Vacuum carbonization of nanometer tungsten powder was investigated in a simple designed apparatus. An X-Y recorder was used to plot differential thermal analysis (DTA) curves to determine starting temperature of carbonization of four samples with different specific surface area. The product was detected by X-ray Diffraction (XRD) and small angle X-ray scattering (SAXS). The results show that finer tungsten powder has lower starting temperature of carbonization. Tungsten powder, which BET surface area is , is completely carbonized to tungsten carbide at , although the starting temperature is . Particle grows sharply before carbonization.