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Investigation of the formation of magnesium titanate phases from xerogels using hot stage X-ray powder diffractometry

Jacob Zabicky 1Giora Kimmel 1Elena Goncharov 1Francesc Guirado 2

1. Ben-Gurion University of the Negev, P.O.Box 653, Beer-Sheva 84105, Israel
2. Universitat Rovira i Virgili (URV), Av. Països Catalans, 26, Tarragona 43007, Spain


Coprecipitated xerogel precursors of nanocrystalline magnesium titanates, with Mg:Ti stoichiometric ratio varying from 1:1 to 2:1, were subjected to thermal treatment at constant temperature in the range from 550 to 1200 °C, in air, using a hot-stage X-ray powder diffractometer. The kinetics during the first hour of the process showed dependence on the temperature and the Mg:Ti stoichiometric ratio of the precursor. At low temperatures, for compositions near 2:1, a single nonstoichiometric metastable nanocrystalline qandilite-like phase is formed; however, when the Mg content is lowered a solubility limit is reached, after which a nonstoichiometric qandilite, of fixed composition depending on the temperature, is in equilibrium with stoichiometric geikielite. The limit moves to higher Mg contents as the temperature rises. In the approximate 900-1000 °C range the metastable qandilite phases decompose into geikielite and periclase. At 1100 °C and above stoichiometric qandilite is obtained in equilibrium with geikielite. At low temperatures nanocrystalline qandilite is formed much faster than nanocrystalline geikielite, probably owing to the isotropic chemical structure of both the amorphous xerogels and qandilite. A phase diagram is proposed for the metastable nanocrystalline phases formed at low temperatures in the composition range of the present study.


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Submitted: 2008-04-21 22:19
Revised:   2009-06-07 00:48