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Figure 5-17. Li2S formation and disappearance during the second cycle. Integrated surface area of (111) reflection as a function of capacity. 5.5.2. The twenty sixth cycle We were also interested in monitoring the Li/S pouch cell during much later cycle, in order to see if any solid phase evolution would still be detectable. For that experiment, a pouch cell was prepared much before the planned synchrotron session, and left for cycling at C/20 in the laboratory (on Arbin® cycler). The cell was then stopped at the end of 25th discharge, transferred to ESRF facilities† and cycled again during following charge and the next 26th full cycle at C/20, while exposed to the beam. Figure 5-18 presents the solid phases evolutions recorded during the 25th charge and the 26th discharge, together with the capacity retention of the pre- cycled pouch cell. One can still observe evolution (formation and disappearance) of crystalline Li2S upon cycling. However, only (111) peak can be detected. The others are probably not intense enough, and are covered by the strong signal of thick polypropylene bag, which was used specially to protect the cell from air during pre-cycling for 2 weeks. It was interesting to observe that the nucleation of crystalline Li2S is starting exactly at the same moment as for the first cycle previously shown, i.e. at the beginning of the low voltage plateau. † ESRF-based results were used for qualitative analysis only, and not quantitative ones. Pouch cell was monitored in one position, where the beam was penetrating through the complete cell. Chapter 5: In situ and operando XRD 184PDF Image | Accumulateur Lithium Soufre
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