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We present a route to synthesize polyacetylene filled multi-walled carbon nanotubes (MCNT) by in situ polymerization. We use supercritical carbon dioxide to fill the nanotubes with toluene and then add the Ziegler-Natta catalyst. In order to assure controlled polymerization inside the nanotube, the catalyst outside is removed before the reaction. The resulting polyacetylene filled nanotubes are characterized by H-1 NMR and scanning electron microscope. (c) 2005 Elsevier B.V. All rights reserved.