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Figure 4-2. SEM photos of Li2S powder (used as-received from Alfa Aesar supplier) manually grinded with SuperP® in an agate mortar, with few drops of cyclohexane. Li2S/SuperP® ratio of 78/22 wt%, aimed for final electrode composition of 70/20/10 wt% after binder addition. Figure 4-3 shows XRD patterns of as-received Li2S samples, purchased from both Sigma Aldrich and Alfa Aesar suppliers, and grinded with SuperP®. Both patterns, as well as the scan of pure Li2S, are identical, and most of the peaks were assigned to the crystalline Li2S (PDF 2 # 00-023-0369; cubic unit cell with lattice parameters: a, b, c = 5.72 Å; α, β, γ = 90°). Small peaks, assigned to lithium hydroxide (LiOH; PDF-2; no. 00-032-0564), were also detected, possibly meaning that some impurities were present in the samples, however, their amount was rather small. Another explanation could be that Kapton® foil did not provide perfect air- tightness, and LiOH got formed because of partial hydrolysis of Li2S in contact with air moisture during measurement. Takeuchi et al. 147 and Hiesgen et al.146 reported on similar presence of LiOH in Li2S samples. Figure 4-3. XRD patterns of Li2S powders: pure (a), after manual grinding with SuperP® in the presence of cyclohexane (b,c) and incorporated into final electrode with composition 70/20/10 wt% = Li2S/SuperP®/PVdF (d). Powders from both suppliers, i.e. Sigma Aldrich and Alfa Aesar, were compared. Chapter 4: Li2S electrode 114PDF Image | Accumulateur Lithium Soufre
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