Boron-doped carbon was prepared by the high-temperature reaction of B2O3 with the highly ordered pyrolytic graphite (HOPG). In order to reveal the effect of the boron doping on the HOPG structure. several experimental tools were employed such as X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning tunneling microscopy (STM). and atomic force microscopy (AFM). While the interlayer spacing of the graphite plane remains virtually unchanged, the boron doping makes the graphite plane of HOPG more disordered. Both the STM and the AFM studies show that the boron-doped HOPG Surface is deformed not only in its bonding geometry, but also in its electronic structure. The overall results imply that the boron atom is substituted for the carbon atom rather than is intercalated into the graphite layers. (C) 2001 Elsevier Science B.V. All rights reserved.