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Comparative X‐ray diffraction study of the crystalline microstructure of tetragonal and monoclinic vanadium–zirconium dioxide solid solutions produced from gel precursors
Author(s) -
Kojdecki Marek Andrzej,
Ruiz de Sola Esther,
Serrano Francisco Javier,
Amigó José María,
Alarcón Javier
Publication year - 2009
Publication title -
journal of applied crystallography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.429
H-Index - 162
ISSN - 1600-5767
DOI - 10.1107/s0021889809005135
Subject(s) - crystallite , materials science , monoclinic crystal system , tetragonal crystal system , microstructure , nucleation , cubic zirconia , vanadium , crystallography , solid solution , x ray crystallography , analytical chemistry (journal) , mineralogy , diffraction , crystal structure , metallurgy , chemistry , ceramic , optics , organic chemistry , physics
The microstructural characteristics of solid solutions, prepared by heating dried gel precursors with nominal compositions V x Zr 1− x O 2 (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.