In this paper, carbon spheres were synthesized by CVD method. These carbon spheres exhibit diameters of about 200 nm. Thermal gravimetric analysis indicated the good stability in high temperature of the carbon spheres. The products were treated by microwave plasma and high temperature vacuum heat treatments respectively. The products were characterized by X-ray diffraction, Raman spectroscopy and Field Emission Scanning Electron Microscope. The study indicated that the original products, with perfect morphology and low graphitization degree, were converted to crystal. The different techniques were considered for the influence on the graphitization degree.