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@PHDTHESIS{Loutati:1043158,
author = {Loutati, Asmaa},
title = {{O}ptimization of {N}a{SICON}-type lithium- ion conductors
for solid-state batteries},
volume = {664},
school = {Duisburg-Essen},
type = {Dissertation},
address = {Jülich},
publisher = {Forschungszentrum Jülich GmbH Zentralbibliothek, Verlag},
reportid = {FZJ-2025-02774},
isbn = {978-3-95806-824-7},
series = {Schriften des Forschungszentrums Jülich Reihe Energie $\&$
Umwelt / Energy $\&$ Environment},
pages = {viii, 104},
year = {2025},
note = {Dissertation, Duisburg-Essen, 2024},
abstract = {The continuing depletion of fossil fuels, rising oil prices
and the need to reduce CO2 emissions have stimulated
intensive research into alternative energy technologies
based on renewable and clean sources. Among the various
technologies, electrochemical energy storage in rechargeable
lithium-ion batteries (LIBs) plays an important role, both
for powering a wide range of electronic devices and electric
vehicles, and for storing electricity generated from
alternative energy sources such as solar and wind.
Commercial LIBs using organic liquid electrolytes dominate
the market. However, the reactivity of liquid electrolytes
at very positive or negative potentials limits the choice of
suitable electrode materials and thus the available energy
density. In addition, the toxicity and flammability of
organic electrolytes raise serious safety concerns. As an
alternative to conventional liquid electrolyte LIBs,
solid-state battery (SSB) concepts using solid electrolytes
(SEs) are currently under intense investigation. Among
numerous classes of materials, ceramic SEs are particularly
attractive due to their non-flammability, relatively high
ionic conductivity at room temperature (RT) and high
chemical stability in air, resulting in potentially very
high intrinsic safety of the batteries. In particular,
Li-containing NaSICONs (Na Super Ionic CONductors) are
currently receiving a great deal of attention due to the
large structural variability and high ionic conductivity
that can be achieved by substituting the lattice framework
with various elements. Within this class of materials,
lithium aluminum germanium phosphate Li1+xAlxGe2-x(PO4)3
(LAGP) and lithium aluminum titanium phosphate
Li1+xAlxTi2-x(PO4)3 (LATP) are solid-state Li-ion conductors
with the highest ionic conductivity at RT. However, the main
drawback of germanium and titanium-containing materials is
the low electrochemical stability at negative potentials
caused by the reduction of Ge4+ to Ge2+ and Ti4+ to Ti3+,
which prevents the use of lithium metal anodes and reduces
the energy density of the battery. To overcome this problem,
the aim of this work was to increase the reduction stability
of NaSICON compounds by replacing Ge and Ti with more
reduction stable ions. To this end, various compositions of
the type Li1+xM3+xZr2-x(PO4)3, where M3+ = Al3+, Sc3+, Y3+,
were synthesized by solution-assisted solid-state reaction.
The effect of Substitution on crystallographic parameters,
relative density, sintering temperature, ionic conductivity,
and electrochemical stability was systematically
investigated. The cationic substitution of M3+ (M = Al, Sc,
Y) for Zr4+ in LiZr2(PO4)3 (LZP) stabilizes the rhombohedral
NaSICON structure (space group 𝑅3̅ c) at RT and
increases the ionic conductivity significantly. Here, at 25
°C and with a comparable relative density of 94-96 $\%,$ an
ionic conductivity of 2.7 × 10-5 S cm-1, 6.7 × 10-5 S cm-1
and 3.6 × 10-6 S cm-1 was achieved with the compositions
Li1.2Sc0.2Zr1.8(PO4)3, Li1.2Y0.2Zr1.8(PO4)3 and
Li1.2Al0.2Zr1.8(PO4)3, respectively. Compared to
Li1+xScxZr2-x(PO4)3, the Y3+ substitution in LZP slightly
enhanced the ionic conductivity and marked the maximum
Li+-ion conductivity at RT with composition x = 0.2 in the
whole system Li1+xM3+xZr2-x(PO4)3. However, the
Al3+-substitution decreased the ionic conductivity at RT. In
addition to cationic substitution, the effect of polyanionic
substitution on ionic conductivity was investigated in the
two materials series Li3+xSc2SixP3-xO12 (0 ≤ x ≤ 0.6)
and Li1.2+xSc0.2Zr1.8SixP3-xO12 (0.3 ≤ x ≤ 2.8). The
substitution of (PO4)3- with (SiO4)4- in the system
Li2O-Sc2O3-ZrO2-SiO2-P2O5 effectively lowers the sintering
temperature. Moreover, the introduction of zirconium can
limit the evaporation of lithium species even at high
sintering temperature. Silicate substitution in
Li3+xSc2SixP3-xO12 (0 ≤ x ≤ 0.6) has been shown to
stabilize the monoclinic Symmetry (space group P21/n)
resulting in the increase of total ionic conductivity. The
ionic conductivity at 25 °C increased from 2 × 10-6 S cm-1
for x = 0 to 1.2 × 10-5 S cm-1 for x = 0.15, which is the
highest ionic Conductivity of the investigated compositions
in the Li2O-Sc2O3-ZrO2-SiO2-P2O5 system. The purity of the
NaSICON materials has a strong influence on the grain
boundary resistance and thus on the ionic conductivity.
Selected ceramic NaSICON electrolytes such as LZP ,
Li1.2Y0.2Zr1.8(PO4)3, and Li3Sc2(PO4)3 (LSP) were found to
be more stable with respect to lithium than LATP and LAGP.
LSP proved to be chemically and electrochemically very
stable and might act as an anode protection material in
combination with lithium metal.},
cin = {IMD-2},
cid = {I:(DE-Juel1)IMD-2-20101013},
pnm = {1222 - Components and Cells (POF4-122)},
pid = {G:(DE-HGF)POF4-1222},
typ = {PUB:(DE-HGF)3 / PUB:(DE-HGF)11},
urn = {urn:nbn:de:0001-2506230903296.203072864795},
doi = {10.34734/FZJ-2025-02774},
url = {https://juser.fz-juelich.de/record/1043158},
}