Precipitates
from different experiments were attached to carbon stickers and coated
with 6 nm of platinum before being examined using a FEI Helios Nanolab
G3 scanning electron microscope (SEM) equipped with a focused ion
beam. Chemical analysis of the precipitates was conducted during the
SEM analysis using energy dispersive X-ray spectroscopy (EDX). Lithium
cannot be analyzed using conventional EDX detectors; therefore, the
presence of C and O, but absence of a cation, was used to identify
the Li-carbonate phase. Crystal aspect analysis was conducted based
on the system described by Um et al.26 (link) for
ice crystals, which show a morphology similar to the crystals formed
in the synthesis experiments. Analysis of crystal morphology aspect
parameters: total length, total width, height from central face to
top of crystal, width of central face, and width of side faces, was
conducted in Adobe Photoshop. Crystals used in the aspect analysis
were chosen that were lying with the longest crystal axis parallel
to the electron beam to limit measurement errors due to image perspective
effects. In addition, only crystals where the entire length of the
crystal could be seen were chosen. These requirements limited the
number of crystals that were measurable, and thus aspect ratios for
10 crystals from each experiment without and with the highest concentration
of additional ions were obtained.
from different experiments were attached to carbon stickers and coated
with 6 nm of platinum before being examined using a FEI Helios Nanolab
G3 scanning electron microscope (SEM) equipped with a focused ion
beam. Chemical analysis of the precipitates was conducted during the
SEM analysis using energy dispersive X-ray spectroscopy (EDX). Lithium
cannot be analyzed using conventional EDX detectors; therefore, the
presence of C and O, but absence of a cation, was used to identify
the Li-carbonate phase. Crystal aspect analysis was conducted based
on the system described by Um et al.26 (link) for
ice crystals, which show a morphology similar to the crystals formed
in the synthesis experiments. Analysis of crystal morphology aspect
parameters: total length, total width, height from central face to
top of crystal, width of central face, and width of side faces, was
conducted in Adobe Photoshop. Crystals used in the aspect analysis
were chosen that were lying with the longest crystal axis parallel
to the electron beam to limit measurement errors due to image perspective
effects. In addition, only crystals where the entire length of the
crystal could be seen were chosen. These requirements limited the
number of crystals that were measurable, and thus aspect ratios for
10 crystals from each experiment without and with the highest concentration
of additional ions were obtained.