Nested multiple-walled coaxial nanotube structures of transition metal oxides, semiconductors, and metals were successfully synthesized by atomic layer deposition (ALD) techniques utilizing nanoporous anodic aluminum oxide (AAO) as templates. In order to fabricate free-standing tube-in-tube nanostructures, successive ALD nanotubes were grown on the interior template walls of the AAO nanochannels. The coaxial nanotubes were alternated by sacrificial spacers of ALD Al(2)O(3), to be chemically removed to release the nanotubes from the AAO template. In this study, we synthesized a novel nanostructure with up to five nested coaxial nanotubes within AAO templates. This synthesis can be extended to fabricate n-times tube-in-tube nanostructures of different materials with applications in multisensors, broadband detectors, nanocapacitors, and photovoltaic cells.