Fe0.65Ni0.35-MgO nanocomposite powders containing approximately 11 wt.
% of metallic phase were prepared by selective reduction of oxide soli
d solutions elaborated by thermal decomposition of mixed oxalic precur
sor The reduction behavior of the oxide solid solution calcinated at 8
00 degrees C was investigated by XRD, Fe-57 Mossbauer spectroscopy and
TEM. These studies have revealed that a reduction temperature of 1300
degrees C is needed to obtain a high reduction rate and to prepare al
loy particles of the desired composition. The metallic alloy particles
dispersed in the MgO matrix have a bimodal size distribution: the lar
ger ones (average size from 50 to 90 nm) are approximately spherical a
nd are located at the surface of the MgO grains; the smaller ones (ave
rage size from 5 to 13 nm) are spherical or cubic and generally grow e
pitaxially inside the oxide grains. (C) 1997 Acta Metallurgica Inc.