The effect of high energy ball milling on the structural refinement of the binary system Ag-Fe has been studied by Transmission and Scanning Electron Microscopy, Small Angle Neutron Scattering and Mössbauer spectroscopy. Samples containng 10 wt% of Fe were submitted to high energy ball milling for times up to 50 hours. The process produces a fine dispersion of Fe into the Ag matrix; the size distribution function is quite broad with an average radius of the order of a few nm. The minimum average particle size is obtained after about 10 hours of milling, longer term processing leads to a detectable particle coarsening. TEM analyses give evidence of a well defined orientation relationships between the Fe particles and the Ag matrix. Mössbauer spectroscopy reveals a modification of the hyperfine field experienced by the Fe atoms only for short term milling. On the basis of the experimental results one can assume that the fine dispersion of Fe into the Ag matrix occurs by mutual solubilisation probably induced by plastic shear, followed by fast decomposition by precipitation. After this step, further milling can induce only coarsening of the microstructure.

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