Straightforward synthesis of Ti-doped YSZ gels by chemical modification of the precursors alkoxides
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Translucent, homogeneous, and monolithic gels of the [(ZrO2)0.92(Y2O3)0.08]1−x(TiO2)x system, where x = 0, 0.05, 0.08, and x = 0.10 (mol), have been reliably obtained, for the first time, by a sol–gel route from zirconium (IV) n-propoxide (Zr(OPrn)4), yttrium acetate hydrate and titanium (IV) isopropoxide (Ti(OPri)4). Chemical modification of both alkoxides, zirconium (IV) n-propoxide and titanium (IV) isopropoxide, by acetic acid allows us to change the hydrolysis and condensation behavior of them. Their modification implies the formation of chelating and bridging acetates avoiding the formation of precipitates. The line width and some shoulders in the FT-IR spectra of the solution, resulting of the mixture of the precursors and the catalysts, during the hydrolysis reaction suggest that both coordinations, chelating and bridging, should occur. Furthermore, the separation of the steps of hydrolysis and condensation allows to achieve conditions under which hydrolysis of the molecular precursor is slowed, whereas condensation is promoted under chemical reversibility to ensure a crystalline product at low calcination temperatures. In addition, the formation of metalloxane bondings (M–O–M’, M and M’ = Zr, Y, and Ti) has been confirmed by FT-IR throughout the sol–gel process. At about 630 °C, the crystallization of yttria stabilized zirconia (YSZ) for x = 0 or a titania-doped yttria stabilized zirconia solid solution (Ti-doped YSZ) for x = 0.05, 0.08, and 0.10 is detected by DTA-TG. By SEM-EDX and TEM-EDX the presence of Zr, Y, and Ti elements, in the adequate proportions according to the nominal compositions, has been proven in both dried and calcined gels.
KeywordsTi-doped YSZ Sol–gel Alkoxides Acetic acid FT-IR SOFCs
This work has been supported by MINECO (Spanish Government) through the MAT2009-14369-C02-01 and MAT2012-31090 projects. I wish also to thank Dr. M.J. Velasco for her useful suggestions and to Mrs. C. Díaz-Dorado for the composition of micrographs and figures of this work.
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