In the present research we employed the newly developed cryosol techni
que for the preparation of nanocrystalline Al(OH)(3). The technique yi
elds sols of aluminum hydroxide stable under a wide range of pH values
and concentrations. Freeze-drying of the sols results in the formatio
n of aluminum hydroxide powders with extremely low density and small p
article size. Thermal behavior and phase evolution of the cryosol-deri
ved aluminum hydroxide has been studied. According to X-ray diffractio
n data, annealing of cryosol-derived aluminum hydroxide results in amo
rphous alumina stable up to 800 degrees C. However DTA, electron diffr
action, and Al-27 NMR studies indicate that the samples amorphous to X
-ray diffraction are composed of crystalline nanoparticles. The therma
l stability of nanocrystals is supposed to be due to the high uniformi
ty of the particles size distribution, the latter resulting from the s
ynthetic method employed.