Synthesis and Characterization of Vanadium-Containing ZrSiO4 Solid Solutions from Gels

A procedure is reported for the preparation of vanadium-doped zircon pigmenting system with different vanadia loadings which enabled their complete formation and further characterization. Vanadium-zircon solid solutions were prepared by gelling mixtures of ZrO2 and V2O5 colloidal sols and tetraethyl...

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Bibliographic Details
Published in:Journal of sol-gel science and technology 1999-09, Vol.15 (3), p.221-230
Main Authors: Valentín, Carla, Muñoz, Mari Carmen, Alarcón, Javier
Format: Article
Language:English
Subjects:
Crystal structure
Crystals
Gelation
Gels
Lattice parameters
Reflectance
Silicon dioxide
Solid solutions
Sols
Ultraviolet reflection
Vanadium pentoxide
X ray powder diffraction
Zircon
Zirconium dioxide
Zirconium silicate
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Summary:A procedure is reported for the preparation of vanadium-doped zircon pigmenting system with different vanadia loadings which enabled their complete formation and further characterization. Vanadium-zircon solid solutions were prepared by gelling mixtures of ZrO2 and V2O5 colloidal sols and tetraethylorthosilicate and studied over the temperature range up to the formation of zircon. The reaction sequence of gels was evaluated by X-ray powder diffraction (XRD) and ultraviolet-visible (UV-Vis) diffuse reflectance. It was found that the first crystalline phase detected was a vanadium-containing tetragonal ZrO2 solid solution where vanadium was stabilized in the reduced V+4 state. The formation of the V-ZrSiO4 solid solution occurred by the reaction between the monoclinic form of V+4-ZrO2 solid solution and the amorphous silica phase. Energy dispersive X-ray microanalysis (SEM/EDX) data, measurements of lattice parameters and UV-Vis diffuse reflectance of V-ZrSiO4 solid solutions revealed that vanadium was dissolved as V+4 replacing Si+4 in tetrahedral sites in the crystal structure of zircon. The solubility limit of vanadium in ZrSiO4 was about 0.01 mole of vanadium per mole of zircon (0.5 wt% as V2O5).
ISSN:0928-0707
1573-4846
DOI:10.1023/A:1008784824917