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NATURE COMMUNICATIONS | DOI: 10.1038/ncomms2513 ARTICLE 3k 2k 1k 70 60 50 40 30 20 10 3k 2k 1k 70 60 50 40 30 20 10 0 Experimental data Peak1-(58 ± 0.5 eV) Li-F Peak2-(55 ± 0.5 eV) Li-O Fit curve 60 55 50 0 s 60 55 50 30 s 60 55 50 Binding energy (eV) 60 55 50 500 s 60 55 50 800 s Li O C 90 s 150 s FS 0N 60 55 50 0 30 90 150 500 800 Etching time (s) 605550 0 s 605550 30 s 605550 Binding energy (eV) Experimental data Peak1-(58 ± 0.5 eV) Li-F Peak2-(55 ± 0.5 eV) Li-O Peak3-(53 ± 0.5 eV) LiO Fit curve LiO 150 s LiO 605550 500 s LiO 605550 800 s Li O C F 60 s 90 s 60 55 50 605550 0 30 60 90 150 500 800 Etching time (s) Figure 6 | X-ray photoelectron spectroscopy (XPS) analysis of metallic lithium anodes. After 100 cycles at a current rate of 0.2C with 2# and SIS-7# electrolytes, (a) XPS Li1 s spectra of metallic lithium electrode using 2# electrolyte before sputtering and after sputtering with different times. (b) Summary of the atomic concentration of Li, C, O, S, N and F on the Li anode surface as a function of sputtering time using 2# electrolyte. (c) XPS Li1 s spectra of metallic lithium electrode using SIS-7# electrolyte before sputtering and after sputtering with different times. (d) Summary of the atomic concentration of Li, C, O, S, N and F on the Li anode surface as a function of sputtering time using SIS-7# electrolyte. gun (Thermo Fisher). Arþ etching was conducted at an argon partial pressure of 10 8 Torr in the x–y scan mode at ion acceleration of 3 kV and ion beam current density of 1mAmm2. The lithium polysulphide dissolution experiments were carried out in the following: Li2S and S with a mole ratio of 1:7 (49.5 and 224 mg) were mixed and added in 2-ml pure solvent, 2 mol salt per 1-l solvent (2#), 4 mol salt per 1-l solvent (4#) and 7 mol salt per 1-l solvent (SIS-7#), respectively. The colour changes of solutions with time were observed and recorded by digital camera. The samples of 2#, 4# and SIS-7# after standing for 18 days were diluted with the corresponding electrolytes in the ratio of 1:7 for UV-Vis measurement, which was carried out on a Cary 5000 UV-Vis spectrophotometry (Varian, America). The control samples are pure electrolytes without Li2S8 (4#0 and SIS-7#0). X-ray powder diffraction analysis was characterized by X’Pert Pro MPD X-ray diffractometer (Philips, Holland) using Cu–Ka radiation (1.5405 Å). Electrochemistry. The electrode was fabricated by mixing C/S composite, carbon nanotube, poly(vinylidene difluoride) in weight ratio of 8:1:1 for cycle life mea- surement and the other weight ratio of 7:2:1 for rate capability measurement. The slurry was cast on carbon-coated Al current collector and dried at 50 °C in vacuum for 10 h. The coin cells CR2032 were assembled with the electrode, pure lithium foil as counter electrode and a glass fibre separator in an argon-filled glove box. The discharge and charge measurements at room temperature and low-temperature range of 20 to 0 °C in a thermostated container were carried out on a Land BT2000 Battery Test System (Wuhan, China). The average cycling efficiency of metallic lithium electrodes in various electrolytes (2#, 4#, SIS-7#) was performed by electrochemically depositing Li on Cu foil (5 C cm 2) followed by Li stripping and deposition cycling (10% depth of discharge-DOD, 0.1mAcm2, 20 cycles). The residual Li was then dissolved electrochemically (charged to 3 V) on a Land BT2000 Battery Test System. The average Li cycling efficiency was calculated according to Aurbach et al.53 NATURE COMMUNICATIONS | 4:1481 | DOI: 10.1038/ncomms2513 | www.nature.com/naturecommunications 7 & 2013 Macmillan Publishers Limited. All rights reserved. N S Atomic concentration (%) Intensity/counts per second Atomic concentration (%) Intensity/counts per secondPDF Image | Solvent-in-Salt electrolyte for high-energy rechargeable metallic lithium batteries
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