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Subject of the Master's internship

Operando characterization of batteries using neutron and synchrotron imaging techniques

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Published on 8 November 2021
Summary
Operando characterization of battery materials is needed to help designing safer and more efficient electrochemical devices. Following lithiation mechanisms during fast charging, in real-time, is particularly challenging since it requires the use non-destructive tools capable of high rate data acquisition. In this regard, synchrotron and neutron techniques provide unique capabilities to access the chemical, morphological and structural changes inside electrodes at relevant length and time scales (from molecular level to nano-, meso and micro-scales, in seconds/minutes). In our team, we focus on developing advanced methodologies to probe in real-time different types of Li-ion batteries. The aim of the internship is to analyze neutron imaging and SAXS/WAXS data and participate to experiments at the European synchrotron, ESRF.



Background
Efficient, safe, and environmentally-friendly energy storage is a key requirement to successfully transitioning from depleting fossil fuels to renewable energy sources. In this regard, Li-ion batteries are playing a decisive role, particularly in meeting the demands of a highly mobile society. Nevertheless, there are great challenges remaining towards the worldwide success of battery-powered electric vehicles, which mostly revolve around increasing the energy density and improving fast charging. Fast charging typically leads to heterogeneous lithiation across the electrodes due to the development of current hot spots. These hot spots can lead to underutilization of active materials and dendrite formation at the anode, both being detrimental for the battery life and safety. Designing effective strategies to mitigate litihiation heterogeneities requires a better understanding of this process, and hence the development of operando technics (monitoring the battery in operation) capable of imaging lithium concentration in materials at high speed (< min). In this regard, synchrotron and neutron techniques provide unique capabilities, in particular with SAXS/WAXS or Neutron Imaging: 

Operando Synchrotron X-ray Small Angle Scattering and Wide Angle Scattering (SAXS/WAXS @ID31 ESRF). In this experiment, WAXS and SAXS patterns are collected, operando, while scanning micron sized beam across the battery electrode. This allows to measure the variation of crystallographic structure (WAXS) and nano-structure (SAXS) associated with lithiation as a function of the position in the electrode, hence leading to the determination of dynamic lithiation heterogeneities.1,2

Operando neutron imaging (@NeXt D50 ILL): Operando imaging of batteries with neutrons is powerful as lithium strongly absorbs neutrons. Therefore mapping of heterogeneities can be obtained with good resolution (a few microns) in thin layers (electrodes/electrolytes), as well as checking the possible growth of dendrites and problems of lithium plating.

The internship
The aim of the internship will be to analyze sets of neutron imaging and SAXS/WAXS data already obtained by the team and to participate to SAXS/WAXS synchrotron experiments (ESRF). Data have been collected on LiNiO2//Graphite full cell being the state of the art high energy density cell chemistry for EV-applications3. Materials have been provided by industries (BASF, CIDETED) through the BIG-MAP project (https://www.big-map.eu/), part of battery 2030+ initiatives (https://battery2030.eu/).The analyzed results will hence be presented and shared across a large consortium of European academic laboratory, with possible collaboration with modelling teams. 
The intern will be working for 6 months at CEA in Grenoble, a major French National Lab focused on the development of low-carbon energies, and more specifically at the IRIG, the fundamental science department of CEA.

Requested skills
M2 master student with a background in data analysis especially using python together with knowledge in condensed matter, physics and/or scattering techniques will be important. Interest in energy storage devices and Li-ion batteries will be appreciated.

Possibility to follow with a PhD
Ecoles Doctorales: Ed Physique

Keywords
Li-ion batteries ; fast charging ; lithiation mechanism ; synchrotron ; diffraction ; neutron imaging

Miscellaneous
Laboratory / Team: SyMMES / STEP
Contacts: Sandrine Lyonnard – 04 38 78 92 86
Quentin Jacquet  

References
1 Berhaut, C. L.; Dominguez, D. Z.; Kumar, P.; Jouneau, P.-H.; Porcher, W.; Aradilla, D.; Tardif, S.; Pouget, S.; Lyonnard, S. Multiscale Multiphase Lithiation and Delithiation Mechanisms in a Composite Electrode Unraveled by Simultaneous Operando Small-Angle and Wide-Angle X-Ray Scattering. ACS Nano 2019, 13 (10), 11538–11551. https://doi.org/10.1021/acsnano.9b05055.

2 Tardif, S.; Dufour, N.; Colin, J.-F.; Gébel, G.; Burghammer, M.; Johannes, A.; Lyonnard, S.; Chandesris, M. Combining Operando X-Ray Experiments and Modelling to Understand the Heterogeneous Lithiation of Graphite Electrodes. J. Mater. Chem. A 2021, 9 (7), 4281–4290. https://doi.org/10.1039/D0TA10735B.

3 Xu, C.; Reeves, P. J.; Jacquet, Q.; Grey, C. P. Phase Behavior during Electrochemical Cycling of Ni-Rich Cathode Materials for Li-Ion Batteries. Adv. Energy Mater. 2021, 11 (7), 2003404. https://doi.org/10.1002/aenm.202003404.