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Henning F. Poulsen

Publications and source records attributed to Henning F. Poulsen.

8 recordsLinked to original sources

In situ mapping of indentation-induced densification and cracking in vitreous silica by nanofocus X-ray scattering

The practical strength of oxide glasses is greatly reduced by surface flaws that form during processing and use. Instrumented indentation can mimic such real-life damage events and induce flaws and cracking under controlled conditions. At the same time, instrumented indentation allows for systematic examination of the deformation and structural changes of the regions of the glass being indented. However, structural probing is nearly always performed after rather than during the sharp contact event, limiting our understanding of the indentation process. To overcome this, we here demonstrate the use of nanofocus X-ray scattering experiments to probe the local mechanical and structural response of vitreous silica during indentation. Two-dimensional mapping of the scattering pattern in the zone below a sharp diamond wedge indenter reveals local changes in the atomic structure and density as well as cracking behavior. These in situ experiments during indentation reveal the formation and evolution of the densification zone and cracking with nanoscale resolution. Understanding the interplay between structural densification and cracking behavior in glasses is deepened through this work, which is crucial for the development of more damage-resistant and thus stronger glasses as well as fundamental understanding of glass deformation mechanisms.

cond-mat.mtrl-sci↗

X-ray induced grain boundary formation and grain rotation in Bi2Se3

Optimizing grain boundary characteristics in polycrystalline materials can improve their properties. Many processing methods have been developed for grain boundary manipulation, including the use of intense radiation in certain applications. In this work, we used X-ray free electron laser pulses to irradiate single-crystalline bismuth selenide (Bi2Se3) and observed grain boundary formation and subsequent grain rotation in response to the X-ray radiation. Our observations with simultaneous transmission X-ray microscopy and X-ray diffraction demonstrate how intense X- ray radiation can rapidly change size and texture of grains.

cond-mat.mtrl-sci↗

Dark-Field X-ray Microscopy for 2D and 3D imaging of Microstructural Dynamics at the European X-ray Free Electron Laser

Dark field X-ray microscopy (DXFM) can visualize microstructural distortions in bulk crystals. Using the femtosecond X-ray pulses generated by X-ray free-electron lasers (XFEL), DFXM can achieve sub-μm spatial resolution and <100 fs time resolution simultaneously. In this paper, we demonstrate ultrafast DFXM measurements at the European XFEL to visualize an optically-driven longitudinal strain wave propagating through a diamond single crystal. We also present two DFXM scanning modalities that are new to the XFEL sources: spatially 3D and 2D axial-strain scans with sub-μm spatial resolution. With this progress in XFEL-based DFXM, we discuss new opportunities to study multi-timescale spatio-temporal dynamics of microstructures.

cond-mat.mes-hall↗

Microstructure and Stress Mapping in 3D at Industrially Relevant Degrees of Plastic Deformation

Strength, ductility, and failure properties of metals are tailored by plastic deformation routes. Predicting these properties requires modeling of the structural dynamics and stress evolution taking place on several length scales. Progress has been hampered by a lack of representative 3D experimental data at industrially relevant degrees of deformation. We present an X-ray imaging based 3D mapping of an aluminum polycrystal deformed to the ultimate tensile strength (32% elongation). The extensive dataset reveals significant intra-grain stress variations (36 MPa) up to at least half of the inter-grain variations (76 MPa), which are dominated by grain orientation effects. Local intra-grain stress concentrations are candidates for damage nucleation. Such data are important for models of structure-property relations and damage.

cond-mat.mtrl-sci↗

3D Microstructural and Strain Evolution During the Early Stages of Tensile Deformation

Dislocation patterning and self-organization during plastic deformation are associated with work hardening, but the exact mechanisms remain elusive. This is partly because studies of the structure and local strain during the initial stages of plastic deformation has been a challenge. Here we use Dark Field X-ray Microscopy to generate 3D maps of embedded $350 \times 900 \times 72 \,μ\mathrm{m}^3$ volumes within three pure Al single crystals, all oriented for double slip on the primary and conjugate slip systems. These were tensile deformed by 0.6$\%$, 1.7$\%$ and 3.6$\%$, respectively. Orientation maps revealed the existence of two distinct types of planar dislocation boundaries both at 0.6$\%$ and 1.7$\%$ but no systematic patterning. At 3.6$\%$, these boundaries have evolved into a well-defined checkerboard pattern, characteristic of Geometrically Necessary Boundaries, GNBs. The GNB spacing is $\approx$ 14 $μ$m and the misorientation $\approx$ 0.2°, in fair agreement with those at higher strains. By contrast to the sharp boundaries observed at higher strains, the boundaries are associated with a sinusoidal orientation gradient. Maps of the elastic strain along the (111) direction exhibit fluctuations of $\pm 0.0002 $ with an average domain size of 3 $μ$m.

cond-mat.mtrl-sci↗

Revisiting neutron propagation-based phase contrast imaging and tomography: use of phase retrieval to amplify the effective degree of brilliance

Propagation-based neutron phase-contrast tomography was demonstrated using the ISIS pulsed spallation source. The proof-of-concept tomogram with Paganin-type phase-retrieval filter applied exhibited an effective net boost of $23\pm 1$ in the signal-to-noise ratio as compared to an attenuation-based tomogram, implying a boost in the effective degree of neutron brilliance of over two orders of magnitude. This comparison is for phase retrieval versus conventional absorption with no additional collimation in place. Expressions are provided for the optimal phase-contrast geometry as well as conditions for the validity of the method. The underpinning theory is derived under the assumption of the sample being composed of a single material. The effective boost in brilliance may be employed to give reduced acquisition time, or may instead be used to keep exposure times fixed while improving the measured contrast.

eess.IV↗

Extensive 3D Mapping of Dislocation Structures in Bulk Aluminum

Thermomechanical processing such as annealing is one of the main methods to tailor the mechanical properties of materials, however, much is unknown about the reorganization of dislocation structures deep inside macroscopic crystals that give rise to those changes. Here, we demonstrate the self-organization of dislocation structures upon high-temperature annealing in a mm-sized single crystal of aluminum. We map a large embedded 3D volume ($100\times300\times300$ $μ$m$^3$) of dislocation structures using dark field x-ray microscopy (DFXM), a diffraction-based imaging technique. Over the wide field of view, DFXM's high angular resolution allows us to identify subgrains, separated by dislocation boundaries, which we identify and characterize down to the single-dislocation level using computer-vision methods. We demonstrate how even after long annealing times at high temperatures, the remaining low density of dislocations still pack into well-defined, straight dislocation boundaries (DBs) that lie on specific crystallographic planes. In contrast to conventional grain growth models, our results show that the dihedral angles at the triple junctions are not the predicted 120$\degree$, suggesting additional complexities in the boundary stabilization mechanisms. Mapping the local misorientation and lattice strain around these boundaries shows that the observed strain is shear, imparting an average misorientation around the DB of $\approx 0.003-0.006 \degree{}$

cond-mat.mtrl-sci↗

Non-destructive determination of phase, size, and strain of individual grains in polycrystalline photovoltaic materials

We demonstrate a non-destructive approach to provide structural properties on the grain level for the absorber layer of kesterite solar cells. Kesterite solar cells are notoriously difficult to characterize structurally due to the co-existence of several phases with very similar lattice parameters. Specifically, we present a comprehensive study of 597 grains in the absorber layer of a 1.64% efficient Cu2ZnSnS4 (CZTS) thin-film solar cell, from which 15 grains correspond to the secondary phase ZnS. By means of three dimensional X-ray diffraction (3DXRD), we obtained statistics for the phase, size, orientation, and strain tensors of the grains, as well as their twin relations. We observe an average tensile stress in the plane of the film of ~ 70 MPa and a compressive stress along the normal to the film of ~ 145 MPa. At the grain level, we derive a 3D stress tensor that deviates from the biaxial model usually assumed for thin films. 41% of the grains are twins. We calculate the frequency of the six types of $Σ$3 boundaries, revealing that 180° rotations along axis <221> is the most frequent. This technique can be applied to polycrystalline thin film solar cells in general, where strain can influence the bandgap of the absorber layer material, and twin boundaries play a role in the charge transport mechanisms.

cond-mat.mtrl-sci↗