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Microstructure Characterisation of Advanced Materials via 2D and 3D X-Ray Refraction Techniques
(2018)
3D imaging techniques have an enormous potential to understand the microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this conference paper we report the use of a powerful, yet not so wide-spread, set of X-ray techniques based on refraction effects. X-ray refraction allows determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with a nanometric detectability. We demonstrate showcases of ceramics and composite materials, where microstructural parameters could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography. We present in situ analysis of the damage evolution in an Al/Al2O3 metal matrix composite during tensile load and the identification of void formation (different kinds of defects, particularly unsintered powder hidden in pores, and small inhomogeneity’s like cracks) in Ti64 parts produced by selective laser melting using synchrotron X-ray refraction radiography and tomography.
In the framework of the Dead Sea Integrated Research project (DESIRE), 59 seismological stations were deployed in the region of the Dead Sea Basin. Twenty of these stations recorded data of sufficiently high quality between May and September 2007 to be used for ambient seismic noise analysis. Empirical Green's functions are extracted from cross-correlations of long term recordings. These functions are dominated by Rayleigh waves, whose group velocities can be measured in the frequency range from 0.1 to 0.5 Hz. Analysis of positive and negative correlation lags of the Green's functions makes it possible to identify the direction of the source of the incoming energy. Signals with frequencies higher than 0.2 Hz originate from the Mediterranean Sea, while low frequencies arrive from the direction of the Red Sea. Travel times of the extracted Rayleigh waves were measured between station pairs for different frequencies, and tomographically inverted to provide independent velocity models. Four such 2D models were computed for a set of frequencies, all corresponding to different sampling depths, and thus together giving an indication of the velocity variations in 3D extending to a depth of 10 km. The results show low velocities in the Dead Sea Basin, consistent with previous studies suggesting up to 8 km of recent sedimentary infill in the Basin. The complex structure of the western margin of the Basin is also observed, with sedimentary infill present to depths not exceeding 5 km west of the southern part of the Dead Sea. The high velocities associated with the Lisan salt diapir are also observed down to a depth of similar to 5 km. The reliability of the results is confirmed by checkerboard recovery tests.
Cryo-electron microscopy (cryo-EM) is a powerful structure determination technique that is well-suited to the study of protein and polymer self-assembly in solution. In contrast to conventional transmission electron microscopy (TEM) sample preparation, which often times involves drying and staining, the frozen-hydrated sample preparation allows the specimens to be kept and imaged in a state closest to their native one. Here, we give a short overview of the basic principles of Cryo-EM and review our results on applying it to the study of different protein and polymer self-assembled nanostructures. More specifically, we show how we have applied cryo-electron tomography (cryo-ET) to visualize the internal morphology of self-assembled poly(ionic liquid) nanoparticles and cryo-EM single particle analysis (SPA) to determine the three-dimensional (3D) structures of artificial protein microtubules.