Free volumes in bulk nanocrystalline metals studied by the complementary techniques of positron annihilation and dilatometry.

Free-volume type defects, such as vacancies, vacancy-agglomerates, dislocations, and grain boundaries represent a key parameter in the properties of ultrafine-grained and nanocrystalline materials. Such free-volume type defects are introduced in high excess concentration during the processes of structural refinement by severe plastic deformation. The direct method of time-differential dilatometry is applied in the present work to determine the total amount and the kinetics of free volume by measuring the irreversible length change upon annealing of bulk nanocrystalline metals (Fe, Cu, Ni) prepared by high-pressure torsion (HPT). In the case of HPT-deformed Ni and Cu, distinct substages of the length change upon linear heating occur due to the loss of grain boundaries in the wake of crystallite growth. The data on dilatometric length change can be directly related to the fast annealing of free-volume type defects studied by in situ Doppler broadening measurements performed at the high-intensity positron beam of the FRM II (Garching, Munich, Germany).

In situ probing of fast defect annealing in Cu and Ni with a high-intensity positron beam.

A high-intensity positron beam is used for specific in situ monitoring of thermally activated fast defect annealing in Cu and Ni on a time scale of minutes. The atomistic technique of positron-electron annihilation is combined with macroscopic high-precision length-change measurements under the same thermal conditions. The combination of these two methods as demonstrated in this case study allows for a detailed analysis of multistage defect annealing in solids distinguishing vacancies, dislocations, and grain growth.