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Characterization of aluminosilicate (mullite) precursors prepared by a mechanochemical process

Published online by Cambridge University Press:  31 January 2011

J. Temuujin ,
K. Okada  and
K. J. D. MacKenzie
J. Temuujin
Affiliation:
Institute of Chemistry of the Mongolian Academy of Sciences, Ulaanbaatar 51, Mongolia
K. Okada
Affiliation:
Department of Inorganic Materials, Tokyo Institute of Technology, 2-12-1 O-okayama, Meguro-ku, Tokyo 152, Japan
K. J. D. MacKenzie
Affiliation:
New Zealand Institute for Industrial Research and Development, Lower Hutt, New Zealand
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Abstract

Aluminosilicate precursors were prepared by mechanochemical treatment of gibbsitesilica gel mixtures. The effect of grinding on their structure and thermal behavior has been examined by 27Al and 29Si MAS NMR, x-ray diffraction (XRD), differential thermal analysis-thermogravimetry (DTA-TG), and Fourier transform infrared (FTIR). After 8 h grinding, the hydrated alumina was completely changed to an amorphous phase which showed a new exothermic DTA peak at about 980 °C due to the formation of γ–Al2O3 or spinel phase. This behavior was related to changes in the Al and Si environments, as deduced from the MAS NMR spectra. With increased grinding time, some 4-coordinated Al appears, together with an Al resonance at about 30 ppm. Simultaneously, a new Si resonance appears at about −90 ppm, indicating a greater degree of homogeneity in the ground samples. Mullite crystallizes at 1200 °C from samples ground for 8–20 h, its XRD intensity increasing with increased milling times, in agreement with the NMR, DTA, and FTIR data. Changes in the Al and Si environments during heat treatment, as reflected by the NMR spectra, are also reported.

Type
Articles
Information
Journal of Materials Research , Volume 13 , Issue 8 , August 1998 , pp. 2184 - 2189
Copyright
Copyright © Materials Research Society 1998

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References

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