Single-shot full strain tensor determination with microbeam X-ray Laue diffraction and a two-dimensional energy-dispersive detector

Abboud, Ali J.; Kirchlechner, Christoph; Kečkéš, Jozef; Nurdan, T. Conka; Send, S.; Micha, Jean‐Sébastien; Ulrich, Olivier; Hartmann, R.; Strüder, L.; Pietsch, U.

doi:10.1107/s1600576717005581

Cited by 16 publications

(10 citation statements)

References 26 publications

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“…13 This limits the application of most such methods to simple in-plane geometries or sections or special materials such as collagen fibrils with an ordered periodic structure at the nanoscale, while in most real-life systems, the 3D morphology may have no particular symmetry or alignment to sample shape. While recent innovative methods like 3D small-angle X-ray scattering (SAXS) tomography 14 and polychromatic X-ray diffraction, 15,16 which reconstruct 3D reciprocal space intensity in a model-free manner, circumvent this 2D limitation, these methods have limitations for in situ studies. SAXS tomography can take several hours of synchrotron time per reconstruction, 14 and the polychromatic X-ray diffraction analysis requires several minutes with a specialized energy-dispersive detector, 15 or scanning the photon energy.…”

Section: Introductionmentioning

confidence: 99%

Towards in situ determination of 3D strain and reorientation in the interpenetrating nanofibre networks of cuticle

et al. 2017

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Determining the in situ 3D nano- and microscale strain and reorientation fields in hierarchical nanocomposite materials is technically very challenging. Such a determination is important to understand the mechanisms enabling their functional optimization. An example of functional specialization to high dynamic mechanical resistance is the crustacean stomatopod cuticle. Here we develop a new 3D X-ray nanostrain reconstruction method combining analytical modelling of the diffraction signal, fibre-composite theory and in situ deformation, to determine the hitherto unknown nano- and microscale deformation mechanisms in stomatopod tergite cuticle. Stomatopod cuticle at the nanoscale consists of mineralized chitin fibres and calcified protein matrix, which form (at the microscale) plywood (Bouligand) layers with interpenetrating pore-canal fibres. We uncover anisotropic deformation patterns inside Bouligand lamellae, accompanied by load-induced fibre reorientation and pore-canal fibre compression. Lamination theory was used to decouple in-plane fibre reorientation from diffraction intensity changes induced by 3D lamellae tilting. Our method enables separation of deformation dynamics at multiple hierarchical levels, a critical consideration in the cooperative mechanics characteristic of biological and bioinspired materials. The nanostrain reconstruction technique is general, depending only on molecular-level fibre symmetry and can be applied to the in situ dynamics of advanced nanostructured materials with 3D hierarchical design.

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Section: Introductionmentioning

confidence: 99%

Towards in situ determination of 3D strain and reorientation in the interpenetrating nanofibre networks of cuticle

et al. 2017

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“…In the present work, all measured (hkl) belong to the same zone in reciprocal space. As demonstrated by Abboud et al (2017), the measurement of reflections belonging to different crystallographic zones provides access to all components of the strain tensor with rather high accuracy. Therefore the technique may serve as an effective tool to evaluate strain variations of nano-objects as a function of different kinds of deformation.…”

Section: Discussionmentioning

confidence: 99%

Energy-dispersive X-ray micro Laue diffraction on a bent gold nanowire

AlHassan¹,

Abboud²,

Cornelius³

et al. 2021

J Appl Cryst

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This article reports on energy-dispersive micro Laue (µLaue) diffraction of an individual gold nanowire that was mechanically deformed in three-point bending geometry using an atomic force microscope. The nanowire deformation was investigated by scanning the focused polychromatic X-ray beam along the nanowire and recording µLaue diffraction patterns using an energy-sensitive pnCCD detector that permits measurement of the angular positions of the Laue spots and the energies of the diffracted X-rays simultaneously. The plastic deformation of the nanowire was shown by a bending of up to 3.0 ± 0.1°, a torsion of up to 0.3 ± 0.1° and a maximum deformation depth of 80 ± 5 nm close to the position where the mechanical load was applied. In addition, extended Laue spots in the vicinity of one of the clamping points indicated the storage of geometrically necessary dislocations with a density of 7.5 × 1013 m−2. While µLaue diffraction with a non-energy-sensitive detector only gives access to the deviatoric strain, the energy sensitivity of the employed pnCCD offers absolute strain measurements with a resolution of 1%. Here, the residual strain after complete unloading of the nanowire amounted to maximum tensile and compressive strains of the order of +1.2 and −3%, which is comparable to the actual resolution limit. The combination of white-beam µLaue diffraction using an energy-sensitive pixel detector with nano-mechanical testing opens up new possibilities for the study of mechanical behavior at the nanoscale.

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“…Accuracies close to 10 À4 were obtained on Áa=a in Ge single-and UO 2 polycrystals (Robach et al, 2013) and a full strain analysis was performed in stressed Ge microstructures (Tardif et al, 2016). Measurements with a two-dimensional energy dispersive X-ray CCD detector in a strained copper single crystal have demonstrated the advantages of single-shot acquisitions for determining the components of the full strain tensor (Abboud et al, 2017). The energy resolution of the pn-junction CCD is of the order of several hundred electronvolts depending on the Laue spot energy (130 eV at 5 keV) and yields strain accuracies close to 10 À3 .…”

Section: Introductionmentioning

confidence: 88%

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

et al. 2017

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OATAO is an open access repository that collects the work of Toulouse researchers and makes it freely available over the web where possible. This is an author-deposited version published in : http://oatao. Laue microdiffraction is used to determine the full elastic strain tensor of the and 0 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 AE2.5 Â 10 À3 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 -0 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 Â 10 À3 Å and the dilatational strains are close to AE1.5 Â 10 À3 depending on the considered phase. For the 2000 nm precipitate size, the lattice mismatch is close to 8 Â 10 À3 Å and almost no elastic strain occurs in the microstructure.

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Single-shot full strain tensor determination with microbeam X-ray Laue diffraction and a two-dimensional energy-dispersive detector

Cited by 16 publications

References 26 publications

Towards in situ determination of 3D strain and reorientation in the interpenetrating nanofibre networks of cuticle

Towards in situ determination of 3D strain and reorientation in the interpenetrating nanofibre networks of cuticle

Energy-dispersive X-ray micro Laue diffraction on a bent gold nanowire

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

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