Probing the Evolution of Surface Chemistry at the Silicon–Electrolyte Interphase via In Situ Surface-Enhanced Raman Spectroscopy

Ha, Yeyoung; Villers, Bertrand J. Tremolet de; Li, Zhifei; Xu, Yun; Stradins, Paul; Zakutayev, Andriy; Burrell, Anthony K.; Han, Sang‐Don

doi:10.1021/acs.jpclett.9b03284

Cited by 25 publications

(21 citation statements)

References 31 publications

(52 reference statements)

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“…[162] Furthermore, in situ Raman spectroscopy was used to investigate the evolution of SEI on nanocrystalline Si in lithium-ion batteries. [373] It was demonstrated that reversible Si peak intensity changed upon lithiation and delithiation, and alkyl carboxylate species (lithium propionate) were one representative of the SEI components. Meanwhile, Nanda et al first employed tip-enhanced Raman spectroscopy to observe nanoscale chemical and topographical heterogeneity of a SEI formed on amorphous Si at different cycle numbers.…”

Section: Advanced In Situ/operando Characterizations On Silicon-basedmentioning

confidence: 99%

Recent Advances in Silicon‐Based Electrodes: From Fundamental Research toward Practical Applications

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Section: Advanced In Situ/operando Characterizations On Silicon-basedmentioning

confidence: 99%

Recent Advances in Silicon‐Based Electrodes: From Fundamental Research toward Practical Applications

et al. 2021

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“…To circumvent this limitation, Raman signal enhancement techniques using the plasmon resonance properties of metal nanostructures were successfully implemented to extract compositions of surface films developed on various electrode materials upon contact with organic carbonate electrolytes. Surface-enhanced Raman spectroscopy (SERS) has been carried out operando on SERS-active silver and gold nanostructured electrodes starting from 2000. − More recently, tip-enhanced Raman spectroscopy (TERS) using silver or gold scanning nanoprobes demonstrated the ex situ mapping of the SEI composition distribution with nanoscale resolution on a non-SERS active electrode material (silicon anode) in a similar way as nanoinfrared mapping was achieved on tin anodes a few years before . TERS, despite recent significant advances since its demonstration under operando conditions, , has not been yet implemented in a LIB electrolyte because of the difficulty to control the atmosphere and prevent the electrolyte evaporation in open cells.…”

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confidence: 99%

Solid Electrolyte Interphase Instability in Operating Lithium-Ion Batteries Unraveled by Enhanced-Raman Spectroscopy

et al. 2021

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The fundamental understanding of the electrode/electrolyte interfacial processes in lithium–sodium ion batteries (LIBs) and of their dynamics upon cycling is of prime importance for the development of new-generation electrode materials. Operando analyses using the utmost sensitive techniques are required to produce an accurate depiction of the underlying processes at the origin of the battery performance decay. Although enhanced Raman spectroscopy through the use of signal nanoamplifiers shows the required sensitivity, its implementation in operando conditions and particularly on functional materials in contact with organic electrolytes remains challenging. This work using extensive optimization of shell-isolated nanoparticle-enhanced Raman spectroscopy conditions for operando diagnosis of LIB materials, including the design of near-infrared active amplifiers and the control of the photon dose, demonstrates the possibility to track the dynamics of composition of the electrode/electrolyte interface upon cycling of LIB coin-cells and uncovers the origin of the irreversible capacity of tin electrodes proposed as an alternative to graphite anodes.

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“…Finally, the surface enhanced Raman scattering (SERS) technique must be mentioned. With SERS the Raman spectra from the electrode/electrolyte interface can be significantly enhanced and in situ experiments can be performed, [40,41] however, there is a need to decorate the surface with nanoparticles based on metals such as Ag and Au or to nanostructure the surface of the sample. The former approach has an implicit problem of alloying the metal particles with lithium and the latter one creates an implicit risk of influencing the mechanism and/or the kinetics of the reactions under study.…”

Section: Raman Microspectroscopy For Batteriesmentioning

confidence: 99%

Nonlinear Electrochemical Analysis: Worth the Effort to Reveal New Insights into Energy Materials

Schlüter

Novák

Schröder

2022

Advanced Energy Materials

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and the effectiveness and durability of the materials applied, researchers always call for reliable and detailed knowledge of the mechanism(s) of both, main and side reactions, and especially for their kinetics. In order to gain the relevant information, a large number of methods have been proposed to characterize battery materials, battery electrodes and their interfaces, and battery cells. But when samples are taken out of the cells and analyzed later, there is a high risk of both, contamination and changes due to possible relaxation processes, and the challenge is to draw sound conclusions in respect to a "living and breathing" battery cell, i.e., to a cell under current flow (cf. Figure 1). Therefore, the so-called in situ and operando (and often online) methods are preferred. Sometimes they are the only option to collect relevant data to understand and improve materials for energy systems. [5] In many cases, results from different techniques need to be combined to obtain sound conclusions. [6,7] The terminology for the aforementioned methods shifted during the last decade and is not always consistent throughout the literature. Nowadays, the general understanding is as follows: An operando experiment means a characterization experiment in an electrochemical cell (e.g., battery, fuel cell, electrolyzer) under current flow, with either the potential or the current controlled. One of the many examples is the operando neutron powder diffraction, a technique analyzing the changes in the structure of battery materials in "real" battery cells under current flow with the help of neutron diffraction. [9] Another example is the operando X-ray photoelectron spectroscopy experiment (normally limited to vacuum-compatible cells with nonvolatile electrolytes) providing information about the changes of the chemical composition of the interfacial species with the potential. [10,11] An in situ experiment is also an experiment in a battery cell, however, the current flow is interrupted when the data are collected. An example here is the in situ X-ray absorption spectroscopy (XAS) experiment in which the cell has to be disconnected for technical reasons during the operation of the detector [7] or the tomography of energy materials by means of neutron or X-ray source. [12,13] Online techniques are understood here as either continuously or periodically analyzed samples that are taken out of the electrochemical cell. A typical example is the online (differential) electrochemical mass spectrometry (often shortened as online electrochemical mass spectrometry (OEMS)/differential electrochemical mass spectrometry (DEMS)) analyzing the volatile products of electrochemical reactions with the help of a mass spectrometer by

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Probing the Evolution of Surface Chemistry at the Silicon–Electrolyte Interphase via In Situ Surface-Enhanced Raman Spectroscopy

Cited by 25 publications

References 31 publications

Recent Advances in Silicon‐Based Electrodes: From Fundamental Research toward Practical Applications

Recent Advances in Silicon‐Based Electrodes: From Fundamental Research toward Practical Applications

Solid Electrolyte Interphase Instability in Operating Lithium-Ion Batteries Unraveled by Enhanced-Raman Spectroscopy

Nonlinear Electrochemical Analysis: Worth the Effort to Reveal New Insights into Energy Materials

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