X-Ray Diffraction, and Raman Scattering Study of Nanostructured ZrO₂-TiO₂ Oxides Prepared by Sol-Gel

Authors: Manriquez, M.E.; Picquart, M.; Bokhimi, X.; López, T.; Quintana, P.; Coronado, J.M.

Source: Journal of Nanoscience and Nanotechnology, Volume 8, Number 12, December 2008 , pp. 6623-6629(7)

Publisher: American Scientific Publishers

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Abstract:

In the present work, we study the phase composition of ZrO₂-TiO₂ system by means of XRD and Raman spectroscopy, using also TG-ATD, and N₂ adsorption isotherms as complementary characterization techniques. TiO₂-ZrO₂ samples of selected compositions (0, 10, 90, 50 and 100% in weight of TiO₂) were prepared by sol-gel method and annealed at three different temperatures (400, 600 and 800 °C). Structural characterization reveals that only the pure oxides are crystalline at 400 °C: TiO₂ as anatasa with a minor brookite component, and ZrO₂ as a mixture of tetragonal (majority) and monoclinic phases. Following the 600 °C calcination, the TiO₂-ZrO₂ 50-50% sample forms the ZrTiO₄ mixed oxide, although this materials remains partly amorphous. In contrast, samples with higher and lower TiO₂ content form solid solutions with, respectively, anatasa and tetragonal ZrO₂ structures. Zirconium incorporation into the TiO₂ lattice leads to the expansion of the unit cell parameters, and it stabilizes the anatase phase, hindering its transformation into rutile. Similarly, dissolving titanium atoms into the ZrO₂ structure delays the transformation from the tetragonal to the monoclinic polymorph.

Keywords: TIO2; ZRO2; MIXED OXIDES; NANOPARTICLES; RIETVELD ANALYSIS; RAMAN SPECTROSCOPY; PHASE DIAGRAM

Document Type: Research article

DOI: http://dx.doi.org/10.1166/jnn.2008.041

Publication date: 2008-12-01

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