Gallium oxide hydroxide (GaOOH.xH(2)O) single crystals were synthesized in aqueous solutions by using two different precipitation techniques: homogeneous decomposition of urea and forced hydrolysis in pure water. Precipitation of crystals started at exactly the same pH value (i.e., 2.05 at 85degreesC) in both cases. The morphology of crystals turned out to be quite different (zeppelin-like with urea, rodlike without urea) in each of the above methods. Calcination of these gallium oxide hydroxide crystals in air at temperatures greater than or equal to500degreesC transformed them into Ga2O3. Characterization of the samples was performed by X-ray diffractometry, scanning electron microscopy, thermogravimetry/differential thermal analysis, Fourier transform infrared spectroscopy, and ICP, carbon, and nitrogen analyses.