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container (inner part of the jar made from agate), with 20 agate beads of Ø 6 mm, as shown on the Figure 4-22a,c. Metallic rings permitted to close tightly the filled container. The more energetic ball-milling (Spex 8000M Mixer) was performed using a 50 mL container and 2 beads of Ø 10 mm, both made of Yttria-Stabilized Zirconia (YSZ), as shown on Figure 4-22b,d. The jar was filled with powders inside the glove box, and then tightly sealed with a black insulating tape. In the further discussion, abbreviations like Li2Splanetary and Li2Senergetical is used for simplicity and clarity. Figure 4-22. Ball-milling equipment and corresponding 50 mL containers used for ball-milling of Li2S powder with SuperP®, in a ratio leading to final electrode composition Li2S/SuperP®/PVdF = 70/20/10 wt%. Planetary ball milling performed in RETSCH (a) in the jar made from agate, filled with 20 Ø 6 mm agate beads (c). High-energy ball milling performed in Spex 8000M Mixer (b), in a jar filled with two beads of Ø 10 mm, both made of YSZ (d). The ball-milling sequence was similar for both sessions, and was as follow: three times milling for 1 h, with 30 min of break in between the cycles, to avoid overheating. ‘Planetary’ milling was performed at 300 rpm, while the speed of the ‘energetic’ one could not be really controlled. The first trial of ‘planetary’ milling was performed in dry conditions (i.e. with only Li2S and SuperP®). However, it appeared that the powders stuck to the walls of the container and were difficult to retrieve. Thus, in the next step, another trial was performed with addition of cyclohexane (~ 2.2 mL added to 0.6 g of Li2S and 0.17 g of SuperP® powders). The ‘energetic’ ball-milling was done in dry conditions, to avoid eventual solvent leakage during milling, since the hermetical protection was hand made with a tape. After ball milling, the jars were brought back to the glove box, and ball-milled Li2S/SuperP® mixtures were recuperated. Concerning the milling with cyclohexane, the jar was left inside Chapter 4: Li2S electrode 138PDF Image | Accumulateur Lithium Soufre
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