The grain boundary excess volume, i.e., the grain boundary expansion, e{GB}, was experimentally determined for high-angle grain boundaries in nickel using the direct technique of high-precision difference dilatometry. Values of e{GB}=(0.35±0.04)×10{-10}  m and e{GB}=(0.32±0.04)×10{-10}  m were obtained by measuring the removal of grain boundary volume upon grain growth for two different types of ultrafine-grained samples. The results are discussed in comparison to values obtained so far from indirect techniques and from computer simulations. It demonstrates the strength of the presented novel, direct approach for grain boundary expansion measurements.

No abstract

A maximum excess volume ΔV/V ≈ 1.9 × 10−3 in ultrafine-grained Fe prepared by high-pressure torsion is determined by measurements of the irreversible length change upon annealing employing a high-resolution differential dilatometer. Since dislocations and equilibrium-type grain boundaries cannot fully account for the observed released excess volume, the present study yields evidence for a high concentration of free volume-type defects inherent to nanophase materials, which is considered to be the main source of their particular properties, such as strongly enhanced diffusivities.

The release of excess volume upon recrystallization of ultrafine-grained Cu deformed by high-pressure torsion (HPT) was studied by means of the direct technique of high-precision difference dilatometry in combination with differential scanning calorimetry (DSC) and scanning electron microscopy. From the length change associated with the removal of grain boundaries in the wake of crystallite growth, a structural key quantity of grain boundaries, the grain boundary excess volume or expansion eGB=(0.46±0.11)×10-10 m was directly determined. The value is quite similar to that measured by dilatometry for grain boundaries in HPT-deformed Ni. Activation energies for crystallite growth of 0.99±0.11 and 0.96±0.06eV are derived by Kissinger analysis from dilatometry and DSC data, respectively. In contrast to Ni, substantial length change proceeds in Cu at elevated temperatures beyond the regime of dominant crystallite growth. In the light of recent findings from tracer diffusion and permeation experiments, this is associated with the shrinkage of nanovoids at high temperatures.

No abstract

No abstract

A model is proposed for directly determining the volume of lattice vacancies by means of dilatometric measurements of the anisotropic irreversible length change which occurs during annealing of lattice vacancies at grain boundaries of shape-anisotropic crystallites. The model is tested using nanocrystalline Ni after the high-pressure torsion deformation which exhibits excess concentration of lattice vacancies and elongated crystallite shape. Different length changes upon annealing parallel and perpendicular to the elongation axis occur from which a vacancy volume can be derived.

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.