The synthesis of an alloy with the composition of 58% Nb, 24% V i 18% Al (a
tomic %) has been performed. The mechanical alloying of elemental powders w
as selected as a method of synthesis. During the course of mechanical alloy
ing the splitting of X-ray peaks on two components was observed. Each compo
nent corresponded to the niobium solid solution (Nb-I and Nb-II) with diffe
rent lattice parameters and different chemical composition. The Nb-I solid
solution and the pure niobium had alike lattice parameters. The intensity o
f peaks corresponding to the Nb-I decreased with the time of milling. The p
eaks disappeared completely after 180 hours of milling. The lattice paramet
er of the Nb-II solid solution decreased with milling time and the intensit
y of corresponding peaks increased. Two brittle phases: Nb3Al-base with A15
crystal structure and Nb2Al-base sigma phase were observed in solid (conso
lidated) material. No phase with B2 crystal structure was observed.