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Mechanical alloying (MA) was employed to produce supersaturated solid solutions of Fe1-xCux,which is virtually immiscible under an equilibrium condition at ambjent temperature. The X-ray diffraction results show that the solutions formed in the concentration ranges of x≤0.1 5 and x≥0.40 are of bcc structure of iron and fcc structure of copper. respectively. For the region in between.however, the alloy obtained is a mixture of bcc plus fcc phases. The Mossbauer spectrum of the solid solution of a single phase could be fitted by two sub-spectra with hyperfine magnetic fields of 200 and 250 kOe. respectively. suggesting that there must exist two forms of coordination in the solution. While to fit the spectrum for the solution with mixed structu re. three Sub-spectra. including a spectrum of α-Fe, should be used. The variation of the Mossbauer spectra of Fe60Cu40 with milling time as well as annealing temperature was systematically studied. This may be ascribed to the changes of the number of nearest neighboring atoms of iron in the processes of formation and decomposition of the solid solution during milling and annealing

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