Ti-Al nanoparticles and have been synthesized by the flow-levitation (FL) method. The morphology, crystal structure and chemical composition of Ti-Al nanoparticles obtained were investigated by transmission electron microscopy, X-ray diffraction and induction-coupled plasma spectroscopy. Results showed that the average grain size of these nanoparticles is about 30 nm, and it can be controlled availably by altering procedure parameters. The structure of powder is mainly double phase Ti-Al particulate composite. In addition, there are certain corresponding relation between the compositions of evaporate source master material and phase composition of alloy compound nanoparticle. The expected nanoparticle, which is mainly composition of nanocrystalline intermetallic compound, can be obtained through changing the compositions of evaporating source mastermaterial.