Carbon nitride powder with an atomic N/C ratio of 1 has been prepared by reaction of cyanuric chloride with sodium metal. X-ray diffraction, Fourier transform infrared spectra, and x-ray photoelectron spectroscopic data provide substantial evidence for a graphite-like sp²-bonded structure composed of building blocks of s-triazine rings bridged by carbon-carbon atoms in the bulk carbon nitride. The electron-microscopy results reveal that the material is spherical particles with an average diameter of 50 nm. The optical properties and thermal stability are also characterized. Based on the experimental results, it is deduced that the structure of as-prepared material carbon nitride has polyether structure.