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Adoption of powder-in-tube method to fabri-cate superconducting wire can realize a large application of Nb3Al prepared by powder metallurgy. Powder metallurgy was used to synthesize Nb3Al under various heat-treatment conditions, annealing temperature was varied from 700 to 1,000 ?C and heating time was varied from 10 to 50 h. X-ray diffraction patterns reveal that a reaction between Nb and Al took place and formed NbAl3 phase. Under current heat-treatment conditions (annealing temperature was varied from 700 to 1,000 ?C and heating time was varied from 10 to 50 h), NbAl3 was so stable that it did not further react with the unreacted Nb and was not sensitive to the heat-treatment condition. By mechanical alloying, adoption of high-energy ball milling significantly decreases particle size and enhances surface free energy, which promotes the formation of Nb3Al phase. X-ray diffraction patterns indicate that relatively pure Nb3Al phase was obtained under the same heat-treatment condition. Energy-disper-sive X-ray analysis measurement demonstrates that the obtained samples were close to the right stoichiometry of A15 structure Nb3Al.