Scanning electrochemical microscopy methods (SECM) and ion-selective microelectrodes for corrosion studies

Traxler, Ines; Singewald, Tanja Denise; Schimo-Aichhorn, Gabriela; Hild, Sabine; Valtiner, Markus

doi:10.1515/corrrev-2021-0104

Cited by 11 publications

(9 citation statements)

References 210 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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“…SECM is one of the scanning probe microscopy techniques using ultramicroelectrodes (UMEs) as a probe [ 23 ]. This allows the probing of electrochemical processes at the micro- or nano-scale, providing spatially resolved information regarding surface electrochemical reactivity and topography [ 24 , 25 ]. SECM offers the unique ability to locally analyse corrosion, material interfaces, and biological systems.…”

Section: Introductionmentioning

confidence: 99%

Localised Electrochemical Impedance Spectroscopy of Gold Nanoparticles Labelled Antibodies Probed by Platinum Microstructured Ultramicroelectrode

Zinovicius,

Morkvenaite-Vilkonciene,

Ramanavicius

2024

Materials

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This research is focused on enhancing the capabilities of scanning electrochemical impedance microscopy (SEIM) for detecting gold nanoparticle-labelled antibodies using electrochemically modified platinum ultramicroelectrode. The primary objective was to address the high resistance issue encountered in previous measurements with SEIM via the utilization of SEIM probes based on micro-electrodes modified by platinum microstructures, which improved the sensitivity and precision of the detection of targeted biomolecules. The modified probe resulted in a lowered charge transfer resistance by over ten times and a decrease in detection to around 100 fg/mL. We suggest potential applications in various biotechnological and biomedical fields, with future research expected to further refine this technique.

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“…The UME can be used amperometrically or potentiometrically while scanned close to the substrate’s surface to collect local current or potential maps of the metal studied. There are different operating modes of SECM that have been used to study corroding metals, including feedback mode, , generation-collection mode, , redox competition mode, , AC mode, , and potentiometric mode. , The use of SECM in corrosion science has been reviewed by many authors over the past decade. − …”

Section: Introductionmentioning

confidence: 99%

Effect of Redox Mediators on Corrosion Behavior and Scanning Electrochemical Microscopy Response

Mena-Morcillo,

Ebrahimzadeh Pilehrood,

Moshrefi

et al. 2024

Anal. Chem.

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Scanning electrochemical microscopy (SECM) is widely used to measure local electrochemical reactivity of corroding surfaces. A major criticism of using SECM in feedback mode for corrosion studies is the requirement of an external redox mediator (RM) as it could react with the metal and affect the Nernst potential at the metal–solution interface. Consequently, it becomes challenging to differentiate the interference caused by the RM from the local reactivity of the metal. Herein, a multiscale electrochemical approach is presented to investigate the effect of RM choice on the corroding substrate. Two common RMs, ferrocenemethanol and hexaammineruthenium(III) chloride, were used to perform SECM over copper and aluminum. It was found during macroscale electrochemical measurements that Ru(NH)6 3+ acted as an oxidant and promoted corrosion. The SECM feedback behavior varied for copper depending on the RM used, suggesting that the corrosion reactions controlled the negative feedback mechanism, not the formation of an insulating passive film. The passivated aluminum surface consistently exhibited negative feedback, regardless of the RM used. SECM approach curves also displayed a distortion in the steady state current, which was caused by the deposition of substrate-generated species on the microelectrode. These deviations in feedback response were accounted for during analysis through incorporation into a finite element model to accurately extract the RM kinetic rate constants. The importance of understanding these processes is highlighted to avoid misinterpretation of passive behavior and advances toward a more quantitative use of SECM for corrosion studies.

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Scanning electrochemical microscopy methods (SECM) and ion-selective microelectrodes for corrosion studies

Cited by 11 publications

References 210 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

Localised Electrochemical Impedance Spectroscopy of Gold Nanoparticles Labelled Antibodies Probed by Platinum Microstructured Ultramicroelectrode

Effect of Redox Mediators on Corrosion Behavior and Scanning Electrochemical Microscopy Response

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