Probing the reactive intermediate species generated during electrocatalysis by scanning electrochemical microscopy

Noël, Jean‐Marc; Kanoufi, Frédéric

doi:10.1016/j.coelec.2022.101071

Cited by 10 publications

(7 citation statements)

References 62 publications

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“…However, some methods have been developed to obtain as close to in situ data as possible using ultrahigh vacuum systems but have a focus on surface characterization rather than in situ electron transfer reactions. , In order to gain a full understanding of the electrode surface properties, electroanalytical techniques are needed to elucidate the electron transfer properties. SECM has become a versatile technique used for a number of different systems including corrosion, , electrocatalysis, and photoelectrocatalyis among many others. In order to gain a thorough understanding of the surface electron transfer reactions, SECM has been coupled with techniques such as Raman spectroscopy for more complex systems such as polymer-based RFBs (discussed in Section ).…”

Section: Discussionmentioning

confidence: 99%

Scanning Electrochemical Microscopy for Chemical Imaging and Understanding Redox Activities of Battery Materials

Strange

Wornyo

et al. 2023

Chemical & Biomedical Imaging

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Improving the charge storage capacity and lifetime and charging/discharging efficiency of battery systems is essential for large-scale applications such as long-term grid storage and long-range automobiles. While there have been substantial improvements over the past decades, further fundamental research would help provide insights into improving the cost effectiveness of such systems. For example, it is critical to understand the redox activities of cathode and anode electrode materials and stability and the formation mechanism and roles of the solid−electrolyte interface (SEI) that forms at the electrode surface upon an external potential bias. The SEI plays a critical role in preventing electrolyte decay while still allowing charges to flow through the system while serving as a charge transfer barrier. While surface analytical techniques such as X-ray photoelectron (XPS), X-ray diffraction (XRD), time-of-flight secondary ion mass spectrometry (ToF-SIMS), and atomic force microscopy (AFM) provide invaluable information on anode chemical composition, crystalline structure, and morphology, they are often performed ex situ, which can induce changes to the SEI layer after it is removed from the electrolyte. While there have been efforts to combine these techniques using pseudo-in situ approaches via vacuum-compatible devices and inert atmosphere chambers connected to glove boxes, there is still a need for true in situ techniques to obtain results with improved accuracy and precision. Scanning electrochemical microscopy (SECM) is an in situ scanning probe technique that can be combined with optical spectroscopy techniques such as Raman and photoluminescence spectroscopy methods to gain insights into the electronic changes of a material as a function of applied bias. This Review will highlight the potential of SECM and recent reports on combining spectroscopic measurements with SECM to gain insights into the SEI layer formation and redox activities of other battery electrode materials. These insights provide invaluable information for improving the performance of charge storage devices.

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Section: Discussionmentioning

confidence: 99%

Scanning Electrochemical Microscopy for Chemical Imaging and Understanding Redox Activities of Battery Materials

Strange

Wornyo

et al. 2023

Chemical & Biomedical Imaging

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“…536 Reactive intermediates play an important role in many electrochemical processes and SECM is well adapted to monitor their formation during electrocatalysis. 537 Chang and Bard reported the detection of the short-lived Sn(III) intermediate and the mechanism of Sn(IV)/Sn(II) electroreduction in bromide media by cyclic voltammetry and operando SECM. 538 The Bard group employed the TG-SC mode to capture the unstable intermediate CO 2…”

Section: Sepm Tip In the Investigation Of Other Reactions For Electro...mentioning

confidence: 99%

Operando Scanning Electrochemical Probe Microscopy during Electrocatalysis

et al. 2023

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Scanning electrochemical probe microscopy (SEPM) techniques can disclose the local electrochemical reactivity of interfaces in single-entity and sub-entity studies. Operando SEPM measurements consist of using a SEPM tip to investigate the performance of electrocatalysts, while the reactivity of the interface is simultaneously modulated. This powerful combination can correlate electrochemical activity with changes in surface properties, e.g., topography and structure, as well as provide insight into reaction mechanisms. The focus of this review is to reveal the recent progress in local SEPM measurements of the catalytic activity of a surface toward the reduction and evolution of O2 and H2 and electrochemical conversion of CO2. The capabilities of SEPMs are showcased, and the possibility of coupling other techniques to SEPMs is presented. Emphasis is given to scanning electrochemical microscopy (SECM), scanning ion conductance microscopy (SICM), electrochemical scanning tunneling microscopy (EC-STM), and scanning electrochemical cell microscopy (SECCM).

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“…82 With the TG/ SC mode, SECM is evidenced to quantitatively determine the *CO 2 À intermediate and its dimerization during CO 2 RR. 155,156 The CO 2 is constantly reduced at a hemisphere-shaped Hg/Pt UME, and the produced *CO 2 À can dimerize to form oxalate within the nanogap between the tip and the substrate and be collected at the Au substrate. The rate of *CO 2 À dimerization is determined to be 6.0 Â 10 8 M À1 s À1 with a half-life of 10 ns by fitting the collection efficiency versus distance curve, which represents the fastest homogeneous coupling reaction that has been measured electrochemically.…”

Section: Build-up Of a Dynamic Interface Toward Co 2 Rrmentioning

confidence: 99%

Spatially and temporally understanding dynamic solid–electrolyte interfaces in carbon dioxide electroreduction

Wang

Tan

et al. 2023

Chem. Soc. Rev.

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Probing the reactive intermediate species generated during electrocatalysis by scanning electrochemical microscopy

Cited by 10 publications

References 62 publications

Scanning Electrochemical Microscopy for Chemical Imaging and Understanding Redox Activities of Battery Materials

Scanning Electrochemical Microscopy for Chemical Imaging and Understanding Redox Activities of Battery Materials

Operando Scanning Electrochemical Probe Microscopy during Electrocatalysis

Spatially and temporally understanding dynamic solid–electrolyte interfaces in carbon dioxide electroreduction

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