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@ARTICLE{Woolley:1025073,
author = {Woolley, Henry Michael and Vargas-Barbosa, Nella},
title = {{E}lectrochemical {C}haracterization of {T}hiophosphate-
{I}onic {L}iquid {H}ybrid {L}ithium {E}lectrolytes {A}gainst
{L}i {M}etal},
journal = {Meeting abstracts},
volume = {MA2023-01},
number = {6},
issn = {1091-8213},
address = {Pennington, NJ},
publisher = {Soc.},
reportid = {FZJ-2024-02661},
pages = {986 - 986},
year = {2023},
abstract = {(Almost) solid-state batteries that utilize thiophosphate
solid electrolytes (SE) are an exciting technology emerging
as a potential alternative to lithium-ion batteries. When
used alongside a lithium metal anode they can offer the high
energy densities [1] required to meet the increasing demand
for energy storage. However, they suffer from numerous
issues which predominately occur at the cathode- or anode-SE
interface. Issues include dendrite propagation through gaps,
pores and grain boundaries of the solid electrolyte which
can eventually puncture electrolyte crystallites and lead to
cell failure. [2] Thiophosphate electrolytes are also
unstable both chemically and electrochemically. As a result
of the SEs having a low electrochemical stability window
reduction or oxidation can occur at the anode or cathode
interface, forming a resistive solid electrolyte interphase
(SEI). [3] Finally, the ionic contact between Li metal anode
and electrolyte is poor and thus high interfacial impedances
can arise. These impedances can be dynamic which increase
during stripping of the lithium and decrease during plating.
[4] To solve some of the interfacial issues there is the
option to add a small of amount of liquid electrolyte at the
lithium metal-electrolyte interface. The liquid electrolyte
can fill in the gaps and pores at the interface thus
improving the ionic contact whilst allowing a more stable
interface. Whilst the ionic contact can be improved the
inherent instability of thiophosphate electrolytes against
the liquid electrolyte means that a new interphase known as
the solid-liquid electrolyte interphase (SLEI) can form. The
presence of this interphase can therefore lower the energy
density and round-trip efficiencies of cells which utilize
hybrid electrolytes meaning that minimizing the SLEI
resistance and maximizing total ionic conductivities is
important in hybrid cells. [5]In this work a hybrid of the
thiophosphate argyrodite Li6PS5Cl and the ionic liquid
x-LiTFSI-1-butyl 1-methylpiperidinium TFSI (BMPipTFSI) with
LiTFSI concentrations of 0.25 M and 0.5 M was studied. The
choice of SE and liquid electrolyte boils down to the high
ionic conductivity of the SE and the electrochemical and
thermal stability of the ionic liquid. Temperature-dependent
ionic conductivity measurements showed that hybrid systems
exhibit lower in room temperature ionic conductivities and
higher total activation energies. This hints at the presence
of a SLEI forming between the LE and SE. To study how the
SLEI resistances changes over time, ion blocking potential
impedance spectroscopy measurements were performed. These
measurements were performed at 10 °C to allow for the
resistance contributions to be better resolved and showed a
SLEI resistance of around 45-50 Ω cm2 for both hybrids.
Over the period of 130 hours this resistance changed
minimally (around 5 Ω cm2 on average) indicating good
stability of the SLEI. To further test the suitability of
this hybrid alongside lithium metal anodes impedance
measurements in symmetrical lithium cells
(Li0|LE|LPCL|LE|Li0) were undertaken. In this case
galvanostatic impedance spectroscopy (GEIS) with an applied
current density of ±0.4 mA cm-2 was used to probe the
changes in resistance contributions in the system over the
period of stripping (positive current) and plating (negative
current). For cells with just SE a large change in the
resistance owing to the electrochemical reaction (ECR) (Li0
↔ Li+ + e-) occurred during stripping and plating
indicating the dynamic nature of the ionic contact at the
interface. For the hybrid electrolyte cells, this ECR
resistance is decreased and becomes more stable however a
larger interphase resistance is present. This resistance is
a combination of the resistances of both the SLEI (the
interphase between the LE and SE) and the SEI (the
interphase between LE and Li anode) and it changes over
stripping and plating showing that the S(L)EIs which are
present are dynamic. Finally, post-mortem SEM/EDX of the
surface of samples show a change in morphology and the
presence of decomposition products from both the liquid and
solid electrolytes. These studies show that the
LPCL-BMPipTFSI hybrid is stable and improve ionic contact at
the lithium metal anode interface. Further testing in half
Li-S cells will determine the suitability of the use of the
ionic liquid at the cathode side of the cell.References[1]
J. Janek and W. G. Zeier, Nat Energy, 2016, 1, 16141. [2] M.
B. Dixit et al. Matter, 2020, 3, 2138-2159 [3] G. Dewald et
al. Chem Mater, 2019, 31, 8328-8337. [4] T. Krauskopf et al.
Chem. Rev, 2020, 7745-7794. [5] H. M. Woolley and N. M.
Vargas-Barbosa, under review.},
cin = {IEK-12},
ddc = {540},
cid = {I:(DE-Juel1)IEK-12-20141217},
pnm = {1221 - Fundamentals and Materials (POF4-122)},
pid = {G:(DE-HGF)POF4-1221},
typ = {PUB:(DE-HGF)16},
doi = {10.1149/MA2023-016986mtgabs},
url = {https://juser.fz-juelich.de/record/1025073},
}