Molybdenum powder was ball milled in a steel vessel with hardened steel bal
ls under Ar, O-2 and N-2 atmosphere, respectively. The milling products wer
e examined by chemical analysis, X-ray diffraction and neutron diffraction.
During milling under Ar or O-2 the iron as well as the oxygen content of t
he samples increases dependent on the number of interruptions of the millin
g process. The presence of dissolved oxygen seems to facilitate the solubil
ity of iron in the molybdenum powder. Milling in a nitrogen gas atmosphere
results in the formation of a nanocrystalline cubic gamma -Mo2N phase and a
Mo-rich amorphous-like grain boundary phase. The microstructural imperfect
ion was characterised by X-ray diffraction-line profile analysis. A method
was proposed for the evaluation of the crystallite size and the microstrain
in nanocrystalline materials, as well as the amount and structure of disor
dered grain boundaries from the reduced pair correlation function. (C) 2001
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d.