The preparation of well-defined nanomaterials using template methods is well established in the materials literature including porous ceramics, open-framework layered structures and porous membranes. In an effort to prepare thermally and electrically conductive nanowire and nanotube materials, we have recently prepared carbon tubes using polymer fibers produced from an electrostatic, non-mechanical “electrospinning” process as templates. Poly(methyl methacrylate) (PMMA) fibers with average diameter of 150–200 nm were initially fabricated as core materials. The fibers were subsequently coated with a thin layer (20∼50 nm) of conductive polypyrrole (PPy) by in-situ polymerization. Upon high temperature (1000 °C) treatment under inert atmosphere, the PMMA core fibers decomposed completely, followed by carbonization of the PPy wall. The structure of the carbon tubes subsequently produced was demonstrated by SEM and TEM. The carbon tubes were analyzed by infrared, elemental analysis and electron diffraction. The results show that the tubes are largely carbon with a small amount of nitrogen and a relatively low crystallinity.