Carbon nanomaterials have been prepared by the thermal chemical vapor deposition (CVD) method in which C2H2 gas was deposited on the Ni-Al(OH)(3) mixture pretreated by mechanochemical treatment with a high-energy mill. As the duration time of grinding for the Ni-Al(OH)(3) mixture by the mixer mill is increased, amorphous Al(OH)(3) and smaller Ni particles agglomerated into spheres. With unground and 120-min ground mixture of Ni-Al(OH)(3), carbon nanomaterials were prepared at 500 and 600 degreesC. As a result, carbon nanomaterials prepared on a ground mixture have more uniform morphologies than those of the unground mixture. The characterization of Ni-Al(OH)(3) mixture and as-prepared carbon samples was done by X-ray diffiractometer (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), Raman spectroscopy and current-voltage (I-P) measurement. (C) 2003 Elsevier Science B.V All rights reserved.