Aerosol Synthesis of Fullerene Nanocrystals in Controlled Flow Reactor Conditions

Abstract

Fullerene nanocrystals in the size range 30–300 nm were produced starting from atomized droplets of C₆₀ in toluene. The experiments were carried out under well-controlled conditions in a laminar flow reactor at temperatures of 20–600°C. Particle transformation and crystallization mechanisms of polydisperse and monodisperse (size classified) fullerene aerosol particles were studied. The results show that fullerene particles are roughly spherical having pores and voids at temperatures of 300°C and below. Particles are already crystalline and likely fine-grained at 20°C and they are polycrystalline at temperatures up to 300°C. At 400°C monodisperse particles evaporate almost completely due to their low mass concentration. Polydisperse particles are crystalline, but sometimes heavily faulted. At 500°C most of the particles are clearly faceted. In certain conditions, almost all particles are hexagonal platelets having planar defects parallel to large (111) faces. We suggest that at 500°C fullerene particles are partially vaporized forming residuals with lamellar defects such as twins and stacking faults, which promote crystal growth during synthesis. Subsequently fullerene vapor is condensed on faces with defects and hexagonal particles are grown by a re-entrant corner growth mechanism. At 600°C particles are single crystals, but they have a less distinct shape due to higher vaporization of fullerene. The final size and shape of the particles are mainly determined at the reactor outlet in the short time when the aerosol cools.