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the oven (integrated to the glove box) for solvent evaporation and drying of the powders, before electrode preparation. Little amounts of both samples were taken for further analysis by XRD and SEM, while the rest was used for electrode preparation, by adding PVdF binder solution and additional volume of NMP, mixing all manually with spatula and coating the inks on the Al current collectors. SEM photos of both samples, obtained by wet ‘planetary’ ball-milling (SEM photos of ‘dry’ ball-milled powders gave similar results as the ‘wet’ one, thus not presented in this paragraph) and dry ‘energetic’ milling, are presented on Figure 4-23. It can be seen that, after less energetic milling (Figure 4-23a,b) Li2S particles diminish to 1-5 μm (initially ~ 10 - 20 μm). However, it seems that the contact between Li2S/carbon was not improved so much as compared with a hand milling protocol in a mortar, as the particles of active material were not completely/uniformly covered by nano-spheres of carbon. Figure 4-23. SEM photos of Li2S/SuperP® powder mixture obtained through: planetary (a, b) and high energetically (c, d) ball milling. On the other hand, when applying highly energetic milling, it is clear that Li2S particle size is decreased, even nano-particles are observed. However, milling protocol also provokes strong agglomeration of carbon particles, leaving Li2S particles ‘naked’ around the agglomerates. Moreover, a visual observation of such highly ball-milled powders as compared with Li2S/SuperP® grinded manually in a mortar, shows significant differences in terms of color: a deep black color is obtained after ball millingenergetical, while a greyish color is obtained for handy mixed powders. Changes in the volume of the powders were also evidenced after being Chapter 4: Li2S electrode 139PDF Image | Accumulateur Lithium Soufre
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