The pH of electrolyte solutions was
measured using a pH meter (Mettler Toledo pH/Ion meter) after sufficient
Ar-gas purging in an Ar-filled glovebox and removed from the glovebox.
It was noted that pH was constant in the Ar-filled glovebox for several
days, while the pH decreased after air exposure. For post-mortem analyses,
LCO electrodes were washed with de-gassed distilled (DI) water and
dried under a vacuum at 60 °C overnight. Soft X-ray absorption
near-edge structure (XANES) was measured in the BL11, Synchrotron
Radiation (SR) center at Ritsumeikan University. The LCO electrodes
were not exposed to air and directly transferred to the XANES chamber
using a hermetic vessel. XRD (Cu Kα, Rigaku) was used to analyze
the long-range order of the crystal structure. XPS (Al Kα, Thermo
VG Scientific) was used for surface analysis. All spectra were calibrated
to the carbon 1s sp2 hybridization signal at 248.5 eV.
TEM (FEI Tecnai GE F30 S-Twin (300 kV)) images were attained to observe
the surface layer. All XRD, XPS, and TEM were used at KARA. The OH
stretching vibrations of aqueous electrolyte solutions were attained
from ATR-IR spectroscopy in the range of 400∼4000 cm–1 (iS50, diamond window, Thermo Scientific). Confocal Raman spectroscopy
(Andor, SR-750-A-R) was used with a laser of 532 nm wavelength to
acquire Raman spectra.
measured using a pH meter (Mettler Toledo pH/Ion meter) after sufficient
Ar-gas purging in an Ar-filled glovebox and removed from the glovebox.
It was noted that pH was constant in the Ar-filled glovebox for several
days, while the pH decreased after air exposure. For post-mortem analyses,
LCO electrodes were washed with de-gassed distilled (DI) water and
dried under a vacuum at 60 °C overnight. Soft X-ray absorption
near-edge structure (XANES) was measured in the BL11, Synchrotron
Radiation (SR) center at Ritsumeikan University. The LCO electrodes
were not exposed to air and directly transferred to the XANES chamber
using a hermetic vessel. XRD (Cu Kα, Rigaku) was used to analyze
the long-range order of the crystal structure. XPS (Al Kα, Thermo
VG Scientific) was used for surface analysis. All spectra were calibrated
to the carbon 1s sp2 hybridization signal at 248.5 eV.
TEM (FEI Tecnai GE F30 S-Twin (300 kV)) images were attained to observe
the surface layer. All XRD, XPS, and TEM were used at KARA. The OH
stretching vibrations of aqueous electrolyte solutions were attained
from ATR-IR spectroscopy in the range of 400∼4000 cm–1 (iS50, diamond window, Thermo Scientific). Confocal Raman spectroscopy
(Andor, SR-750-A-R) was used with a laser of 532 nm wavelength to
acquire Raman spectra.