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Plastic deformation in coarse-grained metals is governed by dislocation-mediated processes. These processes lead to the accumulation of a residual dislocation network, producing inhomogeneous strain and an irreversible broadening of the Bragg peaks in x-ray diffraction. We show that during plastic deformation of electrodeposited nanocrystalline nickel, the peak broadening is reversible upon unloading; hence, the deformation process does not build up a residual dislocation network. The results were obtained during in situ peak profile analysis using the Swiss Light Source. This in situ technique, based on well-known peak profile analysis methods, can be used to address the relationship between microstructure and mechanical properties in nanostructured materials.

The evolution of the grain structure, internal strain, and the lattice misorientations of nanoporous gold during dealloying of bulk (3D) Ag-Au alloy samples was studied by various in situ and ex situ X-ray diffraction techniques including powder and Laue diffraction. The experiments reveal that the dealloying process preserves the original crystallographic structure but leads to a small spread in orientations within individual grains. Initially, most grains develop in-plane tensile stresses, which are partly released during further dealloying. Simultaneously, the feature size of the developing nanoporous structure increases with increasing dealloying time. Finally, microdiffraction experiments on dealloyed micron-sized nanoporous pillars reveal significant surface damage introduced by focused ion beam milling.

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We demonstrate real-time resolved white beam Laue diffraction during compression of micron-sized focused ion beam milled single crystals Au pillars, revealing the dynamical correlation between microstructure and plasticity. The evolution of the Laue patterns of the Au pillars demonstrates the occurrence of crystal rotation and strengthening is explained by plasticity starting on a slip system that is geometrically not predicted but selected because of the character of the preexisting strain gradient.

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While propagation of dislocations in body centered cubic metals at low temperature is understood in terms of elementary steps on {110} planes, slip traces correspond often with other crystallographic or non-crystallographic planes. In the past, characterization of slip was limited to post-mortem electron microscopy and slip trace analysis on the sample surface. Here with in-situ Laue diffraction experiments during micro-compression we demonstrate that when two {110} planes containing the same slip direction experience the same resolved shear stress, sharp slip traces are observed on a {112} plane. When however the {110} planes are slightly differently stressed, macroscopic strain is measured on the individual planes and collective cross-slip is used to fulfill mechanical boundary conditions, resulting in a zig-zag or broad slip trace on the sample surface. We anticipate that such dynamics can occur in polycrystalline metals due to local inhomogeneous stress distributions and can cause unusual slip transfer among grains.