Nanocrystalline boron carbide (B 4 C) was synthesized via a solvothermal reduction of carbon tetrachloride using metallic lithium as reductant in the presence of amorphous boron powder at 6001C in an autoclave. The X-ray diffraction pattern of the product powder was indexed to the hexagonal B 4 C phase, with lattice constants a 5 5.606 and c 5 12.089 Å . The sample was also characterized by Raman spectrum, X-ray photoelectron spectroscopy and inductively coupled plasma atomic emission spectrometry. Transmission electron microscopy revealed that the B 4 C nanocrystallites were slightly agglomerated, with a particle size of approximately 15-40 nm in diameter.