Nanostructured materials are predicted to possess unique physical, chemical, and electronic properties, which have made them attractive for a variety of applications. We have been fabricating metal-carbon composite fibers of Au, Ni, Cu, and Ag prepared via electrospinning process. These high aspect ratio materials have diameters on the order of two hundred nanometers and a uniform, contact-free distribution of nanoparticles on the surface of the carbonized fibers with particle size range of 3 nm – 10 nm. An enhancement in thermal conductivity was observed which has been attributed to the incorporation of metal nanoparticles in the fiber matrix and on the surface of carbon fibers. Integration of these nanostructured materials into real devices can be realized by their incorporation into a matrix. Nanostructured samples were incorporated into industrial epoxy in order to determine thermal conductivity of the materials in situ as thermal interface materials. The resulting nanocomposite at 1 wt% was polished through standard polishing techniques ending with a 6-micron diamond finish. Scanning thermal microscopy study showed that the measured thermal conductivity values are one order of magnitude higher than the commercially available thermal interface materials (TIMs).