Atomic-Site Coordination Tuning for Precise CO2 Electroconversion
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Atomic-Site Coordination Tuning for Precise CO2 Electroconversion
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  • Tianshang Shan
    Tianshang Shan
    School of Materials Science & Engineering, Beijing Institute of Technology, Beijing 100081, China
    Zhongguancun Academy, Beijing 100094, China
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  • Gengxian Zhou
    Gengxian Zhou
    School of Computer Science (National Pilot Software Engineering School), Beijing University of Posts and Telecommunications, Beijing 100876, China
    Zhongguancun Academy, Beijing 100094, China
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  • Hongpan Rong*
    Hongpan Rong
    School of Materials Science & Engineering, Beijing Institute of Technology, Beijing 100081, China
    *E-mail: [email protected]
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    Orcidhttps://orcid.org/0000-0002-3654-9199
  • Jiatao Zhang*
    Jiatao Zhang
    School of Chemistry and Chemical Engineering, Beijing Key Laboratory of Intelligent Molecular Materials and High-throughput Manufacturing, MIIT Key Laboratory of Medical Molecule Science and Pharmaceutical Engineering, MOE Key Laboratory of Cluster Science, Beijing Institute of Technology, Beijing 100081, China
    Beijing Institute of Technology, Zhuhai 519088, China
    *E-mail: [email protected]
    More by Jiatao Zhang
    Orcidhttps://orcid.org/0000-0001-7414-4902
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Precision Chemistry

Cite this: Precis. Chem. 2026, XXXX, XXX, XXX-XXX
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https://doi.org/10.1021/prechem.5c00434
Published March 9, 2026

© 2026 The Authors. Co-published by University of Science and Technology of China and American Chemical Society. This publication is licensed under

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Abstract

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Electrochemical carbon dioxide reduction (ECR) presents a promising avenue for achieving carbon neutrality by converting greenhouse gases into high-value fuels and chemicals. However, the advancement of ECR hinges on the precise design and synthesis of catalysts that exhibit high activity, selectivity, and stability. Single-atom site catalysts (SASCs), benefiting from their maximum atom-utilization efficiency, uniform and tunable active sites, and unique electronic properties arising from strong metal–support interactions, have emerged as a powerful platform for investigating the structure–activity relationship of ECR. By tuning coordination environments (e.g., coordination types and numbers) of isolated metal atoms, the electronic structure of metal active sites can be precisely modified for governing the selective synthesis of ECR products. Herein, this review systematically summarizes the precise synthesis strategies, advanced characterization techniques, and structure–activity relationships of SASCs in various coordination environments. Furthermore, the limitations and necessary precautions associated with the current characterization techniques are also discussed. Finally, we outline the future challenges and potential research directions of SASCs in the field of ECR.

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Published as part of Precision Chemistry special issue “Precision Chemistry for Single-Atom Catalysis”.

1. Introduction

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With the rapid acceleration of global industrialization, the massive consumption of fossil fuels has precipitated a drastic surge in carbon dioxide (CO2) emissions, triggering severe global environmental crises such as the greenhouse effect and ocean acidification. (1) Despite the continuous advancement of renewable energy technologies, projections indicate that fossil fuels will continue to dominate the global energy consumption structure until at least 2030, implying that carbon emissions will not be easily mitigated in the short term. (2) In this background, Carbon Capture, Utilization, and Storage (CCUS) technologies have garnered significant attention for their potential in carbon reduction. (3) Specifically, the CCUS pathway involving the conversion of CO2 into high value-added chemicals offers a promising solution to simultaneously address carbon emissions and energy shortages. (4) Currently, major CO2 conversion technologies include electrocatalysis, (5−12) thermocatalysis, (13−15) photocatalysis, (16−20) and biocoupled catalysis. (21−23) Among these, electrochemical CO2 reduction (ECR) dates back to the 19th century, when the French scientist Royer first achieved the reduction of CO2 to formic acid on a zinc electrode in 1870. (24) Distinguished by its environmental friendliness and sustainability, ECR utilizes clean electricity to drive the direct conversion of CO2 into C1 (e.g., CO, CH4, and HCOOH) and C2+ (e.g., C2H4, C2H5OH, and CH3COOH) value-added carbon-based fuels and chemicals under ambient conditions. (25−27) Consequently, this field has witnessed rapid development over the past century. (28−37)
Nevertheless, the practical implementation of the ECR faces substantial challenges. The core scientific obstacle lies in the high thermodynamic stability of the CO2 molecule, which possesses a strong C═O bond (bond energy: 806 kJ·mol–1). Furthermore, the reaction involves complex proton-coupled electron transfer (PCET) processes, resulting in sluggish kinetics and high reaction overpotentials. (38,39) Simultaneously, the competitive hydrogen evolution reaction (HER) at the cathode often diminishes the faradaic efficiency (FE) of carbon products, (40) while the high energy barrier for C–C coupling makes the selective regulation of high value-added C2+ products particularly difficult. (41) Therefore, the rational design and preparation of electrocatalysts with high activity, selectivity, and long-term stability are critical for the efficient operation of ECR. In recent years, single-atom site catalysts (SASCs), characterized by near 100% atom utilization efficiency and uniform active sites (defined as an isolated metal atom center coordinated with surrounding heteroatoms), have emerged as frontier materials in the ECR field. (42) The concept of such catalysts can be traced back to 1925, when Taylor first proposed a surface catalysis theory involving gaseous Ni single-atom active sites; (43) however, it did not initially attract widespread attention. The field entered a period of rapid expansion in 2011 after Zhang et al. explicitly conceptualized ″single-atom catalysis″ and introduced the M1/Support notation. (44) Since then, Li et al. have established a ″SASCs toolbox″ covering nearly all nonradioactive elements in the periodic table by developing precise synthesis methodologies─such as host–guest strategy, (45−47) in situ coordination strategy, (48,49) and high-temperature solid-phase reactions strategy. (50,51) These advances have significantly propelled the industrialization of SASCs in applications including automotive exhaust purification, (52) alkane dehydrogenation, (53) and ECR. (54) Compared to traditional nanocatalysts (e.g., bulk metals, (55−57) metal oxides, (58−61) and carbon materials (62,63)), SASCs with unique electronic properties arising from strong metal–support interactions offer a revolutionary platform for elucidating the structure–activity relationship in the field of ECR. By precisely regulating the coordination environment (e.g., coordination types and numbers) of metal active sites (64) at the atomic scale, SASCs are primarily categorized into M1-Nx (N: nitrogen), (65−67) M1-M’x (M’: another metal), (68−70) and M1-Ox (O: oxygen). (71,72)
In light of these developments, this Review systematically summarizes the precise synthesis strategies for SASCs with distinct coordination structures. Then, we critically evaluate the developments and intrinsic limitations of high-angle annular dark-field scanning transmission electron microscopy (AC-HAADF-STEM), (73) X-ray absorption fine structure spectroscopy (XAFS) (74) and Mössbauer spectroscopy (75) used for SASCs coordination detection. Next, the intrinsic correlations between these coordination structures and the catalytic ECR performance (C1 and C2+ products) are comprehensively elucidated. Finally, we provide a perspective on the future challenges and potential research directions of SASCs in the field of ECR, aiming to provide a roadmap for the further advancement and practical application.

2. Coordination Types of SASCs

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Driven by the high surface energy, isolated metal atoms are prone to agglomeration into thermodynamically more stable metal nanoparticles or clusters. (76) Thus, the anchoring effect provided by the coordinating atoms of the support is vital for achieving an atomic-level dispersion. In view of this, the term ″single-atom site catalysts″ (SASCs) is adopted in preference to ″single-atom catalysts″ (SACs) to emphasize that the intrinsic active sites are not merely the single metal atoms, but rather the ensembles formed by the isolated metal atoms and their surrounding coordinating atoms (e.g., M’, (77−79) N, (80−82) O, (72,82,83) C, (84−86) and S (87)). Based on the distinction of these coordinating atoms, we herein highlight the specific synthesis strategies for three main types of SASCs (M1-Nx, M1-M’x, and M1-Ox), offering a clear guide for their design principles.

2.1. M1-Nx

M1-Nx generally refers to active sites in carbon-based SASCs where a central metal atom coordinates with a varying number of N atoms and other nonmetal heteroatoms (typically ≤ 4, except for lanthanides (>4) mainly due to their larger ionic radii (1,88)), which have been widely applied in ECR research. (89−91) The more electronegative coordination heteroatoms of M1-Nx can create highly localized acceptor-like states near Fermi energy, leading to electron transfer from the metal atoms, which stabilizes the metal centers and effectively inhibits atomic aggregation. (92) In general, these coordination structures can be categorized into two main groups: symmetric M1-N4 (93−95) and asymmetric M1-NxAy, (96,97) where A represents vacancies (98−100) or nonmetal heteroatoms such as sulfur (S), (101,102) phosphorus (P), (103,104) boron (B), (105,106) O, (107,108) and chlorine (Cl). (109,110)
To construct these SASCs with diverse coordination structures, the synthesis can be broadly summarized as the strategic combination of metal precursors (111−117) with substrate precursors like N sources, (118−124) nonmetal heteroatom sources, (85,89,125) and C sources. (126−130) So far, pyrolysis remains the most widely used combination strategy to synthesize SASCs with symmetric M1-N4 or asymmetric M1-NxAy structures. For example, Li et al. used N-doped porous carbon, derived from the high-temperature carbonization of 2-Methylimidazole zinc salt (ZIF-8), as a support. By precisely adsorbing Ni2+ followed by thermal activation at varying temperatures (400–1200 °C), they successfully achieved fine-tuning of the Ni–Nx coordination structure. Quantitative extended XAFS (EXAFS) fitting revealed that the coordination number of Ni–Nx decreased from ∼4.06 at 900 °C to ∼3.54 at 1200 °C, directly proving that the temperature can drive the transition from symmetric Ni–N4 to asymmetric Ni–N3 (Figure 1a). (131) Besides, He et al. presynthesized NiO nanosheets as self-templates. Then, in an atmosphere of C/N species generated by urea decomposition, NiO was reduced to metallic Ni cores, while an N-doped carbon layer formed simultaneously on the surface. Finally, Ni atoms were anchored into the defects of the N-doped carbon layer via strong Lewis acid–base interactions, thereby forming SASCs with high-density asymmetric Ni–N2 single-atom sites (Figure 1b). (132) Certainly, asymmetric M1-NxAy SASCs can also be prepared via other methods. For instance, Dong et al. applied microwave treatment (1000 W, 5 s) to Cu2+-adsorbed amino-functionalized graphene nanosheets (AGNs) to rapidly synthesize Cu–N3 SASCs, as evidenced by the Cu–N coordination number of ∼ 2.8 from EXAFS fitting (Figure 1c). (133)

Figure 1

Figure 1. (a) Synthesis scheme of the Ni–N–C catalysts by using a N-doped carbon host to absorb Ni ions followed by thermal activation at different temperatures to tune the Ni–N bond structures and establish structure–property correlations. Reproduced from ref (131). Copyright 2022, Royal Society of Chemistry. (b) Schematic illustration for the formation of the Ni-NC@Ni catalyst. In the green circle: the possible atomic structure of the Ni–N species. Reproduced from ref (132). Copyright 2020, Elsevier. (c) Schematic illustration of the preparation strategy for PSB-CuN3 and PS-CuN4. Reproduced from ref (133). Copyright 2023, Springer Nature. (d) Schematic illustration for the preparation of Ni–PxNy. Reproduced from ref (91). Copyright 2023, Springer Nature. (e) The formation process of atomically dispersed SnN3O1 active sites. Reproduced from ref (107). Copyright 2021, Wiley-VCH. (f) Schematic illustration of the proposed formation mechanisms. Reproduced from ref (118). Copyright 2021, Springer Nature.

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In addition to the aforementioned strategies for synthesizing asymmetric SASCs solely via pyrolysis, the introduction of heteroatoms is another common strategy. For example, Qu et al. successfully constructed SASCs with Ni–N4, Ni–P1N3, and Ni–P2N2 coordination by simply regulating the content of triphenylphosphine (PPh3) confined within the MOF (Figure 1d). (91) Guo et al. utilized a vapor transport strategy, where gaseous SnO2 was trapped by N-doped carbon supports at high temperatures to fabricate Sn SASCs. EXAFS analysis quantitatively determined the first coordination shell of Sn was coordinated with N3O1, with no detectable Sn–Sn bonds, thereby definitively proving the successful synthesis Sn-NOC with Sn–N3O1 coordination (Figure 1e). (107) In a different approach, Wang et al. adopted a simultaneous cation–anion diffusion strategy to synthesize Bi1–N3S1 SASCs. In detail, they used Bi2S3 as the Bi source, S source, and sacrificial template. Next, under high-temperature pyrolysis conditions (5% NH3/Ar, 900 °C), Bi and S species can diffuse into the polydopamine (PDA)-derived N-doped carbon coating on the Bi2S3 surface. Followed by HNO3 etching, Bi-SAs-NS/C SASCs with a Bi1–N3S1 coordination was successfully obtained (Figure 1f). (118)
In summary, the current focus on M1-Nx SASCs research mainly lies in engineering coordination atoms. Nevertheless, the role of the carbon matrix, specifically its defect density, graphitization degree, and heteroatom distribution, is also critical for the stability and electronic structure of the single-atom sites. Defects such as vacancies and edges act as vital anchoring points for immobilizing metal atoms, while the graphitization level dictates the support’s conductivity and thus charge transfer efficiency in ECR. (134,135) Moreover, the distribution and local concentration of heteroatoms within the carbon framework fine-tune the electron density and ligand field around the metal center, directly modulating the catalytic behavior. Therefore, these aspects deserve further in-depth exploration. (136) To date, M1-Nx SASCs have emerged as one of the most widely studied electrocatalysts in the field of ECR, largely because they can be synthesized on a gram-scale via simple pyrolysis strategies. (129,137) Also, some special synthesis methods have been developed, such as electroreduction (138) and recrystallization. (139) However, the structure–activity relationship between coordination structures and the CO2 catalytic activity remains to be elucidated.

2.2. M1-M’x

M1-M’x, also known as single-atom alloys (SAAs), denotes a structure where a target single metal atom (M1) is anchored onto a different metal substrate (M’). (140) Generally, the synthesis of SAAs relies on two principles: (1) the bond energy between the target atom and the host metal is stronger than the bond energy between the host atoms themselves; and (2) the target atoms are present at a very low surface concentration (usually <1%) and are isolated by the host metal atoms. (141) Unlike traditional disordered alloys, SAAs not only effectively prevent the migration and aggregation of the target single atoms, but also allow the electronic structure of the active sites to be tuned through electronic interactions between the different metals. (79)
Currently, various strategies have been developed to synthesize SAAs for ECR. These mainly include wet-chemistry, (77,79) galvanic replacement, (142,143) electroreduction, (78,144) and pyrolysis. (68,145) Following this overview, we describe each method individually. As shown in Figure 2a, Liu et al. employed a wet-chemistry method to mix tin (Sn) and copper (Cu) precursors in an alkaline solution, followed by reduction with NaBH4. After washing and vacuum drying, they obtained Sn1Cu-SAA nanobelts with a length of 2–3 μm, in which isolated Sn atoms were embedded in the Cu lattice. (77) In another study, Liu et al. prepared Bi nanoparticles via a hydrothermal method and then used controlled addition of RuCl3 to replace Bi atoms by galvanic replacement method. This achieved uniform dispersion and stabilization of Ru single atoms (0.6 wt %) on the Bi support, constructing a Ru1@Bi SAA catalyst (Figure 2b). (143) Jin et al. successfully synthesized a novel Mo1Cu SAA through a stepwise chemical conversion combined with an in situ electroreduction strategy, which is at ambient temperature in a typical flow cell (Figure 2c). (144) Moreover, Tuo et al. adopted a stepwise pyrolysis approach in which they synthesized a NiZn bimetallic metal organic framework (MOF) precursor via a hydrothermal method and then performed controlled pyrolysis at different temperatures (700, 800, and 900 °C). The volatility of Zn at high temperatures was utilized to adjust its residual content, successfully constructing carbon-supported NiZn bimetallic catalysts. Among them, the NiZn0.03/C sample obtained after pyrolysis at 900 °C possessed a strongly electronically coupled Ni–Zn dual-site structure. This led to a moderate downshift of the d-band center, achieving the Sabatier-optimal adsorption balance during the process of ECR (Figure 2d). (145)

Figure 2

Figure 2. (a) Schematic synthesis process of the Sn1Cu-SAA. Reproduced from ref (77). Copyright 2025, Wiley-VCH. (b) Schematic representation of the preparation of the Ru1@Bi and Run@Bi catalysts. Reproduced from ref (143). Copyright 2024, Wiley-VCH. (c) Schematic diagram for the preparation of Mo1Cu catalysts. Reproduced from ref (144). Copyright 2025, Wiley-VCH. (d) Schematic diagram of the NiZn0.03/C bimetallic catalyst synthesis process. Reproduced from ref (145). Copyright 2023, Wiley-VCH.

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Apart from the synthesis methods introduced above, photodeposition, (146) laser ablation, (147) and physical vapor deposition (PVD) (148) are also used to prepare single-atom alloy catalysts. However, these methods are rarely applied in the field of ECR, possibly due to the limited accessibility of the required specialized equipment, thus presenting research opportunities for further exploration.

2.3. M1-Ox

Similar to the definitions of M1-Nx and M1-M’x, M1-Ox is defined as an active site where a single metal atom is anchored by multiple electronegative O atoms (usually ≤4). (149) However, M1-Ox are mainly supported on metal oxides, (83,150−153) MOFs, (154,155) and MXenes, (156) rather than carbon materials. (7) This sharp contrast to M1-Nx can be attributed to the specific bonding nature of O atoms, which, with six valence electrons and a tendency to form two bonds, typically exist as unstable surface or edge functional group on carbon supports instead of lattice integration. (157,158) In contrast, the O atoms in metal oxides, MOFs, and MXenes are part of the rigid skeleton, allowing them to firmly anchor single metal atoms and form stable M1-Ox structures. (159)
In recent years, metal oxide-supported M1-Ox SASCs have attracted significant attention in the ECR field due to their industrial importance. Their synthesis strategies mainly include impregnation, (159,160) Li-molten salt, (158,161) and coprecipitation. (162) Among them, impregnation can be simply described as introducing metal precursors onto a prepared support and converting them into single-atom sites during subsequent treatment. (52) For example, Guo et al. synthesized pure monoclinic BiVO4 via a solvothermal method. Then, they removed Bi by using NaBH4 reduction to create Bi vacancies. Finally, Cu single atoms were stably anchored onto these vacancies through electrostatic interactions, successfully producing Bi1–xVO4–Cu SASCs with a Cu loading of ∼ 1 wt % (Figure 3a). (160) An alternative synthetic strategy is Li-molten salt, which leverages the low melting point of lithium (180 °C) and its capability to disperse metals. Based on this, SASCs are prepared by achieving atomic-level dispersion through methods like ultrasonication. (163) For instance, Xu et al. successfully synthesized Cu–C catalyst coordinated with O from hydroxyl and carboxyl groups by mixing Cu bulk with molten lithium, followed by steps including ultrasonic dispersion, quenching, air humidification, and water washing (Figure 3b). (158) For the coprecipitation strategy, it can also be used to synthesize SASCs. In this method, two or more metal cations in a solution react with a precipitant, followed by air calcination to obtain SASCs. For example, Yang et al. used the reducing effect of NH3·H2O to coprecipitate Cu(NO3)2·3H2O and ZrO(NO3)2·xH2O into a Co-p-CuZr-0.0 precursor. After calcining at 500 and 900 °C for 3 h, they successfully prepared Cu single-atom catalysts supported on ZrO2 with two different crystal phases, namely Cu1O3-tZrO2 and Cu1O4-mZrO2 (Figure 3c). (83)

Figure 3

Figure 3. (a) Schematic illustration of preparing Bi1–xVO4–Cu. Reproduced from ref (160). Copyright 2024, Wiley-VCH. (b) Step-by-step preparation of the carbon-supported Cu SA catalyst using an amalgamated Cu–Li method. Reproduced from ref (158). Copyright 2020, Springer Nature. (c) Schematic illustration of the support crystal phase engineering and reaction mechanisms on the surface of Cu1O3-tZrO2 and Cu1O4-mZrO2. Reproduced from ref (83). Copyright 2025, American Chemical Society. (d) Illustration of the synthesis of Zr-BTB-In. Reproduced from ref (154). Copyright 2025, Wiley-VCH. (e) Schematic illustration of the fabrication of SA-Cu-MXene via selective etching of quaternary MAX-Ti3(Al1–xCux)C2. Gray, blue, red, yellow, brown, and green balls represent Al, Ti, Cu, O, C, and Cl atoms, respectively. Reproduced from ref (156). Copyright 2021, American Chemical Society.

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In addition to metal oxides, MOFs and MXenes can also serve as supports for the M1-Ox SASCs. For example, Li et al. synthesized an ultrathin 2D MOF (Zr-BTB) using ZrCl4 and 1,3,5-Tris (4-carboxyphenyl) benzene (BTB) via a solvothermal method. Then, they stirred Zr-BTB in InCl3 at 60 °C for 12 h to synthesize Zr-BTB-In catalyst with an In loading of about 2.5 wt % (Figure 3d). (154) Zhao et al. strategically introduced ZnCl2 during the synthesis of the SA-Cu-Mxene catalyst, where it reacts with aluminum (Al) during pyrolysis (600 °C, 5 °C/min, 5 h) to form volatile AlCl3. This allows unreacted Cu to remain loaded on the MXene skeleton. Finally, the SA-Cu-Mxene catalyst with Cu–O3 coordination was successfully synthesized (Figure 3e). (156)
Overall, compared to M1-Nx SASCs mentioned in the previous sections, there are fewer studies on M1-Ox SASCs in the ECR field, which can be attributed to the higher synthetic complexity relative to the simple pyrolysis strategy. In addition, synthesis strategies such as ball milling, (164) atomic layer deposition (ALD), (165) and microemulsion (52) are rarely seen in this area. However, M1-Ox SASCs still represent a promising area for further exploration in ECR research.

3. Coordination Detection of SASCs

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The previous section systematically reviewed the precise synthesis strategies for three main coordination types (M1-Nx, M1-M’x, and M1-Ox) of SASCs, providing practical pathways for their preparation and laying a foundation for investigating their structure–activity relationships in the field of ECR. In particular, it is worth noting that the fine coordination structures of SASCs currently rely on advanced characterization techniques such as AC-HAADF-STEM, XAFS (e.g., X-ray absorption near edge structure (XANES) and EXAFS), and Mössbauer spectroscopy. Nevertheless, these techniques still have intrinsic limits. Therefore, building upon a detailed review of the historical evolution of each technique, this chapter also critically evaluates their respective strengths and limitations to provide reference for future research.

3.1. AC-HAADF-STEM

AC-HAADF-STEM has undergone nearly a century of development. In the 1930s, Manfred von Ardenne attempted to replace visible light with electron beams of extremely short wavelengths, developing the world’s first scanning transmission electron microscope (STEM). (166,167) However, its resolution remained severely limited for decades due to the low brightness of thermal cathodes and the inherent spherical aberration (pointed by Scherzer (168) in 1936) of electromagnetic lenses. A turning point arrived in 1970 when Crewe introduced a high-brightness field emission gun (FEG) combined with an annular dark-field (ADF) detector, successfully capturing blurry images of uranium (U) and thorium (Th) atoms on a carbon film using STEM for the first time. (169) Subsequently, in the 1990s, Pennycook refined the high angle ADF (HAADF) imaging theory, clarifying that collecting high-angle incoherent scattered electrons enables ″atomic number (Z)-contrast″ imaging. In this mode, intensity is proportional to Z2, thereby offering a robust basis for directly distinguishing heavy atoms. (170)
Nevertheless, image clarity remained limited by spherical aberration of lens defects until the late 1990s, when Haider and Krivanek successfully developed the spherical aberration corrector. Acting like ″corrective glasses″ for the microscope, this device historically compressed the electron beam probe to the subangstrom scale (<0.1 nm). (173,174) Thus, the STEM with a perfect combination of aberration correction (AC), the HAADF, and other components (Figure 4a) offers extremely high resolution and exceptional identification of heavy atoms. Following the pioneering work of Zhang et al. in 2011, which achieved the direct observation of Pt single atoms on FeOx (Figure 4b), this technique was established as the ″gold standard″ for characterizing atomic-level microstructures, particularly for visualizing the dispersion of single atoms. (44)

Figure 4

Figure 4. (a) General schematic of an electron microscope in STEM modes with a condenser lens, objective lens, aberration correctors, projector system, retractable detectors, EDS (energy dispersive X-ray spectroscopy), and EELS (electron energy loss spectroscopy) acquisition. p.s. BF (bright-field), ABF (annular bright-field). Reproduced from ref (171). Copyright 2021, Wiley-VCH. (b) Pt single atoms (white circles) are seen to be uniformly dispersed on the iron oxide (FeOx) support (left) and occupy exactly the positions of the Fe atoms (right). Reproduced from ref (44). Copyright 2011, Springer Nature. (c) Schematic diagram of XAFS measurements with fluorescence yield experiment setup. Reproduced from ref (74). Copyright 2024, Springer Nature. (d) Schematic diagram of Pd–O4/BWO and Pd–O3/BWO. (e) Fourier transforms of the EXAFS spectra of the Pd K-edge spectra. Reproduced from ref (172). Copyright 2025, Springer Nature. (f) Schematic diagram of operando Mössbauer spectroscopy for tracking the metastable states of atomically dispersed tin (Sn) in copper oxide (CuO) for selective CO2 electroreduction. Reproduced from ref (162). Copyright 2023, American Chemical Society.

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3.2. XAFS

The evolution of XAFS technology dates back to 1920, when Fricke first observed oscillatory phenomena on the high-energy side (>200 eV) of the K-edge absorption spectra for elements ranging from magnesium (Mg) to chromium (Cr), though the underlying mechanism remained unexplained. (175) In 1931, Kronig attempted to clarify it by proposing the Long-Range Order (LRO) theory. (176) However, he erroneously attributed the oscillations to Bragg diffraction of photoelectrons within the lattice’s periodic potential. This led to a widespread misconception that materials lacking long-range order were incapable of generating XAFS signals, thereby severely impeding the technique’s application.
A paradigm shift was initiated in 1971 by the seminal publication of Sayers, Stern, and Lytle (SSL). (177) They confirmed that oscillatory phenomena on the high-energy side essentially originate from the quantum interference effect between the outgoing photoelectron wave and the backscattered wave from neighboring atoms by proposing Short-Range Order (SRO) theory. Also, they introduced the use of Fourier Transform to convert energy-space (k-space) oscillations into a radial distribution function (R-space), enabling the direct extraction of local structural parameters, including coordination types, numbers and bond lengths. This breakthrough marked the inception of modern XAFS, establishing it as a potent tool for investigating noncrystalline materials. Concurrently, the invention of high-brightness synchrotron radiation sources (104 to 106 times brighter than traditional X-ray tubes) greatly improved data acquisition efficiency and signal-to-noise ratios, paving the way for in situ investigations. (178) On the theoretical front, the multiple scattering theory developed by Rehr and Albers in the 1990s further advanced the field, allowing for the construction of atomic oxidation states and 3D geometries via XANES. (179)
In the 21st century, with the subangstrom resolution in analyzing coordination environments (e.g., coordination types and numbers) of XAFS, SASCs have entered a golden age for identifying single-atom active sites (such as M–N-C). Given the relatively low metal loading of SASCs (typically <1 wt %), XAFS measurements are predominantly conducted in fluorescence mode rather than transmission mode using a multielement solid-state detector (e.g., Ge or Si drift detector) to ensure a sufficient signal-to-noise ratio (Figure 4c). (74,180) For example, Li et al. used EXAFS technique to confirm the Pd–O4 and Pd–O3 coordination structure in the synthesized Pd–O4/BWO and Pd–O3/BWO catalysts with a Pd loading of approximately 0.05 wt % (Figure 4d, e). (172)

3.3. Mössbauer Spectroscopy

In contrast to XAFS that relies on the photoelectric effect excited by X-rays, Mössbauer spectroscopy mainly operates on a unique principle utilizing high-energy γ-rays, which is named as ″recoil-free nuclear resonant fluorescence″ observed by Rudolf Mössbauer in 1958. (181) However, this initial observation required embedding 191Iridium (Ir) atoms in a solid lattice at cryogenic temperatures, suffering from harsh experimental requirements and limited versatility. A major breakthrough occurred with the in-depth investigations by Pound et al. on the Mössbauer effect of 57Fe. Due to its low γ-ray energy (14.4 keV) and ubiquity in nature and industry, 57Fe propelled this technology into an era of rapid development. (182,183)
While XAFS provides coordination structures (e.g., coordination types and numbers) of SASCs, Mössbauer spectroscopy offers site-average resolution sensitive to subtle electronic variations, enabling the precise identification of active sites with identical coordination but different geometries or spins. (184) For instance, Li et al. utilized this technique to deconvolute Fe–N4 sites into two distinct types: D1 (doublet with QS = 0.9–1.2 mm·s–1) and D2 (doublet with QS = 1.8–2.8·s–1). (185) Chen et al. tracked the structural evolution of single Tin (Sn) atoms on a copper oxide (CuO) support under ECR conditions via operando Mössbauer spectroscopy. This finding clearly demonstrated a transformation from Sn4+-O4–Cu2+ to a metastable Sn4+-O3–Cu+ configuration, providing critical insights into the role of single Sn atoms in tuning the electronic structure of the catalyst (Figure 4f). (162)

3.4. Intrinsic Limits

Although AC-HAADF-STEM, XAFS, and Mössbauer spectroscopy collectively constitute the cornerstone for characterizing the coordination environments of SASCs, it must be acknowledged that no single technique offers a flawless resolution of all structural details. In the following section, the intrinsic limits of each advanced characterization technique are critically discussed.
AC-HAADF-STEM, despite its capability to achieve atomic-level resolution, is severely limited by electron irradiation damage (e.g., knock-on damage and ionization damage) arising from high-energy electron beams (accelerating voltage up to 300 kV). (189) For M1-Nx and M1-M’x SASCs, the high density of delocalized electrons can facilitate the ultrafast quenching (<1 fs) of holes generated by incident electrons. Consequently, the typically more destructive ionization damage is effectively suppressed, leaving knock-on damage, where incident electrons elastically displace atoms via momentum transfer, as the dominant mechanism (Figure 5a). (186) To address this, lowering the accelerating voltage (30–80 kV) is a simple but useful strategy to preserve the pristine structure of SASCs. (190) Conversely, for generally poorly conductive M1-Ox SASCs, ionization damage induced by inelastic scattering usually predominates, as holes generated by incident electrons cannot be rapidly neutralized, resulting in lifetimes often exceeding the period of atomic vibration. During this interval, the electronic wave functions can be perturbed (e.g., via vibrational excitation), and a portion of the excitation energy is stored as potential energy, leading to bond destabilization and structural degradation (Figure 5b). (187) Herein, reducing the electron dose or increasing the accelerating voltage energy (to decrease the differential scattering cross-section) are effective to minimize the destruction of SASCs active sites. (191) Also, it is crucial to note that AC-HAADF-STEM only sees a very small area (typically nanometers), which makes it hard to represent the whole sample. In other words, we cannot confirm whether the metal species of SASCs are uniformly dispersed as single atoms based on just a few tiny images. Therefore, it is necessary to combine it with other advanced characterization techniques such as XAFS.

Figure 5

Figure 5. (a) Elastic scattering of electrons from an atomic nucleus, shown schematically (particle model) for a large-angle collision (A) and a 180° collision (B). Sputtering of atoms from the beam-exit surface (C) and the beam-entry surface (D). Reproduced from ref (186). Copyright 2010, Elsevier. (b) Energy-band diagram of a metal (left) and a semiconductor or insulator (right), electron energy being plotted vertically upward. CB and VB represent the conduction and valence bands, f is the work function, Evac, Ef and Eg are the vacuum energy, Fermi energy, and CB-VB energy gap. Upward arrows represent single-electron excitations, while downward arrows are de-excitation processes (filling of a VB or K-shell hole). K-shell excitation in an organic material is shown on the right, with Ekin being the typical kinetic energy of an excited K-shell electron. This process also results in the emission of Auger electrons from the VB, with an energy of about 270 eV. Reproduced from ref (187). Copyright 2013, Elsevier. (c) Schematic diagram of heterogeneous Pt/CeO2 SASCs using EXAFS. (d) Scattering paths for SASCs and small clusters. Schematic depiction of scattering paths present in oxide-supported metal catalysts with a heterogeneity of the metal-site structure including isolated metal sites (middle) as well as metal (left) or oxidized (right) nanoclusters. Bonds are for representation only. Color code: metal (gray), oxygen (red), and support metal cation (brown). (e) R-factor of the 5-path SAC fit to data sets with varying contributions from the Pt/CeO2 SASCs site and metallic Pt13 cluster. The inset shows a zoomed-in region with 70–100% SAC sites (30–0% Pt13 cluster sites). Data are taken over Δk = 3–18 Å–1. (f) Modeled FT EXAFS data for mixtures of the Pt/CeO2 SASCs site and metallic Pt13 cluster. Reproduced from ref (188). Copyright 2023, American Chemical Society.

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Currently, XAFS analysis is a powerful tool for characterizing the coordination environment of SASCs. Specifically, the XANES provides insights into the metal oxidation state, electronic properties, and bonding geometry, while the EXAFS reveals the local coordination environment of atom type, number, and bond length (within ∼5 Å). (192) Therefore, EXAFS is widely employed to detect the absence of metal clusters in SASCs. However, since its signals are dominated by the scattering paths of the major species, the resulting spectrum represents a bulk averaged structure if the sample contains mixed species (e.g., single atoms and nanoclusters), potentially masking the true configuration of the active sites. (193,194) Moreover, the EXAFS peak intensity may also sharply decrease with small particle size. (195,196) For instance, Finzel et al. demonstrated that the R-factor (a quality of fit metric that quantifies the misfit between data and model) of EXAFS lacks sensitivity to the scattering paths (e.g., M-M, M-O, and M-O-M) of small mixed species in Pt/CeO2 (Figure 5c, d). In detail, even when the Pt/CeO2 catalyst contained approximately 40% Pt14O37 clusters (d: ∼1 nm), the R-factor derived from a pure single-atom model remained below 1%, satisfying the conventional standard for a ″good″ fit (Figure 5e, f). Additionally, this insensitivity can be visually confirmed by the barely discernible changes in the simulated Fourier transformation (FT)-EXAFS data. (188) These findings imply that relying solely on a low R-factor is statistically insufficient to confirm the absence of small clusters in SASCs. Therefore, it is recommended to carefully scrutinize the features of scattering paths (e.g., M-M, M-O, and M-O-M) in the high R-space, employ linear combination fitting to quantitatively assess the potential presence of clusters, and incorporate continuous Cauchy wavelet transform (CCWT) to assist in identifying weak cluster signals. (197,198)
For Mössbauer spectroscopy, despite its exquisite sensitivity to electronic structures of SASCs, it also suffers from a critical inherent limitation. Although Mössbauer effect has been observed in approximately 40 elements, suitable Mössbauer-active isotopes (e.g., 57Fe, 119Sn, 121Sb, and 151Eu) remain rare when considering the technical and analytical challenges. (199) Herein, this technique is frequently employed as a specialized complementary technique in conjunction with AC-HAADF-STEM and XAFS to provide unique insights into oxidation states, spin states and coordination symmetries of SASCs. (180)
In summary, to obtain comprehensive and accurate coordination structures of SASCs, researchers must adopt a ″multitechnique combination″ strategy, leveraging the complementary strengths of AC-HAADF-STEM, XAFS, and Mössbauer spectroscopy to cross-validate findings and overcome the inherent bottlenecks of individual characterization techniques.

4. Structure–Activity Relationship of SASCs

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The preceding sections have comprehensively elaborated on the precise synthesis strategies and structural characterization of SASCs with diverse coordination types, establishing a solid material foundation for an atomic-level understanding of the structure–activity relationships in the field of ECR. Then, it is essential to recognize that ECR is intrinsically a complex PCET process (Figure 6). Table 1 presents the standard potentials (E0, vs SHE) for ECR and the competitive HER in aqueous media. Notably, an external driving force is necessary to overcome the barrier for the initial reduction of the mass of CO2. Following this, diverse hydrocarbons are generated via PCET process. (200) As the number of electron transfers increases (2e– to 18e–), the reaction pathways exhibit high diversity, resulting in a broad product distribution from C1 products (e.g., 2e– CO and HCOOH, up to 8e– CH4) to complex C2+ products (e.g., 10e– CH3CHO, 12e– C2H4 and C2H5OH, and even 18e– CH3CH2CH2OH). (39) Although the specific reaction steps of ECR may initially appear intricate, a broad consensus based on the Sabatier principle and density functional theory (DFT) calculations has suggested that the adsorption energy of key intermediates on the highly uniform active centers is the governing factor determining catalytic performance. (201) In light of this, this section discusses the rational design principles of SASCs tuning for specific target products, incorporating current insights into the ECR mechanism.

Figure 6

Figure 6. Overview of reaction pathways for ECR toward different products. Black spheres, carbon; red spheres, oxygen; white spheres, hydrogen; blue spheres, (metal) catalyst. The arrows indicate whether proton, electron or PCETs take place. Reproduced from ref (39). Copyright 2019, Springer Nature.

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Table 1. Standard Potentials of ECR in Aqueous Media at 1 atm and 25 °C
Half-cell reactionStandard potentials(V vs SHE)
2H+ + 2e– → H2–0.42
CO2 + e– → *CO2––1.9
CO2 + 2H+ + 2e– → CO + H2O–0.52
CO2 + 2H+ + 2e– → HCOOH–0.61
CO2 + 4H+ + 4e– → HCHO + H2O–0.51
CO2 + 6H+ + 6e– → CH3OH + H2O–0.38
CO2 + 8H+ + 8e– → CH4 + 2H2O–0.24
2CO2 + 12H+ + 12e– → C2H4 + 4H2O–0.34
2CO2 + 12H+ + 12e– → C2H5OH + 3H2O–0.33

4.1. CO2 to C1 Products

As illustrated in Figure 6, the major C1 products, including CO, HCOOH, CH2O, CH3OH, and CH4, are highlighted in blue boxes. It is generally accepted that *COOH serves as the key intermediate for the conversion of CO2 to CO. This pathway can proceed via a PCET process or a sequential electron transfer-proton transfer (ET-PT) route. (200,202,203) Subsequently, derived from the PCET reduction of *COOH, the *CO species is widely regarded as the pivotal intermediate for the synthesis of CH2O, CH3OH, and CH4. (204) In contrast, the key intermediate for HCOOH or HCOO– remains controversial, and the proposed mechanisms mainly involve either *OCHO adsorbed via single/double oxygen atoms (monodentate/bidentate) or *HCOO formed via an anionic hydride-mediated pathway. (39,205) Based on these consensuses, the following section explores the rational design principles of SASCs tailored for specific C1 products.

4.1.1. CO

ECR-to-CO represents a promising dual-benefit strategy, as it not only mitigates global warming but also facilitates the carbon-neutral cycle by producing CO, a vital feedstock for the Fischer–Tropsch process and other industrial synthesis. (206) Recent literature indicates that catalysts capable of highly efficient CO production are predominantly centered on M1-Nx SASCs, with a smaller portion involving M1-M’x and M1-Ox SASCs. Accordingly, we will discuss these types of SASCs for ECR-to-CO in sequence.
To date, most reported M1-Nx SASCs (particularly those based on transition metals such as Ni, (81) Fe, (207) and Co (115)) have exhibited FECO exceeding 90%. However, it remains challenging to directly compare the intrinsic activities, selectivities, and reaction mechanisms of different metal centers due to the structural heterogeneity inherent in their synthesis. Herein, Chang et al. employed a series of transition-metal porphyrins (TM-Pcs) as well-defined model platforms to systematically investigate the intrinsic roles of isolated transition metals (Fe, Co, Ni, Cu, and Zn) in ECR-to-CO research (Figure 7a). Their findings revealed that Co-Pc exhibited the most superior CO activity (FE = 95%, E = −0.7 V vs RHE, jCO = 8.6 mA·cm–2). In-situ XAFS confirmed that the TM-N4 coordination structure remained unchanged during ECR, which can be attributed to the strong covalent interactions between the transition metal (TM) and N atoms. Further DFT calculations elucidated that the moderate binding strength of the Co-Pc active center toward key intermediates (*HOCO and *CO) was the mechanistic origin of its exceptional performance (Figure 7b). (116) Although Ni-Pc exhibits higher energy barriers for *HOCO and *CO than Co-Pc, leading to lower CO activity, its low-cost and modifiable electronic structure have driven extensive research into Ni-based SASCs for CO production. For instance, Wang et al. introduced the S atom (∼2.58), which is less electronegative than the N atom (∼3.04), to form a Ni–N3S coordination structure, thereby increasing the d-orbital electron density of the Ni atoms. DFT calculations demonstrated that the Ni–N3S site possesses a lower energy barrier for *COOH formation compared to that of the Ni–N4 site. Experimentally, the Ni–N3S–C SASCs achieved maximum FECO of 98.6%, 94.8%, and 90.5% at a current density of 100 mA·cm–2 in alkaline, acidic, and neutral electrolytes, respectively (Figure 7c). (102)

Figure 7

Figure 7. (a) Schematic illustration of CO2RR over a chemical unit of the TM-Pcs. (b) Free energy diagram of TM-PCs for CO2RR at V = 0 V. Reproduced from ref (116). Copyright 2022, American Chemical Society. (c) Stability test of Ni–N3S–C in flow cell with alkaline, acidic, and neutral electrolyte. The electrolytes are 1 M KOH (alkaline, pH = 14), 0.05 M H2SO4 + 1 M KCl (acidic, pH = 1), and 1 M KHCO3 (neutral, pH = 8.2). Reproduced from ref (102). Copyright 2025, Wiley-VCH. (d) Top-left, top-right: Top view and side view optimized adsorption configuration on simulated FeN4 and O–Fe–N-C (Fe, O, N, and C atoms are represented in purple, red, blue, and gray, respectively). Down-left, down-right: Free energy profiles for the CO2RR to CO at 0 V (vs RHE) and at – 0.48 V (vs RHE) on simulated FeN4 and O–Fe–N-C. Reproduced from ref (208). Copyright 2022, Wiley-VCH. (e) Scheme of ECR-to-CO activity for Ni-SAC@NFC. Reproduced from ref (130). Copyright 2024, American Chemical Society. (f) Scheme of ECR-to-CO activity for Ni–N4/C-NH2. Reproduced from ref (209). Copyright 2021, Royal Society Chemistry. (g) Optimized structures of Ni–N4, V1–Ni-N4, V2–Ni-N4, and V3–Ni-N4. (h) Free energy diagram for the ECR-to-CO conversion. Reproduced from ref (81). Copyright 2025, American Chemical Society. (i) Schematic diagram of the orbital matching mechanism, which originated from the characteristic d-d and d-p orbital interactions between the substrate and the dispersed metal atoms. The ″volcano-type″ scaling relationship between the number of valence electrons (nve) of dispersed elements and (j) single atom (k) cluster formation energies. Reproduced from ref (78). Copyright 2025, Wiley-VCH. (l) Different spin states of Co, Fe, and Mn atoms in TM-TCSACs (TM = Co, Fe, and Mn) and CO*. Reproduced from ref (71). Copyright 2025, American Chemical Society.

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Beyond the aforementioned in-plane coordination tuning, out-of-plane (axial) modulation can also break the symmetric electronic structure of M1-N4 sites, thus optimizing the binding energies of *COOH and *CO. For example, Zhang et al. synthesized axial O-coordinated O–Fe–N-C SASCs using O/N-rich MOFs (IRMOF-3) as precursors. The resulting FeN4–O sites exhibited significantly enhanced performance for CO production compared to O-free FeN4 sites, reaching an FECO of 95% at – 0.50 V vs RHE. DFT results indicated that although the *COOH formation barrier for O–Fe–N-C was higher than that for FeN4 at both U = 0 V and U = – 0.48 V, the *CO desorption energy was lower, suggesting that the introduction of axial O coordination facilitates CO release and improves ECR-to-CO selectivity (Figure 7d). (208) In addition to direct coordination tuning, modulating the environment around the metal active sites is another effective strategy to optimize the absorption of key intermediates (e.g., *COOH and *CO) for efficient ECR-to-CO. This includes the introduction of specific functional groups or structural defects, such as C–F bonds, edge-NH2 groups, and edge-rich vacancies. For instance, Wang et al. incorporated F atoms into N-doped carbon-supported Ni SASCs via a simple pyrolysis method. The synthesized Ni-SAC@NFC catalyst achieved a FECO exceeding 99% across a wide potential range and an exceptional CO evolution rate of 9.5 × 104·h–1 at −1.16 V vs RHE (Figure 7e). (130) Similarly, Chen et al. reported a universal amination strategy to significantly boost the current density of M-N/C (M = Ni, Fe, Zn) catalysts for CO production. To be specific, the aminated Ni SASC (Ni–N4/C-NH2) reached a jCO of 450 mA·cm–2 at −0.89 V vs RHE, while maintaining a FECO above 85% over a broad potential window from −0.5 to −1.0 V vs RHE (Figure 7f). (209) Furthermore, Mei et al. employed support vacancy engineering to introduce edge-rich Ni–N4 sites, which enhanced the adsorption of *COOH intermediates. DFT calculations revealed that these edge-rich sites caused an upward shift of the Ni d-band center, which strengthened *COOH binding and improved reaction kinetics in acidic media (Figure 7g, h). (81)
The M1-M’x SASCs, representing a novel alloy design concept, has demonstrated significant performance enhancements by maximizing atomic efficiency, promoting hydrogen spillover, and breaking conventional scaling relations. (210) Currently, studies on M1-M’x SASCs for ECR-to-CO are relatively underexplored, likely due to the instability or aggregation of single atoms during synthesis or under harsh reaction conditions. Therefore, Xu et al. proposed a universal screening principle to evaluate the dispersion stability of M1-M’x combinations based on stabilization energy. Guided by a d-p orbital matching strategy between the substrate and dispersed atoms, they revealed that guest metals with a d1 electronic configuration (or full inner d-orbitals with partially occupied outer s and p orbitals) exhibit superior stability compared to those with only partially occupied d-orbitals (Figure 7i). This study also identified the valence electron number (nve) as the most critical intrinsic factor, showing a volcano-type scaling relationship between nve and formation energy for both single atoms and triatomic clusters (Figure 7j, k). The interesting finding implies that more negative formation energies lead to a higher thermodynamic stability. As a proof of concept, the synthesized Sb1Cu catalyst exhibited a FECO of 99.73 ± 2.5% at 200 mA·cm–2 with other synthesized Cu-based single-atom alloys demonstrated over 70% selectivity for C1 products. (78)
In contrast to M1-Nx and M1-M’x SASCs, M1-Ox SASCs are least applied in ECR-to-CO, which may be explained by their inherent electronic rigidity and the difficulty in tuning their coordination environments. Nevertheless, the emergence of spin-state engineering provides a new dimension for optimizing these systems. For example, Liu et al. have found that unlike octahedral compounds (e.g., transition metal oxides), tetrahedral geometry features three high-energy t2g orbitals (dxy, dyz, dxz) closer to the Fermi level, offering more opportunities for interaction with reactants and intermediates. Consequently, they synthesized tetrahedral coordination single-atom catalysts (TCSACs) by incorporating 3d transition metals (TM = Fe, Mn, Co, etc.) into tetrahedral ZnO sites. The electronic configurations of these TCSACs were elucidated by combining TM oxidation states from X-ray photoelectron spectroscopy (XPS) and magnetic moments from zero-field-cooling (ZFC) measurements. Their findings showed that only Fe and Co maintained intermediate-spin (IS) states before and after CO adsorption (Figure 7l). Notably, Fe, possessing more unpaired electrons, exhibited a moderate binding strength for *CO, which effectively enhanced the CO activation. Experimentally, the Fe-TCSAC achieved a FECO of 91.6% at – 0.9 V vs RHE and demonstrated excellent stability over 30 h, validating the feasibility of spin-state engineering for efficient ECR-to CO. (71)
In summary, the above research collectively demonstrates that precise modulation of the electronic structure of metal active sites─whether through coordination engineering, peripheral environment tuning, or spin-state control─is the core of optimizing the absorption of key intermediates (e.g., *COOH and *CO). These advancements provide a clear theoretical blueprint and a diverse array of material platforms for designing high-performance SASCs for efficient ECR-to-CO.

4.1.2. CH4

CH4 stands out for its high combustion efficiency and the highest energy density (∼56 kJ·g–1) among all hydrocarbons, making it a critical feedstock in both the energy and chemical industries. (211) Currently, ECR-to-CH4 is primarily dominated by M1-Nx and M1-Ox SASCs, whereas M1-M’x SASCs are rarely reported. This phenomenon may be attributed to the limited number of unpaired electrons in M1-M’x sites, which is insufficient to effectively activate *CO and facilitate its continuous hydrogenation to CH4. Based on this, the following section mainly focuses on the applications of M1-Nx and M1-Ox SASCs for ECR-to-CH4 under various modulation strategies.
Among M1-Nx SASCs, Cu-based catalysts have emerged as the most prominent candidates, likely stems from their high energy barriers for C–C coupling and the favorable protonation of key *CHO intermediates. (216) Now, various strategies have been proposed to further enhance the ECR-to-CH4 activity of Cu–Nx SASCs. For instance, Li et al. employed a support geometric engineering strategy using N-doped carbon (NC) and graphite sheets (ss) as primary and secondary supports, respectively. By adjusting the coating amount of polydopamine on the ss, they precisely tuned the site spacing (dsite) of Cu–N4 from 2.2 nm (ssCuNC40) to 0.36 nm (ssCuNC160), achieving uniform anchoring of single-atom sites (Figure 8a, b). DFT calculations revealed that reducing dsite to 0.68 nm (ssCuNC100) induced a positive shift in the Cu 3dx2-y2 orbital, which not only enhanced *CO adsorption but also facilitated the protonation of *OCH3 into *CH4. As a result, the ss-CuNC100 catalyst exhibited an FECH4 of 70% and a jCH4 of 303.9 mA·cm–2, which is more than 1.5 times higher than that of the unmodified CuNC. (113) Furthermore, optimizing the adsorption of key intermediates (e.g., *CO and *CHO) on Cu sites can also be achieved through the introduction of a less electronegative atom to conventional coordination N atoms. For instance, DFT calculations by Dai et al. revealed that incorporating a less electronegative B atom (∼2.04) into the Cu–N4 coordination environment to form Cu–NxBy significantly strengthens the binding of *CO and *CHO, thereby potentially lowering the energy barrier for CH4 formation. Inspired by this, they synthesized BCN-Cu SASCs dominated by Cu–N2B2 sites. Electrochemical tests showed that this catalyst achieved a FECH4 of 73% at −1.46 V vs RHE and a maximum jCH4 of −462 mA·cm–2 at −1.94 V vs RHE (Figure 8c). (105)

Figure 8

Figure 8. (a) Schematic of the synthesis of CuNC and ssCuNC via support engineering. DCD: Dicyandiamide, PNP-Cu: Cu-chelated polydopamine nanoparticles, ss-PNF-Cu: Cu-bound polydopamine nanoparticles and films coated on ss. (b) AC-HAADF-STEM images of (i) ssCuNC40, (ii) ssCuNC80, (iii) ssCuNC100, and (iv) ssCuNC160. Reproduced from ref (113). Copyright 2025, Springer Nature. (c) FE and partial current densities for CH4 of BNC-Cu and NC-Cu as a function of cathodic potentials. Red curve for partial current density and black curve for methane FE. The error bars of FECH4 and jCH4 are calculated based on three independent measurements. Reproduced from ref (105). Copyright 2023, Springer Nature. (d) Conceptual schematic of the self-healing coordination reconstruction process. Reproduced from ref (212). Copyright 2025, Springer Nature. (e) Scheme of ECR-to-CH4 activity for SA-Zn/MNC. Reproduced from ref (213). Copyright 2020, American Chemical Society. (f) Left: Schematic diagram of CO adjacent-adsorption on the Al2O3–CuSAC surface. Right: CO adsorption energy of Al2O3–CuSAC, CeO2–CuSAC, and TiO2–CuSAC. Reproduced from ref (72). Copyright 2025, Springer Nature. (g) Scheme of ECR-toCH4 activity for SA-Zn/MNC. Reproduced from ref (214). Copyright 2022, American Chemical Society. (h) Diagrams of the electroreduction processes over Bi1–xVO4, Bi1–xVO4–Cu, and BiVO4–Cu. Reproduced from ref (160). Copyright 2023, Wiley-VCH. (i) Atomic elemental mapping using the EELS. (j) Comparison of reaction products for pristine Cu and Cu-FeSA. Error bars represent 1 standard deviation on the basis of three independent samples. Reproduced from ref (215). Copyright 2022, Springer Nature.

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Considering that traditional Cu–N4 sites are susceptible to adsorbed protons (*H) induced degradation, incorporating more electronegative O atom (∼3.44) to form Cu–O coordination has been proposed as a potential solution to resist *H attack. (217,218) However, Shen et al. noted that an excessive increase in electronegativity from Cu–O coordination alone might cause an electronic imbalance, failing to resolve the trade-off between activity and stability. Herein, a self-healing strategy enables a one-step Cu–N to Cu–N/O transition, proceeding via HER-induced ″coordination cutting″ and spontaneous O bonding on ZrO2/Cu composites (Figure 8d). As a result, compared to pristine Cu–N4, the synthesized ZrO2/CuN1O2 SASCs demonstrated a 3-fold increase in FECH4 (87.06% vs 27.8%) at −500 mA·cm–2 and a 10-fold increase in FECH4 (80.21% vs 8%) at −1000 mA·cm–2. Meanwhile, minimal performance degradation (<3%) after 25 h of operation in a membrane electrode assembly (MEA) electrolyzer further highlighted its exceptional stability. (212) Parallel to the efforts on Cu SASCs, Zn also demonstrates great potential in the field of ECR-to-CH4. As early as 2017, He et al. found via DFT that the overpotential for CH4 synthesis on Zn single atoms supported on defective graphene (−0.73 V vs RHE) was lower than that of Cu single atoms (−1 V vs RHE). (219) Motivated by this, Han et al. developed a Zn single-atom catalyst supported on microporous N-doped carbon (SA-Zn/MNC) for efficient CH4 production (Figure 8e). In detail, SA-Zn/MNC exhibited a high FECH4 of 85% at −1.8 V vs SCE, with a corresponding partial current density and yield of −31.8 mA·cm–2 and 158 ± 4 μmol·h–1·cm–2, respectively. DFT calculations indicated that during the ECR process, the O atoms (rather than C atoms) in *OCHO prefer to bond with Zn single atoms, thereby blocking CO evolution and promoting CH4 generation. (213)
In the realm of M1-Ox SASCs, Zhang et al. synthesized copper single-atom catalysts supported on Al2O3 (Al2O3–CuSAC), CeO2 (CeO2–CuSAC), and TiO2 (TiO2–CuSAC) via the ALD method to investigate the mechanism of electronic metal–support interaction (EMSI) in ECR-to-CH4. DFT calculations revealed that the electronegativity disparity of Cu (∼1.90) and Ce (∼1.12) allows Cu to withdraw electrons from Ce, markedly reducing electron delocalization around the Cu single atoms. As shown in Figure 8f, the adjacent (site A-C)-adsorption energy of CO (0.35 to −0.65 eV) on the Cu atom of CeO2–CuSAC is significantly lower than the top-adsorption energy, leading to lower CO coverage around the Cu sites and consequently hindering the C–C coupling pathway. Furthermore, compared to Al2O3–CuSAC (1.24 eV) and TiO2–CuSAC (−0.52 eV), CeO2–CuSAC possesses a moderate free energy for *H2O dissociation (−0.24 eV), which facilitates the deep hydrogenation of *CO without excessive activation of the HER. As a result, CeO2–CuSAC delivered the highest FECH4 of 70.3% at 400 mA·cm–2 among the three catalysts. (72) In addition, Chen et al. further investigated the H2O activation issues highlighted above. To address the inherent limitation of Cu in H2O activation due to its high thermal stability, (220) they employed an Ir single-atom doping strategy to induce nucleophilic attack on H2O molecules, thereby accelerating H2O dissociation through abundant electrophilic O species. Simultaneously, they integrated an A-site vacant anti-ReO3 perovskite-type Cu3N with Cu2O, which exhibits favorable affinities for *H2O and *CO, further optimizing the reaction pathway from *CO to *CHO (Figure 8g). Consequently, the Ir1–Cu3N/Cu2O multiactive site catalyst exhibited a high current density of 320 mA·cm–2 at −1.3 V vs RHE, with a maximum FECH4 of 75%. (214) Meanwhile, Guo et al. utilized Bi vacancies (VBi) to both promote H2O dissociation and induce electron transfer toward the Cu single-atom sites in the synthesized Bi1–xVO4–Cu SASCs. This synergistic effect significantly facilitated the formation and stabilization of the key intermediate *CHO, achieving efficient FECH4 of 92% (Figure 8h). (160)
Aside from M1-Nx and M1-Ox SASCs, Hung et al. reported a unique Fe SASC utilizing metallic Cu as the support. By assembling Fe phthalocyanine onto the Cu surface and reducing it during ECR, Fe single atoms were embedded into the Cu host to form Cu-FeSA SASC, which is confirmed by atomic elemental mapping using EELS (Figure 8i). Electrochemical tests demonstrated that Cu-FeSA exhibited a maximum FECH4 of 64% at 200 mA·cm–2, which is far superior to the 2% observed for pure Cu (Figure 8j). DFT calculations suggested that Cu-FeSA favors a pathway involving the hydrogenation of *CO to *COH rather than C–C coupling for CH4 production. (215)
In general, current research on high-efficiency ECR-to-CH4 primarily focuses on the atomic-level precision design and regulation of local coordination environments, support interactions, and interface structures in M1-Nx and M1-Ox SASCs. The purpose is to balance the adsorption of key intermediates (*CO, *CHO/*COH, etc.), proton supply efficiency, and the stability of catalytic sites to achieve high activity, selectivity, and durability. Future efforts could focus on overcoming challenges in the less-explored M1-M’x SASCs to achieve efficient CH4 synthesis. Furthermore, beyond CH4, ECR-to-CH3OH also represents a high-value research direction due to its extensive applications in the energy and chemical sectors. However, as the overall number of studies on SASCs in the field of ECR-to-CH3OH remains limited, it is not discussed in detail in this review. (40,221,222)

4.1.3. HCOOH

HCOOH has long been recognized as a vital liquid feedstock for synthesizing high-value chemicals and an ideal hydrogen carrier, owing to its high volumetric hydrogen storage capacity (53.4 g·L–1) and moderate gravimetric capacity (4.4 wt %) under ambient conditions. (223) Consequently, ECR-to-HCOOH offers a sustainable and efficient pathway for its production. To date, M1-Nx, M1-M’x, and M1-Ox SASCs have been extensively developed for the efficient synthesis of HCOOH, with research primarily focusing on main-group metals (e.g., In, Sn, Bi, and Sb) and transition metals (e.g., Cu, Fe, Mo, and Au).
For M1-Nx SASCs, various structural engineering strategies have been employed to enhance HCOOH electrosynthesis such as in-plane or out-of-plane coordination regulation. For the first type, Shang et al. synthesized In-SAs/NC catalysts featuring unique Inδ+-N4 (0 < δ < 3) atomic interface groups on MOF-derived N-doped carbon substrate via a pyrolysis method (Figure 9a). The catalyst achieved a remarkable turnover frequency (TOF) of 12,500 h–1 at −0.95 V vs RHE, and a high FEHCOOH of 96% at a lower potential of −0.65 V vs RHE, representing a significant advancement in catalytic performance. (224) However, such highly symmetric M1-N4 structures often limit the fine-tuning of the electronic structures of the active metal sites. To overcome this, Dong et al. synthesized a planar-symmetry-broken CuN3 (PSB-CuN3) catalyst using a microwave-assisted method. DFT calculations revealed that reducing the symmetry from planar-like D4h (CuN4) to C2v (CuN3) configuration caused the antibonding 4s and 4p states to shift significantly upward above the Fermi level (Figure 9b). Furthermore, under an applied electric field (URHE = −0.8 V vs RHE), the free-energy difference (ΔGL) for the rate-determining step (RDS) of HCOOH formation (*OCO → *OCHO) on CuN3 was only −0.03 eV, substantially lower than the 0.62 eV observed for CuN4, indicating a strong preference for HCOOH production. Experimental results confirmed that PSB-CuN3 achieved a maximum FEHCOOH of 94.3% at −0.73 V vs RHE, outperforming the symmetric CuN4 catalyst (FEHCOOH = 72.4% at −0.93 V vs RHE). (133) Besides, Wang et al. introduced S atoms, which have lower electronegativity (∼2.58), into the Fe–N4 coordination environment on N-doped carbon supports to form Fe–N2S2 active sites. This modulation of the electronic structure of the central Fe atom optimized the adsorption of key intermediates (e.g., *CO2 and *OCHO). Electron density difference (EDD) maps obtained from DFT calculations showed that the atomic Fe site in Fe–N2S2 exhibited a charge density higher than that in Fe–N4. This suggests that S-substitution breaks the original symmetry of Fe–N4 and induces electronic redistribution, correlating with a higher polarization center in Fe–N2S2 (Figure 9c). Consequently, the Fe–N2S2 catalyst achieved a FEHCOOH of 90.6% at −0.5 V vs RHE, a stark contrast to the Fe–N4 catalyst, which primarily produced CO with a FECO of 58.7% (Figure 9d). (89)

Figure 9

Figure 9. (a) Scheme of ECR-to-HCOOH activity for In Sas/NC. Reproduced from ref (224). Copyright 2020, Wiley-VCH. (b) Schematic diagrams of band shifts and hybridization for the planar CuN4 moiety with local D4h symmetry and the defective CuN3 moiety with lower local C2v symmetry. a.u. arbitrary units. Reproduced from ref (133). Copyright 2023, Springer Nature. (c) EDD plots of FeN4 and FeN2S2. (d) Distribution of ECR products over different Fe-based catalysts at −0.5 V. Reproduced from ref (89). Copyright 2025, American Chemical Society. (e) Schematic illustration for the preparation of SnPc/CNT–OH. Reproduced from ref (128). Copyright 2023, American Chemical Society. (f) Atomic-resolution AC-HAADF-STEM image and intensity profiles of Ru1@Bi. (g) Gibbs free energy landscapes for ECR-to-HCOOH at 0 V versus RHE. The RDS is labeled with a black text. Reproduced from ref (143). Copyright 2024, Wiley-VCH. (h) Comparison of FECO (orange color) and FEHCOO– (green color) on Cu, Cu99In1, Cu95In5, Cu92In8, Cu1In99 and In catalysts. Reproduced from ref (79). Copyright 2025, Wiley-VCH. (i) Electron localization function maps of Op-Ag1In. (j) Charge density difference map of CO2 on Op-Ag1In. Reproduced from ref (225). Copyright 2024, Wiley-VCH. (k) In-situ ATR-FTIR spectra on CuHHTP/Cu(OH)2 at −1.7 V for 60 min in a CO2-saturated 0.1 M KHCO3–KCl electrode. (l) The charge density difference analysis on CuHHTP/Cu(OH)2 and Cu(OH)2. Reproduced from ref (226). Copyright 2025, Wiley-VCH.

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Beyond in-plane strategies, out-of-plane regulation is another effective approach for modulating the electronic structure of SASCs. For example, Deng et al. immobilized tin phthalocyanine (SnPc) onto hydroxylated carbon nanotubes (CNT–OH) through π-π interactions, effectively synthesizing SnPc/CNT–OH with an axially coordinated O structure (O–Sn–N4). In contrast, the SnPc/CNT with planar Sn–N4 sites was prepared using nonhydroxylated carbon nanotubes (CNT) (Figure 9e). Experimental results indicate that the SnPc/CNT–OH catalyst exhibited an FEHCOOH of 89.4% at −1.0 V vs RHE, surpassing SnPc/CNT (70.6%), with a similar trend observed across other potentials. DFT calculations indicated that the energy barrier for the CO2 → *CO2 step was −0.58 eV for the O–Sn–N4 compared to −0.13 eV for Sn–N4, suggesting that the axial O facilitates CO2 activation. Moreover, O–Sn–N4 showed a lower energy barrier for *HCOOH formation (ΔG = 0.8 eV) than Sn–N4 (ΔG = 0.93 eV), leading to enhanced electrocatalytic activity for ECR-to-HCOOH. (128)
For M1-M’x SASCs for ECR-to-HCOOH, their structures can be categorized based on whether the M and M’ atoms are ″pinned″ by other atoms. In the unpinned type, Liu et al. utilized an electrochemical galvanic method to prepare Ru single atoms on Bi substrate (Ru1@Bi, 0.6 wt %) and Ru clusters on Bi substrate (Run@Bi, 1.2 wt %). The AC-HAADF-STEM image of Ru1@Bi is shown in Figure 9f. DFT calculations revealed that Ru1@Bi possesses a more balanced capability for the adsorption and activation of H2O and CO2 compared to Run@Bi (Figure 9g). Consequently, the reaction activity for CO2-to-HCOOH on Ru1@Bi was approximately twice that of Run@Bi, maintaining a high FEHCOOH exceeding 93% within a potential range of −0.8 to −1.2 V vs RHE. (143) Additionally, Du et al. constructed two SAAs catalysts, Cu99In1 and Cu1In99, by inverting the host and guest metals. Regarding Cu1In99, the neighboring In atoms significantly altered the adsorption properties of Cu, stabilizing the bridge-bonded *CO intermediate and promoting the preferential formation of HCOOH, which reached an FEHCOOH of 91% at −1.2 V (Figure 9h). (79) In the pinned category, Fang et al. developed an O-pinned silver–indium SAA (Op-Ag1In) via a mild electrochemical reduction method. This catalyst exhibited a FEHCOOH of 92.03% and a partial current density of 13 mA cm–2 at −0.95 V vs RHE, representing a 1.40-fold increase in selectivity and a 2.23-fold increase in activity compared to pure In catalyst. To elucidate the pinning effect of the O atoms on Ag single atoms, electron localization function (ELF) maps from DFT calculations confirmed the formation of covalent bonds in Op-Ag1In (Figure 9i). Furthermore, the introduction of O-pinning facilitated the adsorption of *CO2 and *H toward HCOOH formation and reduced the kinetic energy barrier of the RDS (Figure 9j). (225)
Finally, catalysts featuring M1-Ox sites constitute a promising frontier for ECR-to-HCOOH, demonstrating significant potential due to their atomically dispersed active centers. Shao et al. strategically anchored phenolic 2,3,6,7,10,11-hexahydroxytriphenylene (HHTP) onto Cu(OH)2 surfaces to construct a CuHHTP/Cu(OH)2 catalyst. The surface phenol-to-quinone transformation regulated the CO2 adsorption configuration, creating a unique reaction pathway for efficient HCOOH production. The optimized CuHHTP/Cu(OH)2 has achieved a high current density of 65.6 mA cm–2 and a FEHCOOH of 88.8% at −1.4 V vs RHE, maintaining FEHCOOH of 83.0% after 66 h of continuous ECR testing. As shown in Figure 9k, in situ electrochemical attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR) for CuHHTP/Cu(OH)2 revealed O–C–O stretching vibrations at 1380 and 1446 cm–1 corresponding to the *OCHO intermediate. In contrast, peaks associated with the *COOH intermediate were absent, indicating the effective suppression of the competing *COOH pathway. DFT calculations further showed that CuHHTP/Cu(OH)2 exhibits stronger electronic interactions with CO2 (Δq = 0.852 e) compared to Cu(OH)2 (Δq = 0.674 e), facilitating electron transfer from Cu to CO2 for stable binding and subsequent reduction (Figure 9l). The calculated free energy barriers for CO2 conversion to *OCHO were 0.67 eV for CuHHTP/Cu(OH)2 and 0.82 eV for Cu(OH)2, confirming that the ECR-to-HCOOH is more energetically favorable on the former. (226)
In summary, M1-Nx, M1-M’x, and M1-Ox SASCs have significantly enhanced the selectivity and efficiency of HCOOH production by precisely tailoring the local coordination environment (e.g., symmetry, ligand species, and axial modification) to optimize the adsorption behavior of key intermediates (such as *CO, *HCOO, and *OCHO). Future research can focus on unraveling the dynamic evolution mechanisms of active sites to drive further breakthroughs in catalytic performance, ultimately advancing ECR-to-HCOOH toward high-efficiency, stability, and industrialization.

4.2. CO2 to C2+ Products

As shown in Figure 6, compared to C1 products (e.g., CO, CH4, and HCOOH), the reaction mechanisms for C2+ products (e.g., C2H4, CH3CH2OH, CH3COOH, and CH3COCH3) are significantly more intricate, typically involving multistep PCET processes. But it is now a wide consensus in the community that *CO serves as the pivotal intermediate for the formation of C2+ species. To date, Cu-based catalysts remain the main class of materials recognized for their ability to efficiently electroreduce CO2 to C2+ products, a property primarily attributed to their moderate binding energy for *CO. However, research into Cu-based SASCs for this specific application remains relatively limited, largely due to the inherent physical isolation of single-atom active sites, which is unfavorable for the C–C coupling step. Consequently, this section will not categorize discussions by individual C2+ products but instead will treat them as a collective whole to provide a systematic and comprehensive overview of the underlying mechanisms and recent advancements.
Currently, research on M1-Nx SASCs for ECR-to-C2+ remains the most extensive, with Cu atoms predominantly serving as active centers. Nevertheless, many Cu-based SACs undergo in situ reconstruction under operating conditions, evolving from isolated Cu sites into Cu clusters or nanoparticles to facilitate C–C coupling, complicating the elucidation of the structure–activity relationships. To address this, Choi et al. elegantly utilized operando high-energy resolution fluorescence detected X-ray spectroscopy (HERFD-XAS) and operando electrochemical liquid-cell scanning transmission electron microscopy (EC-STEM) to quantitatively track the structural and molecular evolution from single atoms to nanocrystals. As illustrated in Figure 10a, the operando EC-STEM images clearly reveal the transformation of a Cu single-atom into metallic Cu nanoparticles on the carbon support during a 120 s ECR process. Compared to Cu-SAC containing less than half the metallic Cu nanocrystals, the nanocarbon supported Cu-SAC (Cu-SAC-NC), comprising almost entirely metallic Cu nanocrystals, achieved a 5-fold increase in the FEC2+. This enhancement was attributed to the superior electronic conductivity of the nanocarbon, which promoted the formation of dense Cu carbonyl (Cu-CO) intermediates, as detected by in situ attenuated total reflection surface enhanced infrared absorption spectroscopy (ATR-SEIRAS). Thus, a higher proportion of active metallic Cu nanocrystallites were formed for efficient C–C coupling and significantly improved C2+ selectivity. (80) However, the specific local coordination environments that trigger Cu reconstruction and their subsequent impact on the ECR-to-C2+ activity remain poorly understood. To clarify this, Lu et al. selected five well-defined mononuclear copper complexes with distinct ligand structures: Cu(II) 5,10,15,20-tetraphenyl-21H,23H-porphine (CuTPP), Cu(II) phthalocyanine (CuPc), fluoro-substituted CuPc (CuPc-F), amino-substituted CuPc (CuPc-NH2), and Cu(II) bis[1-(2-pyridylazo)-2-naphtholato] (CuPAN). Operando XAFS revealed that the Cu–N4 in CuPc is more stable than the Cu–N2O2 in CuPAN, likely due to the easily dissociable Cu–O bonds of the tetrahedral Cu–N2O2 configuration. Furthermore, compared to other model compounds, only CuPc-F exhibited a transition from Cu(II) to Cu(I) during the ECR process, suggesting that the electron-withdrawing F-substituents stabilized the Cu(I) oxidation state (Figure 10b). Interestinglythe unique Cu(I) active site facilitates C2+ production via a distinctive Cu(I)N3H-*CO intermediate, which acts as a bridge for *CO transfer to adjacent Cu(0) sites, achieving a total FE for C2H4 and C2H5OH of approximately 36% at −1.07 V vs RHE (Figure 10c). (82)

Figure 10

Figure 10. (a) Low magnification EC-STEM images of pristine-SAC and Cu nanograins after the CO2RR for 120 s in liquids. Reproduced from ref (80). Copyright 2025, American Chemical Society. (b) Linear combination fitting of Cu oxidation states for CuPc-F. (c) Cu composition ratio and FEs of various products at multiple potentials for CuPc-F. Reproduced from ref (82). Copyright 2025, American Chemical Society. (d) F, O-codrived local coordination environment optimized for CuFONC favors the CO2RR toward C2+. (e) The reaction pathways of CO2 to *COCHO on CuN2O1–FC, CuN2O1–C, and CuN3–C. Reproduced from ref (121). Copyright 2024, Wiley-VCH. (f) Schematic illustration of the modular design of the Cu/Ni-NAC hybrid catalyst for tandem catalysis. In-situ SEIRAS spectra of (g) the Cu/Ni-NAC and (h) the Cu NW catalysts under ECR conditions. Reproduced from ref (95). Copyright 2022, American Chemical Society. (i) A proposed reaction mechanism for the CO2RR to C2H4 and C2H5OH. Reproduced from ref (144). Copyright 2025, Wiley-VCH. (j) Simulated geometry and charge density difference of M1/Cu(111). Reproduced from ref (68). Copyright 2025, Springer Nature. FEs and the product distributions under different polarization potentials over (k) Sn/C-0.12 and (l) Sn/C-1.2 (stacked bar chart) and the geometric partial current densities, J, toward (k) acetate and (l) ethanol (blue line-stars). All FEs are calculated from chronoamperometry measurements. Reproduced from ref (161). Copyright 2024, American Chemical Society. (m) A schematic illustration showing the cascade reaction during CO2 reduction to ethanol over SnS2/Sn1–O3G (gray: S, red: O, yellow: H and purple: Sn). Reproduced from ref (157). Copyright 2023, Springer Nature.

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In addition to studies on Cu-SACs prone to in situ reconstruction, Lv et al. took an alternative approach by developing a highly stable, high-density Cu single-atom catalyst supported on heteroatom-doped carbon (CuFONC) to reveal definitive structure–activity relationships (Figure 10d). The CuFONC catalyst, featuring a high Cu loading (21.9 wt %) and a stable CuN2O1–FC configuration, exhibited an exceptional FEC2+ of ∼80.5% at −1.3 V vs RHE. DFT calculations indicated that CuN2O1–FC possesses the lowest binding energy (−4.19 eV) compared to those of CuN3–C (−2.76 eV) and CuN2O1–C (−4.33 eV), suggesting that the introduction of F and O atoms enhances catalyst stability (Figure 10e). Moreover, the CuN2O1–FC configuration showed the lowest reaction energy barriers for CO2 to *CO and *CO to *CO + *CO, indicating that F and O atoms also synergistically optimize the adsorption of key intermediates, thereby significantly boosting ECR-to-C2+ performance. (121)
Given that *CO is the critical intermediate for C–C coupling, tandem strategies, where one catalyst synthesizes *CO and another facilitates C–C coupling, represent a promising route for efficient ECR-to-C2+ products. For instance, Yin et al. reported a hybrid catalyst integrating Ni single atoms with Cu nanowires for efficient C2H4 synthesis (Figure 10f). The Ni single-atom catalyst on a N-doped carbon support (Ni-NAC) achieved a FE of over 90% for CO2-to-CO conversion over a wide potential range. Therefore, by hybridizing Ni-NAC with Cu nanowires (dominated by {100} facets favorable for C–C coupling) to form Cu/Ni-NAC, this hybrid catalyst achieved an FEC2H4 of 66% in an alkaline flow cell with a current density exceeding 100 mA·cm–2 at – 0.5 V vs RHE. As shown in Figure 10g, h, the hybrid Cu/Ni-NAC catalyst exhibited two strong CO adsorption peaks at 2050 and 1950 cm–1, clearly indicating that *CO generated by the Ni-NAC module was transferred to and enriched on the Cu nanowire surface, providing direct evidence for subsequent C–C coupling. (95)
In contrast to M1-Nx SACs with relatively isolated active sites, M1-M’x SASCs allow for the construction of multiactive sites by doping a second metal atom into another metal substrate, which is more conducive to ECR-to-C2+ requiring C–C coupling. For example, Jin et al. reported a Mo1Cu SAA catalyst that achieved a C2+ partial current density of 1.33 A·cm–2 with an FE exceeding 74.3% (Figure 10i). DFT calculations suggested that the introduced Mo sites promote H2O dissociation to generate active *H, while Cu0 sites distal to Mo act as active centers for CO2 activation to CO. Furthermore, CO and *H are captured by adjacent Cu sites (Cu&+) near the Mo atoms, accelerating CO conversion and the C–C coupling process. (144) Similarly, Huang et al. utilized a single-atom In-alloyed Cu (In1/Cu) catalyst in a high-pressure MEA to convert gas-phase CO2 to C2H4, achieving a maximum FEC2H4 of 85% and a current density of 750 mA·cm–2 under 20 bar (Figure 10j). (68)
Beyond M1-Nx and M1-M’x SASCs, a limited number of M1-Ox SACs have also been explored for C2+ production. For instance, Xu et al. reported a series of carbon-supported Sn electrocatalysts with Sn sizes ranging from single atoms and ultrasmall clusters to nanocrystals (Sn/C-0.12, Sn/C-1.2, and Sn/C-12). By tuning the size of the Sn active sites, the reaction pathway for ECR-to-C2+, including CH3COOH and C2H5OH, has been controlled with high selectivity (FE > 90%) and low onset potentials. Specifically, Sn/C-0.12 converted CO2 to CH3COOH with 90% FE (at −0.6 V), while Sn/C-1.2 yielded C2H5OH with 92% FE (at −0.4 V) (Figure 10k, l). (161) Additionally, Ding et al. reported a Sn-based tandem electrocatalyst for ECR-to-C2H5OH conversion, comprising SnS2 nanosheets and single Sn atoms anchored on a 3D carbon support via local Sn–O3 clusters (Sn1–O3G). They found that SnS2 nanosheets produce HCOOH intermediates, while Sn1–O3G sites generate *OCO(OH) bicarbonate intermediates, followed by C–C coupling at active centers composed of Sn and O atoms. This strategy enabled an ethanol selectivity exceeding 70% over a broad potential range of −0.6 to −1.1 V vs RHE, maintaining 97% FE at current densities up to 17.8 mA·cm–2 of its initial activity after 100 h of continuous operation (Figure 10m). (157)
Overall, the scientific community has developed numerous strategies to tune SASCs to meet the requirements for efficient ECR-to-C2+ conversion. However, constrained by the physical isolation of active sites in conventional SASCs, recent reports have begun to explore dual-atom site catalysts (DASCs) and even multiatom site catalysts with multiple active sites, though these studies remain relatively scarce. (227) Therefore, further in-depth exploration in this direction would be needed to meet the demands for the high-efficiency synthesis of C2+ products.

5. Conclusions and Outlook

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In summary, SASCs, characterized by maximized atom-utilization efficiency and well-defined active sites, serve as an ideal model system to break traditional linear scaling relationships and achieve precise product selectivity in ECR. This stands in contrast to conventional nanoparticle catalysts, which offer controllable size and morphology as well as notable stability but whose activity is often governed by surface sites with low atomic utilization, and to molecular catalysts, which offer structural precision but face challenges in stability and device integration. In this review, we systematically summarize the precise synthesis strategies for the three main SASCs types: M1-Nx, M1-M’x, and M1-Ox. Subsequently, we highlighted the historical evolution and advantages of AC-HAADF-STEM, XAFS, and Mössbauer spectroscopy in probing coordination structures of SASCs. Crucially, we underscored the intrinsic limitations of these advanced techniques, advocating that researchers must adopt a ″multitechnique combination″ strategy to cross-validate findings and overcome the bottlenecks associated with individual methods. Last, we have elucidated the specific structure–activity relationships linking diverse coordination environments to the high selectivity of target C1 and C2+ products. However, despite the remarkable progress in this field, the transition toward large-scale practical application remains fraught with challenges. To address these hurdles, we propose the following potential directions for future research:
1. Tuning for high-selectivity C2+ products: In the field of ECR, *CO is widely recognized as the key intermediate for C2+ product synthesis via C–C coupling. While Cu SASCs possess more suitable *CO adsorption energies than their CO-selective counterparts (e.g., Ag, Ni, Fe, and Mn SASCs), they still struggle to achieve high C2+ selectivity due to the physical isolation of their active sites, which impedes C–C coupling. Therefore, two main strategies have been proposed to overcome this hurdle. The first is the design of multiatom catalysts (e.g., dual-, triple-, or multiatom sites). These catalysts utilize adjacent active sites to coactivate *CO or adsorb various intermediates, thereby lowering the C–C coupling barrier for C2+ products like ethanol and 1-propanol. However, as discussed in Section 3.4, the structural characterization of such multiatom centers is challenging due to the limitations of AC-HAADF-STEM, XAFS, and Mössbauer spectroscopy, making it difficult to establish clear structure–activity relationships. The second strategy entails constructing tandem systems that combine CO-selective SASCs with Cu SASCs to facilitate the sequential conversion of CO2 to CO and subsequently to C2+ products. Currently, tandem catalysis is considered more promising for practical applications as it reduces design complexity while offering superior controllability and predictability.
2. Unveiling the true dynamic active sites: To date, most SASCs research in the field of ECR regards the pristine coordination structure (e.g., M1-N4) as the unchanging active site. However, under the dynamic electrochemical environment, the initial structure may undergo significant reconstruction. For example, Wei et al. synthesized a Zn-SA/CNCl-1000 catalyst via NaCl-assisted pyrolysis and utilized in situ FT-EXAFS to monitor its structural evolution during the process of ECR. They observed that under an applied potential of −0.9 V vs RHE, the Zn–N coordination number decreased from 4 at open circuit voltage (OCV) to approximately 3, whereas the Cl-free Zn-SA/CN-1000 catalyst remained unchanged. DFT calculations revealed that the adjacent C–Cl bond, due to the large electronegativity difference between Cl and N, promotes protonation of the coordinating N atom, triggering dynamic evolution from Zn–N4 to Zn–N3. Consequently, this in situ generated Zn–N3 site exhibits a lower energy barrier, delivering a CO partial current density of 271.7 mA·cm–2 with an FE of 97.5%. (109) Inspired by such insights, advanced in situ/operando characterization techniques (e.g., in situ EXAFS, in situ XAS, and in situ Raman spectroscopy) can accurately unveil the true active sites of SASCs under working conditions. This capability allows performance enhancements to be correctly attributed to specific coordination structures, thereby providing instructive insights rather than misleading other researchers into pursuing further studies based on erroneous foundations. Such efforts will provide a reliable experimental basis for the next generation of efficient SASCs design.
3. Unlocking the rising electronic spin dimension: In addition to the above-mentioned aspects, manipulating the electronic spin state of the central metal atom in SASCs represents a frontier and transformative new dimension beyond optimizing geometric coordination and charge density. Based on crystal field theory (CFT), the like-charge repulsion between transition metal d-orbital electrons and nonbonding electrons of ligand atoms induces the splitting of d-orbital energy levels (e.g., t2g and eg orbitals in an octahedral field), which directly dictates the electronic spin state. (228) In brief, when the ligand field splitting energy is smaller than the electron pairing energy, the central metal of SASCs will form a high-spin (HS) state; conversely, it adopts a low-spin (LS) state. (229) This theoretical understanding enables deliberate spin-state engineering for investigating its potential impact on SASCs catalysts. For instance, Zeng et al. introduced a strong-field-O atom axially to the Fe–N4 active site, increasing the ligand field splitting energy and facilitating the formation of low-spin Fe(III) sites. At a cathodic potential of −0.7 V vs RHE, this catalyst achieved a CO Faradaic efficiency of up to 99% and an exceptionally high turnover frequency (TOF) of 5.3 × 104·h–1, representing a performance improvement of over 20-fold compared to high-spin Fe(III) sites. (230) In addition to the aforementioned internal regulation strategies, external field regulation (including magnetic, electric, and light field modulation) serves as an innovative strategy to achieve precise control over catalytic performance through noncontact physical interactions, deserving deeper exploration in the field of ECR. Meanwhile, it is imperative to develop and integrate high-sensitivity in situ spin-sensitive characterization techniques, such as in situ X-ray magnetic circular dichroism (XMCD), (231) in situ electron paramagnetic resonance (EPR), and in situ Mössbauer spectroscopy. The application of these methods is essential to precisely capture the dynamic evolution of spin states under reaction conditions, thereby establishing a clear spin-activity relationship of SASCs.
4. Advancing AI-driven full-lifecycle development: With the increasing demand for efficiency and precision in SASCs development, the traditional ″trial-and-error″ paradigm has become insufficient to navigate the vast coordination space of SASCs for precise synthesis of high-value ECR products. Artificial intelligence (AI) is leading a paradigm shift from ″passive discovery″ to ″proactive design″, aiming to achieve the full-lifecycle development of SASCs, which covers theoretical prediction, precision synthesis, and performance evaluation. For instance, Bai et al. employed AI for large-scale literature embedding analysis and deep model screening to extract key design features (e.g., magnetic metal centers such as Fe/Co and heteroatom coordination structures such as M-N/S). Then, they constructed binary catalytic descriptors by integrating d-band centers and adsorption Gibbs free energy (ΔG) from DFT calculations, enabling the precise and efficient AI screening of high-performance SASCs. (232) Furthermore, the ″AI-driven automated laboratory″ represents a highly promising frontier for future ECR studies. Szymanski et al. developed an A-Lab platform, which integrates computational simulations, historical literature data, machine learning (ML), and active learning to autonomously plan and execute robotic experiments. During 17 days of continuous operation, A-Lab successfully synthesized 41 new compounds from 58 targets, including various oxides and phosphates. (233) Based on this, integrating such platforms with operando characterization and electrochemical testing feedback loops would establish a closed-loop automated optimization process that encompasses SASCs construction, structural verification, and performance testing. Such a data-driven paradigm will drastically shorten development timelines and facilitate the commercialization of SASCs, effectively bridging the gap between laboratory-scale discovery and industrial-scale implementation.

Author Information

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  • Corresponding Authors
    • Hongpan Rong - School of Materials Science & Engineering, Beijing Institute of Technology, Beijing 100081, China;  Orcidhttps://orcid.org/0000-0002-3654-9199;  Email: [email protected]
    • Jiatao Zhang - School of Chemistry and Chemical Engineering, Beijing Key Laboratory of Intelligent Molecular Materials and High-throughput Manufacturing, MIIT Key Laboratory of Medical Molecule Science and Pharmaceutical Engineering, MOE Key Laboratory of Cluster Science, Beijing Institute of Technology, Beijing 100081, China;  Beijing Institute of Technology, Zhuhai 519088, China;  Orcidhttps://orcid.org/0000-0001-7414-4902;  Email: [email protected]
  • Authors
    • Tianshang Shan - School of Materials Science & Engineering, Beijing Institute of Technology, Beijing 100081, China;  Zhongguancun Academy, Beijing 100094, China
    • Gengxian Zhou - School of Computer Science (National Pilot Software Engineering School), Beijing University of Posts and Telecommunications, Beijing 100876, China;  Zhongguancun Academy, Beijing 100094, China
  • Author Contributions

    H.R. and J.Z. conceived of and supervised the project. T.S. conducted the comprehensive literature review. All authors participated in drafting the manuscript, reviewing the results, and providing critical feedback.

  • Notes
    The authors declare no competing financial interest.

Acknowledgments

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This work was supported by the National Natural Science Foundation of China (52272186).

References

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  • Abstract

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    Figure 1

    Figure 1. (a) Synthesis scheme of the Ni–N–C catalysts by using a N-doped carbon host to absorb Ni ions followed by thermal activation at different temperatures to tune the Ni–N bond structures and establish structure–property correlations. Reproduced from ref (131). Copyright 2022, Royal Society of Chemistry. (b) Schematic illustration for the formation of the Ni-NC@Ni catalyst. In the green circle: the possible atomic structure of the Ni–N species. Reproduced from ref (132). Copyright 2020, Elsevier. (c) Schematic illustration of the preparation strategy for PSB-CuN3 and PS-CuN4. Reproduced from ref (133). Copyright 2023, Springer Nature. (d) Schematic illustration for the preparation of Ni–PxNy. Reproduced from ref (91). Copyright 2023, Springer Nature. (e) The formation process of atomically dispersed SnN3O1 active sites. Reproduced from ref (107). Copyright 2021, Wiley-VCH. (f) Schematic illustration of the proposed formation mechanisms. Reproduced from ref (118). Copyright 2021, Springer Nature.

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    Figure 2

    Figure 2. (a) Schematic synthesis process of the Sn1Cu-SAA. Reproduced from ref (77). Copyright 2025, Wiley-VCH. (b) Schematic representation of the preparation of the Ru1@Bi and Run@Bi catalysts. Reproduced from ref (143). Copyright 2024, Wiley-VCH. (c) Schematic diagram for the preparation of Mo1Cu catalysts. Reproduced from ref (144). Copyright 2025, Wiley-VCH. (d) Schematic diagram of the NiZn0.03/C bimetallic catalyst synthesis process. Reproduced from ref (145). Copyright 2023, Wiley-VCH.

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    Figure 3

    Figure 3. (a) Schematic illustration of preparing Bi1–xVO4–Cu. Reproduced from ref (160). Copyright 2024, Wiley-VCH. (b) Step-by-step preparation of the carbon-supported Cu SA catalyst using an amalgamated Cu–Li method. Reproduced from ref (158). Copyright 2020, Springer Nature. (c) Schematic illustration of the support crystal phase engineering and reaction mechanisms on the surface of Cu1O3-tZrO2 and Cu1O4-mZrO2. Reproduced from ref (83). Copyright 2025, American Chemical Society. (d) Illustration of the synthesis of Zr-BTB-In. Reproduced from ref (154). Copyright 2025, Wiley-VCH. (e) Schematic illustration of the fabrication of SA-Cu-MXene via selective etching of quaternary MAX-Ti3(Al1–xCux)C2. Gray, blue, red, yellow, brown, and green balls represent Al, Ti, Cu, O, C, and Cl atoms, respectively. Reproduced from ref (156). Copyright 2021, American Chemical Society.

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    Figure 4

    Figure 4. (a) General schematic of an electron microscope in STEM modes with a condenser lens, objective lens, aberration correctors, projector system, retractable detectors, EDS (energy dispersive X-ray spectroscopy), and EELS (electron energy loss spectroscopy) acquisition. p.s. BF (bright-field), ABF (annular bright-field). Reproduced from ref (171). Copyright 2021, Wiley-VCH. (b) Pt single atoms (white circles) are seen to be uniformly dispersed on the iron oxide (FeOx) support (left) and occupy exactly the positions of the Fe atoms (right). Reproduced from ref (44). Copyright 2011, Springer Nature. (c) Schematic diagram of XAFS measurements with fluorescence yield experiment setup. Reproduced from ref (74). Copyright 2024, Springer Nature. (d) Schematic diagram of Pd–O4/BWO and Pd–O3/BWO. (e) Fourier transforms of the EXAFS spectra of the Pd K-edge spectra. Reproduced from ref (172). Copyright 2025, Springer Nature. (f) Schematic diagram of operando Mössbauer spectroscopy for tracking the metastable states of atomically dispersed tin (Sn) in copper oxide (CuO) for selective CO2 electroreduction. Reproduced from ref (162). Copyright 2023, American Chemical Society.

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    Figure 5

    Figure 5. (a) Elastic scattering of electrons from an atomic nucleus, shown schematically (particle model) for a large-angle collision (A) and a 180° collision (B). Sputtering of atoms from the beam-exit surface (C) and the beam-entry surface (D). Reproduced from ref (186). Copyright 2010, Elsevier. (b) Energy-band diagram of a metal (left) and a semiconductor or insulator (right), electron energy being plotted vertically upward. CB and VB represent the conduction and valence bands, f is the work function, Evac, Ef and Eg are the vacuum energy, Fermi energy, and CB-VB energy gap. Upward arrows represent single-electron excitations, while downward arrows are de-excitation processes (filling of a VB or K-shell hole). K-shell excitation in an organic material is shown on the right, with Ekin being the typical kinetic energy of an excited K-shell electron. This process also results in the emission of Auger electrons from the VB, with an energy of about 270 eV. Reproduced from ref (187). Copyright 2013, Elsevier. (c) Schematic diagram of heterogeneous Pt/CeO2 SASCs using EXAFS. (d) Scattering paths for SASCs and small clusters. Schematic depiction of scattering paths present in oxide-supported metal catalysts with a heterogeneity of the metal-site structure including isolated metal sites (middle) as well as metal (left) or oxidized (right) nanoclusters. Bonds are for representation only. Color code: metal (gray), oxygen (red), and support metal cation (brown). (e) R-factor of the 5-path SAC fit to data sets with varying contributions from the Pt/CeO2 SASCs site and metallic Pt13 cluster. The inset shows a zoomed-in region with 70–100% SAC sites (30–0% Pt13 cluster sites). Data are taken over Δk = 3–18 Å–1. (f) Modeled FT EXAFS data for mixtures of the Pt/CeO2 SASCs site and metallic Pt13 cluster. Reproduced from ref (188). Copyright 2023, American Chemical Society.

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    Figure 6

    Figure 6. Overview of reaction pathways for ECR toward different products. Black spheres, carbon; red spheres, oxygen; white spheres, hydrogen; blue spheres, (metal) catalyst. The arrows indicate whether proton, electron or PCETs take place. Reproduced from ref (39). Copyright 2019, Springer Nature.

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    Figure 7

    Figure 7. (a) Schematic illustration of CO2RR over a chemical unit of the TM-Pcs. (b) Free energy diagram of TM-PCs for CO2RR at V = 0 V. Reproduced from ref (116). Copyright 2022, American Chemical Society. (c) Stability test of Ni–N3S–C in flow cell with alkaline, acidic, and neutral electrolyte. The electrolytes are 1 M KOH (alkaline, pH = 14), 0.05 M H2SO4 + 1 M KCl (acidic, pH = 1), and 1 M KHCO3 (neutral, pH = 8.2). Reproduced from ref (102). Copyright 2025, Wiley-VCH. (d) Top-left, top-right: Top view and side view optimized adsorption configuration on simulated FeN4 and O–Fe–N-C (Fe, O, N, and C atoms are represented in purple, red, blue, and gray, respectively). Down-left, down-right: Free energy profiles for the CO2RR to CO at 0 V (vs RHE) and at – 0.48 V (vs RHE) on simulated FeN4 and O–Fe–N-C. Reproduced from ref (208). Copyright 2022, Wiley-VCH. (e) Scheme of ECR-to-CO activity for Ni-SAC@NFC. Reproduced from ref (130). Copyright 2024, American Chemical Society. (f) Scheme of ECR-to-CO activity for Ni–N4/C-NH2. Reproduced from ref (209). Copyright 2021, Royal Society Chemistry. (g) Optimized structures of Ni–N4, V1–Ni-N4, V2–Ni-N4, and V3–Ni-N4. (h) Free energy diagram for the ECR-to-CO conversion. Reproduced from ref (81). Copyright 2025, American Chemical Society. (i) Schematic diagram of the orbital matching mechanism, which originated from the characteristic d-d and d-p orbital interactions between the substrate and the dispersed metal atoms. The ″volcano-type″ scaling relationship between the number of valence electrons (nve) of dispersed elements and (j) single atom (k) cluster formation energies. Reproduced from ref (78). Copyright 2025, Wiley-VCH. (l) Different spin states of Co, Fe, and Mn atoms in TM-TCSACs (TM = Co, Fe, and Mn) and CO*. Reproduced from ref (71). Copyright 2025, American Chemical Society.

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    Figure 8

    Figure 8. (a) Schematic of the synthesis of CuNC and ssCuNC via support engineering. DCD: Dicyandiamide, PNP-Cu: Cu-chelated polydopamine nanoparticles, ss-PNF-Cu: Cu-bound polydopamine nanoparticles and films coated on ss. (b) AC-HAADF-STEM images of (i) ssCuNC40, (ii) ssCuNC80, (iii) ssCuNC100, and (iv) ssCuNC160. Reproduced from ref (113). Copyright 2025, Springer Nature. (c) FE and partial current densities for CH4 of BNC-Cu and NC-Cu as a function of cathodic potentials. Red curve for partial current density and black curve for methane FE. The error bars of FECH4 and jCH4 are calculated based on three independent measurements. Reproduced from ref (105). Copyright 2023, Springer Nature. (d) Conceptual schematic of the self-healing coordination reconstruction process. Reproduced from ref (212). Copyright 2025, Springer Nature. (e) Scheme of ECR-to-CH4 activity for SA-Zn/MNC. Reproduced from ref (213). Copyright 2020, American Chemical Society. (f) Left: Schematic diagram of CO adjacent-adsorption on the Al2O3–CuSAC surface. Right: CO adsorption energy of Al2O3–CuSAC, CeO2–CuSAC, and TiO2–CuSAC. Reproduced from ref (72). Copyright 2025, Springer Nature. (g) Scheme of ECR-toCH4 activity for SA-Zn/MNC. Reproduced from ref (214). Copyright 2022, American Chemical Society. (h) Diagrams of the electroreduction processes over Bi1–xVO4, Bi1–xVO4–Cu, and BiVO4–Cu. Reproduced from ref (160). Copyright 2023, Wiley-VCH. (i) Atomic elemental mapping using the EELS. (j) Comparison of reaction products for pristine Cu and Cu-FeSA. Error bars represent 1 standard deviation on the basis of three independent samples. Reproduced from ref (215). Copyright 2022, Springer Nature.

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    Figure 9

    Figure 9. (a) Scheme of ECR-to-HCOOH activity for In Sas/NC. Reproduced from ref (224). Copyright 2020, Wiley-VCH. (b) Schematic diagrams of band shifts and hybridization for the planar CuN4 moiety with local D4h symmetry and the defective CuN3 moiety with lower local C2v symmetry. a.u. arbitrary units. Reproduced from ref (133). Copyright 2023, Springer Nature. (c) EDD plots of FeN4 and FeN2S2. (d) Distribution of ECR products over different Fe-based catalysts at −0.5 V. Reproduced from ref (89). Copyright 2025, American Chemical Society. (e) Schematic illustration for the preparation of SnPc/CNT–OH. Reproduced from ref (128). Copyright 2023, American Chemical Society. (f) Atomic-resolution AC-HAADF-STEM image and intensity profiles of Ru1@Bi. (g) Gibbs free energy landscapes for ECR-to-HCOOH at 0 V versus RHE. The RDS is labeled with a black text. Reproduced from ref (143). Copyright 2024, Wiley-VCH. (h) Comparison of FECO (orange color) and FEHCOO– (green color) on Cu, Cu99In1, Cu95In5, Cu92In8, Cu1In99 and In catalysts. Reproduced from ref (79). Copyright 2025, Wiley-VCH. (i) Electron localization function maps of Op-Ag1In. (j) Charge density difference map of CO2 on Op-Ag1In. Reproduced from ref (225). Copyright 2024, Wiley-VCH. (k) In-situ ATR-FTIR spectra on CuHHTP/Cu(OH)2 at −1.7 V for 60 min in a CO2-saturated 0.1 M KHCO3–KCl electrode. (l) The charge density difference analysis on CuHHTP/Cu(OH)2 and Cu(OH)2. Reproduced from ref (226). Copyright 2025, Wiley-VCH.

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    Figure 10

    Figure 10. (a) Low magnification EC-STEM images of pristine-SAC and Cu nanograins after the CO2RR for 120 s in liquids. Reproduced from ref (80). Copyright 2025, American Chemical Society. (b) Linear combination fitting of Cu oxidation states for CuPc-F. (c) Cu composition ratio and FEs of various products at multiple potentials for CuPc-F. Reproduced from ref (82). Copyright 2025, American Chemical Society. (d) F, O-codrived local coordination environment optimized for CuFONC favors the CO2RR toward C2+. (e) The reaction pathways of CO2 to *COCHO on CuN2O1–FC, CuN2O1–C, and CuN3–C. Reproduced from ref (121). Copyright 2024, Wiley-VCH. (f) Schematic illustration of the modular design of the Cu/Ni-NAC hybrid catalyst for tandem catalysis. In-situ SEIRAS spectra of (g) the Cu/Ni-NAC and (h) the Cu NW catalysts under ECR conditions. Reproduced from ref (95). Copyright 2022, American Chemical Society. (i) A proposed reaction mechanism for the CO2RR to C2H4 and C2H5OH. Reproduced from ref (144). Copyright 2025, Wiley-VCH. (j) Simulated geometry and charge density difference of M1/Cu(111). Reproduced from ref (68). Copyright 2025, Springer Nature. FEs and the product distributions under different polarization potentials over (k) Sn/C-0.12 and (l) Sn/C-1.2 (stacked bar chart) and the geometric partial current densities, J, toward (k) acetate and (l) ethanol (blue line-stars). All FEs are calculated from chronoamperometry measurements. Reproduced from ref (161). Copyright 2024, American Chemical Society. (m) A schematic illustration showing the cascade reaction during CO2 reduction to ethanol over SnS2/Sn1–O3G (gray: S, red: O, yellow: H and purple: Sn). Reproduced from ref (157). Copyright 2023, Springer Nature.

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