Synthesis and thermal stability of zirconia and yttria-stabilized zirconia microspheres

Elisabeth W Leib; Ulla Vainio; Robert M Pasquarelli; Jonas Kus; Christian Czaschke; Nils Walter; Rolf Janssen; Martin Müller; Andreas Schreyer; Horst Weller; Tobias Vossmeyer

doi:10.1016/j.jcis.2015.02.049

Synthesis and thermal stability of zirconia and yttria-stabilized zirconia microspheres

J Colloid Interface Sci. 2015 Jun 15:448:582-92. doi: 10.1016/j.jcis.2015.02.049. Epub 2015 Feb 27.

Authors

Affiliations

¹ Institute of Physical Chemistry, University of Hamburg, Grindelallee 117, D-20146 Hamburg, Germany.
² Institute of Materials Research, Helmholtz-Zentrum Geesthacht, Max-Planck-Straße 1, 21502 Geesthacht, Germany.
³ Institute of Advanced Ceramics, Hamburg University of Technology (TUHH), Denickestraße 15, 21073 Hamburg, Germany.
⁴ Institute of Physical Chemistry, University of Hamburg, Grindelallee 117, D-20146 Hamburg, Germany; The Hamburg Centre for Ultrafast Imaging, Luruper Chaussee 149, 22761 Hamburg, Germany; Department of Chemistry, Faculty of Science, King Abdulaziz University, Jeddah, Saudi Arabia.
⁵ Institute of Physical Chemistry, University of Hamburg, Grindelallee 117, D-20146 Hamburg, Germany. Electronic address: tobias.vossmeyer@chemie.uni-hamburg.de.

PMID: 25796070
DOI: 10.1016/j.jcis.2015.02.049

Abstract

Hypothesis: Zirconia microparticles produced by sol-gel synthesis have great potential for photonic applications. To this end, identifying synthetic methods that yield reproducible control over size uniformity is important. Phase transformations during thermal cycling can disintegrate the particles. Therefore, understanding the parameters driving these transformations is essential for enabling high-temperature applications. Particle morphology is expected to influence particle processability and stability. Yttria-doping should improve the thermal stability of the particles, as it does in bulk zirconia.

Experiments: Zirconia and YSZ particles were synthesized by improved sol-gel approaches using fatty acid stabilizers. The particles were heated to 1500 °C, and structural and morphological changes were monitored by SEM, ex situ XRD and high-energy in situ XRD.

Findings: Zirconia particles (0.4-4.3 μm in diameter, 5-10% standard deviation) synthesized according to the modified sol-gel approaches yielded significantly improved monodispersities. As-synthesized amorphous particles transformed to the tetragonal phase at ∼450 °C with a volume decrease of up to ∼75% and then to monoclinic after heating from ∼650 to 850 °C. Submicron particles disintegrated at ∼850 °C and microparticles at ∼1200 °C due to grain growth. In situ XRD revealed that the transition from the amorphous to tetragonal phase was accompanied by relief in microstrain and the transition from tetragonal to monoclinic was correlated with the tetragonal grain size. Early crystallization and smaller initial grain sizes, which depend on the precursors used for particle synthesis, coincided with higher stability. Yttria-doping reduced grain growth, stabilized the tetragonal phase, and significantly improved the thermal stability of the particles.

Keywords: Ceramic; Microspheres; Phase transformation; Thermal barrier coating; YSZ; Zirconia.