Invited talk: Operando synchrotron and neutron based techniques to probe battery materials

Invited talk: Operando synchrotron and neutron based techniques to…

Presenter:  Claire Villevieille
Title: Operando synchrotron and neutron based techniques to probe battery materials
Affiliation: Université Grenoble-Alpes, Grenoble INP, LEPMI laboratory, France


The Li-ion chemistry is thus far the most advanced chemistry employed in battery technology. To date, Li-ion batteries dominate the market of the electronics and portables devices. However, in the field of electric and hybrid vehicles further improvements are required in terms of performance, safety, and cost. The same set of criteria concerns other systems based on alternative chemistries such as Na-ion and solid-state batteries. Advanced Li-ion batteries and the pre-cited novel systems utilize less understood electroactive materials and thus show new reaction mechanisms during electrochemical cycling, the understanding of which requires new characterization tools and techniques.

Unfortunately, in most cases the electrochemical cells used for operando measurement are not ideal and suffer from low internal pressure (i.e. poor contact between the electrodes). It shorts the lifespan of the cell and as a consequence most of the studies presented in the literature focus on the first/second cycle. Herein we present different cell designs developed in our laboratory and used for operando/in situ studies. Having overcome earlier mentioned obstacle our operando/in situ cells are able to sustain more than 100 cycles and simultaneously to perform structural studies such as X-ray and neutron diffraction. For the latter one, we also developed a new set-up called stroboscopic mode. It allows operando study of the batteries that are cycling at very high rates (e.g. 10C) with a neutron patterns collected each 1 s along 200 cycles and more.

Additionally, we will use bulk, surface and imaging techniques to better understand the limitation of all solid state batteries. As an example, Operando neutron imaging has been employed to understand the Li diffusion within the electrode and inside an all-solid state batteries employing Li3PS4 as solid electrolyte whereas operando X-ray microscopic tomography was employed to follow the possible electro-mechanical fracture occurring during cycling and the possible impact on the electrochemical performance.

Other examples based on different operando/in situ techniques such as X-ray diffraction, neutron diffraction, neutron imaging, and X-ray tomography microscopic used to characterize batteries will be presented during the talk.

Dr. Claire Villevieille was the leader of the Battery Materials group at the Paul Scherrer Institute in Switzerland. Her research is especially dedicated to study the reaction mechanisms of battery systems such as Li-ion, Na-ion, Li-S, and recently all-solid-state cells by means of various operando techniques. Moreover, her work centers on the proper design and/or adjustments of the measurement cells so that they meet the requirements of selected characterization techniques. Her research involves both, in-house devices as well as large facilities such as Swiss Light Source (PSI, Switzerland), Swiss Spallation Neutron Source (PSI, Switzerland), ERSF (Grenoble, France), ILL (Grenoble, France), and Soleil (Paris, France). In 2010 she accepted the position of a scientist at the Paul Scherrer Institute in Switzerland in the “Electrochemical Energy Storage Section” lead by Prof. Petr Novák. In 2006 she graduated with a Master degree in Materials Science (2006) at the University of Montpellier II in France. In 2009 she obtained her doctoral degree from the Science, Physics, and Chemistry Department (ICGM-AIME Laboratory) of the University of Montpellier II in France. Her doctoral studies focused on the conversion and insertion-based negative electrodes for Li-ion batteries and the elucidation of the complex reaction mechanisms using in situ X-Ray Diffraction (XRD), Mössbauer spectroscopy, SQUID measurements, etc. Her primary interests include development of operando techniques to investigate batteries, solid state synthesis, electrochemical properties, and bulk–surface relationship of the various electrode materials.