Cone-stacked nanotubes with thick layers of deposited carbon obtained by a catalytic chemical vapor deposition method are annealed at high temperature. Phase separation between cone-stacked nanotubes and amorphous carbon layers occurs during annealing due to different structural transformation behaviors, resulting in the formation of multi-wall carbon nanotubes containing a cone-type multi-shell arrangement. The apex angles of the nanocones are about 40degrees. This type of carbon nanotube shows different physical and electrical properties. 2002 Elsevier Science B.V. All rights reserved.