In-situ scanning electron microscope observation of electrode reactions related to battery material

Tsuda, Toshitaka; Hosoya, Kei; Sano, Teruki; Kuwabata, Susumu

doi:10.1016/j.electacta.2019.06.165

Cited by 17 publications

(12 citation statements)

References 35 publications

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“…Methods such as in-situ Scanning Electron Microscopy and Wide and Small Angle X-ray Scattering will be applied in our future studies to investigate the mechanism of plating in detail in order to gain a deeper understanding of the deposition of the sodium in the matrix. [34,35]…”

Section: Resultsmentioning

confidence: 99%

“…Overall, although the capacity retention in the first cycle in both cases is not astonishing as displayed in Figure 2(c and d), the PDC exhibited excellent cycling stability for at least 100 cycles whether during insertion or plating. Methods such as in‐situ Scanning Electron Microscopy and Wide and Small Angle X‐ray Scattering will be applied in our future studies to investigate the mechanism of plating in detail in order to gain a deeper understanding of the deposition of the sodium in the matrix [34,35] …”

Section: Resultsmentioning

confidence: 99%

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On the Reversible Sodium Plating/stripping Reaction in Porous SiCN(O) Ceramic: A Feasibility Study

d’Eril

Graczyk‐Zajac

Riedel

2023

Batteries & Supercaps

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Sodium‐ion batteries (SIBs) are a cost‐effective and sustainable alternative to lithium‐ion batteries (LIBs), which might be independent of rare raw materials. These advantages come at the expense of low energy density. Sodium metal batteries (SMBs) can provide a possible solution. In this work, we present the use of a porous silicon carbonitride (SiCN(O)) ceramic as an anodic matrix for reversible Na‐plating. The role of the pores is investigated and the plating mechanism allowing reversible and uniform plating/stripping of sodium is also presented. Electrochemical studies show a stable and reversible capacity gain of around 60 mAh/g beyond the insertion capacity of the SiCN(O) ceramic over 100 cycles.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

On the Reversible Sodium Plating/stripping Reaction in Porous SiCN(O) Ceramic: A Feasibility Study

d’Eril

Graczyk‐Zajac

Riedel

2023

Batteries & Supercaps

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“…14). [114][115][116][117] Although the electrolyte that we can select is limited, the cell setup and the replacement of electrode become a greater ease. This approach may be not good for getting atomic scale information concerning battery reaction, but nano-scale one can be obtained with relatively little effort.…”

Section: Electron Microscopy (Sem Tem)mentioning

confidence: 99%

Electrochemical In Situ/<i>operando</i> Spectroscopy and Microscopy Part 2: Battery Applications

et al. 2022

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In situ/operando techniques for electrochemical systems are useful for understanding the electrochemical reactions, as we presented in Part 1. Here we present a series of in situ/operando techniques for battery applications. Now the in situ/operando techniques presented in this paper has become powerful tools for the development of advanced battery systems such as Li-ion batteries, solid-state batteries, and other beyond Li-ion batteries. In the present paper we introduce the in situ/operando cell design of each measurement technique and discuss how we apply each technique for in the advanced battery materials development.

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“…Unrepresentative spots due to natural inhomogeneity of the composite electrode structure and artifacts due to sample preparation can cause misinterpretation of these local SEM images and EDX spectra. Therefore, in situ/operando techniques were developed to obtain a detailed understanding of the degradation mechanisms of Si-based anodes − as well as of Si/C anodes . In recent articles, ,,− operando measurements have been described as performing the analysis during the charge/discharge procedure, while in situ means the charge/discharge procedure is suspended and the measurement is carried out at open-circuit potential.…”

Section: Introductionmentioning

confidence: 99%

Visualization of Degradation Mechanisms of Negative Electrodes Based on Silicon Nanoparticles in Lithium-Ion Batteries via Quasi In Situ Scanning Electron Microscopy and Energy-Dispersive X-ray Spectroscopy

2022

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Understanding the degradation mechanisms of negative electrodes based on nanoparticles like silicon is key for developing solutions against active material cracking, pulverization, or extensive growth of the solid electrolyte interphase (SEI). Scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) are common ex situ methods for post mortem analysis of lithium (ion) battery materials. Beyond that, in situ/ operando methods provide more accurate insights but require specially designed cells and electrolytes with a high evaporation temperature. This study combines aspects of in situ and ex situ SEM/EDX measurements to enable detailed insights on the degradation mechanisms of silicon nanoparticle-based electrodes during charge/discharge cycling. Therein, a protective quasi in situ environment was ensured by handling electrodes of repeatedly disassembled cells under an inert atmosphere and performing a same-spot analysis by SEM and EDX in the pristine state and after formation and subsequent cycles. This so-called quasi in situ analysis allowed accurate tracking of the degradation mechanisms such as irreversible expansion, cracking, and pulverization of active material particles and evolution of the SEI. Thus, extensive irreversible volume expansion of silicon nanoparticles was detected during charge/discharge cycling at low C rates, while higher C rates facilitated pulverization. Furthermore, EDX analysis revealed pronounced SEI growth at conductive additive-rich areas.

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In-situ scanning electron microscope observation of electrode reactions related to battery material

Cited by 17 publications

References 35 publications

On the Reversible Sodium Plating/stripping Reaction in Porous SiCN(O) Ceramic: A Feasibility Study

On the Reversible Sodium Plating/stripping Reaction in Porous SiCN(O) Ceramic: A Feasibility Study

Electrochemical In Situ/<i>operando</i> Spectroscopy and Microscopy Part 2: Battery Applications

Visualization of Degradation Mechanisms of Negative Electrodes Based on Silicon Nanoparticles in Lithium-Ion Batteries via Quasi In Situ Scanning Electron Microscopy and Energy-Dispersive X-ray Spectroscopy

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