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@ARTICLE{Hahn:829015,
author = {Hahn, H. and Wagner, Ralf and Schappacher, F. and Winter,
M. and Nowak, S.},
title = {{I}n operando {X}-shaped cell online electrochemical mass
spectrometry ({OEMS}): {N}ew online analysis enables insight
into lab scale lithium ion batteries during operation},
journal = {Journal of electroanalytical chemistry},
volume = {772},
issn = {1572-6657},
address = {New York, NY [u.a.]},
publisher = {Elsevier},
reportid = {FZJ-2017-02832},
pages = {52 - 57},
year = {2016},
abstract = {A new method for the in operando analysis of evolving gases
during cyclic aging of lithium ion batteries (LIBs) was
developed to better assess safety concerning cell processes,
especially those arising from the electrochemical
degradation of the lithium hexafluorophosphate LiPF6/organic
carbonate solvent based electrolyte. For electrochemical
characterization at lab-scale, a cell in the shape of
T-connector (“T-cell”) is usually used, offering
connections to working, counter and reference electrode. To
maintain comparability to this established system, an in
operando X-shaped cell, i.e., a T-cell (“X-cell”), which
varies only by an additional connector from the original
setup, was designed. The new OEMS cell based on DEMS cell
designs was linked to a modified GC–MS System and a
potentiostat for in operando analysis of the evolving gases
and the voltammetry experiments, respectively. This work
comprises the evaluation of this new OEMS method in
potentiostatic aging experiments of the conventional
electrolyte 1M LiPF6 in EC:EMC (1:1, by wt.) in
LiNi1/3Co1/3Mn1/3O2 (NCM)/Li half cells as a function of the
applied cut-off potential. Mainly CO2 release at onset
potentials > 4.6 V vs. Li/Li+ could be identified. At a
potential of > 5.4 V vs. Li/Li+, the evolution of silicon
tetrafluoride (SiF4) was observed mainly stemming from the
HF induced degradation of the used glass fiber separator.
Furthermore, triethyl phosphate (TEP) evolved from the LiPF6
decomposition at > 5.5 V vs. Li/Li+. Oxygen evolution either
coming from the oxidative decomposition of the electrolyte
or degradation of the NCM cathode material was not detected
at even 5.5 V vs. Li/Li+ and at 20 °C.},
cin = {IEK-12},
ddc = {540},
cid = {I:(DE-Juel1)IEK-12-20141217},
pnm = {131 - Electrochemical Storage (POF3-131)},
pid = {G:(DE-HGF)POF3-131},
typ = {PUB:(DE-HGF)16},
UT = {WOS:000377321400007},
doi = {10.1016/j.jelechem.2016.04.023},
url = {https://juser.fz-juelich.de/record/829015},
}