Nanocrystalline Fe
xNi
1−x alloys (
x = 0.15, 0.20, 0.22, 0.25, 0.30, 0.50 and 0.65) were produced by a wet chemical method. The metal concentration ratios in the solutions were preserved in the precipitated pow
der alloys and no metal segregation was
detected. The FCC phase was observed from
x = 0.15 to 0.50. For
x = 0.65 both FCC and BCC phases were observed. The materials obtained consist of nanoparticles with a mean diameter of 90 nm. The latter are composed of several nanocrystallites surroun
ded by a low
density structurally disor
dered region. The crystallite size in the FCC phase increased as the at. % Fe
decreased from
der=0>10 nm for
x = 0.50 to
der=0>20 nm for
x = 0.15. A different thermal behavior was observed for the
x = 0.50 in comparison to the
x = 0.22 sample.