Comparative X-ray diffraction study of the crystalline microstructure of tetragonal and monoclinic vanadium-zirconium dioxide solid solutions produced from gel precursors

• Published in: Journal of applied crystallography 2009-04, Vol.42 (2), p.198-210
• Main Authors: Kojdecki, Marek Andrzej, Ruiz de Sola, Esther, Serrano, Francisco Javier, Amigó, José María, Alarcón, Javier
• Format: Article
• Language: English
• Subjects: Comparative studies; Crystal structure; crystalline microstructure; crystallite shape; Crystallography; Diffraction; line profile analysis; Mineralogy; powder pattern analysis; second-order crystalline lattice strain distribution; vanadium-doped zirconium dioxide; volume-weighted crystallite size distribution
• ISSN: 1600-5767; 0021-8898; 1600-5767
• DOI: 10.1107/S0021889809005135

The microstructural characteristics of solid solutions, prepared by heating dried gel precursors with nominal compositions VxZr1−xO2 (0 ≤x≤ 0.1) at 723 and 1573 K, were determined from X‐ray diffraction patterns. The crystalline microstructure of the resulting specimens, characterized by a prevalent crystallite shape, a volume‐weighted crystallite size distribution and a second‐order lattice strain distribution, was found to depend on the vanadium content. A characteristic feature of all size distributions was their bimodality, explained as a result of transformations between tetragonal and monoclinic phases during thermal treatment. A comparative study of the microstructure of both zirconia phases has been carried out, enabling reconstruction of a probable course of crystallization of both pure and vanadium‐doped zirconias: on heating a sample, nucleation and the early growth stages involve crystallites of both phases; then on annealing and cooling, the crystallites of one phase transform into the other, depending on the thermal treatment temperature. Each logarithmic normal component of the crystallite size distribution of the resulting phase can be attributed to one of these processes. The limit of solubility of vanadium in tetragonal and monoclinic zirconia is estimated from the microstructural characteristics.