催化学报 ›› 2021, Vol. 42 ›› Issue (6): 920-937.DOI: 10.1016/S1872-2067(20)63718-4
都京a,†, 马媛媛d,†, 谭华桥a,*(), 康振辉b,c,#(), 李阳光a,$()
收稿日期:
2020-07-22
接受日期:
2020-09-03
出版日期:
2021-06-18
发布日期:
2021-01-30
通讯作者:
谭华桥,康振辉,李阳光
作者简介:
†共同第一作者.
基金资助:
Jing Dua,†, Yuan-Yuan Mad,†, Huaqiao Tana,*(), Zhen-Hui Kangb,c,#(), Yangguang Lia,$()
Received:
2020-07-22
Accepted:
2020-09-03
Online:
2021-06-18
Published:
2021-01-30
Contact:
Huaqiao Tan,Zhen-Hui Kang,Yangguang Li
About author:
$E-mail: liyg658@nenu.edu.cn†These authors contributed equally.
Supported by:
摘要:
随着工业发展和全球人口的持续增长, 人类对化石燃料的消耗日益增加, 从而导致大气中二氧化碳含量的显著增加以及与之相伴的一系列环境问题. 电化学还原二氧化碳制备高附加值的燃料和化学品具有稳定的效率和较高的经济可行性等特点, 目前已成为一种有前景的策略来缓解当前全球面临的能源短缺和气候变暖问题. 然而, 电催化二氧化碳还原过程存在反应能垒高和复杂的多电子/质子耦合过程等不足, 因此, 合理有效的电催化剂设计成为该领域的关键问题. 近年, 理解和明确电化学二氧化碳还原反应过程的活性起源、选择性调控机制和催化反应机理已成为高效电催化剂设计过程中的重要指导原则. 作为一类独特的纳米尺度的金属氧簇, 多金属氧酸盐(多酸)已成为二氧化碳还原领域的热点材料. 尤其是, 多酸明确的结构、优越的电子/质子存储转移能力和二氧化碳吸附活化能力有助于探究二氧化碳还原反应过程中的活性起源和构效机制. 因此, 利用多酸阐明电化学二氧化碳还原反应中的这些关键问题对于开发高效、可实用化的电催化剂意义重大.
本文综述了近年多酸在电催化二氧化碳还原反应中取得的进展, 重点介绍了多酸阴离子均相分子催化剂、多酸基无机-有机杂化材料催化剂、多酸电解质溶液、多酸-纳米复合材料在电催化二氧化碳还原反应中的应用. 利用密度泛函理论结合原位实验证据推测了可能的反应机理, 探讨了多酸对电催化活性和产物选择性的影响, 揭示了电子/质子存储-转移过程和多酸表面修饰工程在电催化二氧化碳还原过程中的重要作用. 最后, 本文还分析了多酸基材料存在的问题与面临的挑战, 并对多酸基材料在二氧化碳还原领域的未来发展进行了展望, 这对理解电催化二氧化碳还原反应中的关键步骤和开发新型高效的电催化二氧化碳还原电催化剂具有启发意义.
都京, 马媛媛, 谭华桥, 康振辉, 李阳光. 多金属氧酸盐材料在二氧化碳电催化还原领域中的研究进展[J]. 催化学报, 2021, 42(6): 920-937.
Jing Du, Yuan-Yuan Ma, Huaqiao Tan, Zhen-Hui Kang, Yangguang Li. Progress of electrochemical CO2 reduction reactions over polyoxometalate-based materials[J]. Chinese Journal of Catalysis, 2021, 42(6): 920-937.
Possible half-reactions in electrochemical CO2RRs | Electrode potentials (V vs. SHE) |
---|---|
CO2 (g) + e- → *COO- | -1.90 |
CO2 (g) + 2H+ + 2e- → CO (g) + H2O (l) | -0.52 |
CO2 (g) + 8H+ + 8e- → CH4 (g) + 2H2O (l) | -0.24 |
2CO2 (g) + 12H+ + 12e- → C2H4 (g) + 4H2O (l) | -0.34 |
CO2 (g) + 2H+ + 2e- → HCOOH (l) | -0.61 |
CO2 (g) + 4H+ + 4e- → HCHO (l) + H2O (l) | -0.51 |
CO2 (g) + 6H+ (l) + 6e- → CH3OH (l) + H2O (l) | -0.38 |
2H+ + 2e- → H2 (g) | -0.42 |
Table 1 Electrochemical potentials of reactions that may occur during electrocatalytic CO2 reduction in aqueous solutions.
Possible half-reactions in electrochemical CO2RRs | Electrode potentials (V vs. SHE) |
---|---|
CO2 (g) + e- → *COO- | -1.90 |
CO2 (g) + 2H+ + 2e- → CO (g) + H2O (l) | -0.52 |
CO2 (g) + 8H+ + 8e- → CH4 (g) + 2H2O (l) | -0.24 |
2CO2 (g) + 12H+ + 12e- → C2H4 (g) + 4H2O (l) | -0.34 |
CO2 (g) + 2H+ + 2e- → HCOOH (l) | -0.61 |
CO2 (g) + 4H+ + 4e- → HCHO (l) + H2O (l) | -0.51 |
CO2 (g) + 6H+ (l) + 6e- → CH3OH (l) + H2O (l) | -0.38 |
2H+ + 2e- → H2 (g) | -0.42 |
Fig. 1. Kinetic volcano plot for CO evolution at a 0.35 V overpotential from the (211) step of TMs. The TMs fall along a trendline that does not pass over the top of the volcano. However, the noble metals occupy near-optimum positions along this trend line. The speci?c CO evolution current for the ChCODH II and MbCODH enzyme models is comparable or better than those of the noble metals. Reprinted with the permission of Ref. [75]. Copyright 2013, American Chemical Society.
Fig. 2. (a) Visible spectra of tetraheptylammonium salts of (I) α-[SiW11O39Co(OH2)]6-, (II) α-[SiW11O39Co(_)]6-, and (III) a-[SiW11O39Co(CO2)]6- in toluene. (b) Infrared spectrum of the tetraheptylammonium salt of α-[SiW11O39Co(CO2)]6- in CCl4. The two peaks marked with arrows appear after the CO2 is bubbled, and are assigned to vibrations of CO2 complexed to cobalt. (c) Difference spectrum between α-[SiW11O39Co(CO2)]6- and α-[SiW11O39Co(_)]6-. The peak at 2335 cm-1 originates from the CO2 gas dissolved in the solvent. (d) 13C NMR spectra of 0.1 M α-[SiW11O39Co(CO2)]6- in toluene at temperatures from -40 °C to + 35 °C. (e-h) Proposed hypothetical bonding modes for CO2 with cobalt in α-[SiW11O39Co(CO2)]6-, stabilized by hydrogen bonding utilizing both hydrogen atoms from water. Reprinted with the permission of Ref. [88]. Copyright 1998, American Chemical Society (ACS).
Fig. 3. Synthesis of the organometallic derivative [α-H2PW11O39{RhIIICp*(OH2)}]3- (the POM skeleton is displayed in polyhedral representation). Reprinted with the permission of Ref. [98]. Copyright 2019 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
Fig. 4. (a) Structural representation of Mn(III), Ni(II), and Zn(II) μ-(meso-5,10,15,20-tetra(pirydil)porphyrin)tetrakis{bis(bipyridine)chloride ruthenium(II)}; Linear sweep voltammogram of bare ITO electrode (b), [MnIIITRP]5+/[SiW12O40]4- multilayer modi?ed electrode (c) [ZnIITRP]4+/[SiW12O40]4- multilayer modi?ed electrode (d) and [NiIITRP]4+/[SiW12O40]4- multilayer modi?ed electrode the in presence (solid line) and absence (dash line) of CO2 and 0.1 M NaClO4 solution at 5 mV s-1 (e). Reprinted with the permission of Ref. [100]. Copyright 2013 Elsevier Ltd.
Electrode | Products and TOF (s-1) | ||
---|---|---|---|
CO | HCOOH | CH3OH | |
[MnIIITRP]5-/[SiW12O40]4-/ITO | N.D.a | 0.48 b | 0.023 |
[ZnIITRP]5-/[SiW12O40]4-/ITO | 0.0037 | N.D. a | 8.2 |
[NiIITRP]5-/[SiW12O40]4-/ITO | 0.24 | 0.083 | N.D. a |
Table 2 Electrocatalytic CO2RR activity and products of [MTRP]/[SiW12O40]/ITO electrodes.
Electrode | Products and TOF (s-1) | ||
---|---|---|---|
CO | HCOOH | CH3OH | |
[MnIIITRP]5-/[SiW12O40]4-/ITO | N.D.a | 0.48 b | 0.023 |
[ZnIITRP]5-/[SiW12O40]4-/ITO | 0.0037 | N.D. a | 8.2 |
[NiIITRP]5-/[SiW12O40]4-/ITO | 0.24 | 0.083 | N.D. a |
Fig. 5. (a) Schematic illustration of the structures of M-PMOFs (M = Co, Fe, Ni, Zn). M-PMOFs consist of 4-connection TCPP linkers and zigzag POM chains; (b) Linear sweep voltammetry (LSV) curves of M-PMOFs; (c) Faradaic ef?ciencies for CO; (d) Durability test of Co-PMOF at a potential of -0.8 V vs. RHE. Reprinted with the permission of Ref. [37]. Copyright 2018, Springer Nature.
Fig. 6. (a) Schematic diagram of the reaction mechanism induced by POM-MnL; (b) TEM image of SiW12-MnL/KB (inset: HR-TEM image of SiW12-MnL/KB, scale bar: 5 nm); (c) The CV curves for MnL/KB, CsSiW12/KB, and SiW12-MnL/KB in 0.5 mol L-1 N2-saturated KHCO3 at a 0.05 V s-1 scan rate; (d) The LSV curves of SiW12-MnL/KB and MnL/KB in 0.5 M N2-(black curve) or CO2-(red curve) saturated KHCO3 electrolyte; (e) The FE for CO at di?erent potentials for MnL/KB and SiW12-MnL/KB (the line is drawn only to guide the eye); (f) The FEs for CO and H2 at the overpotential of the highest FE for CO of MnL/KB and POM-MnL/KB. Reprinted with the permission of Ref. [101]. Copyright 2020, Royal Society of Chemistry (RSC).
Fig. 7. Square reaction scheme representing the interaction between the reduced forms of [α-SiW12O40]4- and CO2 during electrochemical reduction. [α-SiW12O40]4- is represented as SiW4- for convenience. Reprinted with the permission of Ref. [102]. Copyright 2016 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim.
Fig. 8. The Faradaic e?ciencies of products of In cathode in SiW9V3 (a) and SiW11Mn (b) electrolyte. (c) XPS spectra of In 3d for the indium electrode before and after electrolysis with 1 and 12 h. (d) XPS spectra of W 4f for the indium electrode after 1 h electrolysis. (e) The FTIR spectroscopy characterization for the 2 mM SiW9V3-0.1 M Na2SO4 electrolyte during electrolysis, in which the peak at 2071 cm-1 corresponds to the adsorbed CO*. (f) Current density with electrolysis time at different potential for 1 h; The inset is the current density with electrolysis time at -1.15 V vs. Ag/AgCl for 12 h. Reprinted with the permission of Refs. [103,104]. Copyright 2020 Elsevier Ltd.
Fig. 9. (a) SEM images of Ag-PMo nanocomposite-modi?ed ITO glasses; (b) TEM images of Ag-PMo nanocomposites, inset: Schematic diagram of Ag-PMo catalytic CO2 reduction; (c) Comparison of cyclic voltammograms obtained at an Ag-PMo nanocomposite-modi?ed GC electrode in DMF (0.1 M [n-Bu4N]PF6) with 0.5% (v/v) added H2O under a CO2 (black line) or a N2b(red line) atmosphere (Scan rate: 100 mV s-1); (d) Potentiostatic i-t curves obtained at an Ag-PMo nanocomposite modified GC electrode in DMF (0.1 M [n-Bu4N]PF6) with 0.5% (v/v) added water under CO2 or N2 atmospheres. Applied potential: -1.9 V vs. Fc0/+. Reprinted with the permission of Ref. [105]. Copyright 2018, American Chemical Society.
Fig. 10. (a) SEM image of the film deposited on an FTO electrode in aqueous 0.25 M HNO3 solutions containing 1.0 mM Bi(NO3)3; (b) Atomic force microscopy (AFM) image and height profile of Bi-PMo nanosheets; (c) Raman spectra of Bi-PMo nanosheets before (black) and after electrolysis (red), and H3PMo12O40 (blue); (d,e) High-resolution XPS spectra recorded for Mo 3d and Bi 4f regions of the Bi-PMo nanosheets; (f) Cyclic voltammograms obtained for Bi-PMo nanosheet (solid lines) and Bi nano-dendrite (dash lines) modified GC electrodes in CO2-(black) or N2-(red) saturated 0.5 M NaHCO3 aqueous solutions, scan rate: 0.1 V s-1; (g) Faradaic efficiencies for formate produced on Bi-PMo nanosheets (black) and Bi nano-dendrites (red) at various applied potentials in CO2-saturated 0.5 M NaHCO3 solutions; (h) Long term stability study of Bi-PMo nanosheets during controlled potential electrolysis at -0.86 V vs. RHE in a CO2-saturated 0.5 M NaHCO3 solution; (i) Tafel plots obtained for Bi-PMo nanosheets (black) and Bi nano-dendrites (red). Reprinted with the permission of Ref. [106]. Copyright 2019 Wiley‐VCH Verlag GmbH & Co. KGaA, Weinheim.
Electrocatalyst | Electrolyte | Potential | Principal product | FE (%) | TON | Ref. |
---|---|---|---|---|---|---|
(TOA)6[α-SiW11O39Co(_)] | CH2Cl2 | -1.5 V vs. Hg2Cl2/Hg | CO | 18 | — | [ |
(TBA)3[H2PW11O39{RhIIICp* (OH2)}] | CH3CN | -1.8 V vs. Hg2Cl2/Hg | HCOOH | 4.5 | 0.8 | [ |
[Cp*RhIII(bpy)Cl]+ | CH3CN | -1.8 V vs. Hg2Cl2/Hg | HCOOH | 60 | 18 | [ |
[Mn(III)TRP]5+/[SiW12O40]4-/ITO | 0.1 M NaClO4 | -0.8 V vs. Ag/AgCl | HCOOH | — | 1.06 × 104 | [ |
[Zn(II)TRP]4+/[SiW12O40]4-/ITO | 0.1 M NaClO4 | -0.8 V vs. Ag/AgCl | Methanol | — | 1.76 × 105 | [ |
[Ni(II)TRP]5+/[SiW12O40]4-/ITO | 0.1 M NaClO4 | -0.8 V vs. Ag/AgCl | CO | — | 3.85 × 103 | [ |
[Ni(II)TRP]5+ | DMF | -0.8 V vs. SHE | CO | — | — | [ |
Co-PMOF | 0.5 M KHCO3 | -0.8 V vs. RHE | CO | 98.7 | 7693 | [ |
Fe-PMOF | 0.5 M KHCO3 | -0.8 V vs. RHE | CO | 28.8 | — | [ |
Ni-PMOF | 0.5 M KHCO3 | -0.8 V vs. RHE | CO | 18.5 | — | [ |
Zn-PMOF | 0.5 M KHCO3 | -0.8 V vs. RHE | CO | 0.95 | — | [ |
Co-TMCP | 0.5 M KHCO3 | -0.9 V vs. RHE | CO | ~50 | — | [ |
MOF-525(Co) | 0.5 M KHCO3 | -0.8 V vs. RHE | CO | 47.9 | — | [ |
CoPPC/CNT | 0.5 M KHCO3 | -0.58 V vs. RHE | CO | ~90 | — | [ |
SiW12-MnL/KB | 0.5 M KHCO3 | -0.72 V vs. RHE | CO | 95 | — | [ |
PW12-MnL/KB | 0.5 M KHCO3 | -0.72 V vs. RHE | CO | 80 | — | [ |
PMo12-MnL/KB | 0.5 M KHCO3 | -0.52 V vs. RHE | CO | 65 | — | [ |
MnL/KB | 0.5 M KHCO3 | -0.72 V vs. RHE | CO | 65 | — | [ |
[Mn(L)(CO)3Br (MnL) | CH3CN | -1.7 V vs. Ag/Ag+ | CO | 85 | 34 | [ |
AgNC@BSA | 1 mM [Bu4N]4[α-SiW12 O40] in DMF | -2.32 V vs. Fc0/+ | CO | 75.6 | — | [ |
Ag-PMo | DMF | -1.9 vs. Fc0/+ | CO | 90 ± 5 | — | [ |
Ag/N-doped graphene/carbon foam | 0.1 M KHCO3 | -0.6 V vs. RHE | Ethanol | 85.2 | — | [ |
Ag QDDCs | 0.5 M KHCO3 | -0.3 V vs. RHE | CO | 95 | — | [ |
Indium sheet | 2 mM SiW9V3 + 0.1 M Na2SO4 | -1.15 vs. Ag/AgCl | CH3COOH | 96.5 | — | [ |
Indium sheet | 2 mM SiW11Mn+ 0.1 M Na2SO4 | -1.0 V vs. RHE | CH3COOH | 72.1 | — | [ |
In2O3-rGO | 0.1 M KHCO3 | -1.2 V vs. RHE | HCOOH | 84.6 | — | [ |
Sulfur-doped indium | 0.5 M KHCO3 | -0.98 V vs. RHE | HCOOH | 93 | — | [ |
Bi-PMo nanosheets | 0.5 M KHCO3 | -0.86 V vs. RHE | CH3COOH | 93 | — | [ |
Bi nano-dendrites | 0.5 M KHCO3 | -0.96 V vs. RHE | CH3COOH | 81 | — | [ |
Bi nanoflakes | 0.1 M KHCO3 | -0.6 V vs. RHE | HCOOH | ~100 | — | [ |
Table 3 Performance of major POM-based electrocatalysts and other representative electrocatalysts used in electrocatalytic CO2RRs.
Electrocatalyst | Electrolyte | Potential | Principal product | FE (%) | TON | Ref. |
---|---|---|---|---|---|---|
(TOA)6[α-SiW11O39Co(_)] | CH2Cl2 | -1.5 V vs. Hg2Cl2/Hg | CO | 18 | — | [ |
(TBA)3[H2PW11O39{RhIIICp* (OH2)}] | CH3CN | -1.8 V vs. Hg2Cl2/Hg | HCOOH | 4.5 | 0.8 | [ |
[Cp*RhIII(bpy)Cl]+ | CH3CN | -1.8 V vs. Hg2Cl2/Hg | HCOOH | 60 | 18 | [ |
[Mn(III)TRP]5+/[SiW12O40]4-/ITO | 0.1 M NaClO4 | -0.8 V vs. Ag/AgCl | HCOOH | — | 1.06 × 104 | [ |
[Zn(II)TRP]4+/[SiW12O40]4-/ITO | 0.1 M NaClO4 | -0.8 V vs. Ag/AgCl | Methanol | — | 1.76 × 105 | [ |
[Ni(II)TRP]5+/[SiW12O40]4-/ITO | 0.1 M NaClO4 | -0.8 V vs. Ag/AgCl | CO | — | 3.85 × 103 | [ |
[Ni(II)TRP]5+ | DMF | -0.8 V vs. SHE | CO | — | — | [ |
Co-PMOF | 0.5 M KHCO3 | -0.8 V vs. RHE | CO | 98.7 | 7693 | [ |
Fe-PMOF | 0.5 M KHCO3 | -0.8 V vs. RHE | CO | 28.8 | — | [ |
Ni-PMOF | 0.5 M KHCO3 | -0.8 V vs. RHE | CO | 18.5 | — | [ |
Zn-PMOF | 0.5 M KHCO3 | -0.8 V vs. RHE | CO | 0.95 | — | [ |
Co-TMCP | 0.5 M KHCO3 | -0.9 V vs. RHE | CO | ~50 | — | [ |
MOF-525(Co) | 0.5 M KHCO3 | -0.8 V vs. RHE | CO | 47.9 | — | [ |
CoPPC/CNT | 0.5 M KHCO3 | -0.58 V vs. RHE | CO | ~90 | — | [ |
SiW12-MnL/KB | 0.5 M KHCO3 | -0.72 V vs. RHE | CO | 95 | — | [ |
PW12-MnL/KB | 0.5 M KHCO3 | -0.72 V vs. RHE | CO | 80 | — | [ |
PMo12-MnL/KB | 0.5 M KHCO3 | -0.52 V vs. RHE | CO | 65 | — | [ |
MnL/KB | 0.5 M KHCO3 | -0.72 V vs. RHE | CO | 65 | — | [ |
[Mn(L)(CO)3Br (MnL) | CH3CN | -1.7 V vs. Ag/Ag+ | CO | 85 | 34 | [ |
AgNC@BSA | 1 mM [Bu4N]4[α-SiW12 O40] in DMF | -2.32 V vs. Fc0/+ | CO | 75.6 | — | [ |
Ag-PMo | DMF | -1.9 vs. Fc0/+ | CO | 90 ± 5 | — | [ |
Ag/N-doped graphene/carbon foam | 0.1 M KHCO3 | -0.6 V vs. RHE | Ethanol | 85.2 | — | [ |
Ag QDDCs | 0.5 M KHCO3 | -0.3 V vs. RHE | CO | 95 | — | [ |
Indium sheet | 2 mM SiW9V3 + 0.1 M Na2SO4 | -1.15 vs. Ag/AgCl | CH3COOH | 96.5 | — | [ |
Indium sheet | 2 mM SiW11Mn+ 0.1 M Na2SO4 | -1.0 V vs. RHE | CH3COOH | 72.1 | — | [ |
In2O3-rGO | 0.1 M KHCO3 | -1.2 V vs. RHE | HCOOH | 84.6 | — | [ |
Sulfur-doped indium | 0.5 M KHCO3 | -0.98 V vs. RHE | HCOOH | 93 | — | [ |
Bi-PMo nanosheets | 0.5 M KHCO3 | -0.86 V vs. RHE | CH3COOH | 93 | — | [ |
Bi nano-dendrites | 0.5 M KHCO3 | -0.96 V vs. RHE | CH3COOH | 81 | — | [ |
Bi nanoflakes | 0.1 M KHCO3 | -0.6 V vs. RHE | HCOOH | ~100 | — | [ |
Fig. 11. The DFT calculation and proposed reaction mechanism. (a) The free energy diagrams of CO2 reduction to CO for POM (orange), Co-TCPP (green), and Co-PMOF (pink). The rate-determining step and the corresponding free energy of each material are indicated (Note that an asterisk represents a surface-active site for reaction); (b) Comparison of the free energy of each elementary reaction (ΔG1, ΔG2, and ΔG3 represent the free energy of *COOH formation, *CO formation, and CO desorption, respectively) during CO2RRs for Co-PMOF, Fe-PMOF, Ni-PMOF, and Zn-PMOF, respectively; (c,d) Proposed mechanism scheme for the CO2RRs on Co-PMOF (POMs as electron-donors, porphyrins as charge transfer ligands, and TMs as electron-acceptors). Reprinted with the permission of Ref. [37]. Copyright 2018, Springer Nature.
Fig. 12. (a) Computed frontier orbitals (compositions and energies) for MnL, SiW12-MnL, PW12-MnL, and PMo12-MnL (the green lines represent the unoccupied molecular orbitals (MO) contributed by MnL in POM-MnL); (b) The electronic con?gurations for the di?erent reduction degree states of SiW12-MnL, PW12-MnL, and PMo12-MnL; (c) The transient photovoltage curves of powder POM-MnL and MnL; (d) Potential energy surfaces for H+ and CO2 addition to the respective active CO2 and H adducts. Reprinted with the permission of Ref. [101]. Copyright 2020, Royal Society of Chemistry (RSC).
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