Journal of The Electrochemical Society, 161 (10) A1731-A1741 (2014) A1731 0013-4651/2014/161(10)/A1731/11/$31.00 © The Electrochemical Society An In-Situ Electrochemical Cell for Neutron Diffraction Studies of Phase Transitions in Small Volume Electrodes

The design and performance of a novel in-situ electrochemical cell that greatly facilitates the neutron diffraction study of complex phase transitions in small volume electrodes of Li-ion cells, is presented in this work. Diffraction patterns that are Rietveld-refinable could be obtained simultaneously for all the electrodes, which demonstrates that the cell is best suited to explore electrode phase transitions driven by the lithiation and delithiation processes. This has been facilitated by the use of single crystal (100) Si sheets as casing material and the planar cell configuration, giving improved signal-to-noise ratio relative to other casing materials. The in-situ cell has also been designed for easy assembly and to facilitate rapid experiments. The effectiveness of cell is demonstrated by tracking the neutron diffraction patterns during the charging of graphite/LiCoO2 and graphite/LiMn2O4 cells. It is shown that good quality neutron diffraction data can be obtained and that most of the finer details of the phase transitions, and the associated changes in crystallographic parameters in these electrodes, can be captured