First In Situ Observation of the LiCoO₂ Electrode/Electrolyte Interface by Total‐Reflection X‐ray Absorption Spectroscopy

Abstract

Oberflächenanalyse: Mittels In‐situ‐Totalreflexions‐Röntgenfluoreszenz‐Absorptionsspektroskopie wurde gefunden, dass Cobalt an der Oberfläche einer LiCoO2‐Elektrode vom flüssigen Elektrolyten reduziert wird. Ein irreversibles Verhalten wurde an der LiCoO2‐Oberfläche während des ersten Lade‐/Entladeprozesses beobachtet, wohingegen das Bulk‐Material ein reversibles Verhalten zeigte. Die Cobalt‐Reduktion ist Auslöser für den Abbau der Elektrode.

Intrinsic rapid Na+ intercalation observed in NaxCoO2 thin film

“…Very recently, Takamatsu et al have performed in-situ x-ray absorption near-edge structure (XANES) measurement to investigate the LiCoO 2 electrode/electrolyte interface during charge/discharge process using a polycrystalline LiCoO 2 thin film. 13 They observed a rather poor cyclability where its capacity almost vanishes after 20 cycles in a 1:1 volumetric mixture of EC and DEC containing 1 mol/l LiClO 4 between 3.2-4.2 V (v.s. Li/Li + ).…”

In Situ Three‐Dimensional Synchrotron X‐Ray Nanotomography of the (De)lithiation Processes in Tin Anodes

“…In recent years, a few in situ studies have provided valuable information on the electrode behavior of LIBs. [4][5][6][7][8][9][10] However, most of the reported in situ methods are based on two-dimensional (2D) rather than 3D measurements. [8][9][10][11] Recently, X-ray tomography at micronscale resolution was used for tracking the degradation in lithium-ion batteries and provided valuable 3D images.…”

In situ Raman and UV-Vis spectroscopic analysis of lithium-ion batteries

“…It turns out to be a particular challenge to develop and apply in situ techniques that provide information on the electrolyte/electrode interfaces and/or offer sufficient spatial (~μm) resolution to monitor single electrode particles. While recent applications of X-ray absorption spectroscopy (XAS) [3] and sum-frequency generation (SFG) [4] have highlighted their use for studies on LiCoO2 electrode/electrolyte interfaces, Raman micro-spectrometry has been shown to be a powerful tool to access spatially-resolved information of electrode materials of lithiumion batteries [5][6][7][8].…”