In situ electron microscopy and X-ray photoelectron spectroscopy for high capacity anodes in next-generation ionic liquid-based Li batteries

Tsuda, Toshitaka; Imanishi, Akihito; Sano, Teruki; Sawamura, Amane; Kamidaira, Toshiki; Chen, Chih-Yao; Uchida, Satoshi; Kusumoto, Shohei; Ishikawa, Masashi; Kuwabata, Susumu

doi:10.1016/j.electacta.2018.05.081

Cited by 21 publications

(13 citation statements)

References 47 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Herein, a window‐less TEM holder has been designed for in situ observations of electrochemical reactions in less and nonvolatile electrolytes by applying our prior knowledge of electron microscope techniques with ionic liquids (ILs). [ 27–29 ] The unique properties of ILs make them alternative electrolyte candidates for advanced batteries with improved performance and great safety, including LMA‐based secondary batteries. [ 10,30–32 ] Their extremely low vapor pressure, antistatic property, and remarkable physicochemical stability entirely fulfil the requirements for long‐period TEM characterization.…”

Section: Introductionmentioning

confidence: 99%

In Situ Monitoring of Lithium Metal Anodes and Their Solid Electrolyte Interphases by Transmission Electron Microscopy

et al. 2021

Self Cite

View full text Add to dashboard Cite

Lithium (Li) metal anodes (LMAs) are considered to be the holy grail of electrodes to enable advanced battery chemistry for energy‐intensive applications. However, the formation of Li dendrites and their intricate interplay with the solid electrolyte interphase (SEI) remain unclear to date. Herein, a simple yet efficient methodology for in situ transmission electron microscopy (TEM) observation is reported, and the relationship between the SEI chemistry and the morphology of LMAs is unraveled by a combination of TEM imaging and selected area electron diffraction analysis in an unprecedented way. The authors find that the coexistence of LiF and Li3N in the SEI layer helps realize dendrite‐free Li deposition and directly visualize the deposition–dissolution behavior of individual Li deposits with different microstructures. The approach should be applicable to scrutinize a broad range of interfacial reactions in nonvolatile electrolytes (e.g., ionic liquid, glass‐, and ceramic‐based electrolytes) relevant to future energy storage devices, including magnesium secondary batteries.

show abstract

Section: Introductionmentioning

confidence: 99%

In Situ Monitoring of Lithium Metal Anodes and Their Solid Electrolyte Interphases by Transmission Electron Microscopy

et al. 2021

Self Cite

View full text Add to dashboard Cite

show abstract

“…28 Electrical potential distribution/variations in solid/liquid electrolyte interfaces, as revealed by XPS, are even more informative since the sign, the magnitude, and also the variations in cation/ anion ratios are directly quantifiable. 47−49 Tsuda et al have reported earlier on a combined SEM and XPS investigation of anodes of IL-based Li batteries, 50 followed by a more recent report by Benayad et al 51 The potential distribution at the electrified liquid/solid interfaces has been recently probed via careful deconvolution of XPS signatures of the special molecular probes. 52 This present work reports on a comparative XPS and SEM operando study of a model coplanar electrochemical device consisting of two metal electrodes deposited on a porous polyethylene membrane (PEM) film coated with an IL as the electrolyte medium.…”

Section: ■ Introductionmentioning

confidence: 99%

“…Tsuda et al have reported earlier on a combined SEM and XPS investigation of anodes of IL-based Li batteries, followed by a more recent report by Benayad et al The potential distribution at the electrified liquid/solid interfaces has been recently probed via careful deconvolution of XPS signatures of the special molecular probes …”

Section: Introductionmentioning

confidence: 99%

Comparative Operando XPS and SEM Spatiotemporal Potential Mapping of Ionic Liquid Polarization in a Coplanar Electrochemical Device

2021

View full text Add to dashboard Cite

The polarization response of a coplanar electrochemical capacitor covered with an ionic liquid as the electrolyte has been examined using a combination of two powerful analytic techniques, X-ray photoelectron spectroscopy (XPS) and scanning electron microcopy (SEM). Spatiotemporal distribution of the ionic liquid surface potential, upon DC or AC (square wave) biasing, has been monitored via chemical element binding energy shifts using XPS and secondary electron intensity variations using SEM. SEM's high spatial resolution and speedy imaging together with application of a data mining algorithm made mapping of the surface potential distribution across the capacitor possible. Interestingly, despite the differences in the detection principles, both techniques yield similar polarization relaxation time constants. The results demonstrate the power of a synergistic combination of the two techniques with complementary capabilities and pave the way to a deeper understanding of liquid/solid interfaces and for performance evaluation and diagnostics of electrochemical devices.

show abstract

“…Facilitated by their high vacuum compatibility, over the past decade ILs have been fairly well characterized in‐vacuo by X‐ray photoelectron spectroscopy (XPS) as a function of electrochemical potential [34–58] . XPS allows for the determination of surface composition of an IL while also probing the binding energy shifts in the ions ( U XPS ; units of eV) as a function of an external electrochemical potential ( U ; units of V).…”

Section: Introductionmentioning

confidence: 99%

The Influence of Water Vapor on the Electrochemical Shift of an Ionic Liquid Measured by Ambient Pressure X‐ray Photoelectron Spectroscopy

2021

View full text Add to dashboard Cite

Ionic liquids (ILs) are considered to be one of the steppingstones to fabricate next generation electrochemical devices given their unique physical and chemical properties. The addition of water to ILs significantly impact electrochemical related properties including viscosity, density, conductivity, and electrochemical window. Herein we utilize ambient pressure X‐ray photoelectron spectroscopy (APXPS) to examine the impact of water on values of the electrochemical shift (S), which is determined by measuring changes in binding energy shifts as a function of an external bias. APXPS spectra of C 1s, O 1s and N 1s regions are examined for the IL 1‐butyl‐3‐methylimidazolium acetate, [C4mim][OAc], at the IL/gas interface as a function of both water vapor pressure and external bias. Results reveal that in the absence of water vapor there is an IL ohmic drop between the working electrode and quasi reference electrode, giving rise to chemical specific S values of less than one. Upon introducing water vapor, S values approach one as a function of increasing water vapor pressure, indicating a decrease in the IL ohmic drop as the IL/water mixture becomes more conductive and the potential drop is driven by the electric double layer at the electrode/IL interface.

show abstract

In situ electron microscopy and X-ray photoelectron spectroscopy for high capacity anodes in next-generation ionic liquid-based Li batteries

Cited by 21 publications

References 47 publications

In Situ Monitoring of Lithium Metal Anodes and Their Solid Electrolyte Interphases by Transmission Electron Microscopy

In Situ Monitoring of Lithium Metal Anodes and Their Solid Electrolyte Interphases by Transmission Electron Microscopy

Comparative Operando XPS and SEM Spatiotemporal Potential Mapping of Ionic Liquid Polarization in a Coplanar Electrochemical Device

The Influence of Water Vapor on the Electrochemical Shift of an Ionic Liquid Measured by Ambient Pressure X‐ray Photoelectron Spectroscopy

Contact Info

Product

Resources

About