Published online by Cambridge University Press: 31 January 2011
Glass-ceramic powders with a composition of Li2O · Al2O3 · 4SiO2 (LAS) have been synthesized by the sol-gel technique using LiOCH3, Al(OC2H5)3, Si(OC2H5)4, Ti(OC2H5)4, and Zr(OC2H5)4 as starting materials and the phase transformation behavior during calcination has been investigated. Differential thermal analysis (DTA), x-ray diffraction (XRD), and scanning electron microscopy (SEM) were utilized to determine the thermal behavior of the gels. Considering the LAS gels with 6.0 wt. % TiO2 and various wt. % ZrO2 content, and peak position of the β-spodumene phase formation in DTA curves was shifted to a higher temperature when the ZrO2 content was increased. The activation energy of β-spodumene crystallization was 283.8 kcal/mol for LAS gels with 6.0 wt. % TiO2 and 2.0 wt. % ZrO2. Unlike foregoing studies for LAS gels, during calcination of the dried LASTZ gels from 800 °C to 1200 °C neither β-eucryptite nor γ-spodumene was noted to be present. The crystallized phases comprised of β-spodumenes as the major phase and rutile (TiO2) together with zirconia (ZrO2) are precipitated as minor phases.