In the past decades, the development of nano- carbon materials with well-defined characteristics such as fullerenes, nanotubes and graphene have been a very active area of research. Carbon nanospheres (CNSs) are other class of nanostructured carbon materials, and have shown good prospects for application as alternative LIB anodes. CNSs possess some remarkable characteristics such as high specific capacity and good rate capability as anode materials in LIB. Those specific characteristics are attributed to a combination of several factors, including a short diffusion paths for Li⁺ ions; good porosity and high surface area. In this study, carbon nanospheres (CNSs) were synthesized by thermal assisted pyrolysis process using palm oil as carbon precursors, Fe-catalyst and activated carbon support. Prior to the synthesis of carbon nanospheres, Fe-catalyst on carbon supports was prepared by deposition precipitation by varying the amount of catalyst (10%, 20% and 30% w with respect to the mass of carbon support). The effect of catalyst amount on the morphology and structural characteristics of carbon products was investigated by x-ray diffraction (XRD), Raman spectroscopy and transmission electron microscope (TEM). The study indicated that structural properties are changed when a Fe catalyst amount is increased from 10 to 30 wt%. The stable cycle performances of carbon products were demonstrated when they are utilized as anode materials in lithium ion batteries. However, it can be observed that the highest specific capacity was shown by the carbon samples produced at the highest content of Fe catalyst.