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together with XRD samples preparation, was conducted in the glove box, due to sensitivity of Li2S powder. The recorded XRD patterns (Figure 5-11) allowed to determine the correlation between the peak areas (i.e. of (222) and (111) reflections, for S8 and for Li2S, respectively) and the S8/Li2S molar ratio, according to equation (13). Chapter 5: In situ and operando XRD (a) /&#* #$&# (111) 01 ↔ 5-6& 01 (13) /&#* #$&# (222) 2 30 5-6& 2 30 (b) Figure 5-11. XRD patterns (a) recorded on three different mass ratios of S8/Li2S: 2/1 (in blue), 1/2 (in red) and 1/1 (in black). A linear relation between integrated peak surface area ratio vs. molar ratio S8/Li2S of prepared samples was obtained (b). Only the most intensive reflection of sulfur (222) and Li2S (111) were taken into account. Therefore, knowing the initial amount of sulfur in the electrode (27 mg) and the integrated peak surface areas for both Li2S and S8, it was possible to estimate the real quantity of Li2S produced upon discharge and consumed upon charge. Even if micrometric Li2S powder (commercial one) was used to prepare these Li2S/S8 samples for quantitative purposes, while the electrochemical processes in a real Li/S cell rather involves nanometric Li2S particles, we made the assumption that the effect of the particle size would be negligible for evaluation of molar ratios through correlation with XRD patterns. For the three investigated S8/Li2S compositions, the relation between the peak area and the molar ratio gives a straight line, with a slope equal to A = 1.13. One should note that this correlation was found to be stable during the time necessary for the XRD measurement. This indicates that, even if a large reactivity between S8 and Li2S is expected, the use of micrometric powders combined with a prior mixing with SuperP® permits to perform XRD measurements of these batches before observing any S8/Li2S reaction. 174PDF Image | Accumulateur Lithium Soufre
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