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Accumulateur Lithium Soufre

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Accumulateur Lithium Soufre ( accumulateur-lithium-soufre )

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Chapter 5: In situ and operando XRD studies: insight into the structural changes of the active material....................................................157 5.1. Motivation of the work ...............................................................................................157 5.2. Experimental section...................................................................................................158 5.2.1. Measurements description and synchrotron beam line characteristics................158 5.2.2. Cells design..........................................................................................................159 5.3. The initial cycle evolution at C/20..............................................................................161 5.3.1. XRD and electrochemistry – results ....................................................................161 5.3.2. End of charge: β-Sulfur formation.......................................................................163 5.3.2.a) β-Sulfur: physical characteristics..................................................................164 5.3.2.b) Unusual formation of metastable β-S8: supporting experiments..................165 5.3.3. ‘Reference’ holes evaluation................................................................................167 5.4. Quantitative analysis – insight into evolution of solid active material phases ...........168 5.4.1. Sulfur reduction and re-oxidation........................................................................169 5.4.2. Lithium sulfide (Li2S) formation and disappearance...........................................171 5.4.3. Ex situ XRD – supporting data for analysis.........................................................173 5.4.4. Conclusions..........................................................................................................181 5.5. Further cycles evolution at C/20.................................................................................181 5.5.1. The second cycle..................................................................................................181 5.5.2. The twenty sixth cycle .........................................................................................184 5.6. Influence of C-rate: C/8 studies..................................................................................185 5.6.1. XRD and electrochemistry – results ....................................................................186 5.6.2. Quantitative interpretation ...................................................................................188 5.7. Conclusions.................................................................................................................190 Chapter 6: Application of Electrochemical Impedance Spectroscopy and low temperature tests..................................................................191 6.1. Motivation of the work ...............................................................................................191 6.2. Experimental part........................................................................................................191 6.2.1. Coin cell design....................................................................................................191 6.2.2. EIS measurements................................................................................................192 6.3. Impedance response – Nyquist plot features ..............................................................193 6.3.1. Symmetric coin cells approach............................................................................194 6.4. Li/S cells upon storage – evidence of self-discharge..................................................197 6.5. Li/S battery upon cycling – initial cycle.....................................................................200 6 Table of context

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