Mossbauer spectroscopy and X-ray diffraction were used to investigate the s
ynthesis of nanocomposite powders by reactive milling of a variety of blend
s of aluminium and metallic oxides corresponding to the target compositions
: Al2O3-(Fe,Cr,Ni) alloys. Particular emphasis was given to the (Fe,Cr) and
(Fe,Ni) binaries with chromium contents ranging between 0.13 and 0.60 and
nickel contents between 0.10 and 0.80, respectively. Several compositions i
n the iron-rich part of the ternary with chromium in the 0.18-0.20 range we
re also investigated. The essential steps of the reaction mechanisms were i
dentified as functions of milling time and initial composition. A number of
transient phases, some metastable under normal conditions at room temperat
ure were observed. Chemical heterogeneities and their changes in the metall
ic phases were also characterized semi-quantitatively and the possibility o
f side effects, such as partial dissolution of not yet reacted Cr2O3 into n
ewly formed Al2O3, was considered. Finally, some of the as-milled powders w
ere subsequently heat treated for 1 h at 1100 degrees C to explore their st
ructural changes and progress towards homogenization via the same experimen
tal techniques. (C) 1998 Kluwer Academic Publishers.