Hollow polyhedral graphite particles with 200~400 nm in diameter have been synthesized by heating oxalic acid, ferrocene and metallic magnesium at 580 °C, typically forming diamond-like octahedral structure. Combined with SEM, TEM, SAED patterns, and Raman spectroscopy, it was shown that the surface of graphite polyhedrons is composed of approximately 30-40 graphene shells; the four-or six-fold symmetric diffraction spots disclosed the nature of octahedral graphite particles; the edge of the graphite polyhedrons exists sp 3 -hybridized bonding, which would act as dangling bonds and localized defects in the polyhedron.