J. Alarcon, Synthesis and characterization of vanadium-containing ZrO2 solid solutionspigmenting system from gels, J MATER SCI, 36(5), 2001, pp. 1189-1195
A procedure is reported for the synthesis of vanadium-doped zirconia pigmen
ting system with different vanadium loadings which permitted their complete
formation and further characterization. Monoclinic vanadium-zirconia solid
solutions were prepared by gelling mixtures of zirconium n-propoxide and v
anadyl acetylacetonate and studied over the range of temperature up to 1300
degreesC. Succesive steps of the reactions leading to the final monoclinic
vanadium-zirconia solid solution phase were investigated by X-ray powder d
iffraction. It was found that the formation of the monoclinic solid solutio
n took place by a phase transformation from a phase with the structure of t
etragonal zirconia. The transformation temperature of metastable tetragonal
to monoclinic phase was found to be governed by the nominal vanadium amoun
t. Measurements of lattice parameters of monoclinic vanadium-zirconia solid
solutions as a function of the nominal vanadium amount revealed that vanad
ium was dissolved in the zirconia lattice. Energy dispersive X-ray microana
lysis and lattice parameters variation indicates that the maximum amount of
vanadium into the monoclinic zirconia lattice was about 5 mol % of vanadiu
m (3.7 wt % as V2O5). UV-Vis diffuse reflectance of monoclinic V-ZrO2 solid
solutions indicated that vanadium was dissolved as V+4 and that the color
of vanadium-zirconia yellow pigments was produced by the dissolved vanadium
. (C) 2001 Kluwer Academic Publishers.