Ion
conductivity of ceramic electrolytes sets a limit to their
use in batteries; correct analysis of this parameter opens a gate
for further material optimization. Electrochemical impedance spectroscopy
(EIS) is the only way to characterize ionic conductivity, but the
data obtained could vary from researcher to researcher for a number
of reasons. Our goal was to propose a unified approach on the basis
of both the published data and our own experience. We synthesized
pure Li1.3Al0.3Ti1.7(PO4)3 and analyzed it using EIS, powder X-ray diffraction
analysis, scanning electron microscopy, and energy-dispersive X-ray
spectroscopy. We show how to (1) obtain reliable EIS spectra; (2)
verify the equivalent circuit by adjusting the temperature; and (3)
estimate the error of measurement via three approaches highlighting
their use for special research aims. Finally, we summarized parameters
that should be checked when describing results and benchmarking the
results with literature. The article will be useful for those who
work with ion-conducting ceramics.
The interest in alternative
energy sources grows rapidly and demands
improved materials. The cutting-edge investigations focus attention
on the development and optimization of solid electrolytes for advanced
energy storage. Their chemical and structural stability defines both
battery performance and lifetime, yet it is studied poorly even for
well-known superionic conductors such as NASICON-based compounds.
In this work, we studied the Li1.3Al0.3Ti1.7(PO4)3 (LATP) stability toward water.
Corresponding ceramics were synthesized in pellet form through the
solid-state reaction and had been immersed in deionized water for
different periods of time with subsequent electrochemical (electrochemical
impedance spectroscopy), structural (powder X-ray diffraction analysis,
Raman spectroscopy, computational modeling), chemical (ceramicsenergy-dispersive
X-ray spectroscopy; mother-solutionsinductively coupled plasma
mass spectrometry), and morphological (scanning and transmission electron
microscopy) analyses. Water exposure triggers drastic conductivity
losses (64% for σt) with accompanying lithium elution (exceeds
13 atomic%) and unit cell shrinkage. All these changes reach a plateau
after 2 h of water exposure.
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