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In Situ Lithiated Reference Electrode: Four Electrode Design for In-operando Impedance Spectroscopy

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In Situ Derived Impedance-Structure Correlation during LaNiO₃ Decomposition.

Christoph Malleier¹, Thomas F Winterstein¹, Marc Heggen²

¹Institute of Physical Chemistry, University of Innsbruck, Innrain 52c, A-6020 Innsbruck, Austria.

Journal of the American Chemical Society

|November 20, 2025

Summary

This summary is machine-generated.

In situ impedance spectroscopy effectively tracks LaNiO3 decomposition during hydrogen reduction, revealing chemical and structural changes. This method is potent for detecting bulk and surface transitions in perovskites.

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Area of Science:

Materials Science
Electrochemistry
Surface Science

Background:

Lanthanum nickelate (LaNiO3) is a perovskite material with potential applications in catalysis and energy storage.
Understanding its decomposition pathways under reductive conditions is crucial for optimizing its performance and stability.
In situ characterization techniques are needed to probe dynamic transformations during redox processes.

Purpose of the Study:

To demonstrate the utility of in situ impedance spectroscopy as a marker for LaNiO3 decomposition.
To correlate electrochemical properties with chemical and structural transitions during hydrogen reduction.
To investigate the influence of redox cycling on the material's behavior.

Main Methods:

In situ impedance spectroscopy coupled with in situ X-ray diffraction (XRD).
Differential thermoanalysis (DTA) and in situ near-ambient pressure X-ray photoelectron spectroscopy (NAP-XPS).
Redox cycling under H2 and O2 atmospheres at various temperatures.

Main Results:

In situ impedance spectroscopy successfully monitored LaNiO3 decomposition, identifying bulk and surface transitions.
Combined impedance and XRD revealed electrochemical properties of oxygen-deficient phases and decomposition products (La2O3, Ni).
Distinct exothermic events correlated with LaNiO2.5 and La2O3 + Ni formation; impedance changes indicated surface redox transformations and kinetic delays.

Conclusions:

In situ impedance spectroscopy is a powerful, non-invasive tool for tracking redox-induced transformations in perovskites like LaNiO3.
The technique offers high sensitivity to surface chemistry, defect dynamics, and structural changes during redox cycling.
Understanding these transformations is key for designing stable and efficient perovskite-based materials.