), Ni-Se-N3-C (e), and Ni-Te-N3-C (f) in the range of 1350-1900 cm-1. (g) Reaction pathways for electrochemical CO2-to-CO reduction at Ni-X-N3-C (X: S, Se, and Te).

Fig. 4. Theoretical investigations. (a) Bader charge analysis of Ni-S, Ni-Se, and Ni-Te moieties. (b) Calculated projected density of states (PDOS) of Ni-N4-C, Ni-S-N3-C, Ni-Se-N3-C, and Ni-Te-N3-C for *COOH adsorption. Reaction pathways and free energy diagrams of eCO2RR (c) and HER (d) over Ni-N4-C, Ni-S-N3-C, Ni-Se-N3-C, and Ni-Te-N3-C at 0 V vs. RHE. (e) Calculated limiting potential differences between eCO2RR and HER at Ni-N4-C, Ni-S-N3-C, Ni-Se-N3-C, and Ni-Te-N3-C.

Fig. 5. Electrochemical performance of Ni-Se-N3-C SAC based Zn-CO2 battery. (a) Schematic illustration of the Ni-Se-N3-C SAC based Zn-CO2 battery. Charging and discharging curves (b) and power density curve (c) of Ni-Se-N3-C SAC based Zn-CO2 battery. (d) LEDs powered by the Ni-Se-N3-C SAC based Zn-CO2 battery. (e) Galvanostatic discharge-charge curves of Ni-Se-N3-C SAC based Zn-CO2 battery at 2 mA cm-2.

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具有非对称配位结构的硫族杂原子掺杂Ni-N-C单原子催化剂及其电化学二氧化碳还原性能

Chalcogen heteroatoms doped nickel-nitrogen-carbon single-atom catalysts with asymmetric coordination for efficient electrochemical CO₂ reduction

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具有非对称配位结构的硫族杂原子掺杂Ni-N-C单原子催化剂及其电化学二氧化碳还原性能

Chalcogen heteroatoms doped nickel-nitrogen-carbon single-atom catalysts with asymmetric coordination for efficient electrochemical CO2 reduction

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Chalcogen heteroatoms doped nickel-nitrogen-carbon single-atom catalysts with asymmetric coordination for efficient electrochemical CO₂ reduction