Well-crystallized graphitic carbon nitride (g-C3N4) nanocrystallites have been prepared via a novel benzene-thermal reaction between C3N3Cl3 and NaNH2 at 180-220 degreesC for 8-12 h. X-ray diffraction patterns strongly indicated that the synthesized carbon nitride is g-C3N4. Transmission electron microscopy images reveal that the product mainly consists of particles with coexistence of minor hollow balls, and square frameworks. The atomic N/C ratio (1.39) determined by X-ray photoelectron spectroscopy analysis is good agreement with the C3N4 stoichiometry. The chemical bonding and optical properties of the sample have been investigated by Fourier transform infrared spectroscopy, UV, and photoluminescence spectrum. (C) 2003 Elsevier B.V. All rights reserved.