Jean-Sébastien Micha

A new white beam x-ray microdiffraction setup on the BM32 beamline at the European Synchrotron Radiation Facility

A white beam microdiffraction setup has been developed on the bending magnet source BM32 at the European Synchrotron Radiation Facility. The instrument allows routine submicrometer beam diffraction to perform orientation and strain mapping of polycrystalline samples. The setup features large source to optics distances allowing large demagnification ratios and small beam sizes. The optics of the beamline is used for beam conditioning upstream a secondary source, suppressing any possible interference of beam conditioning on beam size and position. The setup has been designed for an easy and efficient operation with position control tools embedded on the sample stage, a high magnification large aperture optical microscope, and fast readout detectors. Switching from the white beam mode to the monochromatic mode is made easy by an automatic procedure and allows the determination of both the deviatoric and hydrostatic strain tensors.

Dislocation storage in single slip-oriented Cu micro-tensile samples: new insights via X-ray microdiffraction

Synchrotron X-ray microdiffraction was used to characterize the deformation structure of single crystalline Cu micro-tensile specimens which were oriented for single slip. The 3-µm thick samples were strained in situ in a scanning electron microscope (SEM). Electron microscopy observations revealed glide steps at the surface indicating single slip. While the slip steps at the surface must have formed by the predominant activation of the primary glide system, analysis of Laue peak streaking directions revealed that, even at low strains, dislocations had been activated and stored on an unpredicted slip system. Furthermore, the µLaue scans showed that multiple slip takes over at a later state of deformation.

Strain field in silicon on insulator lines using high resolution x-ray diffraction

Symmetric and asymmetric reciprocal space maps (RSMs) of silicon on insulator (SOI) lines are obtained using high resolution x-ray diffraction. RSMs calculated from the displacement field simulated using finite element calculations show a good agreement with the experimental RSMs. These calculations indicate the large influence of the displacement field created by the silicon nitride cap and the sensitivity of the RSMs to the gradients of displacement at the edge of the SOI lines. They further show that the RSMs are influenced by local strains but also by local rotations of the crystal lattice connected with the strain distribution.

Investigation of reversible plasticity in a micron-sized, single crystalline copper bending beam by X-ray μLaue diffraction

The observed mechanical behaviour of micron-sized samples raises fundamental questions about the influence of size on the underlying dislocation plasticity. In situ µLaue diffraction on a single crystalline copper bending beam was performed to study the feasibility of bending tests and their contribution to our understanding of size-dependent dislocation plasticity. Theoretical considerations lead to a minimum sample size where in situ µLaue experiments are useable. A critical size is evidenced below which, depending on Youngs modulus and maximum stress, the elastic and plastic contributions to the lattice curvature cannot be separated. The experiment shows the increase in geometrically necessary dislocations during plastic deformation followed by a decrease during unloading. This can be explained by the formation and dissolution of a dislocation pile-up at the neutral axis of the bending cantilever. The dissolution of the dislocation pile-up is caused by the back stress of the pile-up and a direct observation of the Bauschinger effect, which is consistent with the non-purely elastic mechanical behaviour when unloading the sample.

New reactor dedicated to in operando studies of model catalysts by means of surface x-ray diffraction and grazing incidence small angle x-ray scattering

A new experimental setup has been developed to enable in situ studies of catalyst surfaces during chemical reactions by means of surface x-ray diffraction (SXRD) and grazing incidence small angle x-ray scattering. The x-ray reactor chamber was designed for both ultrahigh-vacuum (UHV) and reactive gas environments. A laser beam heating of the sample was implemented; the sample temperature reaches 1100 K in UHV and 600 K in the presence of reactive gases. The reactor equipment allows dynamical observations of the surface with various, perfectly mixed gases at controlled partial pressures. It can run in two modes: as a bath reactor in the pressure range of 1-1000 mbars and as a continuous flow cell for pressure lower than 10(-3) mbar. The reactor is connected to an UHV preparation chamber also equipped with low energy electron diffraction and Auger spectroscopy. This setup is thus perfectly well suited to extend in situ studies to more complex surfaces, such as epitaxial films or supported nanoparticles. It offers the possibility to follow the chemically induced changes of the morphology, the structure, the composition, and growth processes of the model catalyst surface during exposure to reactive gases. As an example the Pd(8)Ni(92)(110) surface structure was followed by SXRD under a few millibars of hydrogen and during butadiene hydrogenation while the reaction was monitored by quadrupole mass spectrometry. This experiment evidenced the great sensitivity of the diffracted intensity to the subtle interaction between the surface atoms and the gas molecules.

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

The in situ three-point bending of a single self-suspended Au nanowire is visualized by micro Laue diffraction. The nanowire deflection is inferred from the displacement of Laue spots and it is well described by finite element analysis taking into account geometric nonlinearities and the elastic constants of bulk Au.

Strains in light-ion-implanted polycrystals: influence of grain orientation

The implantation of He ions in UO2 polycrystals induces a strain in the implanted layer which can be characterized using Laue micro X-ray diffraction (µ-XRD). The strain tensor resulting from the ion implantation may not be reduced to a single out-of-plane strain component: it also has nonzero shear components. Their strong dependence upon crystal orientation is modeled using elasticity theory. This work demonstrates the potential of Laue µ-XRD for characterizing radiation effects in materials.

Laue-DIC: a new method for improved stress field measurements at the micrometer scale

The increment of elastic strain distribution, with a micrometer spatial resolution, is obtained by the correlation of successive Laue images. Application to a bent Si crystal allows evaluation of the accuracy of this new Laue-DIC method, which is about 10−5.

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.

The effect of size on the strength of FCC metals at elevated temperatures: annealed copper

Abstract As the length scale of sample dimensions is reduced to the micron and sub-micron scales, the strength of various materials has been observed to increase with decreasing size, a fact commonly referred to as the ‘sample size effect’. In this work, the influence of temperature on the sample size effect in copper is investigated using in situ microcompression testing at 25, 200 and 400 °C in the SEM on vacuum-annealed copper structures, and the resulting deformed structures were analysed using X-ray μLaue diffraction and scanning electron microscopy. For pillars with sizes between 0.4 and 4 μm, the size effect was measured to be constant with temperature, within the measurement precision, up to half of the melting point of copper. It is expected that the size effect will remain constant with temperature until diffusion-controlled dislocation motion becomes significant at higher temperatures and/or lower strain rates. Furthermore, the annealing treatment of the copper micropillars produced structures which yielded at stresses three times greater than their un-annealed, FIB-machined counterparts.