Radiation damage of liquid electrolyte during focused X-ray beam photoelectron spectroscopy

Arble, Christopher; Guo, Hongxuan; Strelcov, Evgheni; Hoskins, Brian D.; Zeller, Patrick; Matteo, Amati; Gregoratti, Luca; Kolmakov, Andrei

doi:10.1016/j.susc.2020.121608

Cited by 11 publications

(6 citation statements)

References 52 publications

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“…However, this approach suffers from beam damage requiring graphene of high quality to ensure stability during data acquisition. The illumination of an aqueous electrolyte, with an intense X-ray beam, yields the formation of radicals from water radiolysis; these radicals damage the graphene layer [15,52,53]. To solve this issue, the stability of the graphene layer can be increased by stacking more layers of graphene one on top of the other.…”

Section: Can the Operando Approaches Based In Photoelectron Spectrosc...mentioning

confidence: 99%

The rise of electrochemical NAPXPS operated in the soft X-ray regime exemplified by the oxygen evolution reaction on IrO_x electrocatalysts

et al. 2022

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Section: Can the Operando Approaches Based In Photoelectron Spectrosc...mentioning

confidence: 99%

The rise of electrochemical NAPXPS operated in the soft X-ray regime exemplified by the oxygen evolution reaction on IrO_x electrocatalysts

et al. 2022

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“…In combination with graphene (and similar) liquid cells, the proposed SEM imaging method can become a standard approach for studying a wide variety of practically relevant electrochemical systems where laterally heterogeneous interfaces are present and high-resolution polarization mapping is required, and this is the subject of the ongoing research. As we and others have shown recently, dose reduction is required to avoid (or to minimize) the radiation damage of the electrolyte. In this regard, we note that damage-free quantification and mapping of the polarization potentials of radiation sensitive electrolytes can also be done using Kelvin probe force microscopy …”

Section: Discussionmentioning

confidence: 97%

“…The proposed method is most useful for studying electrochemical systems where laterally heterogeneous interfaces are present and highresolution polarization mapping is required. As we have shown recently, care has to be taken in these cases to minimize the radiation damage of the electrolyte 32 and damage-free quantification and mapping of the polarization potentials of radiation sensitive electrolytes can be also done using Kelvin Probe Force Microscopy. 33…”

Section: Discussionmentioning

confidence: 99%

“…The cell bias range used for polarization studies was restricted to ca. 1 V to avoid water splitting or Cu plating reactions, which manifest themselves as gas bubbles or characteristic particulate Cu deposit formation under the graphene . Pt was also selected as a counter electrode to widen the non-faradaic window.…”

Section: Methodsmentioning

confidence: 99%

“…1 V to avoid water splitting or Cu plating reactions, which manifest themselves as gas bubbles or characteristic particulate Cu deposit formation under the graphene. 34 Pt was also selected as a counter electrode to widen the non-faradaic window. To minimize the effect of the bias on SE trajectories to the detector, the MCA's front Gr reference electrode was grounded, and a polarization bias was applied to the Pt bottom electrode instead (Figure 1d,e).…”

Section: ■ Introductionmentioning

confidence: 99%

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Probing Electrified Liquid–Solid Interfaces with Scanning Electron Microscopy

Guo

Yulaev

Strelcov

et al. 2020

ACS Appl. Mater. Interfaces

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Electrical double layers play a key role in a variety of electrochemical systems. The mean free path of secondary electrons in aqueous solutions is on the order of a nanometer, making them suitable for probing of ultrathin electrical double layers at solid-liquid electrolyte interfaces. Employing 2 graphene as an electron-transparent electrode in a two-electrode electrochemical system, we show that the secondary electron yield of the graphene-liquid interface depends on the ionic strength and concentration of electrolyte and applied bias at the remote counter electrode. These observations have been related to polarization-induced changes in the potential distribution within the electrical double layer and demonstrate the feasibility of using scanning electron microscopy to examine and map electrified liquid-solid interfaces.

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Interfaces and Interphases in Batteries: How to Identify and Monitor Them Properly Using Surface Sensitive Characterization Techniques

Villevieille

2022

Adv Materials Inter

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design, characterization, equipment, modelling, artificial intelligence, engineering, etc. [3] The main challenges are quite frequently addressed in the literature, including i) the development of a new electroactive material with higher operating voltage/specific capacity, which would increase the overall energy density of the battery; ii) the safety issues concerning the Li metal counter electrode and its uncontrollable interface, called dendrites; iii) the power density of the system, which merits proper electrode architecture and material design; and iv) the replacement of organic liquid electrolytes that are responsible for certain safety issues such as flammability and decomposition caused by electrochemical stability windows smaller than 4 V. [4] Understanding the underlying reaction mechanisms governing the electrochemical processes is an engaging yet challenging task. This is because of the complexity of battery technology: multiple interactions exist that can concern several length scales, from the mm to the nm scale, including the bulk, the surface, the interphase, and their own interactions between each other. [5,6] Another way to actively ensure the development of better/ safer battery systems is a thorough investigation using several advanced characterization techniques (ideally operando, that is, during battery operation) that can probe multiscale lengths. [7,8] Bulk reactions are typically well-understood and monitored because these processes generally occur on a microscopic scale. Furthermore, several characterization techniques were initially developed to monitor bulk reactions, providing substantial knowledge at the macroscopic scale, such as structural evolution. [9] Surface/interphase/interface investigation is more complex primarily because of the size of the "surface" layer (only a few nanometres) and the "fragility" (mechanical and transient nature) of this layer due to its chemical composition. [10,11] Indeed, the surface layer is mainly composed of organic/polymeric species that can easily "burn" during the investigation. A persistent issue that has not yet been properly addressed in the literature is beam damage, which is one of the most common threats to proper interface/interphase investigation. [8,12] This is because the chemical composition of the layer changes rapidly during beam damage. Moreover, interphase/interface/surface chemistries evolve faster than the time-scale resolution of various applied characterization techniques and are primarily Interfaces, interphases, surfaces, and bulk are the main elements in a battery that require to be monitored and understood to control battery life during cycling and electrochemical ageing. To date, bulk-related processes are generally easier to address in terms of characterization techniques because in-depth investigations of most of these processes can be performed in operando mode (that is, during battery cycling). However, investigations of surfaces, interfaces, and interphases possess some challenges due to the involved nanosize dim...

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Radiation damage of liquid electrolyte during focused X-ray beam photoelectron spectroscopy

Cited by 11 publications

References 52 publications

The rise of electrochemical NAPXPS operated in the soft X-ray regime exemplified by the oxygen evolution reaction on IrO_x electrocatalysts

The rise of electrochemical NAPXPS operated in the soft X-ray regime exemplified by the oxygen evolution reaction on IrO_x electrocatalysts

Probing Electrified Liquid–Solid Interfaces with Scanning Electron Microscopy

Interfaces and Interphases in Batteries: How to Identify and Monitor Them Properly Using Surface Sensitive Characterization Techniques

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Radiation damage of liquid electrolyte during focused X-ray beam photoelectron spectroscopy

Cited by 11 publications

References 52 publications

The rise of electrochemical NAPXPS operated in the soft X-ray regime exemplified by the oxygen evolution reaction on IrOx electrocatalysts

The rise of electrochemical NAPXPS operated in the soft X-ray regime exemplified by the oxygen evolution reaction on IrOx electrocatalysts

Probing Electrified Liquid–Solid Interfaces with Scanning Electron Microscopy

Interfaces and Interphases in Batteries: How to Identify and Monitor Them Properly Using Surface Sensitive Characterization Techniques

Contact Info

Product

Resources

About

The rise of electrochemical NAPXPS operated in the soft X-ray regime exemplified by the oxygen evolution reaction on IrO_x electrocatalysts

The rise of electrochemical NAPXPS operated in the soft X-ray regime exemplified by the oxygen evolution reaction on IrO_x electrocatalysts