Pecs 682

Powder X-ray diffraction patterns were obtained using a Stoe STADI/P diffractometer employing CuKα₁ radiation operating in transmission mode with the samples sealed in 0.2 mm capillaries, expect for the experiments on air sensitivity, which were carried out in air. Time-of-flight powder neutron diffraction data were collected on the POLARIS high-intensity; medium resolution instrument at ISIS, Rutherford Appleton Laboratory (UK) with samples sealed in 2 mm quartz capillaries. The structures were refined by the Rietveld method using TOPAS Academic36 . Samples with different Li amounts for X-ray diffraction were prepared electrochemically. After cycling, cells were transferred to an argon-filled glove box before opening and active material removed. The electrodes were then rinsed with a small amount of dry dimethyl carbonate to remove residual electrolyte. They were left under dynamic vacuum overnight to ensure all solvent had evaporated before measurements were collected. SEM studies were carried out using a Carl Zeiss Merlin instrument. Electrodes for cross-sectional imaging were rotary-etched in a Gatan Precision Etching Coating System (PECS 682).

For the scanning electron microscopy analysis, the nanogel solutions were cast on silicone surface and the samples were sputter-coated before imaging, using a precision etching coating system (PECS, 682, Gatan Inc, Pleasanton, CA) with 8 nm thick gold/palladium. The size and shape of the nanogels were investigated using a scanning electron microscope (ESEM, FEI Quanta 200 FEG, FEI Company). The analyses were made in high vacuum and at relatively low acceleration voltage (5 kV) using backscattered electron technique.

Microstructure
analyses were performed on thermally etched (1150 °C in air for
15 min) cross sections using a scanning electron microscope (SEM;
Thermo Fisher Quanta 650 ESEM, Massachusetts, USA) with a thermionic
electron source.
Samples for scanning transmission electron
microscopy (STEM) were prepared by cutting a 3 mm disk from the ceramic
pellet, mechanical thinning to ∼100 μm, dimpling to ∼20
μm in the disc center (Dimple grinder, Gatan Inc., Warrendale),
and finally, ion milling to perforation using 3.8 keV Ar ions at an
angle of 8° from both sides (PIPS 691, Gatan Inc., Pleasanton,
USA). After perforation, the energy was gradually lowered, finally
to 500 eV for 5 min to minimize the thickness of the amorphous surface
layer. STEM analyses were performed using a probe-corrected atomic-resolution
microscope (JEOL ARM200 CF, Jeol Ltd., Tokyo, Japan) operated at 200
kV and equipped with a high-angle annular dark-field (HAADF) detector
with inner and outer semiangles of 68 and 180 mrad, respectively.
EELS spectra were acquired using a Gatan DualEELS Quantum ER spectrometer.
Samples for STEM analyses were coated with 2 nm of amorphous carbon
(PECS 682, Gatan Inc., Pleasanton, USA) to prevent charging under
the electron beam.