Oxygen <i>K</i>-edge X-ray absorption spectra of liquids with minimization of window contamination

Vogt, Linda; Cotelesage, Julien J. H.; Titus, Charles J.; Sharifi‐Asl, Samin; Butterfield, Albert E.; Hillman, P.; Pickering, Ingrid J.; George, Graham N.; George, Simon J.

doi:10.1107/s1600577521009942

Cited by 4 publications

(2 citation statements)

References 7 publications

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“…At even lower potentials, the electrolyte peaks are no longer discernable and the features above 534 eV are similar to those of the as-deposited a-Si (see supplementary Figure S3), with the main peak maximum found at ∼538.0 eV and a post-peak at ∼540.0 eV. This lineshape closely resembles SiO 2 [50,51] or possibly oxidized Si 3 N 4 [52]. We also performed measurements of as-deposited a-Si/Ni/Cu (as used in the coin cells), and a-Si/Ni/Si 3 N 4 and Ni/Si 3 N 4 membranes which all show the features of SiO 2 in their O and Si K-edges (see supplementary Figure S3).…”

Section: Operando X-ray Absorption Spectroscopymentioning

confidence: 56%

Revealing Solid Electrolyte Interphase Formation Through Interface-Sensitive Operando X-ray Absorption Spectroscopy

Swallow

Fraser

Kneusels

et al. 2022

Preprint

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The solid electrolyte interphase (SEI) that forms on Li-ion battery anodes is critical to their long-term performance, however observing SEI forma- tion processes at the buried electrode-electrolyte interface is a significant challenge. Here we show that operando soft X-ray absorption spectroscopy in total electron yield mode can resolve the chemical evolution of the SEI during electrochemical formation in a Li-ion cell, with nm-scale interface sensitivity. O, F, and Si K-edge spectra, acquired as a function of potential, reveal when key reactions occur on high-capacity amorphous Si anodes cycled with and without fluoroethylene carbonate (FEC). The sequential formation of inorganic (LiF) and organic (-(C=O)O-) components is thereby revealed, and results in layering of the SEI. The addition of FEC leads to SEI formation at higher potentials which is implicated in the rapid healing of SEI defects and the improved cycling performance observed. Operando TEY-XAS offers new insights into the formation mechanisms of electrode-electrolyte interphases and their stability for a wide variety of electrode materials and electrolyte formulations.

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Section: Operando X-ray Absorption Spectroscopymentioning

confidence: 56%

Revealing Solid Electrolyte Interphase Formation Through Interface-Sensitive Operando X-ray Absorption Spectroscopy

Swallow

Fraser

Kneusels

et al. 2022

Preprint

View full text Add to dashboard Cite

show abstract

“…Pre-edge region exhibits two structures-One centered at 534 eV (A1) and second centered at 531.8 eV shown by arrow. Presence of second structure in the pre-edge region may be due to presence of oxygen adsorbed from the environment on the surface (Singh et al, 2018;Vogt et al, 2021) in the form of hydroxyls (Nagasaka et al, 2003;Kim et al, 2011). Post-edge region of these spectra also exhibits major changes and three distinct structures A2, A3 and A4 are clearly visible.…”

Section: Resultsmentioning

confidence: 97%

Effect of Heating/Cooling Rate on the Local Electronic Structure of Amorphous Calcium Carbonate

Lim,

Song

2024

Prabha Materials Science Letters

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Here, in the impact of heating/cooling rate was investigated on the formation of amorphous calcium carbonate (calcite) during sol-gel synthesis by probing local electronic structure. The amorphous calcium carbonate was synthesized by annealing precursor at 400oC at different heating/cooling rates i.e., 1.5 and 3oC /min. X-ray diffraction studies revealed amorphous nature at both heating/cooling rates. Fourier transformed infrared spectroscopic measurements characteristics bands in the spectra of both materials. Near edge X-ray absorption fine structure measurements at Ca L-edge, C K-edge and O K-edge were utilized to reveal the associated changes in the local electronic structure during synthesis. Local electronic structure investigation using near edge X-ray absorption fine structure measurements shows onset of moisture absorption on the surface particles when kept in the open environment.

show abstract

Revealing solid electrolyte interphase formation through interface-sensitive Operando X-ray absorption spectroscopy

et al. 2022

View full text Add to dashboard Cite

The solid electrolyte interphase (SEI) that forms on Li-ion battery anodes is critical to their long-term performance, however observing SEI formation processes at the buried electrode-electrolyte interface is a significant challenge. Here we show that operando soft X-ray absorption spectroscopy in total electron yield mode can resolve the chemical evolution of the SEI during electrochemical formation in a Li-ion cell, with nm-scale interface sensitivity. O, F, and Si K-edge spectra, acquired as a function of potential, reveal when key reactions occur on high-capacity amorphous Si anodes cycled with and without fluoroethylene carbonate (FEC). The sequential formation of inorganic (LiF) and organic (-(C=O)O-) components is thereby revealed, and results in layering of the SEI. The addition of FEC leads to SEI formation at higher potentials which is implicated in the rapid healing of SEI defects and the improved cycling performance observed. Operando TEY-XAS offers new insights into the formation mechanisms of electrode-electrolyte interphases and their stability for a wide variety of electrode materials and electrolyte formulations.

show abstract

Oxygen K-edge X-ray absorption spectra of liquids with minimization of window contamination

Cited by 4 publications

References 7 publications

Revealing Solid Electrolyte Interphase Formation Through Interface-Sensitive Operando X-ray Absorption Spectroscopy

Revealing Solid Electrolyte Interphase Formation Through Interface-Sensitive Operando X-ray Absorption Spectroscopy

Effect of Heating/Cooling Rate on the Local Electronic Structure of Amorphous Calcium Carbonate

Revealing solid electrolyte interphase formation through interface-sensitive Operando X-ray absorption spectroscopy

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