Positron lifetime measurements on different nanocrystalline iron samples sh
ow that the microstructure, with respect to the inherent free volumes in th
e samples, can be determined Three distinct defect types can be detected i)
a vacancy-like defect in the interface, ii) a microvoid at the intersectio
n of interfaces and iii) larger free volumes (missing grains) where the ann
ihilation of ortho-positronium is observed. The effect of the crystallite s
ize and preparation conditions of the samples are discussed (C) 1999 Acta M
etallurgica Inc.