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The use of high brilliance and partial coherent synchrotron light for radiography and computed tomography (CT) allows to image micro-structured, multi-component specimens with different contrast modes and resolutions up to submicrometer range. This is of high interest for materials research, life science and non-destructive evaluation applications. An imaging setup for microtomography and radiography installed at BESSY II (a third generation synchrotron light source located in Berlin, Germany) as part of its first hard X-ray beamline (BAMline) can now be used for absorption, refraction as well as phase contrast dedicated to inhouse research and applications by external users. Monochromatic synchrotron light between 6 keV and 80 keV is attained via a fully automated double multilayer monochromator. For imaging applications the synchrotron beam transmitted by the sample is converted with a scintillator into visible light. By use of microscope optics this luminescence image is then projected onto, e.g., a CCD chip. Several scintillating materials are used in order to optimise the performance of the detector system. Different optical systems are available for imaging ranging from a larger field of view and moderate resolutions (macroscope up to 14 mm x 14 mm field of view) to high resolution (microscope down to 0.35 μm pixel size), offering magnifications from 1.8× to 40×. Additionally asymmetric cut Bragg crystals in front of the scintillator can be used for a further magnification in one dimension by a factor of about 20. Slow and fast cameras are available, with up to 16 bit dynamic range. We show the suitability of the setup for numerous applications from materials research and life science.
X-ray refraction topography techniques are based on ultra-small angle scattering by micro-structural elements causing phase-related effects such as refraction and total reflection at a few minutes of arc as the refractive index of X-rays is nearly unity. The refraction contrast is several times higher than true absorption and results in images of cracks, pores and fibre debonding separations below the spatial resolution of the detector. In most cases the investigated inner surface and interface structures correlate to mechanical properties. For the exploration of micro structured materials the refraction technique has been improved by a 3D Synchrotron Refraction Computed Tomography test station. The specimen is placed in an X-ray beam between two single crystals, which suppresses all sample scattering. In addition, an asymmetric cut second crystal can magnify the image up to 50 times revealing nano meter resolution. The technique is an alternative to other attempts on raising the spatial resolution of CT machines.
Erstmals wurden MMCs mit Hilfe der Interface-Kontrast verstärkenden Röntgen-Refraktions-Technik in Kombination mit der 3D-CT-Technik untersucht. Die Methode der Röntgen-Refraktions-Topography sowie der Röntgen-Refraktions-Tomography wurden in den letzten Jahren speziell für die zerstörungsfreie Charakterisierung von Leichtbau-Hochleistungs-Werkstoffen wie Verbund-Werkstoffen und Keramiken entwickelt. Die Technik basiert auf der Refraktion von Röntgenlicht an Grenzflächen zwischen Bereichen unterschiedlicher Elektronendichte wie z.B. Faser- und Matrix-Werkstoff. Auf Grund der kurzen Röntgen-Wellenlänge hat der Brechungsindex einen Wert dicht bei eins, sodass der Streuwinkel nur wenige Bogenminuten beträgt. Der Vorteil der kurzen Wellenlänge besteht jedoch darin, dass Poren und Risse detektiert werden können, deren Größe im Nanometerbereich liegen. Damit kann die Refraktions-Technik zum besseren Verständnis von Mikro- und Submikro-Strukturen in der Materialwissenschaft eingesetzt werden. Mit der hier vorgestellten Refraktions-CT wurden Ermüdungsmechanismen an MMCs, bestehend aus SiC-Faser verstärktem Titan (Ti6242) untersucht. Die Messungen wurden am Röntgen-Messplatz der BAM (BAMline) am Synchrotron-Speicherring-BESSY in Berlin Adlershof durchgeführt.
Microstructural aspects of composites such as reinforcement particle size, shape, and distribution play important roles in deformation behavior. In addition, Fe-rich inclusions and porosity also influence the behavior of these composites, particularly under fatigue loading. Three-dimensional (3-D) visualization of porosity and Fe-rich inclusions in three dimensions is critical to a thorough understanding of fatigue resistance of metal matrix composites (MMCs), because cracks often initiate at these defects. In this article, we have used X-ray synchrotron tomography to visualize and quantify the morphology and size distribution of pores and Fe-rich inclusions in a SiC particle-reinforced 2080 Al alloy composite. The 3-D data sets were also used to predict and understand the influence of defects on the deformation behavior by 3-D finite element modeling.
Evaluating porosity in cordierite diesel particulate filter materials, part 1 X-ray refraction
(2013)
Bi-continuous porous ceramics for filtration applications possess a particularly complicated microstructure, with porosity and solid matter being intermingled. Mechanical, thermal, and filtration properties can only be precisely estimated if the morphology of both solid matter and porosity can be quantitatively determined. Using x-ray absorption and refraction, we quantitatively evaluate porosity and pore orientation in cordierite diesel particulate filter ceramics. Porosity values turn out to agree with mercury intrusion measurements, while pore orientation factors agree with published crystallographic texture data.
X-ray computed tomography is an important tool for non-destructively evaluating the 3-D microstructure of modern materials. To resolve material structures in the micrometer range and below, high brilliance synchrotron radiation has to be used. The Federal Institute for Materials Research and Testing (BAM) has built up an imaging setup for micro-tomography and -radiography (BAMline) at the Berliner storage ring for synchrotron radiation (BESSY). In computed tomography, the contrast at interfaces within heterogeneous materials can be strongly amplified by effects related to X-ray refraction. Such effects are especially useful for materials of low absorption or mixed phases showing similar X-ray absorption properties that produce low contrast. The technique is based on ultra-small-angle scattering by microstructural elements causing phase-related effects, such as refraction and total reflection. The extraordinary contrast of inner surfaces is far beyond absorption effects. Crack orientation and fibre/matrix debonding in plastics, polymers, ceramics and metal-matrix-composites after cyclic loading and hydro-thermal aging can be visualized. In most cases, the investigated inner surface and interface structures correlate to mechanical properties. The technique is an alternative to other attempts on raising the spatial resolution of CT machines.
High-density polyethylene becomes optically transparent during tensile drawing when previously saturated with diesel fuel. This unusual phenomenon is investigated as it might allow conclusions with respect to the material behavior. Microscopy, differential scanning calorimetry, density measurements are applied together with two scanning X-ray scattering techniques: wide angle X-ray scattering (WAXS) and X-ray refraction, able to extract the spatially resolved crystal orientation and internal surface, respectively. The sorbed diesel softens the material and significantly alters the yielding characteristics. Although the crystallinity among stretched regions is similar, a virgin reference sample exhibits strain whitening during stretching, while the diesel-saturated sample becomes transparent. The WAXS results reveal a pronounced fiber texture in the tensile direction in the stretched region and an isotropic orientation in the unstretched region. This texture implies the formation of fibrils in the stretched region, while spherulites remain intact in the unstretched parts of the specimens. X-ray refraction reveals a preferred orientation of internal surfaces along the tensile direction in the stretched region of virgin samples, while the sample stretched in the diesel-saturated state shows no internal surfaces at all. Besides from stretching saturated samples, optical transparency is also obtained from sorbing samples in diesel after stretching.
The performance of grating interferometers coming up now for Imaging interfaces within materials depends on the efficiency (visibility) of their main component, namely the phase grating. Therefore, experiments with monochromatic synchrotron radiation and corresponding simulations are carried out. The visibility of a Phase grating is optimized by different photon energies, varying detector to grating distances and continuous rotation of the phase grating about the grid lines. Such kind of rotation changes the projected grating shapes, and thereby the distribution profiles of phase shifts. This yields higher visibilities than derived from ideal rectangular shapes. By continuous grating rotation and variation of the propagation distance, we achieve 2D visibility maps. Such maps provide the visibility for a certain combination of grating orientation and detector position. Optimum visibilities occur at considerably smaller distances than in the standard setup.
In order to investigate their microcracking behaviour, the microstructures of several β-eucryptite ceramics, obtained from glass precursor and cerammed to yield different grain sizes and microcrack densities, were characterized by laboratory and synchrotron x-ray refraction and tomography. Results were compared with those obtained from scanning electron microscopy (SEM). In SEM images, the characterized materials appeared fully dense but computed tomography showed the presence of pore clusters. Uniaxial tensile testing was performed on specimens while strain maps were recorded and analyzed by Digital Image Correlation (DIC). X-ray refraction techniques were applied on specimens before and after tensile testing to measure the amount of the internal specific surface (i.e., area per unit volume). X-ray refraction revealed that (a) the small grain size (SGS) material contained a large specific surface, originating from the grain boundaries and the interfaces of TiO2 precipitates; (b) the medium (MGS) and large grain size (LGS) materials possessed higher amounts of specific surface compared to SGS material due to microcracks, which decreased after tensile loading; (c) the precursor glass had negligible internal surface. The unexpected decrease in the internal surface of MGS and LGS after tensile testing is explained by the presence of compressive regions in the DIC strain maps and further by theoretical arguments. It is suggested that while some microcracks merge via propagation, more close mechanically, thereby explaining the observed X-ray refraction results. The mechanisms proposed would allow the development of a strain hardening route in ceramics.