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Coming back to the electrochemical processes occurring during discharge, we aimed at determining the quantity of Li2S produced experimentally versus the theoretical quantity. All steps were investigated by looking at S8 disappearance towards Li2S formation, i.e. following the global process of discharge. According to the fact that the reduction of 1 mole of S8 consumes 2 moles of electrons, and the reduction of two moles of S42- leads to 8 moles of S2-, while consuming 12 electrons, the ratio of S8 disappearance towards Li2S appearance, in terms of exchanged capacity, and normalized to the number of moles exchanged, is equal to 4/3 (R), and calculated according to equation (14): S8 +2e- →S82- 2S42- +12e- →8S2- 01 #77&#$# !& 2& −81 5-6& 4 = 3 = < (14) This ratio was further derived in order to take into account the correlation between the peaks areas of (111) and (222) reflections, and the molar ratio between S8 and Li2S, i.e. the slope A (A = 1.13), that was determined experimentally thanks to ex situ XRD measurements. An additional parameter, so called R’, was determined as follow: 01 #77&#$# !& × /&#* #$&# (111) 01 ↔ < × 1.13 = 0.849 = <′ (15) 2 30 #77&#$# !& /&#* #$&# (222) 2 30 This theoretical coefficient R’, representing correlation between S8 disappearance and Li2S appearance in terms of exchanged capacity and peaks areas of ex situ XRD patterns, was then compared with experimental data. Experimental coefficient Rexp was extracted from in situ XRD patterns, by correlation of the Li2S and S8 peaks areas evolution upon discharge with the practical capacity (Figure 5-12). 2 30 #77&#$# !& ↔ 12& −8 8 5-6& Chapter 5: In situ and operando XRD 175PDF Image | Accumulateur Lithium Soufre
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