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Exploring Metastable Phases in Cerium-Doped Zirconia: Insights from X-ray Diffraction, Raman, X-ray Absorption, and
Luiza B F Dos Santos1,2, Volodymyr Svitlyk3, Selina Richter1
1Institute of Resource Ecology, Helmholtz-Zentrum Dresden-Rossendorf, Bautzner Landstraße 400, 01328 Dresden, Germany.
Inorganic Chemistry
|May 8, 2025
Summary
This study clarifies the complex ZrO2-CeO2 phase diagram, identifying a miscibility gap and metastable phases using Eu3+ as a probe. Findings enable optimized material properties for applications like solid oxide fuel cells.
Area of Science:
- Materials Science
- Solid-state Chemistry
- Crystallography
Background:
- The Zirconium Dioxide-Cerium Dioxide (ZrO2-CeO2) system is crucial for advanced technologies but has unresolved questions about cation miscibility and metastable phases.
- Understanding the Zr1-xCexO2 phase diagram is essential for optimizing material performance in demanding applications.
Purpose of the Study:
- To comprehensively investigate the Zr1-xCexO2 phase diagram, focusing on cation miscibility and the formation of metastable crystalline phases.
- To utilize Europium (Eu3+) as a luminescent probe for detailed characterization of phase transformations and local atomic environments.
Main Methods:
- Synchrotron powder X-ray diffraction (XRD) was employed to determine phase compositions and identify a miscibility gap.
- Raman spectroscopy and High Energy Resolution Fluorescence Detected X-ray Absorption Near Edge Structure (HERFD-XANES) spectroscopy were used to probe structural distortions and oxygen ion behavior.
- Luminescence spectroscopy of Eu3+ was utilized to distinguish between different crystalline phases and metastable structures.
Main Results:
- A miscibility gap was identified in the Zr1-xCexO2 system between 20 and 50 mol % cerium.
- Beyond the miscibility gap, solid solutions formed, including tetragonal prime (t') and tetragonal double prime (t″) phases, with unique Raman signatures.
- HERFD-XANES analysis indicated oxygen ion displacement in the t' phase, and Eu3+ luminescence distinctly identified all metastable phases.
Conclusions:
- The ZrO2-CeO2 system exhibits complex polymorphism, with identified metastable phases crucial for understanding its behavior.
- Precise control over phase composition through controlled synthesis is achievable, paving the way for property optimization.
- These findings have significant implications for developing advanced materials for oxygen sensors, three-way catalysts, and solid oxide fuel cells.
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