Scanning electrochemical microscopy: a versatile tool for inspecting the reactivity of battery electrodes

Sarbapalli, Dipobrato; Mishra, Abhiroop; Hatfield, Kendrich O.; Gossage, Zachary T.; Rodríguez‐López, Joaquín

doi:10.1088/978-0-7503-2682-7ch9

Cited by 4 publications

(6 citation statements)

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“…lower probe currents. [41] For simplifying the analysis, the measured tip current, i t , was normalized to the current far away from the substrate, i t /i ∞ . [42] By tracking changes in i t /i ∞ at the probe during raster we could reliably evaluate electron transfer and interphase formation across the MLG surface through feedback imaging (Figure 1b).…”

Section: Resultsmentioning

confidence: 99%

Tracking Passivation and Cation Flux at Incipient Solid‐Electrolyte Interphases on Multi‐Layer Graphene using High Resolution Scanning Electrochemical Microscopy

et al. 2022

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The solid electrolyte interphase (SEI) is a dynamic, electronically insulating film that forms on the negative electrode of Li+ batteries (LIBs) and enables ion movement to/from the interface while preventing electrolyte breakdown. However, there is limited comparative understanding of LIB SEIs with respect to those formed on Na+ and K+ electrolytes for emerging battery concepts. We used scanning electrochemical microscopy (SECM) for the in situ interfacial analysis of incipient SEIs in Li+, K+ and Na+ electrolytes formed on multi‐layer graphene. Feedback images using 300 nm SECM probes and ion‐sensitive measurements indicated a superior passivation and highest cation flux for a Li+‐SEI in contrast to Na+ and K+‐SEIs. Ex situ X‐ray photoelectron spectroscopy indicated significant fluoride formation for only Li+ and Na+‐SEIs, enabling correlation to in situ SECM measurements. While SEI chemistry remains complex, these electroanalytical methods reveal links between chemical variables and the interfacial properties of materials for energy storage.

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Section: Resultsmentioning

confidence: 99%

Tracking Passivation and Cation Flux at Incipient Solid‐Electrolyte Interphases on Multi‐Layer Graphene using High Resolution Scanning Electrochemical Microscopy

et al. 2022

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“…The working principle of approach curves is discussed in greater detail elsewhere. 26 In brief, the Pt UME was biased at 3.6 V vs Li + /Li to oxidize ferrocene at its surface (Fig. S3) and simultaneously moved towards the cathode at a speed of 1 μm s −1 .…”

Section: Resultsmentioning

confidence: 99%

“…24 In recent years, SECM has emerged as a powerful tool to study processes at the electrode-electrolyte interfaces in electrochemical energy storage systems. 25,26 In this work, SECM was utilized to investigate oxygen evolution from electroplated LiCoO 2 . We strategically chose electrodeposition as the synthesis method to produce samples with different facets exposed at the surface, 27 enabling us to investigate the facet dependence of oxygen loss.…”

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confidence: 99%

In Situ Investigation of Lattice Oxygen Loss from Preferentially Faceted Electrodeposited LiCoO₂ via Scanning Electrochemical Microscopy

Mishra,

Lin,

Zahiri

et al. 2024

J. Electrochem. Soc.

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Lattice oxygen loss from transition metal oxide cathodes in Li-ion batteries (LiBs) is a key factor responsible in their gradual capacity decline over time. Understanding and mitigating this phenomenon is crucial for the development of next-generation LiBs. The effect of various parameters on lattice oxygen loss, such as cathode chemical composition, has been studied extensively. However, there is a lack of experimental investigation into the lattice oxygen stability across different crystallographic facets within the same cathode composition. Here, we employed in situ scanning electrochemical microscopy (SECM) to investigate oxygen evolution from preferentially faceted, electrodeposited LiCoO2 cathodes. Samples predominantly exposing the (003) basal planes and the (101), (102), (110) fast Li-ion diffusing facets exhibited oxygen evolution at potentials exceeding 3.5 V vs Li+/Li. Finite element simulations helped quantify the flux of oxygen evolution on the first charge cycle to 33±5 pmol/cm2s for the basal plane and 37±9 pmol/cm2s for the faceted samples at potentials above 4 V based on single spot measurements. However, spatially resolved measurements showed that faceted samples exhibited significant heterogeneity in their oxygen evolution, reaching twofold values compared to the basal plane samples at potentials beyond 4.5 V.

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“…ESPTs utilize local physical or electrochemical interactions between a small probe (or tip) and the sample (or substrate) enabling micro-to nanoscale investigations of the changes in these properties. For further details regarding in-depth working principles of these ESPTs, we direct readers to additional literature on EC-AFM (14), SECM (13,16), SECCM (17)(18)(19), and SICM (20,21)…”

Section: A Primer On Espts Applied To Eesssmentioning

confidence: 99%

“…In addition, comprehensive chemical, morphological, and electrochemical characterization can be performed via correlative experiments, or by coupling spectroscopy-(5-7) or X-ray- (8,9) based measurements to ESPTs. The interested reader is referred to previous reviews covering analytical methods for EESSs (10), including nanoscale electrochemistry (11,12) and focused reviews covering the application of an individual ESPT (13,14). The scope of this review is limited to recent in situ and operando studies utilizing these ESPTs on LiBs and other novel battery chemistries beyond Li ion.…”

Section: Introductionmentioning

confidence: 99%

Electrochemical Imaging of Interfaces in Energy Storage via Scanning Probe Methods: Techniques, Applications, and Prospects

Mishra

Sarbapalli

Rodríguez

et al. 2023

Annual Rev. Anal. Chem.

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Developing a deeper understanding of dynamic chemical, electronic, and morphological changes at interfaces is key to solving practical issues in electrochemical energy storage systems (EESSs). To unravel this complexity, an assortment of tools with distinct capabilities and spatiotemporal resolutions have been used to creatively visualize interfacial processes as they occur. This review highlights how electrochemical scanning probe techniques (ESPTs) such as electrochemical atomic force microscopy, scanning electrochemical microscopy, scanning ion conductance microscopy, and scanning electrochemical cell microscopy are uniquely positioned to address these challenges in EESSs. We describe the operating principles of ESPTs, focusing on the inspection of interfacial structure and chemical processes involved in Li-ion batteries and beyond. We discuss current examples, performance limitations, and complementary ESPTs. Finally, we discuss prospects for imaging improvements and deep learning for automation. We foresee that ESPTs will play an enabling role in advancing EESSs as we transition to renewable energies. Expected final online publication date for the Annual Review of Analytical Chemistry, Volume 16 is June 2023. Please see http://www.annualreviews.org/page/journal/pubdates for revised estimates.

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Scanning electrochemical microscopy: a versatile tool for inspecting the reactivity of battery electrodes

Cited by 4 publications

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Tracking Passivation and Cation Flux at Incipient Solid‐Electrolyte Interphases on Multi‐Layer Graphene using High Resolution Scanning Electrochemical Microscopy

Tracking Passivation and Cation Flux at Incipient Solid‐Electrolyte Interphases on Multi‐Layer Graphene using High Resolution Scanning Electrochemical Microscopy

In Situ Investigation of Lattice Oxygen Loss from Preferentially Faceted Electrodeposited LiCoO₂ via Scanning Electrochemical Microscopy

Electrochemical Imaging of Interfaces in Energy Storage via Scanning Probe Methods: Techniques, Applications, and Prospects

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Scanning electrochemical microscopy: a versatile tool for inspecting the reactivity of battery electrodes

Cited by 4 publications

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Tracking Passivation and Cation Flux at Incipient Solid‐Electrolyte Interphases on Multi‐Layer Graphene using High Resolution Scanning Electrochemical Microscopy

Tracking Passivation and Cation Flux at Incipient Solid‐Electrolyte Interphases on Multi‐Layer Graphene using High Resolution Scanning Electrochemical Microscopy

In Situ Investigation of Lattice Oxygen Loss from Preferentially Faceted Electrodeposited LiCoO2 via Scanning Electrochemical Microscopy

Electrochemical Imaging of Interfaces in Energy Storage via Scanning Probe Methods: Techniques, Applications, and Prospects

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In Situ Investigation of Lattice Oxygen Loss from Preferentially Faceted Electrodeposited LiCoO₂ via Scanning Electrochemical Microscopy