Following dislocation patterning during fatigue

Precursors of failure are dislocation mechanisms at the nanoscale and dislocation organization at the mesoscale responsible for long-range internal stresses and lattice rotation. Detailed information on the link between both scales is missing, computationally and experimentally. Here we present a method based on x-ray Laue diffraction scanning providing time and sub -micron spatially resolved evolution of geometrical necessary dislocations in volumes that are similar to what advanced computational models can achieve. The approach is used to follow dislocation patterning during accumulation of fatigue cycles using a newly developed miniaturized shear device. Performed on Cu during cyclic shear, it reveals early dislocation patterning influenced by pre-existing dislocation structures. The quantitative information on non -homogeneous structure formation and its evolution corresponds to the need for synergies with continuum dislocation plasticity simulations of fatigue or any other type of plastic deformation. (C) 2016 Acta Materialia Inc. Published by Elsevier Ltd. This is an open access article under the CC BY -NC ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

In-situ Laue diffraction to follow dislocation patterning during fatigue

Ainara Irastorza Landa

The macroscopic strength of metals is determined by the dislocation arrangements that are formed when dislocations slip in the crystal lattice in response to the applied stress. Despite the extensive research carried out, the transition from uniform to non-uniform dislocation structures is not yet fully understood. This information is however essential to support the development of computational models that aim to predict dislocation patterning. Lattice rotation caused by the presence of dislocations is, for instance, a parameter that is often not taken into account in computational models although it plays a role in the development of dislocation ensembles. Experimentally following in-situ dislocation patterning including involved lattice rotations at lengthscales comparable to those in simulations is not straightforward. In fact, the current available techniques that have the necessary spatial and angular resolution are either destructive (3D-EBSD) or very time consuming (3D X-ray Laue diffraction). In this dissertation we present a new experimental approach that allows following lattice rotation and dislocation ensembles time-resolved during deformation. The technique is based on X-ray Laue diffraction scanning in transmission mode, which provides a sub-micron spatial resolution in 2D and statistical information on orientation spread in the third dimension. The in-situ mechanical tests are performed at the microXAS beamline of the Swiss Light Source Synchrotron. The method has been applied to understand dislocation pattering of copper single crystals occurring in the earlier phases of low cycle fatigue. Samples with different crystal orientations (single crystal, coplanar and collinear) have been cyclically deformed up to a maximum of 120 cycles. A dedicated miniaturized shear-fatigue device compatible with Laue diffraction has been constructed for that purpose and a sample preparation based on picosecond laser ablation has been developed. The developed procedure analyzes the evolving dislocation microstructures in terms of lattice rotation, lattice curvature and geometrically necessary dislocation densities at lengthscales similar to those addressable in computational models. It sacrifices on the fully 3D aspect but it brings the time resolution required to validate ongoing simulations. It has been shown that the error made by integration depends on the dislocation network expected. For instance, the technique can be used to validate 3DDD models or density based dislocation dynamics models when applied in deformation geometries where the formation of 2D dislocation patterns are expected (e.g. vein-channel structure in single slip oriented fatigued samples). The greatest advantage of this technique is that the evolving regions are easy to follow due to the high rotational sensitivity and time resolution of the method. What is more, the influence of the initial microstructure can be evaluated and quantitative values can be provided. On the other hand, the principal drawbacks are related to the gauge thickness of the samples. Even if the technique can estimate the orientation spread along the third direction, the approach cannot physically resolve the integrated signal along the thickness. This is source of uncertainty when providing actual values of lattice curvatures and geometrically necessary dislocation densities. Another shortcoming is the sensitivity of the method to the energy distribution of the X-ray beam provided in the beamline, which determines the collected signal - the principal basis of the subsequent analysis and interpretation.

EPFL2016

Nanocrystalline metals: transient testing during in situ X-ray diffraction and molecular dynamics

Zhen Sun

Nanocrystalline (NC) metals have attracted widespread interest in materials science due to their high strength compared to coarse-grained counterparts. It is well know that during uniaxial deformation, the stress-strain behaviour exhibits an extraordinary work-hardening followed by an early observation of constant flow stress. Information on possible deformation mechanisms have been gathered by extensive research combining in situ deformation experiments, electron microscopy observations and computational modelling. Generally, these mechanisms are categorized into two types: dislocation slip and grain boundary (GB) accommodation processes, as for instance, GB sliding based mechanisms and GB migration eventually coupled to the shear stress. However, the interplay between these mechanisms resulting in the constant deformation resistance is not fully understood. Transient testing has proven to be a suitable tool to gather information on the rate limiting deformation mechanisms that are activated during the deformation path. In particular in stress reduction experiments, after an intermediate/large stress drop thermally activated dislocation slip is suppressed so that other underlying mechanisms are brought into foreground during subsequent transient creep. Those mechanisms may play a minor role in the determination of the flow stress but might still be essential to the development of a constant deformation resistance. Within this thesis, transient testing is combined with in situ X-ray diffraction at the Swiss Light Source. Therefore, the transient responses are captured in terms of evolution of macrostrain as well as diffraction peak broadening. Since dislocation slip and GB accommodation have an opposite footprint on the peak broadening, the presence of these two types of mechanisms can be distinguished. Three electrodeposited NC materials with different grain sizes are investigated: two NC Ni batches and one NC Ni50Fe50 batch. The results reveal that the constant flow stress reached during uniaxial deformation of electrodeposited NC metals reflects a quasi-stationary balance between dislocation-based mechanisms and GB-mediated accommodation. The latter plays an important role in producing plastic strain and recovering the defects and internal stress. Depending on the magnitude of the stress drop, a non-monotonic behaviour of the diffraction peak width is observed, suggesting an alternation of mechanisms. Also, by comparing transient responses among different NC materials, the relative contributions of dislocation slip and GB accommodation mechanisms are discussed in terms of grain size and alloying. Finally, different magnitudes of stress reduction are carried out by molecular dynamics (MD) simulations with the aim to verify in situ experimental results and explore the mechanisms responsible for GB accommodation. MD simulations confirm that dislocation slip is reduced after a moderate stress drop, however can continue to operate after adaption of the GB structures by a variety of GB accommodation mechanisms explaining the non-monotonic behaviour of the peak broadening during transient creep.

EPFL2016

In-situ Laue diffraction to follow dislocation patterning during fatigue

Ainara Irastorza Landa

EPFL2016

Nanocrystalline metals: transient testing during in situ X-ray diffraction and molecular dynamics

Zhen Sun

EPFL2016