A new vertical floating catalytic technique is developed and used to prepare both single-walled carbon nanotubes (SWNTs) and carbon fibers (CFs). Scanning electron microscopy (SEM) observation shows a clear separation of these two materials. Thin films of SWNTs can be peeled easily from the CF substrate which just acts as a catalyst support for the SWNT growth. The production process is also semicontinuous, resulting in a yield of ~1.0gh - 1 of SWNTs film with high purity. Structure and vibrational properties of these materials are investigated by electron microscopy and Raman spectroscopy, respectively.