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volumes (20–30 μL) of this mixture were dropped directly onto ACFC with a digital micropipette (Nichipet EX II 100, 10–100 μL, Nichiryo Co., Ltd.), and the DME solvent was allowed to evaporate at 120 °C under vacuum. The final amount of sulfur loading was controlled within the ACFC in the range of 4–6.5 mg cm−2. ECF was fabricated by electrospinning. Polyacrylonitrile (average MW 150,000, Sigma- Aldrich) and polymethylmethacrylate (MW = 120 000, Sigma-Aldrich) were dispersed at a 5:1 wt% ratio in anhydrous N,N-dimethylformamide (Sigma-Aldrich) and magnetically stirred for 20 h at 80 °C. Vacuum-dried silica nanoparticles (12 nm, LUDOX HS-30 colloidal silica, 30 wt % suspension in water, Sigma-Aldrich) were then added to this solution 2 wt %at a time. The as- prepared solution was fed through a syringe needle (BD 10 mL syringe, Luer-Lok tip) with the aid of an infusion syringe pump (78-0100C, Cole Parmer Instrument company, USA) at a constant flow rate of 1.20 mL h−1 and a DC voltage of 15 kV. The distance between the needle and the collector was 15 cm. The polymer composite membranes were stabilized in air at 250 °C for 1 h and subsequently carbonized at 700 °C for 3 h under Ar/H2 flow (96:4, 100 cc min−1). The membrane thickness ranged from 100 to 250 μm, and the mass loading was between 1.4 and 3.0 mg cm−2. ECF-Li2S8 cathodes were prepared in the same way as ACFC_Li2S8 to assemble the Li- S cell. In the operando XAS measurement, SiO2 was not added for the thin specimen of ECF_Li2S8. Materials characterization XPS measurements were performed with a Physical Electronics Quantera scanning X-ray microprobe. This system uses a focused, monochromatic, Al Kα X-ray (1486.7 eV) source for excitation and a spherical section analyzer. The instrument has a 32-element multichannel detection system. The X-ray beam is incident normal to the sample, and the photoelectron detector is at 45° off normal. High energy resolution spectra were collected using a pass energy of 69.0 eV with a step size of 0.125 eV. For the Ag 3d5/2 line, these conditions produced a full width at half maximum of 0.92 eV 0.05 eV. The binding energy scale was calibrated using the Cu 2p3/2 feature at 932.62 0.05 eV and that of Au 4f7/2 at 83.96 0.05 eV. All samples were rinsed with DME several times to remove residual electrolyte and then dried under vacuum for 20 min. To avoid side reactions or electrode contamination with ambient oxygen and moisture, electrodeposited Li was transported from the glovebox to the XPS and scanning electron microscope (SEM) instruments in a hermetically sealed container filled with Ar. The morphology of Li electrodeposited onto Cu was investigated using a Quanta focused-ion-beam SEM (FEI, Quanta 650 ESEM). All EPR measurements were performed on a Bruker ELEXSYS E580 spectrometer at both 298 K and 125 K. All samples were prepared inside a glove box filled with nitrogen immediately before EPR experiments to minimize the influence of air and moisture. For liquid samples, a capillary with ID 0.8 mm and OD 1 mm was used to hold the solution in the EPR cavity with both ends sealed by CritosealTM Leica Microsystems capillary tube sealant; the capillary was further placed inside a 4 mm EPR tube with the open end sealed inside a glove box. The typical settings for the spectra were microwave frequency = 9.32 GHz, sweep width = 1000 G, sweep time = 42 s, time constant = 40.96 ms, power = 20 mW, field modulation amplitude = 15 G. Absolute spin concentrations of the samples were determined by calibration Page 12 of 24PDF Image | A lithium-sulfur battery with a solution-mediated pathway
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