Dynamic Imaging of Nanostructures in an Electrolyte with a Scanning Electron Microscope

Yoon, Aram; Herzog, Antonia; Grosse, Philipp; Alsem, Daan Hein; Chee, See Wee; Cuenya, Beatriz Roldán

doi:10.1017/s1431927620024769

Cited by 9 publications

(13 citation statements)

References 46 publications

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“…not the electrolyte, it is often hard to interpret how and why the structure of the electrode changed during the degradation process. To overcome this limitation, operando liquid cells have been developed for STEM [151][152][153] and also for SEM [154] that permit structure/chemistry changes in the electrodes to be observed during electrochemical cycling in all forms of liquid electrolytes. For these liquid cells, the low mass/density of Li metal causes a contrast reversal in the experimental images that makes the identification and tracking of Li metal easily quantifiable [151].…”

Section: Statusmentioning

confidence: 99%

Roadmap for a sustainable circular economy in lithium-ion and future battery technologies

et al. 2023

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The market dynamics, and their impact on a future circular economy for lithium-ion batteries (LIB), are presented in this roadmap, with safety as an integral consideration throughout the life cycle. At the point of end-of-life, there is a range of potential options – remanufacturing, reuse and recycling. Diagnostics play a significant role in evaluating the state of health and condition of batteries, and improvements to diagnostic techniques are evaluated. At present, manual disassembly dominates end-of-life disposal, however, given the volumes of future batteries that are to be anticipated, automated approaches to the dismantling of end-of-life battery packs will be key. The first stage in recycling after the removal of the cells is the initial cell-breaking or opening step. Approaches to this are reviewed, contrasting shredding and cell disassembly as two alternative approaches. Design for recycling is one approach that could assist in easier disassembly of cells, and new approaches to cell design that could enable the circular economy of LIBs are reviewed. After disassembly, subsequent separation of the black mass is performed before further concentration of components. There are a plethora of alternative approaches for recovering materials; this roadmap sets out the future directions for a range of approaches including pyrometallurgy, hydrometallurgy, short-loop, direct, and the biological recovery of LIB materials. Furthermore, anode, lithium, electrolyte, binder and plastics recovery are considered in the range of approaches in order to maximise the proportion of materials recovered, minimise waste and point the way towards zero-waste recycling. The life-cycle implications of a circular economy are discussed considering the overall system of LIB recycling, and also directly investigating the different recycling methods. The legal and regulatory perspectives are also considered. Finally, with a view to the future, approaches for next-generation battery chemistries and recycling are evaluated, identifying gaps for research.

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Section: Statusmentioning

confidence: 99%

Roadmap for a sustainable circular economy in lithium-ion and future battery technologies

et al. 2023

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“…A c c e p t e d M a n u s c r i p t and are exploring the use of a commercial closed cell system (Figure 5(c)) with integrated flow and regular reference/counter electrodes [163] for operando electrochemical studies.…”

Section: (F))mentioning

confidence: 99%

In situ and operando electron microscopy in heterogeneous catalysis—insights into multi-scale chemical dynamics

Chee

Lunkenbein

Schlögl

et al. 2021

J. Phys.: Condens. Matter

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This review features state-of-the-art in situ and operando electron microscopy (EM) studies of heterogeneous catalysts in gas and liquid environments during reaction. Heterogeneous catalysts are important materials for the efficient production of chemicals/fuels on an industrial scale and for energy conversion applications. They also play a central role in various emerging technologies that are needed to ensure a sustainable future for our society. Currently, the rational design of catalysts has largely been hampered by our lack of insight into the working structures that exist during reaction and their associated properties. However, elucidating the working state of catalysts is not trivial, because catalysts are metastable functional materials that adapt dynamically to a specific reaction condition. The structural or morphological alterations induced by chemical reactions can also vary locally. A complete description of their morphologies requires that the microscopic studies undertaken span several length scales. EMs, especially transmission electron microscopes, are powerful tools for studying the structure of catalysts at the nanoscale because of their high spatial resolution, relatively high temporal resolution, and complementary capabilities for chemical analysis. Furthermore, recent advances have enabled the direct observation of catalysts under realistic environmental conditions using specialized reaction cells. Here, we will critically discuss the importance of spatially-resolved operando measurements and the available experimental setups that enable (1) correlated studies where EM observations are complemented by separate measurements of reaction kinetics or spectroscopic analysis of chemical species during reaction or (2) real-time studies where the dynamics of catalysts are followed with EM and the catalytic performance is extracted directly from the reaction cell that is within the EM column or chamber. Examples of current research in this field will be presented. Challenges in the experimental application of these techniques and our perspectives on the field’s future directions will also be discussed.

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“…Therefore, studies of operando characterizations at the solid–liquid interface ( i.e., in situ characterization under electrochemical reaction in the liquid phase) have recently received attention. In situ and in real space the morphology changes and surface reconstruction of a model Cu electrocatalyst on atomic scale during the electrochemical CO 2 reduction reaction (CO 2 RR) were observed with an electrochemical atomic force microscope (AFM) which enabled the direct observation of oxidized copper surfaces entering different morphological regimes when certain cathodic CO 2 RR potential ranges are set. , Indeed, using both cyclic voltammetry and in situ electrochemical STM, it was shown that the electrochemical signal and the roughening of its surface are well-related. , Recently, by using liquid cell transmission electron microscopy (TEM) and scanning electron microscopy (SEM), it was found that Cu 2 O nanocatalysts restructure under CO 2 RR conditions. − These well-established operando technologies allow us to observe key information on catalytic behaviors by monitoring the changes in interfaces on an atomic scale.…”

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confidence: 99%

Hot Electron Phenomena at Solid–Liquid Interfaces

Lee

Jeon

Lee

et al. 2022

J. Phys. Chem. Lett.

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Understanding the role of energy dissipation and charge transfer under exothermic chemical reactions on metal catalyst surfaces is important for elucidating the fundamental phenomena at solid–gas and solid–liquid interfaces. Recently, many surface chemistry studies have been conducted on the solid–liquid interface, so correlating electronic excitation in the liquid-phase with the reaction mechanism plays a crucial role in heterogeneous catalysis. In this review, we introduce the detection principle of electron transfer at the solid–liquid interface by developing cutting-edge technologies with metal–semiconductor Schottky nanodiodes. The kinetics of hot electron excitation are well correlated with the reaction rates, demonstrating that the operando method for understanding nonadiabatic interactions is helpful in studying the reaction mechanism of surface molecular processes. In addition to the detection of hot electrons excited by a catalytic reaction, we highlight recent results on how the transfer of the hot electrons influences surface chemical and photoelectrochemical reactions.

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Dynamic Imaging of Nanostructures in an Electrolyte with a Scanning Electron Microscope

Abstract: Abstract

Cited by 9 publications

References 46 publications

Roadmap for a sustainable circular economy in lithium-ion and future battery technologies

Roadmap for a sustainable circular economy in lithium-ion and future battery technologies

In situ and operando electron microscopy in heterogeneous catalysis—insights into multi-scale chemical dynamics

Hot Electron Phenomena at Solid–Liquid Interfaces

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