Carbon Nanospheres (CNSs) have been synthesized by thermal pyrolysis method. A mixture of Fe-catalyst supported activated carbons and palm oil was used in the furnace to produce CNSs. Prior to the synthesis of CNSs, Fe-catalyst was deposited onto the surface of activated carbons by wet incipient impregnation method. The ratio of carbon support and palm oil was varied (1:1, 1: 2 and 1:3) to obtain CNSs. The characteristics of produced CNSs were then evaluated with BET surface area analysis, pore size distribution analysis, scanning electron microscope (SEM), transmission electron microscope (TEM) and X-ray photoelectron spectroscopy (XPS). It was found that some impurities were still found in the CNSs in the forms of iron oxide and amorphous carbons.