Amorphous and nanostructural Fe-B alloys made by mechanical alloying of ele
mental Fe and amorphous B powders have been studied using X-ray diffraction
, differential scanning calorimetry and Mossbauer spectroscopy. It has been
shown that the milling conditions have a strong effect on the alloying. Th
e single phase amorphous alloy, which is limited at nominal composition of
Fe60B40, has been produced only by milling in Ar atmosphere and in other co
mposition range the mixture of nanostructure Fe-like phase and Fe2B compoun
d with a little amorphous phase are obtained. While by milling in air atmos
phere the introduction of oxygen in air may suppress the formation of amorp
hous phase, thus the compounds Fe2B may be synthesized with no trace of amo
rphous phase. The crystallization temperatures of amorphous phase in the re
sultant products are higher than those of a single amorphous alloy Fe60B40,
and hardly independent of the milling conditions and the composition. In a
ddition, it is revealed that detectable B content in the final products is
lower than the nominal composition of all the initial samples, which indica
tes that some B atoms may be located in the disordered interfacial regions
of the nanostructural alloyed mixtures.