Thesis. (M.Tech. (Chemistry)) -- Vaal University of Technology, 2011. / Bis(acetylacetonato)oxovanadium(IV), Manganese(III) acetylacetonate, Co-Zn and Co-Al were prepared as catalyst precursors for the synthesis of carbon materials in a catalytic chemical vapor deposition (CCVD) reactor. The carbon materials produced were characterized with Raman spectroscopy, Scanning electron microscope (SEM), Energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), High resolution transmission electron microscopy (TEM) and Thermogravimetric analysis, (TGA). Carbon material prepared from bis(acetylacetonato)oxovanadium(IV) catalyst precursor showed the presence of carbon spheres with average diameter of 104μm together with small traces of carbon nanotubes or amorphous carbon. Synthesis of bis(acetylacetonato)oxovanadium(IV) catalyst precursor yielded approximately 92% of carbon material. Carbon material prepared from Manganese(III) acetylacetonate catalyst precursor showed the presence of carbon spheres with diameter of 87.5μm. Synthesis of Manganese(III) acetylacetonate catalyst precursor yielded approximately 97% of carbon material. Carbon material produced from Co-Zn and Co-Al catalyst precursors showed the presence of carbon nanotubes with small amounts of amorphous carbon. The use of Co-Zn catalyst precursor yielded approximately 80% of carbon nanotubes, whereas Co-Al catalyst precursor yielded approximately 98% of carbon nanotubes. / Vaal University of Technology; NRF; SASOL