Positron annihilation spectroscopy on nanocrystalline Pd85Zr15 shows the segregation of Zr at the interfaces and a decrease of the fraction of nanovoids the size of 10 to 15 missing atoms upon isochronal annealing up to Ta=1100 K by which the grain size increases up to d=185 nm. In this state, the positron trapping at interfacial free volumes reversibly changes contingent upon the temperature whereas the interfacial composition is unchanged when the measuring temperature varies.

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