Strategies for efficient CO2 electroreduction in acidic conditions

doi:10.1016/S1872-2067(23)64511-5

Abstract

Abstract:

CO₂ electroreduction is a promising technique to convert renewable electricity and CO₂ to high-value fuels and chemicals. Selectivity, energy efficiency, carbon efficiency and sustainability are the criteria for CO₂ electroreduction techniques suitable for industrial application. With alkaline and neutral electrolytes, carbonate formation from CO₂ leads to low carbon efficiency. High energy consumption to regenerate alkaline electrolyte and high resistance of neutral electrolyte cause low energy efficiency. Recently, CO₂ reduction with acidic electrolyte becomes a hot topic due to its potential to increase carbon efficiency and energy efficiency. Improving the selectivity towards CO₂ reduction is challenging in acidic condition. Diverse approaches were proposed to suppress H⁺ reduction and promote CO₂ reduction. However, fundamental issues about cation effect and local pH effect on CO₂ reduction in acidic condition are still under debate. Moreover, bicarbonate precipitation in gas diffusion electrode limits the sustainability with acidic electrolyte. This review tries to rationalize the reported strategies to improve the selectivity towards CO₂ reduction in acidic condition from mass transport and electrode reactions. Different approaches, including adding alkali cations, surface decoration, nanostructuring, and electronic structure modulation, are designed based on these two aspects. This review also introduces the recent progress in CO₂ electroreduction with metal cation-free acidic electrolyte. This strategy is deemed to improve the sustainability.

Key words: Carbon dioxide reduction, Electrocatalysis, Acidic electrolyte, Mass transport, Cation effect

Xinyi Zou, Jun Gu. Strategies for efficient CO₂ electroreduction in acidic conditions[J]. Chinese Journal of Catalysis, 2023, 52: 14-31.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(23)64511-5

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Figures/Tables 25

Fig. 1. Advantages and challenges of CO2RR techniques with acidic electrolyte and strategies to suppress HER and promote CO2RR.

Fig. 2. Schematic illustration of flow cell with KOH solution as electrolyte for CO2RR. Green and brown arrows indicate the flows of CO2 converted to reduction products and consumed by OH-, respectively. Advantages and disadvantages of CO2RR with alkaline electrolyte are shown.

Fig. 3. Schematic illustration of flow cell with near neutral KHCO3 solution as electrolyte for CO2RR. Green and brown arrows indicate the flows of CO2 converted to reduction products and consumed by OH-, respectively. Advantages and disadvantages of CO2RR with alkaline electrolyte are shown.

Fig. 4. Schematic illustration of flow cell with acidic electrolyte for CO2RR. CO2 molecules consumed by OH- are regenerated near the cathode and finally converted to reduction products.

Table 1 Summary of reported CO2RR performances in acidic condition.

Catalyst	Electrolyte	Type of cell	Major product	FE* (%)	SPCE* (%)	Ref.
Ag	0.2 mol L^‒1 H₂SO₄ + 0.01 mol L^‒1 Cs₂SO₄ (anolyte)	MEA with PEM	CO	80	90	[31]
Au/C	0.1 mol L^‒1 H₂SO₄ + 0.4 mol L^‒1 K₂SO₄	flow cell	CO	91	—	[34]
Ni₃N/CNTs	NaCl + HCl (pH 2.5)	H-cell	CO	50	—	[57]
Au	H₂SO₄ + Cs₂SO₄ (pH 2)	flow cell	CO	80	—	[58]
Ni-N-C	0.5 mol L^‒1 H₂SO₄ + 0.5 mol L^‒1 K₂SO₄ (anolyte)	MEA with PEM	CO	95	85	[56]
Ni@N-doped-C	1 mmol L^‒1 H₂SO₄ + 0.25 mol L^‒1 Na₂SO₄	flow cell	CO	84	—	[59]
Fe/porous C	0.2 mmol L^‒1 H₂SO₄ + 0.1 mol L^‒1 KCl	flow cell	CO	90	—	[60]
Ni-N-C	H₂SO₄ + Cs₂SO₄ (pH 2)	flow cell	CO	100	76	[61]
NiPc-OMe/CNTs	0.05 mol L^‒1 H₂SO₄ + 0.45 mol L^‒1 K₂SO₄	flow cell	CO	98	—	[62]
Ni-N-C	H₃PO₄ + KH₂PO₄ + KCl (pH 2)	flow cell	CO	99	—	[63]
Bi nanosheets	0.05 mol L^‒1 H₂SO₄ + 1 mol L^‒1 KCl	flow cell	HCOOH	92	27	[16]
S doped Sn	H₂SO₄ + K₂SO₄ (pH 3)	flow cell	HCOOH	92	35	[18]
SnO₂/C	0.1 mol L^‒1 H₂SO₄ + 0.4 mol L^‒1 K₂SO₄	flow cell	HCOOH	88	—	[34]
SnBi/SiC /PTFE	0.05 mol L^‒1 H₂SO₄ + 3 mol L^‒1 KCl	flow cell	HCOOH	90	65	[47]
Cs₃Bi₂Br₉/C	0.05 mol L^‒1 H₂SO₄ + 0.5 mol L^‒1 CsBr	flow cell	HCOOH	92	47	[54]
Bi porous electrode	H₂SO₄ + Na₂SO₄ (pH 2.7)	flow cell	HCOOH	89	—	[64]
Cu	1 mol L^‒1 H₃PO₄ + 3 mol L^‒1 KCl	flow cell	C₂₊	48	77 (50 for C₂₊)	[30]
Cu/C	0.1 mol L^‒1 H₂SO₄ + 0.4 mol L^‒1 K₂SO₄	flow cell	C₂₊	50	—	[34]
Cu	0.05 mol L^‒1 H₂SO₄ + 2.5 mol L^‒1 KCl	flow cell	C₂₊	90	70 for C₂₊	[46]
COF:PFSA/Cu	1 mol L^‒1 H₃PO₄ + 3 mol L^‒1 KCl	flow cell	C₂₊	75	45 for C₂₊	[49]
Cu porous nanosheets	0.05 mol L^‒1 H₂SO₄ + 3 mol L^‒1 KCl	flow cell	C₂₊	84	54 for C₂₊	[65]
Pd-Cu	H₂SO₄ + K₂SO₄ (pH 2)	flow cell	C₂₊	89	60 for C₂₊	[66]
Modified Cu	H₃PO₄ + KH₂PO₄ (pH 2)	flow cell	C₂₊	70	—	[67]
Ag	0.1 mol L^‒1 H₂SO₄	flow cell	CO	95	—	[32]
In	0.1 mol L^‒1 H₂SO₄	flow cell	HCOOH	76	—	[32]
Cu	0.2 mol L^‒1 H₂SO₄	flow cell	C₂₊	80	90	[50]

Table 1 Summary of reported CO2RR performances in acidic condition.

Catalyst	Electrolyte	Type of cell	Major product	FE* (%)	SPCE* (%)	Ref.
Ag	0.2 mol L^‒1 H₂SO₄ + 0.01 mol L^‒1 Cs₂SO₄ (anolyte)	MEA with PEM	CO	80	90	[31]
Au/C	0.1 mol L^‒1 H₂SO₄ + 0.4 mol L^‒1 K₂SO₄	flow cell	CO	91	—	[34]
Ni₃N/CNTs	NaCl + HCl (pH 2.5)	H-cell	CO	50	—	[57]
Au	H₂SO₄ + Cs₂SO₄ (pH 2)	flow cell	CO	80	—	[58]
Ni-N-C	0.5 mol L^‒1 H₂SO₄ + 0.5 mol L^‒1 K₂SO₄ (anolyte)	MEA with PEM	CO	95	85	[56]
Ni@N-doped-C	1 mmol L^‒1 H₂SO₄ + 0.25 mol L^‒1 Na₂SO₄	flow cell	CO	84	—	[59]
Fe/porous C	0.2 mmol L^‒1 H₂SO₄ + 0.1 mol L^‒1 KCl	flow cell	CO	90	—	[60]
Ni-N-C	H₂SO₄ + Cs₂SO₄ (pH 2)	flow cell	CO	100	76	[61]
NiPc-OMe/CNTs	0.05 mol L^‒1 H₂SO₄ + 0.45 mol L^‒1 K₂SO₄	flow cell	CO	98	—	[62]
Ni-N-C	H₃PO₄ + KH₂PO₄ + KCl (pH 2)	flow cell	CO	99	—	[63]
Bi nanosheets	0.05 mol L^‒1 H₂SO₄ + 1 mol L^‒1 KCl	flow cell	HCOOH	92	27	[16]
S doped Sn	H₂SO₄ + K₂SO₄ (pH 3)	flow cell	HCOOH	92	35	[18]
SnO₂/C	0.1 mol L^‒1 H₂SO₄ + 0.4 mol L^‒1 K₂SO₄	flow cell	HCOOH	88	—	[34]
SnBi/SiC /PTFE	0.05 mol L^‒1 H₂SO₄ + 3 mol L^‒1 KCl	flow cell	HCOOH	90	65	[47]
Cs₃Bi₂Br₉/C	0.05 mol L^‒1 H₂SO₄ + 0.5 mol L^‒1 CsBr	flow cell	HCOOH	92	47	[54]
Bi porous electrode	H₂SO₄ + Na₂SO₄ (pH 2.7)	flow cell	HCOOH	89	—	[64]
Cu	1 mol L^‒1 H₃PO₄ + 3 mol L^‒1 KCl	flow cell	C₂₊	48	77 (50 for C₂₊)	[30]
Cu/C	0.1 mol L^‒1 H₂SO₄ + 0.4 mol L^‒1 K₂SO₄	flow cell	C₂₊	50	—	[34]
Cu	0.05 mol L^‒1 H₂SO₄ + 2.5 mol L^‒1 KCl	flow cell	C₂₊	90	70 for C₂₊	[46]
COF:PFSA/Cu	1 mol L^‒1 H₃PO₄ + 3 mol L^‒1 KCl	flow cell	C₂₊	75	45 for C₂₊	[49]
Cu porous nanosheets	0.05 mol L^‒1 H₂SO₄ + 3 mol L^‒1 KCl	flow cell	C₂₊	84	54 for C₂₊	[65]
Pd-Cu	H₂SO₄ + K₂SO₄ (pH 2)	flow cell	C₂₊	89	60 for C₂₊	[66]
Modified Cu	H₃PO₄ + KH₂PO₄ (pH 2)	flow cell	C₂₊	70	—	[67]
Ag	0.1 mol L^‒1 H₂SO₄	flow cell	CO	95	—	[32]
In	0.1 mol L^‒1 H₂SO₄	flow cell	HCOOH	76	—	[32]
Cu	0.2 mol L^‒1 H₂SO₄	flow cell	C₂₊	80	90	[50]

Fig. 5. Comparison of single pass carbon efficiency (SPCE) and FE of CO2RR with acidic (pH < 3) and neutral or alkaline (pH > 7) electrolytes.

Fig. 6. Suppression of H+ reduction by cathodic reactions. (a) Schematic of the suppression of H+ reduction by OH- generated from CO2RR. Reprinted with permission from Ref. [68]. Copyright 2020, American Chemical Society. (b) Simulated pH profile at varied cathodic current density in 1 mol L?1 H3PO4 + 3 mol L?1 KCl based on reaction-diffusion model. (c) FE of H2 and methane from CO2RR on sputtered Cu GDE in 1 mol L?1 H3PO4 + 3 mol L?1 KCl at varied current density. Reprinted with permission from Ref. [30]. Copyright 2021, American Association for the Advancement of Science.

Fig. 7. Suppressing the migration of H+ by alkali cations. (a) HER polarization curves of Au RDE in 10 mmol L?1 HClO4 + 0?100 mmol L?1 LiClO4. The red dashed line indicates the limiting diffusion current density deduced from Levich equation. (b) GMPNP-simulated migration rate of H+ (in the form of current density) on Au RDE in 10 mmol L?1 HClO4 + 0?100 mmol L?1 LiClO4 at the limiting mass-transport condition. Reprinted with permission from Ref. [35]. Copyright 2022, American Chemical Society. Schematic illustrations of the migration of H+ in acidic solutions with alkali cations (c) and without alkali cations (d). Reprinted with permission from Ref. [34] with permission. Copyright 2022, Springer Nature.

Fig. 8. The distribution of pH value near the cathode under the condition that H+ reduction reaches the plateau current density (limiting mass-transport condition). (a) In acidic electrolyte free of alkali cations. (b) In acidic electrolyte containing alkali cations.

Fig. 9. Approaches to suppress H+ diffusion. (a) Covering the catalyst with organic adlayers. (b) Depositing porous materials onto the catalyst. (c) Constructing nano-catalysts with confinement structure.

Fig. 10. Suppressing H+ diffusion by covering the catalyst with organic adlayer. (a) Organic layer from N-tolyl pyridinium (tolyl-pyr) electrodeposition polymer on Cu electrode. (b) Limiting diffusion current of H+ reduction on bare Cu RDE and organic adlayer modified Cu RDE in HClO4-KClO4 solution (pH = 2.2). The diffusion coefficient of H+ (DH+) decreased by 23% after the modification. Reprinted with permission from Ref. [67]. Copyright 2023, Wiley-VCH GmbH.

Fig. 11. Physical obstacles for the diffusion of H+ towards cathode surface. (a) Simulation of H+ diffusion without and with the coating layers of polystyrene beads. Simulated pH distribution on Cu surface (b) without the coating and (c) with the coating. Reprinted with permission from Ref. [49]. Copyright 2023, Springer Nature.

Fig. 12. Schematic illustration of Ni nanoparticles encapsulated in N-doped carbon nanocage for CO2RR in acidic solution containing alkali cations. Reprinted with permission from Ref. [59]. Copyright 2022, American Chemical Society.

Fig. 13. Proposed reaction pathways of HER and CO2RR to diverse reduction products. The free energy differences of key intermediates determine the selectivity of reduction products are labeled by grey arrows.

Fig. 14. Modulation of kinetics of C?C coupling step. (a) Screening of M-Cu bimetallic (111) facets. The descriptors of C2+ activity (ΔGOCCOH*) and C2+ selectivity (ΔGOCCOH* ? ΔGCHO*) were calculated. Reprinted with permission from Ref. [66]. Copyright 2022, Springer Nature. (b) Free energy diagram of *CO-*CO coupling on Cu (100) facet without *OH and with *OH on the site nearby. In the right panel, red and blue balls indicate the top and sublayer of Cu atoms, respectively, and the numbers indicate the site of *OH adsorption. Reprinted with permission from Ref. [46]. Copyright 2023, Springer Nature.

Fig. 15. Simulated concentration profiles of H+ and alkali cations in acidic electrolyte at varied electrode potential. (a) The concentration profile of H+ in 10 mmol L?1 HClO4. (b) The concentration profile of Li+ in 10 mmol L?1 HClO4 + 10 mmol L?1 LiClO4. The electrode is Au.

Fig. 16. Effect of cations on the interfacial electric field strength. (a) Schematic illustration of the Gaussian surface to deduce the value of EStern. ρ is the spatial charge density in the diffuse layer, ε0 is the vacuum permittivity, εr is the relative permittivity, F is the Faradaic constant, zi is the number of charge of species i (i = H+, M+, ClO4-). (b) Schematic illustrations of hydrated Li+ and Cs+ accumulated at OHP. Reprinted with permission from Ref. [78]. Copyright 2020, Royal Society of Chemistry. (c) Simulated plots of electric field strength in Stern layer depending on electrode potential in acidic electrolyte with and without alkali cations. Reprinted with permission from Ref. [35]. Copyright 2022, American Chemical Society.

Fig. 17. Correlation between electric field strength and the kinetics of CO2RR. (a) Illustration of the Frumkin correction. The blue curve indicates the potential profile in the EDL. CO2 molecule located at the OHP is regarded as the acceptor of electron. (b) Schematic illustration of the interaction between the dipole moment of *CO2 intermediate and the electric field in Stern layer.

Fig. 18. Interaction between alkali cations and intermediates of CO2RR. (a) Schematic of the interaction between partially dehydrated Cs+ and *CO2 in the CO2-to-CO process. Reprinted with permission from Ref. [33]. Copyright 2021, Springer Nature. (b) Schematic of the proposed CO-to-C2H4 pathways with the coordination of alkali cations. *OCCO, *OCCOH, and *HOCCOH were identified to be coordinated by alkali cations. (c) Coordination with alkali cations stabilize *CO2 on Ag (111) facet and *OCCO on Cu (100) facet and promotes the electron transfer from the metal surface to the adsorbed intermediates. Isosurface shows the charge difference between the cation-coordinated case and the cation-uncoordinated case (isosurface value is 0.0006 e·a0?3). Yellow and cyan colors indicate charge accumulation and depletion, respectively. Reprinted with permission from Ref. [83]. Copyright 2022, Springer Nature.

Fig. 19. Strategies to accumulate alkali cations near the catalyst. (a) Schematic of Cu cathode decorated by perfluorosulfonic acid ionomer as cation-augmenting layer (CAL). Reprinted with permission from Ref. [30]. Copyright 2021, American Association for the Advancement of Science. (b) Simulated surface K+ density and current density distribution on the surface of Au needle with the tip radius of 5 nm. Reprinted with permission from Ref. [84]. Copyright 2016, Springer Nature. Simulated K+ distribution on (c) porous Cu nanosheet and (d) flat Cu nanosheet. Reprinted with permission from Ref. [65]. Copyright 2022, Springer Nature.

Fig. 20. CO2RR in metal cation-free acidic conditions. (a) Sustainability issues of CO2RR in alkali cation-containing acidic electrolyte. Schematic illustrations of the process of bicarbonate precipitation and alkali cation permeation through the PEM. (b) Schematic illustration of cathode decorated by c-PDDA in metal cation-free acidic electrolyte. The layer of c-PDDA suppresses H+ migration and enhances the interfacial electric field. (c) FE of CO from CO2RR with c-PDDA decorated Ag catalyst in 0.1 mol L?1 H2SO4 (orange) and bare Ag catalyst in 0.1 mol L?1 H2SO4 + 0.4 mol L?1 K2SO4 (blue). Reprinted with permission from Ref. [32]. This work is licensed under a CC BY 4.0 License.

Fig. 21. CO2RR with quaternary ammonium salts as supporting electrolyte. (a) Partial current density of ethylene from CO2RR on bare Cu foil (blue) and QAPPT decorated Cu foil (orange) in PipCl solution as the electrolyte. Modified from Ref. [91] with permission. Copyright 2023, Elsevier. (b) Partial current density of CO from CO2RR on Au/PTFE electrode (blue) and Ag/PTFE electrode (orange) at about ?0.95 V vs. RHE in solution with different bicarbonate salts as supporting electrolyte. Modified from Ref. [92] with permission. Copyright 2023, American Chemical Society.

Fig. 22. Schematic illustration of the combination of atomic-level DFT simulation, micro-kinetics of electrode reactions and finite element analysis of mass transport and homogeneous reactions in diffuse and diffusion layers for the simulation of CO2RR process in acidic condition.

Fig. 23. Four approaches to promote CO2RR in acidic electrolyte and the effects induced by each approach.

Fig. 24. Schematic illustration of MEA based on bipolar membrane (BPM) with non-noble metal-based catalyst for OER.

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Strategies for efficient CO₂ electroreduction in acidic conditions

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