Structural and interfacial engineering of well-defined metal-organic ensembles for electrocatalytic carbon dioxide reduction

doi:10.1016/S1872-2067(21)63980-3

Abstract

Abstract:

Electrochemical carbon dioxide reduction (CO₂RR) has been generally regarded as green technologies that can convert renewable energy such as sunlight and wind into fuels and valuable chemicals. However, the large-scale implementation of CO₂RR is severely hindered by the lack of high-performance CO₂RR electrocatalysts. Heterogeneous molecular catalysts and metal-organic framework with well-defined structure and high tunability of the metal centers and ligands show great promise for CO₂RR in terms of both fundamental understanding and practical application. Here, structural and interfacial engineering of these well-defined metal-organic ensembles is summarized. This review starts from the fundamental electrochemistry of CO₂RR and its evaluation criteria, and then moves to the heterogeneous molecular catalysts and metal-organic framework with emphasis on the engineering of metal centers and ligands, their interaction with supports, as well as in situ reconstruction of metal-organic ensembles. Summary and outlook are present in the end, with the hope to inspire and provoke more genuine thinking on the design and fabrication of efficient CO₂RR electrocatalysts.

Key words: Carbon dioxide reduction, Electrocatalysis, Heterogeneous molecular catalyst, Metal-organic frameworks, In situ reconstruction

Fenglei Lyu, Wei Hua, Huirong Wu, Hao Sun, Zhao Deng, Yang Peng. Structural and interfacial engineering of well-defined metal-organic ensembles for electrocatalytic carbon dioxide reduction[J]. Chinese Journal of Catalysis, 2022, 43(6): 1417-1432.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(21)63980-3

https://www.cjcatal.com/EN/Y2022/V43/I6/1417

Figures/Tables 13

Fig. 1. Schematic illustration of structural and interfacial engineering on heterogeneous molecular catalysts and MOFs for CO2RR.

Table 1 Standard potentials for CO2RR and hydrogen evolution reaction [33,34].

Equation	E⁰ vs. NHE at pH = 7	Electron transfer number
CO₂ + e^- → CO₂^•-	-1.90	1
CO₂ + 2e^-+ 2H⁺ → CO + H₂O	-0.53	2
CO₂ + 2e^- + 2H⁺ → HCOOH	-0.61	2
CO₂ + 6e^- + 6H⁺ → CH₃OH + H₂O	-0.38	6
CO₂ + 8e^- + 8H⁺ → CH₄ + 2H₂O	-0.24	8
2CO₂ + 12e^- + 12H⁺ → C₂H₄ + 4H₂O 2CO₂ + 12e^- + 12H⁺ → C₂H₅OH + 3H₂O 2H⁺ + 2e^- → H₂	-0.34 -0.33 -0.42	12 12 2

Fig. 2. Molecular structure of PorCu (a), Faradaic efficiencies (b) and partial current densities (c) for the gas-phase products at -0.976 V vs. RHE. (a?c) Reprinted with permission from Ref. [42]. Copyright 2016, American Chemical Society. (d) Chemical structures of the PorZn and H2Por, (e) CO Faradaic efficiencies and CO partial current densities at different potentials and (f) CO Faradaic efficiencies and total current densities after electrolysis at -1.7 V vs. standard hydrogen electrode (SHE). (d?f) Reprinted with permission from Ref. [43]. Copyright 2017, American Chemical Society. (g) Calculated free-energy diagram for all the MePc electrodes, (h) LSV tests in CO2-saturated 0.5 mol/L KHCO3 and (i) CO current density of MePcs at various potentials. (g?i) Reprinted with permission from Ref. [44]. Copyright 2018, Wiley-VCH.

Fig. 3. Molecular structures of CoPc1 (a) and CoPc2 (b). (c) Current density and TOF for CoPc1@MWCNTs and CoPc2@MWCNTs for CO production in CO2-saturated 0.5 mol/L KHCO3. (a?c) Reprinted with permission from Ref. [48]. Copyright 2019, the Springer-Nature. (d) Molecular structures of NiPc, NiPc-OMe and NiPc-CN. (e) Linear sweep voltammetry of neat NiPc, P-NiNC, NiPc MDE, NiPc-OMe MDE and NiPc-CN MDE in CO2-saturated 0.5 mol/L KHCO3 at scan rate of 5 mV s-1. (f) Chronoamperometry of NiPc MDE at -0.68 V, NiPc-CN MDE at -0.56 V and NiPc-OMe MDE at -0.64 V. (d?f) Reprinted with permission from Ref. [49]. Copyright 2020, the Springer-Nature. (g) Molecular structures of CoPc-A; Total current density (h) and Faradic efficiencies (i) for CO and H2 of CCG/CoPc-A and CCG/CoPc hybrids in CO2-saturated 0.1 mol/L KHCO3. (g?i) Reprinted with permission from Ref. [51]. Copyright 2019 American Chemical Society.

Fig. 4. Molecular structure comparison of Co-porphine (a) and Co(II)CPY (b). LSV curves (c) and FE (d) of CO for Co(II)CPY/CNT and CoTPP/CNT in CO2-saturated 0.1 mol/L KHCO3 at a scan rate of 1 mV s-1. (a?d) Reprinted with permission from Ref. [54]. Copyright 2020, Wiley-VCH. (e) Molecular structure of Co-salophen-X. FECO (f) and jCO (g) at selected potentials over the three Co-salophen-X samples. (e?g) Reprinted with permission from Ref. [40]. Copyright 2021 Elsevier. Molecular structure of Ni-N4-TPP (h) and Ni(-Cl)-N3O-TPP (i). FETotal and FECO (j) and jTotal and jCO (k) acquired for 1 h CO2RR operation at various potentials in a H-cell. (h?k) Reprinted with permission from Ref. [55]. Copyright 2021, American Chemical Society.

Fig. 5. (a) An illustration of CoPc immobilized in P4VP. Reprinted with permission from Ref. [56]. Copyright 2016, The Royal Society of Chemistry. (b) A proposed mechanism for CO2 reduction by CoPc showing pathway for competitive H2 generation. Reprinted with permission from Ref. [57]. Copyright 2019, the Springer-Nature. Interaction between pyridine and central Co (c) and Co 3d orbital splitting of Co centers (d) in MTPyP-Co and STPyP-Co obtained from multiplet fitting of Co L-edge absorption. (c,d) Reprinted with permission from Ref. [58]. Copyright 2019, Wiley-VCH.

Fig. 6. Schematic illustrations of adsorbed CoPc molecules on GDY/G (a) and graphene (b). (c) Linear sweep voltammetry with a scan rate of 20 mV s-1. (d) FECO and FEH2 of CoPc, CoPc/G, and CoPc/GDY/G. (a?d) Reprinted with permission from Ref. [63]. Copyright 2021, American Chemical Society. (e) Schematics showing the structure of Co-Nx (x = 2-5) centers in the MOLs; Linear sweep voltammetry (f) and Faradaic efficiencies (g) of MOL-Co-N3, MOL-Co-N4, MOL-Co-N5, and MOL-Co-N2 in CO2-saturated 1.0 mol/L KHCO3. (e?g) Reprinted with permission from Ref. [64]. Copyright 2021, American Chemical Society. (h) Supramolecular structure of Fe-PB composed of six Fe-TPP monomer building blocks. Faradaic efficiencies of CO and H2 (i) and CO specific current densities (j) for Fe-PB and Fe-TPP. (h?j) Reprinted with permission from Ref. [65]. Copyright 2018, Wiley-VCH.

Table 2 Comparisons of different heterogeneous molecular catalysts for CO2RR.

Catalyst	Cell	Electrolyte	j (mA cm^-2)	Product FE	Stability	Ref.
PorCu	H	0.5 mol/L KHCO₃	49	CH₄27%, C₂H₄ 17%	—	[42]
CoPc	H	0.5 mol/L KHCO₃	~8	CO 99%	60h@-0.8V	[44]
NiPc-OMe	flow	1 mol/L KHCO₃	300	CO 99.5%	40h@150mA cm^-2	[49]
CoTMAPc	flow	1 mol/L KOH	239	CO 95.6%	15h@-0.4V	[52]
CoCPY	H	0.1 mol/L KHCO₃	10.73	CO 96%	11h@-0.55V	[54]
STPyP-Co	H	0.5 mol/L KHCO₃	6.5	CO 96%	48h@-0.62V	[58]
CoPc/GDY/G	H	0.1 mol/L KHCO₃	9	CO 96%	24h@-0.81V	[63]
MOL-Co-N₃	H	1 mol/L KHCO₃	13.3	CO 99%	1.5h@-0.5V	[64]
Fe-PB	H	0.5 mol/L KHCO₃	~1.6	CO 100%	24h@-0.63V	[65]

Fig. 7. (a) Schematic structure of PcCu-O8-Zn (the dashed rectangular indicates the unit cell); partial current (b) and Faradaic (c) efficiency of CO for PcCu-O8-Zn/CNT, PcCu-O8-Cu/CNT, PcZn-O8-Zn/CNT and PcZn-O8-Cu/CNT at different potentials. (a?c) Reprinted with permission from Ref. [77]. Copyright 2020, the Springer-Nature. (d) Illustration of the preparation of NiPc-NiO4. Faradaic efficiencies (e) of CO, and CO partial current density (f) for NiPc-NiO4 and NiPc-OH. (d?f) Reprinted with permission from Ref. [78]. Copyright 2021, Wiley-VCH. (g) Illustration of the structure of PcCu-Cu-O; CV curves (h) and FEs (i) of C2H4, CH4, CO, and H2 for PcCu-Cu-O. (h,i) Reprinted with permission from Ref. [79]. Copyright 2021, American Chemical Society.

Fig. 8. (a) Design and synthetic scheme for isoreticular MOF series MPc-Cu-X (M = Co, Ni, X = NH, O) containing CoPc and NiPc units connected by Cu bis(diimine) and Cu bis(dioxolene) linkages. Reprinted with permission from Ref. [80]. Copyright 2020, American Chemical Society. (b) Illustration of the preparation for phenanthroline-doped ZIF-8; (c) FECO at various potentials on pristine ZIF-8, ZIF-A-LD, pristine ZIF-8/CB, and ZIF-A-LD/CB. (b,c) Reprinted with permission from Ref. [82]. Copyright 2019, Wiley-VCH. (d) Schematic illustration of the crystal structure of ZIF-8 and CALF20; (e) CO Faradaic efficiencies at different applied potentials for CALF20 and ZIF-8 in 1.0 mol/L KOH. (d,e) Reprinted with permission from Ref. [83]. Copyright 2021, American Chemical Society.

Fig. 9. (a) Scheme illustrating the synthesis of Ag@Al-PMOF hybrids. Reprinted with permission from Ref. [84]. Copyright 2020, Wiley-VCH. (b) Schematics for the Ag nanoparticle incorporated MOF structure. Reprinted with permission from Ref. [85]. Copyright 2020, American Chemical Society. (c) Schematic illustration of the synthetic procedure to obtain Zn-CoTAPc/PMo12 MLSs. Reprinted with permission from Ref. [86]. Copyright 2021, American Chemical Society.

Fig. 10. Structures of Cu8 clusters and unit cell in NNU-33(S) (a) and NNU-33(H) (b). (a,b) Reprinted with permission from Ref. [88]. Copyright 2021, American Chemical Society. (c) Illustration of the solvothermal synthesis of CuHHTP and preparation of Cu2O@CuHHTP via electrochemical treatment of CuHHTP. Reprinted with permission from Ref. [89]. Copyright 2020 Wiley-VCH. (d) Schematic of the two-step reconstruction process, including (1) the electrolyte-mediated chemical and structural transformation from Bi-MOF NR to Bi2O2CO3 NS, and (2) electrochemical reduction of Bi2O2CO3 NS to Bi NS, (e) SEM image for Bi-MOF NR, (f) Bi2O2CO3 NS and (g) TEM image for the final Bi NS. (e?g) Reprinted with permission from Ref. [90]. Copyright 2021 Wiley-VCH.

Table 3 Comparisons of different MOFs-based catalysts for CO2RR.

Catalyst	Cell	Electrolyte	J (mA cm^-2)	Product FE	Stability	Ref.
Cu₃(HHTQ)₂	H	0.1 mol/L KHCO₃	~0.5	CH₃OH 53.6%	10h@-0.4V	[76]
PcCu-O₈-Zn	H	0.1 mol/L KHCO₃	~8	CO 88%	10h@-0.7V	[77]
NiPc-NiO₄	H	0.5 mol/L KHCO₃	34.5	CO 98.4%	10h@-0.85V	[78]
PcCu-Cu-O	H	0.1 mol/L KOH	7.3	C₂H₄ 50%	4h@-1.2V	[79]
NNU-33(H)	flow	1 mol/L KOH	391	CH4 82%	5h@-0.9V	[88]
Cu₂O@CuHHTP	H	0.1 mol/L KCl/0.1 mol/L KHCO₃	10.8	CH₄ 73%	5h@-1.4V	[89]
Bi-MOF	H	0.1 mol/L KHCO₃	15	HCOO^‒ 92%	10h@-1.1V	[90]

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