A Sealed Liquid Cell for &lt;italic&gt;In Situ&lt;/italic&gt; Transmission Electron Microscopy of Controlled Electrochemical Processes

Leenheer, Andrew Jay; Sullivan, John P.; Shaw, Michael J.; Harris, Charles Thomas

doi:10.1109/jmems.2014.2380771

Cited by 61 publications

(74 citation statements)

References 20 publications

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“…The spacer may be a solid layer with a channel, or spherical particles. The liquid may be inserted through an entry port etched into one chip (14)(15)(16)(17)(18) or flowed in through the gap between the chips (19). Electrodes can be patterned lithographically inside the closed cell and controlled by an external potentiostat (14).…”

Section: The Rapidly Developing Liquid Cell Microscopy Techniquementioning

confidence: 99%

Opportunities and challenges in liquid cell electron microscopy

Ross

2015

Science

480

434

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Advances in seeing small things Electron microscopes, particularly those with aberration correction, can view materials at the subnanometer scale. Additional improvements make it possible to obtain images at lower electron doses, thus minimizing the damage to the sample. However, for a number of materials, particularly those of biological origin, samples need to be imaged in solution. Ross reviews recent advances that have made it possible to do liquid cell electron microscopy, which opens up the possibility of studying problems such as the changes inside a battery during operation, the growth of crystals from solution, or biological molecules in their native state. Science , this issue p. 10.1126/science.aaa9886

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Section: The Rapidly Developing Liquid Cell Microscopy Techniquementioning

confidence: 99%

Opportunities and challenges in liquid cell electron microscopy

Ross

2015

Science

480

434

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“…Even EDLs associated with liquid organic electrolyte in batteries have arguably only recently received systematic experimental studies. [26][27][28] Modeling efforts have made much progress in elucidating the structures of solid-solid [29][30][31] transfer like parasitic reactions and undesirable metal plating, have arguably received less theoretical attention. In this work, we apply electronic Density Functional Theory (DFT) calculations to investigate how voltages affect the structures and stoichiometries of thin solid films, their interfaces, and their EDL at atomic lengthscales.…”

Section: Introductionmentioning

confidence: 99%

How Voltage Drops Are Manifested by Lithium Ion Configurations at Interfaces and in Thin Films on Battery Electrodes

Leung

Leenheer

2015

J. Phys. Chem. C

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Battery electrode surfaces are generally coated with electronically insulating solid films of thickness 1-50 nm. Both electrons and Li + can move at the electrode-surface film interface in response to the voltage, which adds complexity to the "electric double layer" (EDL). We apply Density Functional Theory (DFT) to investigate how the applied voltage is manifested as changes in the EDL at atomic lengthscales, including charge separation and interfacial dipole moments. Illustrating examples include Li 3 PO 4 , Li 2 CO 3 , and Li x Mn 2 O 4 thin-films on Au(111) surfaces under ultrahigh vacuum conditions. Adsorbed organic solvent molecules can strongly reduce voltages predicted in vacuum. We propose that manipulating surface dipoles, seldom discussed in battery studies, may be a viable strategy to improve electrode passivation. We also distinguish the computed potential governing electrons, which is the actual or instantaneous voltage, and the "lithium cohesive energy"-based voltage governing Li content widely reported in DFT calculations, which is a slower-responding self-consistency criterion at interfaces. This distinction is critical for a comprehensive description of electrochemical activities on electrode surfaces, including Li + insertion dynamics, parasitic electrolyte decomposition, and electrodeposition at overpotentials. keywords: lithium ion batteries; voltage prediction; density functional theory; computational electrochemistry

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“…7,9 The former point relates to the welldescribed importance of electrolyte volume and electrode placement in thin-layer electrochemistry. 29 However, the exact origins of how and to what extent the e − beam can alter electrochemical measurements of interest is unclear.…”

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confidence: 99%

Electrochemical Measurements in In Situ TEM Experiments

Fahrenkrug

Alsem

Salmon

et al. 2017

J. Electrochem. Soc.

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Potential sources of measurement error in electroanalytical analyses performed in-situ within a transmission electron microscope (TEM) are reported. Some relevant aspects of experimental set-up that impact noise are identified. The possibility of ground loops and recommendations that minimize them are presented. Offsets in the measured open circuit potential of working electrodes caused by the presence of the electron beam in TEM are demonstrated and discussed. This work also highlights the possibility of erroneous potential measurements when the electrode area exposed to electrolyte is significantly larger than the beam illumination area. General design criteria are proposed to assist in future electrochemical cell designs to mitigate electrochemical measurement artifacts inside a TEM.

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A Sealed Liquid Cell for <italic>In Situ</italic> Transmission Electron Microscopy of Controlled Electrochemical Processes

Cited by 61 publications

References 20 publications

Opportunities and challenges in liquid cell electron microscopy

Opportunities and challenges in liquid cell electron microscopy

How Voltage Drops Are Manifested by Lithium Ion Configurations at Interfaces and in Thin Films on Battery Electrodes

Electrochemical Measurements in In Situ TEM Experiments

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