In-operando photoelectron spectroscopy for batteries: Set-up using pristine thin film cathode and first results on NaxCoO2

A model all-solid-state battery cell with a thin film NaxCoO2 cathode was assembled under ultra-high vacuum conditions and cycled inside the vacuum chamber, using a dedicated sample holder. We present in-operando x-ray photoelectron spectroscopy measurements of a NaxCoO2 cathode at different chargin...

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Bibliographic Details
Published in:Review of scientific instruments 2018-07, Vol.89 (7), p.073104-073104
Main Authors: Guhl, Conrad, Kehne, Philipp, Ma, Qianli, Tietz, Frank, Alff, Lambert, Komissinskiy, Philipp, Jaegermann, Wolfram, Hausbrand, René
Format: Article
Language:English
Subjects:
Batteries
Cathodes
Electrode materials
High vacuum
Interface reactions
Measurement techniques
Oxidation
Photoelectron spectroscopy
Pollution monitoring
Sample holders
Scientific apparatus & instruments
Spectrum analysis
Surface layers
Thin films
Vacuum chambers
Valence
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Summary:A model all-solid-state battery cell with a thin film NaxCoO2 cathode was assembled under ultra-high vacuum conditions and cycled inside the vacuum chamber, using a dedicated sample holder. We present in-operando x-ray photoelectron spectroscopy measurements of a NaxCoO2 cathode at different charging states. During battery operation, the change in sodium content, the change in cobalt oxidation state, and the evolution of the O1s and VB emissions could be monitored. Comparison with a conventional post-mortem analysis technique showed that the new measurement technique produces comparable results regarding the oxidation state of the transition metal, but sodium and oxygen results show differences due to cathode/electrolyte interfacial reactions for conventional analysis. By using surface layer-free samples in the presented techniques, we could circumvent such reactions and obtain reliable spectra for the pure bulk-like active cathode material.
ISSN:0034-6748
1089-7623
DOI:10.1063/1.5022616