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frequency range of 1 MHz – 10 mHz, with voltage amplitude of 10 mV. The experimental data were analyzed with ZView software. Morphology of the samples (mainly electrodes) was investigated with the use of a Scanning Electron Microscope (SEM; LEO 1530, Gemini). 5 kV accelerating voltage was used. A sample was placed on SEM stubs onto adhesive conductive carbon tape. Air-sensitive samples (i.e. discharged electrodes with Li2S deposit) were transferred to the SEM with a special transfer box as shown on Figure 2-3a. (a) (b) (c) Figure 2-3. SEM transfer box permitting to keep the analyzed samples under argon protective atmosphere without air exposure at any step of the measurement (a,b); XRD sample protected by thin Kapton® film (c). The structural characterization was performed by X-Ray Diffraction (XRD) technique via BRÜKER powder diffraction system (model D8 Advance), using CuKα as the radiation source. In case of air-sensitive samples (mostly post mortem analysis), electrode was recuperated from a coin cell inside the glove box, washed gently with DIOX and left for solvent evaporation for 10-15 minutes. Once dried, the electrode was stuck on a glass plate with the use of double side tape and covered with a thin (13 μm) Kapton® foil to protect from air (Figure 2-3b). 2.2.4. Discussion concerning the results’ margin of error All results presented here were carefully selected to keep the best reproducibility and reliability, i.e. (i) sulfur electrodes prepared not far from each other in terms of date, (ii) same batch of electrolyte used, (iii) same conditions for battery assembly and testing (room temperature for Arbin® cycler), etc. In most of the cases, the data were obtained from few cells in parallel. Nevertheless, despite of all precautions taken, different natures of error were still present, which could influence the experimental capacity. The error related with the electrode weight was rather low, and estimated according to the equation (4): Chapter 2: S8 electrode on Aluminum 48PDF Image | Accumulateur Lithium Soufre
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