A solvothermal method has been successfully applied to prepare crystalline carbon nitride from C(3)N(3)Cl(3) and NaN(3) in CCl(4) at 180 degrees C without any catalyst. The final product was a reddish brown powder. X-ray diffraction pattern indicated that the prepared powder was well-crystallized graphitic carbon nitride. The atomic N/C ratio determined by combustion method was 1.63, indicating a high nitrogen concentration. XPS and FTIR studies showed that graphite-like sp(2) bonded structure existed in the sample. Nanometer scale spherical particles and crinkly lamellas were found in the TEM morphologies. (C) 2008 Elsevier Ltd. All rights reserved.