Experimental Considerations for Operando Metal‐Ion Battery Monitoring using X‐ray Techniques. Issue 6 (7th May 2021)

• Record Type: Journal Article
• Authors: Saurel, D.; Pendashteh, A.; Jáuregui, M.; Reynaud, M.; Fehse, M.; Galceran, M.; Casas‐Cabanas, M.
• Is Part Of: Chemistry methods. Volume 1:Issue 6(2020)
• Page Start: 249
• Page End: 260
• Publication Date: 2021-05-07
• Subjects: electrochemical cell -- in situ -- operando -- SAXS -- XAS -- XRD; Chemistry, Analytic -- Periodicals; 543
• DOI: 10.1002/cmtd.202100009
• Languages: English
• ISSNs: 2628-9725

Abstract

Abstract: Operando experiments represent a powerful tool for the monitoring of internal processes upon battery cycling that provide valuable insights regarding the fundamental electrochemical redox mechanisms and ageing phenomena in battery materials. However, obtaining high‐quality, representative and exploitable data from operando measurements requires careful control of many experimental parameters such as the cell configuration, the nature of the cell components, the electrode preparation approach, the optical/goniometer geometry, data acquisition protocols and data interpretation methodology. In this work we discuss the impact of all these factors in X‐ray scattering and spectroscopic techniques based on experimental results obtained from different electrode materials using a multifunctional electrochemical in situ cell developed at our laboratory. Abstract : Practical tips for conducting successful operando measurements of battery materials are provided, based on extensive experience. The examples were obtained using a universal electrochemical cell, specifically designed by the lab for the investigation under operando conditions. Besides cell design considerations, the importance of instrumental setup parameters and experimental conditions on the outcome of the experiment are highlighted.