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@ARTICLE{Malkowski:910690,
author = {Malkowski, Thomas F. and Boeding, Ethan D. and
Fattakhova-Rohlfing, Dina and Wettengl, Nadine and
Finsterbusch, Martin and Veith, Gabriel M.},
title = {{D}igestion processes and elemental analysis of oxide and
sulfide solid electrolytes},
journal = {Ionics},
volume = {28},
number = {7},
issn = {0947-7047},
address = {Heidelberg},
publisher = {Springer},
reportid = {FZJ-2022-04062},
pages = {3223 - 3231},
year = {2022},
abstract = {Detailed elemental analysis is essential for a successful
development and optimization of material systems and
synthesis methods. This is especially relevant for Li- and
Na-containing compounds, found in state-of-the-art and
next-generation battery systems. Their materials’
properties and thus the final device performance strongly
depend on the crystal structure, the stoichiometry, and
defect chemistry, e.g., influencing charge carrier
concentration and activation energies for vacancy transport.
However, a detailed quantitative analysis of light elements
in a heavy matrix, featuring a broad range of solubilities
and vapor pressures, is often difficult and associated with
large uncertainties and thus neglected in favor of just
reporting the stoichiometry as “weighed in.” In this
work, we report several approaches to digest and dissolve
various oxide and sulfide-based materials, used in
next-generation Li batteries, for elemental analysis via
optical emission spectroscopy. These include the most common
solid electrolytes Li-La-Ti–O, a perovskite material
(LLTO), and Li-La-Zr-O which has garnet structure (LLZO).
Additionally, a facile thermal digestion process is reported
for a surrogate sulfide solid electrolyte (Na2S). The
digestion procedures reported here are suitable for almost
any laboratory environment and, when applied, will improve
understanding of the synthesis-structure–property
correlations needed to advanced batteries with all
solid-state configurations.},
cin = {IEK-1 / ZEA-3},
ddc = {530},
cid = {I:(DE-Juel1)IEK-1-20101013 / I:(DE-Juel1)ZEA-3-20090406},
pnm = {1221 - Fundamentals and Materials (POF4-122)},
pid = {G:(DE-HGF)POF4-1221},
typ = {PUB:(DE-HGF)16},
UT = {WOS:000788507700002},
doi = {10.1007/s11581-022-04536-0},
url = {https://juser.fz-juelich.de/record/910690},
}