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Abstract: Nanocrystalline Mo2C powders were successfully synthesized at 500°C by reacting molybdenum chloride (MoCl5) with C (graphite or carbon nanotube) in metallic sodium medium. X-ray powder diffractometer (XRD), transmission electron microscope (TEM), X-ray photoelectron spectroscope (XPS) and surface area analyzer (BET method) were used to characterize the samples. Experiments reveal that the carbon source used for the carbide synthesis has a great effect on the particle size and the surface area of the samples. When micro-sized graphite was used as C source the obtained nanocrystalline Mo2C powder consists of particles of 30∼100nm, with a surface area of 2.311m2/g. When carbon nanotubes were used as C source, the as-synthesized Mo2C sample is composed of particles of 20∼50nm, with a surface area of 23.458m2/g, which is an order of magnitude larger than that of the carbide prepared from the graphite. [Copyright &y& Elsevier]