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Nb3Al nanoparticles were directly synthesized by metallothermic reduction process in the molten salts with mNbCl5–nAlCl3 powders as raw materials and sodium as reducing reagent. The effects of different feeding material orders, soaking time, Nb content in raw materials, and 3NbCl5–AlCl3 content in molten salts on the obtained Nb3Al powder were discussed. The as-prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). It is found that the only phase Nb3Al nanoparticles are obtained by controlling the variation of the feeding material orders, soaking time, and Nb content in raw materials. And the morphologies of as-prepared nanoparticles change owning to different 3NbCl5–AlCl3 contents in molten salts. [ABSTRACT FROM AUTHOR]