Among the various synthesizing technologies of carbon nanofibers (CNFs), chemical vapor deposition (CVD) technology, which uses hydrocarbon gas or carbon monoxide as a carbon source gas and pyrolyzes it to grow CNFs on transition metal catalysts, such as Ni, Fe, and Co, has been regarded as the most inexpensive and convenient method to produce CNFs for industrial use. Experimental variables for CVD are source gas, catalyst layers, temperature, and reaction time. Since the particle size of metal catalysts has an influence on the diameter of CNFs, it is possible to control the diameter of CNFs by varying particle sizes of the metal. As such, it is possible to synthesize CNFs selectively through the selective deposition of catalyst metals. In this study, CNFs were grown by CVD on C-fiber textiles, which had catalysts deposited via electrophoretic deposition. The CNFs were coated with a silica layer via hydrolysis of TEOS (tetraethyl orthosilicate), and the CNFs were oxidized by nitric acid. Due to oxidation, a hydroxyl group was created on the CNFs, which was then able to be used as an activation site for the SiO2. CNFs and the CNFs/SiO2 composite can be used in various applications, such as a composite material, electromagnetic wave shielding material, ultrathin display devices, carbon semiconductors, and anode materials of Li secondary batteries. In particular, there is an increasing demand for lightweight, small-scale, and high-capacity batteries for portable electronic devices, such as laptop computers or smart phones, along with the escalating concern of fossil energy depletion. Accordingly, CNFs and CNFs/SiO2 composites are receiving attention for their use as anode materials of Li secondary batteries, which are eco-friendly, lightweight, and high capacity. Therefore, the physicochemical properties and electrochemical performance data of synthesized CNFs and CNFs/SiO2 composite are described in this chapter
