Nanocrystalline yttrium aluminum garnet (YAG, Y(3)AI(5)O(12)) was synthesized by pyrolysis of complex compounds of aluminum and yttrium with triethanolamine [(HOCH2CH2)(3)N, (TEA)]. Loose and porous precursor was obtained on complete dehydration of the metal ion-triethanolamine complexes. Pure YAG powder was obtained by calcination of the precursor at 950degreesC. The precursor was characterized by simultaneous thermogravimetry, differential scanning calorimetry, and mass spectra analyses (TG-DSC-MS). The heat-treated powders were characterized by X-ray diffractometry (XRD), specific surface area measurements, and transmission electron microscopy (TEM). The average crystallite size as determined from X-ray line broadening and transmission electron microscopy studies was similar to40 nm. The effects of the calcination temperature and the ratio of triethanolamine to mixed metal ions were also studied.