Circular in situneutron powder diffraction cell for study of reaction mechanism in electrode materials for Li-ion batteries

The study of reaction mechanisms in materials for Li-ion batteries mainly involves localization of lighter elements like Li, O, or even H in the structure. Thus, in order to facilitate in situlocalization of lighter elements and in situstudy of structural evolution in the electrode materials, a circ...

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Bibliographic Details
Published in:RSC advances 2013, Vol.3 (3), p.757-763
Main Authors: Godbole, Vikram A., Heß, Michael, Villevieille, Claire, Kaiser, Hermann, Colin, Jean-François, Novák, Petr
Format: Article
Language:English
Subjects:
Batteries
Design engineering
Deuteration
Diffraction
Diffraction patterns
Electrode materials
Electrolytes
Electrolytic cells
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Summary:The study of reaction mechanisms in materials for Li-ion batteries mainly involves localization of lighter elements like Li, O, or even H in the structure. Thus, in order to facilitate in situlocalization of lighter elements and in situstudy of structural evolution in the electrode materials, a circular in situneutron diffraction cell capable of cycling small amounts of electrode materials (0.2-0.3 g) was developed for primary use at the D20 beamline at ILL, Grenoble, France. The circular cell design was tested using LiFePO sub(4) and graphite as the model electrode materials. The effect of using deuterated electrolyte versusprotonated electrolyte on the quality of the in situneutron diffraction data was also investigated. First in situneutron powder diffraction measurements at ILL, Grenoble, were successfully conducted where each neutron diffraction pattern was recorded in only 24 min, delivering very good time resolution. It was also found that a circular cell design holding only a small amount of material soaked in deuterated electrolyte was best to perform quantitative analysis using the Rietveld method over the complete 2 theta range. The pattern shows no apparent anisotropic absorption of the diffracted neutron beams.
ISSN:2046-2069
2046-2069
DOI:10.1039/C2RA21526H