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Nitrogen‐substituted graphite thin films were prepared by chemical vapor deposition (CVD) using pyrrole as a starting material. Ni was used as the substrate material whose temperature was kept in the range 700–1000 °C. The interlayer spacing of these films, determined by x‐ray diffraction, was close to that of single‐crystal graphite. Two XPS peaks were observed in the N 1s spectra at around 398 and 401 eV. The former can be assigned to nitrogen atoms substituting for carbon atoms in the graphite layer and the latter to nitrogen atoms bonded to the layer edge. © 1994 American Institute of Physics.