CO2 laser pyrolysis has been used to synthesize carbon black (particle diameter ∼30 nm) via a catalytically driven pyrolysis of benzene vapor. The H : C ratio is found to be ∼1 : 10, which is unusually high for carbon blacks. Subsequent heat treatment of the “laser black” to temperatures up to ∼2800 °C produces well-graphitized faceted particles with central polygonal cavities. High resolution TEM lattice imaging, Raman scattering, and x-ray diffraction have been used to characterize the morphological structure of these carbon particles in their as-synthesized and heat-treated forms. Furthermore, KOH treatment at ∼800 °C has been employed to activate the as-synthesized particles, producing a tenfold increase in the surface area from 50 to 700 m2/g. Possible pore structures generated during this activation process have been identified by high resolution TEM imaging.