Chemical and bonding analysis of liquids using liquid cell electron microscopy

Ercius, Peter; Hachtel, Jordan A.; Klie, Robert F.

doi:10.1557/mrs.2020.230

Cited by 8 publications

(3 citation statements)

References 72 publications

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“…The latest advances in chip fabrication and TEM holder design have significantly increased the effective solid-angle range of the detector, thereby increasing the X-ray collection efficiency. Additionally, the invention of large solid-angle X-ray detectors and high-sensitivity EELS spectrometers have enabled outstanding signal detection, with a higher efficiency than before [86][87][88] . In addition, the high electron dose required to generate sufficient secondary signals for EDS or EELS, which is generally several orders of magnitude higher than that needed to produce annular dark-field images [89] , might produce a large number of gas bubbles in the liquid, thereby affecting the imaging process.…”

Section: Discussionmentioning

confidence: 99%

Applications of in situ electron microscopy in oxygen electrocatalysis

Wu¹,

Zhang²,

Chen³

et al. 2022

Microstructures

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Oxygen electrocatalysis involving the oxygen reduction reaction (ORR) and oxygen evolution reaction (OER) plays a vital role in cutting-edge energy conversion and storage technologies. In situ studies of the evolution of catalysts during oxygen electrocatalysis can provide important insights into their structure - activity relationships and stabilities under working conditions. Among the various in situ characterization tools available, in situ electron microscopy has the unique ability to perform structural and compositional analyzes with high spatial resolution. In this review, we present the latest developments in in situ and quasi-in situ electron microscopic techniques, including identical location electron microscopy, in situ liquid cell (scanning) transmission electron microscopy and in situ environmental transmission electron microscopy, and elaborate their applications in the ORR and OER. Our discussion centers on the degradation mechanism, structural evolution and structure - performance correlations of electrocatalysts. Finally, we summarize the earlier discussions and share our perspectives on the current challenges and future research directions of using in situ electron microscopy to explore oxygen electrocatalysis and related processes.

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Section: Discussionmentioning

confidence: 99%

Applications of in situ electron microscopy in oxygen electrocatalysis

Wu¹,

Zhang²,

Chen³

et al. 2022

Microstructures

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“…We then applied liquid-phase TEM techniques to maintain the volatile liquids under vacuum. Now, most liquid cell experiments are based on imaging with mass thickness and/or phase contrast, requiring a large input radiation dose ( 33 ). However, a large radiation dose is incompatible with radiation-sensitive materials, such as organic liquids, even at low temperatures.…”

Section: Introductionmentioning

confidence: 99%

Spatially resolved structural order in low-temperature liquid electrolyte

et al. 2023

Self Cite

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Determining the degree and the spatial extent of structural order in liquids is a grand challenge. Here, we are able to resolve the structural order in a model organic electrolyte of 1 M lithium hexafluorophosphate (LiPF 6 ) dissolved in 1:1 (v/v) ethylene carbonate:diethylcarbonate by developing an integrated method of liquid-phase transmission electron microscopy (TEM), cryo-TEM operated at −30°C, four-dimensional scanning TEM, and data analysis based on deep learning. This study reveals the presence of short-range order (SRO) in the high–salt concentration domains of the liquid electrolyte from liquid phase separation at the low temperature. Molecular dynamics simulations suggest the SRO originates from the Li + -(PF 6 − ) n ( n > 2) local structural order induced by high LiPF 6 salt concentration.

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“…We then applied liquid phase TEM techniques to maintain the volatile liquids under vacuum. Currently, most liquid cell experiments are based on imaging with mass-thickness and/or phase contrast requiring a large input radiation dose (33). However, a large radiation dose is incompatible with radiation-sensitive materials, such as organic liquids, even at low temperatures.…”

Section: Introductionmentioning

confidence: 99%

Spatially Resolved Structural Order in Low-Temperature Liquid Electrolyte

Xie

Ophus

Ercius

et al. 2023

Microscopy and Microanalysis

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Determining the degree and the spatial extent of structural order in liquids is a significant grand challenge. Here, we are able to resolve the structural order in a model organic electrolyte of 1 M lithium hexafluorophosphate (LiPF6) dissolved in 1:1 (v/v) ethylene carbonate (EC):dimethyl carbonate (DEC) by developing an integrated method of liquid-phase TEM, cryogenic transmission electron microscopy (cryo-TEM) operated at -30°C, four-dimensional scanning transmission electron microscopy (4D-STEM), and data analysis based on deep learning. This study reveals the presence of short-range order (SRO) in the high salt-concentration domains of the liquid electrolyte from liquid phase separation at the low temperature. Molecular dynamics simulations suggest the SRO originates from the Li + -(PF6 -)n (n>2) local structural order induced by high LiPF6 salt concentration. TeaserAn integrated advanced transmission electron microscope operated at -30°C reveals short-range order in liquid electrolyte.

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Chemical and bonding analysis of liquids using liquid cell electron microscopy

Abstract: Abstract

Cited by 8 publications

References 72 publications

Applications of in situ electron microscopy in oxygen electrocatalysis

Applications of in situ electron microscopy in oxygen electrocatalysis

Spatially resolved structural order in low-temperature liquid electrolyte

Spatially Resolved Structural Order in Low-Temperature Liquid Electrolyte

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