Carbon materials with different morphology were prepared by reacting CCl 4 and Mo at 873–1173 K. At 873–973 K, hollow spheres (diameter: 1–3 μm, shell thickness: 50 nm) were obtained. At 1073 K, particles (diameter: 50–100 nm) encapsulated in spherical shells (diameter: 1–5 μm) were collected. At 1173 K, formation of particles (diameter: 200–300 nm) was observed. Mo acted as a reagent to remove chlorine atoms from the carbon source and a template for the formation of the spherical structures. We propose that reaction temperature and polymerization of chlorinated species formed from the pyrolysis of CCl 4 affect the morphology of carbon products greatly.