簇状Bi28O32(SO4)10原位Bi晶格畸变增强电催化CO2还原为甲酸

doi:10.1016/S1872-2067(24)60287-1

催化学报 ›› 2025, Vol. 72: 199-210.DOI: 10.1016/S1872-2067(24)60287-1

簇状Bi₂₈O₃₂(SO₄)₁₀原位Bi晶格畸变增强电催化CO₂还原为甲酸

孙静涵^a, 许峥嵘^a, 刘邓^a, 孔爱国^b^,^*(), 张其春^c^,^*(), 刘睿^a^,^*()

^a同济大学材料科学与工程学院, 先进土木工程材料教育部重点实验室, 上海 201804
^b华东师范大学化学与分子工程学院, 上海 200241
^c香港城市大学材料科学与工程学院, 香港 999077

收稿日期:2024-12-04 接受日期:2025-02-03 出版日期:2025-05-18 发布日期:2025-05-20
通讯作者: *电子信箱: agkong@chem.ecnu.edu.cn (孔爱国),qiczhang@cityu.edu.hk (张其春),ruiliu@tongji.edu.cn (刘睿).
基金资助:
中央高校基本科研业务费(22120230104)

In-situ distortion of Bi lattice in Bi₂₈O₃₂(SO₄)₁₀ cluster boosted electrocatalytic CO₂ reduction to formate

Jinghan Sun^a, Zhengrong Xu^a, Deng Liu^a, Aiguo Kong^b^,^*(), Qichun Zhang^c^,^*(), Rui Liu^a^,^*()

^aKey Laboratory of Advanced Civil Engineering Materials of Ministry of Education, School of Materials Science and Engineering, Tongji University, Shanghai 201804, China
^bSchool of Chemistry and Molecular Engineering, East China Normal University, Shanghai 200241, China
^cDepartment of Materials Science and Engineering, City University of Hong Kong, Hong Kong SAR 999077, China

Received:2024-12-04 Accepted:2025-02-03 Online:2025-05-18 Published:2025-05-20
Contact: *E-mail: agkong@chem.ecnu.edu.cn (A. Kong), qiczhang@cityu.edu.hk (Q. Zhang), ruiliu@tongji.edu.cn (R. Liu).
Supported by:
Fundamental Research Funds for the Central Universities(22120230104)

摘要/Abstract

摘要：

利用可再生电力将二氧化碳还原(CO₂RR)为甲酸等高附加值产物是一种高效的二氧化碳资源利用策略. 提高CO₂RR性能的关键在于设计低成本、高性能的新型电催化剂, 同时显著抑制竞争性析氢反应(HER)的发生. 簇型催化剂因其独特的几何构型和电子结构以及多原子之间的协同作用, 受到越来越多的关注. 在电催化CO₂RR过程中, 簇型催化剂的真实活性位点演变以及催化机理仍有待阐明. 因此, 设计高效的簇型电催化剂并探究其原位重构及催化机理是本文的主要研究内容.

本文通过在空气氛围中硫化煅烧铋-鞣花酸金属有机框架, 分别在500和600 °C煅烧制备了两种铋基化合物: 具有[Bi₂O₂]²⁺层状结构的Bi₂O₂SO₄和具有[Bi₁₄O₁₆]¹⁰⁺簇的Bi₂₈O₃₂(SO₄)₁₀. 在H型电解池中测试了上述两种铋基化合物的电催化CO₂RR性能. 结果表明, 簇状Bi₂₈O₃₂(SO₄)₁₀电催化剂在−0.9 V_RHE到−1.3 V_RHE的宽电位范围内实现了超过90%的甲酸法拉第效率(FE_formate), 并在−1.1 V_RHE时FE_formate最高可达96.2%, 表现出比层状结构Bi₂O₂SO₄更高的CO₂RR性能. 原位表征技术、X射线衍射、透射电子显微镜、X射线光电子能谱及X射线吸收谱等测试结果证明了Bi₂₈O₃₂(SO₄)₁₀和Bi₂O₂SO₄不同的原位重构过程对它们电催化性能差异的影响. 簇状的Bi₂₈O₃₂(SO₄)₁₀在CO₂RR过程中经历了特殊的Bi₂₈O₃₂(SO₄)₁₀ → Bi_−2.1/ Bi₂O₂CO₃ → Bi_−2.1/Bi_−0.6两步重构过程, 即在第一步发生阴离子交换和原子重排得到了晶格畸变较高的金属Bi_−2.1, 在第二步发生电化学还原又形成了晶格畸变较弱的金属Bi_−0.6. 相比之下, Bi₂O₂SO₄层状化合物在重构过程中只发生了阴离子交换生成了Bi₂O₂CO₃, 并进一步还原为Bi_−0.6. 通过密度泛函理论计算比较了这两种不同晶格应变铋(Bi_−2.1和Bi_−0.6)对电催化CO₂RR性能的影响. 与弱晶格畸变的Bi_−0.6相比, 高晶格畸变的Bi_−2.1在CO₂吸附和活化过程中所需的吉布斯自由能更低, 从而更高效地促进甲酸生成. 同时, Bi_−2.1对竞争性HER的抑制作用也显著增强. 原位表征和理论计算结果为簇状Bi₂₈O₃₂(SO₄)₁₀催化剂表现出更好CO₂RR性能提供了进一步的理论支持.

综上, 本文为CO₂RR提供了一种高效的无机簇型电催化剂, 并证明了具有Bi-O簇结构的化合物引发的原位重构过程可以调控金属Bi的非稳态程度进而提高CO₂RR催化性能, 为从电化学重构角度设计新型电催化剂提供了一种新思路.

关键词: 无机金属氧簇, Bi₂₈O₃₂(SO₄)₁₀, 电催化CO₂还原, 原位重构, 晶格应变

Abstract:

To convert carbon dioxide into high-value-added liquid products such as formate with renewable electricity (CO₂RR) is a promising strategy of CO₂ resource utilization. The key is to find a highly efficient and selective electrocatalyst for CO₂RR. Herein, clustered Bi₂₈O₃₂(SO₄)₁₀ was found to show a high formate Faradaic efficiency (FE_formate) of 96.2% at -1.1 V_RHE and FE_formate above 90% in a wide potential range from -0.9 to -1.3 V_RHE in H-type cell, surpassing the corresponding layered Bi₂O₂SO₄ (85.6% FE_formate at -1.1 V_RHE). The advantageous CO₂RR performance of Bi₂₈O₃₂(SO₄)₁₀ over Bi₂O₂SO₄ was ascribed to a special two-step in-situ reconstruction process, consisting of Bi₂₈O₃₂(SO₄)₁₀ → Bi_-2.1/Bi₂O₂CO₃ → Bi_-2.1/Bi_-0.6 during CO₂RR. It gave metallic Bi_-2.1 with lattice distortion of -2.1% at the first step and metallic Bi_-0.6 with lattice distortion of -0.6% at the second step. In contrast, the usual layered Bi₂O₂SO₄ only formed metallic Bi_-0.6 with weaker lattice strain. The metallic Bi_-2.1 revealed higher efficiency in stabilizing *CO₂ intermediate and reducing the energy barrier of CO₂RR, while suppressing hydrogen evolution reaction and CO formation. This work delivers a high-performance cluster-type Bi₂₈O₃₂(SO₄)₁₀ electrocatalyst for CO₂RR, and elucidates the origin of superior performance of clustered Bi₂₈O₃₂(SO₄)₁₀ electrocatalysts compared with layered Bi₂O₂SO₄.

Key words: Inorganic metal-oxygen clusters, Bi₂₈O₃₂(SO₄)₁₀, Electrocatalytic CO₂ reduction, In-situ reconstruction, Lattice strain

孙静涵, 许峥嵘, 刘邓, 孔爱国, 张其春, 刘睿. 簇状Bi₂₈O₃₂(SO₄)₁₀原位Bi晶格畸变增强电催化CO₂还原为甲酸[J]. 催化学报, 2025, 72: 199-210.

Jinghan Sun, Zhengrong Xu, Deng Liu, Aiguo Kong, Qichun Zhang, Rui Liu. In-situ distortion of Bi lattice in Bi₂₈O₃₂(SO₄)₁₀ cluster boosted electrocatalytic CO₂ reduction to formate[J]. Chinese Journal of Catalysis, 2025, 72: 199-210.

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图/表 6

Fig. 1. Schematic illustration of the synthesis and reconstruction of layer-type Bi2O2SO4 and cluster-type Bi28O32(SO4)10.

Fig. 2. XRD patterns (a), FT-IR spectra (b) and XPS survey spectra (c), high resolution XPS spectra of Bi 4f (d), S 2p (e), O 1s (f) of Bi2O2SO4 and Bi28O32(SO4)10. SEM and HRTEM images of Bi2O2SO4 (g,h) and Bi28O32(SO4)10 (i,j).

Fig. 3. Electrochemical performances of Bi2O2SO4 and Bi28O32(SO4)10 in H-type cell. (a) LSV curves of Bi2O2SO4 and Bi28O32(SO4)10. FEformate and jformate on Bi2O2SO4 (b) and Bi28O32(SO4)10 (c). (d) Comparison of performances with reported Bi-based electrocatalysts for the CO2RR to formate in H-type cell. (e) Durability test of Bi28O32(SO4)10 at the potential of -1.1 VRHE. Cdl (f), Tafel slopes (g), single oxidative LSV curves (h) in N2-saturated 0.05 mol L-1 NaOH and (i) Nyquist plots of Bi2O2SO4 and Bi28O32(SO4)10.

Fig. 4. In-situ time-resolved XRD patterns (a,b) and Raman spectra (c,d) of Bi2O2SO4 and Bi28O32(SO4)10.

Fig. 5. XRD patterns (a), enlarged XRD diffraction peaks (b) and Bi L3-edge FT-EXAFS spectra (c) of Bi2O2SO4-2h and Bi28O32(SO4)10-2h. SEM, HRTEM images and GPA strain maps of Bi2O2SO4-2h (d-f) and Bi28O32(SO4)10-2h (g-i).

Fig. 6. In-situ ATR-IR spectra of Bi2O2SO4 (a) and Bi28O32(SO4)10 (b). (c) Schematic illustration of CO2RR on the catalyst surface (Bi: purple, C: brown, O: red, H: blue). Gibbs free energy for CO2RR to formate (d), bond length between *CO2 and the surface Bi atom (e), PDOS of p-orbitals of O atom of the absorbed *CO2 intermediate (Fermi level was at 0 eV) (f), Gibbs free energy for H2 formation (g), adsorption energy comparisons of *CO2 and *H (h) over Bi-0.6 and Bi-2.1.

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簇状Bi₂₈O₃₂(SO₄)₁₀原位Bi晶格畸变增强电催化CO₂还原为甲酸

In-situ distortion of Bi lattice in Bi₂₈O₃₂(SO₄)₁₀ cluster boosted electrocatalytic CO₂ reduction to formate

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