Emanuel Larsson

Coherent X-ray imaging techniques, such as in-line holography, exploit the high brilliance provided by diffraction-limited storage rings to perform imaging sensitive to the electron density through contrast due to the phase shift, rather than conventional attenuation contrast. Thus, coherent X-ray imaging techniques enable high-sensitivity and low-dose imaging, especially for low-atomic-number (Z) chemical elements and materials with similar attenuation contrast. Here, the first implementation of in-line holography at the NanoMAX beamline is presented, which benefits from the exceptional focusing capabilities and the high brilliance provided by MAX IV, the first operational diffraction-limited storage ring up to approximately 300 eV. It is demonstrated that in-line holography at NanoMAX can provide 2D diffraction-limited images, where the achievable resolution is only limited by the 70 nm focal spot at 13 keV X-ray energy. Also, the 3D capabilities of this instrument are demonstrated by performing holotomography on a chalk sample at a mesoscale resolution of around 155 nm. It is foreseen that in-line holography will broaden the spectra of capabilities of MAX IV by providing fast 2D and 3D electron density images from mesoscale down to nanoscale resolution.

When subjecting cast irons to mechanical loading the deformation and damage mechanisms occur on a microstructural level and are dependent on the inherent microstructure. A deeper understanding of the relation between the different microstructural constituents and the macroscopic mechanical behaviour would be beneficial in material development efforts and for the ability to design and cast components with tailored properties. Traditionally, microscopy examinations on sectioned cast iron samples have been used when analysing the microstructure in cast irons. Since all microstructural heterogeneity is in three-dimensions (3D), methods that provide a three-dimensional characterisation are essential for a deeper understanding of, both the microstructural features as well as the deformation and damage of cast irons. Therefore, different cast iron grades have been studied using synchrotron X-ray tomography and 3D x-ray diffraction (3DXRD) at ESRF in Grenoble, France. The samples were stepwise loaded and unloaded in-situ at in the tomography/3DXRD set-up to study the deformation with regard to microstructural constituents and the microstructural evolution in 3D. Based on the 3D tomography image sequences, digital volume correlation (DVC) was used for full strain field analysis and for the analysis of damage and deformation mechanisms. In addition, 3DXRD data were analysed to provide details on the lattice parameters and lattice strain of individual ferrite grains. This work shows the possibilities of such synchrotron experiments for advanced study of the mechanical behaviour of cast iron.

High-energy synchrotron radiation has been demonstrated to be a powerful tool for materials characterization. The development of novel methodologies is still ongoing, driven by major technological advances regarding the available source brilliance and efficient large area detectors. The Swedish Materials Science beamline at PETRA III is dedicated to materials characterization by high-energy X-rays and scheduled to enter into user operation starting August 2019. The beamline has been designed in particular for the combination of two complementary techniques: wide and small angle scattering and imaging. The beamline design is presented briefly and the different techniques are reviewed with regard to the contrast mechanisms and the ability to obtain spatially resolved information.

Biomaterials often display outstanding combinations of mechanical properties thanks to their hierarchical structuring, which occurs through a dynamically and biologically controlled growth and self-assembly of their main constituents, typically mineral and protein. However, it is still challenging to obtain this ordered multiscale structural organization in synthetic 3D-nanocomposite materials. Herein, we report a new bottom-up approach for the synthesis of macroscale hierarchical nanocomposite materials in a single step. By controlling the content of organic phase during the self-assembly of monodisperse organically-modified nanoparticles (iron oxide with oleyl phosphate), either purely supercrystalline or hierarchically structured supercrystalline nanocomposite materials are obtained. Beyond a critical concentration of organic phase, a hierarchical material is consistently formed. In such a hierarchical material, individual organically-modified ceramic nanoparticles (Level 0) self-assemble into supercrystals in face-centered cubic superlattices (Level 1), which in turn form granules of up to hundreds of micrometers (Level 2). These micrometric granules are the constituents of the final mm-sized material. This approach demonstrates that the local concentration of organic phase and nano-building blocks during self-assembly controls the final material’s microstructure, and thus enables the fine-tuning of inorganic-organic nanocomposites’ mechanical behavior, paving the way towards the design of novel high-performance structural materials.

Full-field transmission X-ray microscopy (TXM) is a well established technique, available at various synchrotron beamlines around the world as well as by laboratory benchtop devices. One of the major TXM challenges, due to its nanometre-scale resolution, is the overall instrument stability during the acquisition of the series of tomographic projections. The ability to correct for vertical and horizontal distortions of each projection image during acquisition is necessary in order to achieve the effective 3D spatial resolution. The effectiveness of such an image alignment is also heavily influenced by the absorption properties and strong contrast of specific features in the scanned sample. Here it is shown that nanoporous gold (NPG) can be used as an ideal 3D test pattern for evaluating and optimizing the performance of a TXM instrument for hard X-rays at a synchrotron beamline. Unique features of NPG, such as hierarchical structures at multiple length scales and high absorbing capabilities, makes it an ideal choice for characterization, which involves a combination of a rapid-alignment algorithm applied on the acquired projections followed by the extraction of a set of both 2D- and 3D-descriptive image parameters. This protocol can be used for comparing the efficiency of TXM instruments at different synchrotron beamlines in the world or benchtop devices, based on a reference library of scanned NPG samples, containing information about the estimated horizontal and vertical alignment values, 2D qualitative parameters and quantitative 3D parameters. The possibility to tailor the ligament sizes of NPG to match the achievable resolution in combination with the high electron density of gold makes NPG an ideal 3D test pattern for evaluating the status and performance of a given synchrotron-based or benchtop-based TXM setup.