Twins and their boundaries during homoepitaxy on Ir(111)

The growth and annealing behavior of strongly twinned homoepitaxial films on Ir(111) has been investigated by scanning tunneling microscopy, low energy electron diffraction and surface X-ray diffraction. In situ surface X-ray diffraction during and after film growth turned out to be an efficient tool for the determination of twin fractions in multilayer films and to uncover the nature of side twin boundaries. The annealing of the twin structures is shown to take place in a two step process, reducing first the length of the boundaries between differently stacked areas and only then the twins themselves. A model for the structure of the side twin boundaries is proposed which is consistent with both the scanning tunneling microscopy and surface X-ray diffraction data.Comment: 13 pages, 11 figure

Full elastic strain tensor determination at the phase scale in a powder metallurgy nickel-based superalloy using X-ray Laue microdiffraction

Laue microdiffraction is used to determine the full elastic strain tensor of the γ and γ′ phases in grains of a nickel-based superalloy with a coarse-grained microstructure. A `rainbow' filter and an energy dispersive point detector are employed to measure the energy of Bragg reflections. For the two techniques, an uncertainty of ±2.5 × 10−3 Å is obtained for the undetermined crystal lattice parameter. Our measurements show that the filter method provides better confidence, energy resolution, accuracy and acquisition time. The sensitivity of each method with respect to the γ–γ′ lattice mismatch is demonstrated with measurements in samples with average precipitate sizes of 200 and 2000 nm. For the 200 nm precipitate size, the lattice mismatch is less than 2 × 10−3 Å and the dilatational strains are close to ±1.5 × 10−3 depending on the considered phase. For the 2000 nm precipitate size, the lattice mismatch is close to 8 × 10−3 Å and almost no elastic strain occurs in the microstructure

3D-Laue micro diffraction to characterize fatigue damage in bi-crystalline micro cantilevers

Laue microdiffraction (µLaue) – a synchrotron based technique applying sub-micron sized (0.5x0.5µm²), polychromatic x-ray beams – has proven to shed unprecedented light onto the deformation behaviour of small volumes. So far, µLaue was used in situ as well as for 2D mapping to understand the tensile, compression and fatigue behaviour of metals. 3D-µLaue – also called “Differential Aperture X-ray microscopy” [1] – extend the capabilities of µLaue to achieve submicron 3D spatial characterization. An absorbing wire is moved between the sample surface and the detector. It is used to partially shadow the Laue pattern in order to reconstruct depth-resolved Laue patterns (see Fig.1). The achieved depth-resolution is in the order of 0.5µm³. In recent years we have adopted the 3D approach and coupled it with an in situ deformation rig. In this work we present the in situ characterization of low cycle fatigue damage in focussed ion beam (FIB) milled, micron sized copper single and bi-crystalline cantilevers (5x5x25µm³). Each bi-crystalline sample contains one single grain boundary located at the neutral plane. The experiments were performed at BM32 of the European Synchrotron (ESRF), using a combination of a micro straining rig and 3D-µLaue. From the measurements the lattice orientation, deviatoric strain tensor and the density of unpaired dislocations are extracted with sub-micron resolution. This is done at several different deformation stages, i.e. after ¼, ½, ¾ and full cycle. Please click Additional Files below to see the full abstract

In situ bending of an Au nanowire monitored by micro Laue diffraction

International audienceThis article reports on the first successful combination of micro Laue (µLaue) diffraction with an atomic force microscope for in situ nanomechanical tests of individual nanostructures. In situ three-point bending on self-suspended gold nanowires was performed on the BM32 beamline at the ESRF using a specially designed atomic force microscope. During the bending process of the self-suspended wire, the evolution of µLaue diffraction patterns was monitored, allowing for extraction of the bending angle of the nanowire. This bending compares well with finite element analysis taking into account elastic constant bulk values and geometric nonlinearities. This novel experimental setup opens promising perspectives for studying mechanical properties at the nanoscale

Lattice strain and tilt mapping in stressed Ge microstructures using X-ray Laue micro-diffraction and rainbow-filtering

Micro-Laue diffraction and simultaneous rainbow-filtered micro-diffraction were used to measure accurately the full strain tensor and the lattice orientation distribution at the sub-micron scale in highly strained, suspended Ge micro-devices. A numerical approach to obtain the full strain tensor from the deviatoric strain measurement alone is also demonstrated and used for faster full strain mapping. We performed the measurements in a series of micro-devices under either uniaxial or biaxial stress and found an excellent agreement with numerical simulations. This shows the superior potential of Laue micro-diffraction for the investigation of highly strained micro-devices.Comment: 28 pages, 10 figure

Evidence of 3D strain gradients associated with tin whisker growth

We have used Differential Aperture X-ray Microscopy (DAXM) to measure grain orientations and deviatoric elastic strains in 3D around a tin whisker. The results show strain gradients through the depth of the tin coating, revealing a higher strain deeper in the Sn layer. These higher strains are explained by the volume change occurring during growth of the intermetallic phase Cu6Sn5 at the interface between the Cu substrate and the Sn coating and at grain boundaries between Sn grains

Validity of Crystal Plasticity Models Near Grain Boundaries: Contribution of Elastic Strain Measurements at Micron Scale

Synchrotron Laue microdiffraction and digital image correlation measurements were coupled to track the elastic strain field (or stress field) and the total strain field near a general grain boundary in a bent bicrystal. A 316L stainless steel bicrystal was deformed in situ into the elasto-plastic regime using a four-point bending setup. The test was then simulated using finite elements with a crystal plasticity model comprising internal variables (dislocation densities on discrete slip systems). The predictions of the model are compared with both the total strain field and the elastic strain field obtained experimentally. While activated slip systems and total strains are reasonably well predicted, elastic strains appear overestimated next to the grain boundary. This suggests that conventional crystal plasticity models need improvement to correctly model stresses at grain boundaries

Direct measurement of local constitutive relations, at the micrometre scale, in bulk metallic alloys

Multiscale models involving crystal plasticity are essential to predict the elastoplastic behavior of structural materials with respect to their microstructure. However, those models are often limited by a poor knowledge of the local constitutive behavior. This article reports a method to measure the mechanical behavior directly, at the micrometre scale, in bulk crystalline materials. Local strain and stress states were evaluated at the surface of a bent stainless steel crystal by combining total strain measurements – performed with the digital image correlation technique on optical images – with elastic strain measurements obtained by Laue microdiffraction. A local constitutive relation was measured, in an efficient nondestructive way, without the need for full-field simulations. The method was validated by a comparison between the measured local behavior and the macroscopic behavior of the single crystal