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Mechanochemical changes in mixture of magnesium and aluminium hydroxides

Author(s): Števulová Nadežda | Luxová Mária

Journal: Acta Montanistica Slovaca
ISSN 1335-1788

Volume: 5;
Issue: 3;
Start page: 279;
Date: 2000;
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Keywords: amorphisation | mechanosynthesis | mechanochemical dehydration | spinel

Complex oxides with the spinel structure often called “spinels” belong to the group of strategic materials which are used in the wide area of modern technologies. They exhibit excellent magnetic, refractory, semiconducting, catalytic and sorption properties. Spinels based on magnesium aluminate (MA spinels) are used for the preparation of refractory ceramic materials and bricks. Due to its good properties MA spinel is predestinated for special applications in electronics.Several methods and precursors for the synthesis of MA spinel have been studied experimentally. The conventional process of MA spinel preparation based on the high temperature solid state reaction of precursors is connected with the difficulty to obtain the high spinel phase purity required for its special applications. From the viewpoint of final material properties and of intensification of solid state reactions, the non-standard mechanochemical techniques are suitable.In the paper, results of the mechanochemical modification of the mixture of crystalline hydroxide precursors caused by the high-energy milling and subsequent heating in the temperature range 300-1500 °C are presented.Mixtures of brucite and gibbsite in the molar ratio 1:2 were submitted to grinding in a planetary mill using the corundum chamber for various milling times (0.5-12 hours). The specific surface area of the milled samples was determined by the BET method. Changes in the structure of mechanosynthesized products and the evolution of the spinel phase during the subsequent calcination of both mechanosynthesized samples and reference homogenised mixtures were monitored by the X-ray diffraction analysis and IR spectroscopy. The degree of conversion of hydroxide mixture to the MA spinel was determined by chelatometry.During the early stage of grinding (up to 1 hour), a considerable refinement of hydroxide mixture occurs. With the increasing grinding time, amorphisation of structure as well as a gradual mechanochemical dehydration and formation of aggregates take place. A structural metastability of high reactive products of dehydration and a large area of particle contacts lead to the solid state mechanochemical reaction with the formation of nucleation centres of amorphous magnesium aluminate. By the combination of mechanosynthesis with the subsequent thermal treatment, crystalline magnesium aluminate with the spinel structure is prepared at temperatures which are by 300 K lower than those at which the spinel is synthesized by conventional ceramic method.
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