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Organisationseinheit der BAM
We present an experimental approach to study the three-dimensional microstructure of gas diffusion layer (GDL) materials under realistic compression conditions. A dedicated compression device was designed that allows for synchrotron-tomographic investigation of circular samples under well-defined compression conditions. The tomographic data provide the experimental basis for stochastic modeling of nonwoven GDL materials. A plain compression tool is used to study the fiber courses in the material at different compression stages. Transport relevant geometrical parameters, such as porosity, pore size, and tortuosity distributions, are exemplarily evaluated for a GDL sample in the uncompressed state and for a compression of 30 vol.%. To mimic the geometry of the flow-field, we employed a compression punch with an integrated channel-rib-profile. It turned out that the GDL material is homogeneously compressed under the ribs, however, much less compressed underneath the channel. GDL fibers extend far into the channel volume where they might interfere with the convective gas transport and the removal of liquid water from the cell.
We present a synchrotron X-ray tomographic study on the morphology of carbon fiber-based gas diffusion layer (GDL) material under compression. A dedicated compression device is used to provide well-defined compression conditions. A flat compression punch is employed to study the fiber geometry at different degrees of compression. Transport relevant geometrical parameters such as porosity, pore size and tortuosity distributions are calculated. The geometric properties notably change upon compression which has direct impact on transport conditions for gas and fluid flow. The availability of broad 3D paths, which are most important for the transport of liquid water from the catalyst layer through the GDL, is markedly reduced after compression. In a second experiment, we study the influence of the channel-land-pattern of the flow-field on shape and microstructure of the GDL. A flow-field compression punch is employed to reproduce the inhomogeneous compression conditions found during fuel cell assembly. While homogenously compressed underneath the land the GDL is much less and inhomogeneously compressed under the channel. The GDL material extends far into the channel volume where it can considerably influence gas and fluid flow. Loose fiber endings penetrate deeply into the channel and form obstacles for the discharge of liquid water droplets.
Aiming at ceramic materials of low thermal radiation emittance titania yttrium oxide ceramics have been prepared by sintering in air at 1,100 and 1,400 °C, respectively, and characterised. Due to its high infrared refractive index, average pore sizes up to 1 µm for optimal Mie scattering cross sections and over 35% porosity the material is a promising candidate for elevated temperature insulations. The essentially in large pore growth is achieved by graphitic nano and micro particle additives.
The microstructure parameters of porosity, specific surface area, median and average pore sizes are determined by mercury intrusion porosimetry. Beyond this classical technique supplementary measurements by X-ray Absorption and X-ray refractometry reveal considerably larger average pore sizes due to closed pores not accessible for mercury. An additional advantage of the X-ray techniques is their non-destructive application, which allows other treatments afterwards. The combined application of both methods provides additional information and reliability in case of complex ceramic microstructures and may serve for improved developments of porous ceramics with optimised thermal scattering for energy savings in high temperature applications.
The morphology and thermal behaviour of polypropylenegraftmaleic anhydride (PPgMA) layered silicate (montmorillonite) nanocomposites were investigated using X-ray diffraction, transmission electron microscopy, differential scanning calorimetry and thermogravimetry. The study focuses on the influence of the presence of oxygen during the preparation of PPgMAnanocomposite using two different modified clays. The nanocomposites show tactoid, intercalated and exfoliated structures side by side with different dominant states depending on the clay used and on the processing conditions. The systems are described as multi-component blends rather than binary blends since the organic ions do not only change the mixing behaviour, but also influence material properties. Beside the physical barrier property of the clay layers also chemical processes were found to play an important role.
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.
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.
A novel approach is suggested to strongly suppress artifacts in radiography and computed tomography caused by the effect of diffuse background signals 'backlighting' of 2D X-ray detectors. Depending on the detector geometry the mechanism may be different. Either based on the optical scattering of the fluorescent screen materials into the optical detection devices or Compton or X-ray fluorescence scattering by the detector components. Consequently, these erroneous intensity portions result in locally different violations of Lambert Beer's law in single projections (radiographs) as a function of the detector area coverage and the magnitude of the attenuation. The absorption of multiple metal sheets is investigated by monochromatic synchrotron radiation, thus excluding beam hardening. The proposed correction procedure simply requires the individual subtraction of one and the same fraction of the primary and transmitted mean intensity, as a constant (non-local) scattering mechanism is assumed.
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.
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.
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.
The employment of synchrotron radiation for refraction topography of materials has considerable advantages over standard x-ray sources. The much higher beam intensity and the parallel and monochromatic radiation provide faster measurements and better angular and spatial resolution. X-ray refraction techniques image the inner surface and interface concentration of micro-structured materials. This effect of x-ray optics is additional to small-angle scattering by diffraction, when the scattering objects reach micrometre dimensions. We have developed x-ray refraction techniques within the last decade in order to meet the growing demands for improved non-destructive characterization of high-performance composites, ceramics and other low-density materials. Sub-micron particle dimensions, the pore size of ceramics, the crack density distribution and single fibre debonding within damaged composites can be measured and visualized by computer-generated interface topographs. For this purpose investigations are now being performed at the new hard x-ray beamline of the Federal Institute for Materials Research and Testing (BAM) at BESSY, Berlin. This BAMline provides monochromatic radiation of photon energies from 5 to 60 keV from a double multilayer and/or a double-crystal monochromator. A separate instrument is dedicated to the further development and application of synchrotron radiation refraction (SRR) topography. Different from conventional small-angle scattering cameras with collimating slits and pinholes, scattering angles down to a few seconds of arc are selected by a single-crystal analyser, similar to a Bonse-Hart diffractometer. A 20 µm spatial resolution of the scattering micro-structures is achieved by a CCD camera with a fluorescent converter. First SRR topographs of aircraft composites [carbon fibre-reinforced plastics (CFRP), carbon fibre-reinforced ceramics (C/C), metal matrix ceramics (MMC)] will be reported.
The first hard X-ray beamline at BESSY II will be installed by BAM and PTB at a superconducting 7 T wavelength shifter. The main optical elements of the beamline are a Double-Multilayer-Monochromator and a Double-Crystal-Monochromator. The two devices can be used separately or in-line. Main applications of monochromatic radiation with photon energies up to 50 keV are X-ray fluorescence analysis, micro-computed tomography, X-ray topography, detector calibration and reflectometry. Calculable undispersed radiation up to 200 keV will be available for radiometric applications.
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.
Neutron tomography was applied to study the 3D water distribution in full polymer electrolyte membrane fuel cell (PEMFC) stacks. The water distribution after switch-off of the fuel cell was analyzed over a period of 36 h. We found a slowly increasing water amount in the fuel cell, but only few changes within a time period of 5 h, which is about the time necessary for neutron tomography. In this way, the requirement for successful tomography was obtained. It is demonstrated how the quasi in-situ tomography technique enables us to study the water content in individual flow field channels of three-fold stacks. Flow field as well as stack design issues are addressed by this visualization method showing weak points due to a non-uniform water distribution that can be identified by means of neutron imaging.
Magnetic domains have been the subject of much scientific investigation since their theoretical existence was first postulated by P.-E. Weiss over a century ago. Up to now, the three-dimensional (3D) domain structure of bulk magnets has never been observed owing to the lack of appropriate experimental methods. Domain analysis in bulk matter thus remains one of the most challenging tasks in research on magnetic materials. All current domain observation methods are limited to studying surface domains or thin magnetic films. As the properties of magnetic materials are strongly affected by their domain structure, the development of a technique capable of investigating the shape, size and distribution of individual domains in three dimensions is of great importance. Here, we show that the novel technique of Talbot-Lau neutron tomography with inverted geometry enables direct imaging of the 3D network of magnetic domains within the bulk of FeSi crystals.
This paper gives a brief overview on3D imaging of magnetic domains with shearing grating neutron tomography. We investigated the three-dimensional distribution of magnetic domain walls in the bulk of a wedge-shaped FeSi single crystal. The width of the magnetic domains wasanalyzed at different locations within the crystal. Magnetic domains close to the tip of the wedge are much smaller than in the bulk. Furthermore, the three-dimensional shape of individual domains wasinvestigated. We discuss prospects and limitations of the applied measurement technique.
CT (computed tomography) reconstructions of fuel cell components of a yet unrivaled spatial resolution and quality are presented. This is achieved by application of the novel DIRECTT (Direct Iterative Reconstruction of Computed Tomography Trajectories) algorithm. We focus on two different key issues which essentially rule the fuel cell's durability on different length scales and physical interactions. On the resolution scale of some 100 µm agglomerations of condensed water in flow-field channels are detected by means of quasi-in situ neutron CT (after operation). Five orders of magnitude below nanometer sized Ru catalyst particles on carbon black support are visualized by electron tomography. Both types of experiments are especially adapted to the type of material involved but they are accompanied by severe deviations from ideal CT measuring conditions, as well. In order to overcome the tremendous reconstruction artifacts of standard algorithms, we employ DIRECTT which is described in detail. Comparisons of DIRECTT reconstructions to the conventional filtered back projection, prove the significant improvements in both experimental methods.
A novel approach to strongly suppress artifacts in radiography and computed tomography caused by the effect of diffuse background signals ('backlighting') of 2D X-ray detectors is suggested. Depending on the detector geometry the mechanism may be different, either based on the optical scattering by the fluorescent screen materials into optical detection devices or Compton or X-ray fluorescence scattering by the detector components. Consequently, these erroneous intensity portions result in locally different violations of Lambert–Beer's law in single projections (radiographs). When used as input data for computed tomography these violations are directly observed via modulation of the projected mass as a function of the rotation phase and the samples aspect ratio (dynamics). The magnitude of the diffuse background signal depends on the detector area covered by the projected sample. They are more pronounced the smaller the shadowed area and the stronger the total attenuation. This implies that the reconstruction suffers from additional anisotropic artifacts caused by elongated sample structures. This issue is studied simply by absorption of flat plates in a conventional laboratory radiography set-up and at a synchrotron radiation facility. In the latter case beam hardening artifacts can be excluded due to the monochromatic radiation. The proposed correction procedure requires simple integral intensity offsets as a constant (non-local) light scattering mechanism is assumed.
X-ray compton tomography
(2014)
The potentials of incoherent X-ray Scattering (Compton) tomography are investigated. Imaging materials of very different density or atomic number at once is a perpetual challenge for X-ray tomography or radiography, in general. In a basic laboratory set-up for simultaneous perpendicular Compton Scattering and direct beam attenuation tomographic scans are conducted by single channel photon counting. This results in asymmetric distortions of the projection profiles of the scattering CT-data set. ln a first approach corrections of Compton scattering data by taking advantage of rotational symmetry yield tomograms without major geometric artefacts.
A cylindrical sample composed of PE, PA, PVC, glass and wood demonstrates similar Compton contrast for all the substances, while the conventional absorption tomogram only reveals the two high order materials.
Compärison to neutron tomography reveals astonishing similarities except for the glass component (without hydrogen). Therefore, Compton CT bears the potential to replace neutron tomography, which requires much more efforts.