Toward Standardization of Electrochemical Impedance Spectroscopy Studies of Li-Ion Conductive Ceramics

Abstract

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.

Complex Investigation of Water Impact on Li-Ion Conductivity of Li1.3Al0.3Ti1.7(PO4)3—Electrochemical, Chemical, Structural, and Morphological Aspects

“…We attribute these reflections to the same main LATP phase and justify their appearance with the residual low-intensity X-ray irradiation, namely CuK β and WL α1 . 29,43,45,46 Therefore, based on the SEM, EDX, and PXRD combined results, we may consider the reference 0h-sample as a pure target LATP phase. After the water exposure, samples tend to be contaminated with undefined, nanosized, X-ray amorphous phases.…”

“…Gold electrodes (30 nm thickness; 8 mm diameter) were sputtered on both plane faces of the pellet using the magnetron-sputtering machine Quorum Q150T ES and the 8 mm diameter mask. 29 The EIS results were registered 43 using a two-electrode cell 29 with copper electrodes (the EIS registration scheme is given in the Supporting Information, Section 4). Impedance studies were carried out at a galvanostat/potentiostat Metrohm Autolab (ambient conditions, RT = 23 °C, frequency range 1 MHz − 0.1 Hz, amplitude 10 mV vs Root Mean Square).…”

“…For further procedural details, please refer to our recent publications. 29,43 2.7. Mother-Solution Analysis.…”

Electrochemical Impedance Spectroscopy for All‐Solid‐State Batteries: Theory, Methods and Future Outlook

“…-is hugely influential on the resulting impedance spectra and a critical part of any EIS experiment. [15] Three general types of electrodes are used in electrochemical measurements: ion-blocking, electron-blocking and reversible. [16] In all cases, the contacting material should be inert and stable against the sample being tested.…”

Methods & Protocols of 2020

“…This emphasis remained in 2020, spanning both hard and soft, inorganic and organic materials (Table ). − Often, these methods are described in the context of classical material systems and provide a foundation for their application to new materials. Second are manuscripts focused on the application of materials (Table ), , with both contributions from 2020 putting emphasis on rigorous, quantitative electrochemical methods.…”