EN
Ni_3Fe nanoparticles prepared by calcination of the iron-nickel oxalate were investigated by X-ray diffraction, Mössbauer spectroscopy and magnetic measurements. The high temperature X-ray diffraction shows two stages of transformation of oxalate: (i) amorphization and (ii) formation of nanocrystalline Ni_3Fe particles. The development of coercivity, magnetization and mean coherence length ( ≈ particle size) is discussed.