This work was carried out in order to prepare precursor powders with a spodumene composition (Li2O . Al2O3 . 4SiO(2), LAS) and to investigate their crystallization behaviours during calcination. A fine beta-spodumene type amorphous powder was obtained through set-gel techniques using LiOCH3, Al(OC2H5)(3), Si(OC2H5)(4) and Zr(OC2H5)(4) as the starting metal alkoxides. The process included well controlled hydrolysis polycondensation of the raw alkoxides. Differential thermal analysis (DTA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED) analyses were utilized to study the crystallization behaviour of the gels. The activation energy of beta-spodumene crystallization was 192 kJ mol(-1) for LAS gels with 4 wt % ZrO2, being much smaller than those of LAS gel without ZrO2, 382 kJ mol(-1). For calcination at 800-1200 degrees C, the crystallized phases comprised a major phase of beta-spodumene and a minor phase of zirconia (ZrO2).