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Organisationseinheit der BAM
Eingeladener Vortrag
- nein (34)
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 Techniques
(2005)
Enhanced Spatial Resolution in 2D CT-Reconstruction without Filtered Back Projection: DIRECTT
(2008)
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.
Synchrotron-Refraktions-Computer-Tomographie - EIne neue Methode zur Erkennung von Grenzflächen
(2009)
Rekonstruktion unvollständiger computertomografischer Modelldatensätze mit Directt-Algorithmus
(2010)
Modellrechnungen zur Rekonstruktion unvollständiger computertomographischer Datensätze werden zur Ermittlung der Vorteile des neuen Directt-Algorithmus gegenüber der konventionellen gefilterten Rückprojektion durchgeführt, insbesondere auch zur Vermeidung experimentell begründeter Unwägbarkeiten. Ein entsprechender Bedarf entsteht seitens erweiterter Forschungsaktivitäten und industrieller Bedürfnisse, wo die Rekonstruktion limitierter Messdatensätze von Artefakten dominiert wird. Die bekanntesten Einschränkungen betreffen das Limited-View- und Few-Angles-Problem sowie die ROI-Situation, die jeweils unabhängig voneinander untersucht werden, in der Anwendung jedoch zumeist undefiniert vermischt sind, wie etwa in der Elektronen-Tomografie. Die hochauflösende Rekonstruktion von Einzelpixeln wird durch die Wahl eines kleinen Modells von nur 1012 Pixeln visualisiert und ist ohne Filterung möglich. Rekonstruktionen von 90°-Sektoren oder 50 % -ROI-Querschnitten sind fast ohne Auflösungseinschränkungen realisierbar. Die bisher nicht bekannte Möglichkeit, auch außerhalb der ROI präzise zu rekonstruieren, wurde als "Extended ROI"-Methode erfolgreich erprobt.
Die Aufklärung spezifischer Fragestellungen zur Funktionalität von PEM(polymer electrolyte membrane)- und DMFC(Direct Methanol)-Brennstoffzellen bedarf der 3D-Abbildung der spezifischen Komponenten mit unterschiedlichen Strahlungsarten: des Wassergehalts in den Flow Fields mit Neutronen, der Katalysator-Alterung in der MEA (membrane electrode assembly) mit Synchrotronstrahlung und der freien (reaktiven) Katalysator-Oberfläche von Nano-Partikeln mit TEM-Elektronen-Tomografie. Diese Messungen im Bereich der mm- bis nm-Skala unterliegen dabei erheblichen Restriktionen: einer ortsabhängigen Verschmierung der Neutronenradiogramme, Manipulatorinstabilitäten der Synchrotronmessungen sowie einer Kombination von Limited-View-Datensätzen, wenigen Projektionswinkeln und teilweiser Nichtdurchstrahlbarkeit in der Elektronen-CT. Die Vorteile eines fortentwickelten Directt-Algorithmus für die Bewältigung dieser Randbedingungen gegenüber gefilterten Rückprojektionen werden aufgezeigt.
The presence of elongation, streak and blurring artifacts in tomograms recorded under a missing wedge of rotation angles presents a major challenge for the quantitative analysis of tomographic image data. We show that the missing wedge artifacts of standard reconstruction algorithms may be reduced by the innovative reconstruction technique DIRECTT. For the comparison of missing wedge artifacts we apply techniques from spatial statistics, which have been specifically designed to investigate the shape of phase boundaries in tomograms.
In order to demonstrate the challenging tasks in current R&D applications in the field of renewable energy
sources experimental neutron and electron tomographic data sets of PEM fuel cell components are processed by
an advanced version of the DIRECTT algorithm. The neutron measurements of the water distribution suffer from
several intrinsic limitations such as massive position dependent focal smearing due to the large primary neutron
beam aperture. Electron (TEM) tomography allows characterisation of nanometre sized catalyst particles but is
hampered by the following restrictions: partial opacity, a limited sector of projections (missing wedge), very few
projections, samples exceeding the detector size (region of interest) and improper angular alignment. Beyond the
capabilities of other algorithms DIRECTT proves to overcome these essential reconstruction problems, in
comparison to FBP and SIRT. Nevertheless, careful data pre-processing is an inevitable requirement in order to
fully exploit the algorithm's potentials.
Incomplete tomographic data sets such as limited view (missing wedge) data represent a well-known challenge
for reconstruction algorithms, since they unavoidably lead to substantial image artefacts. Such data sets may
occur in industrial computed tomography of limited access (e.g. extended components, fixed objects), directional
opacity, limited sample life time or laminographic set-up. We present strategies to effectively suppress the
typical elongation artefacts (e.g. lemon-like deformed pores) by our iterative algorithm DIRECTT which offers
the opportunity to vary the versatile reconstruction parameters within each cycle. Those strategies are applied to
experimental data obtained from metallic foams as well as model simulations. Comparison is drawn to state-ofthe-
art techniques (filtered backprojection and algebraic techniques). Further reference is made to reconstructions
of complete data sets serving as gold standards. For quantitative assessment of the reconstruction
quality adapted techniques based on spatial statistics are introduced.
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 of 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 Beers law in
single projections (radiographs) as 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.
The relevance of nano sized structures and interfaces in upcoming technologies requires new non-destructive Xray
techniques exploiting attenuation as well as scattering. In the course of driving the resolution and the contrast
of modern radiography into micro and nano metre dimension the inevitable scattering effects require increased
attention. Several radiologists interpret the observed edge artefacts simply by 'phase contrast' due to different
X-ray path lengths within the sample and others refer to Fresnel scattering. The ultra small angle scattering is of
high intensity and may reach the level of the primary beam. We present monochromatic synchrotron
measurements on rather simply shaped objects (such as plates and cylinders) which prove clearly the dominance
of refraction intensity over total reflection and coherent small angle scattering. The refraction conditions hold for
angles of incidence of several degrees to the surface, but typical deflection angles range from several seconds to
minutes of arc. Additionally to the concept of 'phase contrast' of the primary beam its deflection becomes the
essential issue. The appropriate removal of the attenuation contribution enables the imaging of inner surfaces and
interfaces by refraction scanning topography. The presented measurements of reference particles demonstrate the
reliability of laboratory refraction scanners applying X-ray tubes.
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.
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.
Complementary to Part 1 of this work, the bi-continuous microstructure of porous synthetic cordierite ceramics for filtration applications was investigated using 3D x-ray computed tomography at different resolutions. Applying both Fast Fourier Transform and a newly developed image analysis algorithm, we quantitatively evaluated porosity and pore orientation. The statistical approach allows extraction of spatially resolved or average values. Porosity values based on x-ray absorption agree with mercury intrusion measurements, while pore orientation factors agree with x-ray refraction data (Part 1 of this work), and with published crystallographic texture data.
Typische 'Missing Wedge'(MW)-Artefakte in Rekonstruktionen der Computertomografie können mit dem iterativen DIRECTT-Algorithmus (Direkte iterative Rekonstruktion computertomografischer Trajektorien) unterdrückt werden. Die durch fehlende Projektionswinkel bedingten MW-Restriktionen betreffen bisher nur Sonderapplikationen der Röntgen- und Neutronentomografie, müssen in der Nanometer auflösenden Elektronentomografie jedoch als Standard akzeptiert werden. Die MW-Artefakte werden besonders effektiv mit einer spezifischen DIRECTT-Prozedur partiell diskreter Zwischenlösungen beseitigt. Für die Beurteilung der Abbildungsqualität werden Rekonstruktionen von vollständigen und unvollständigen Mess- und Modell-Datensätzen erzeugt und mit Ergebnissen anderer Algorithmen (gefilterte Rückprojektion (FBP) und ART-Methoden) verglichen. Die Fourier-Transformierten der Rekonstruktionen demonstrieren die erfolgreiche Ergänzung der fehlenden Information im MW-Bereich. Die quantitative Bewertung der lokalen Rekonstruktionsqualität mit Methoden der räumlichen Statistik ergibt auch für unterschiedliche Signal-Rausch-Verhältnisse signifikante Vorteile gegenüber FBP und ART.
Anhand von computertomografischen Messungen und Modellrechnungen werden DIRECTT-Rekonstruktionen im Vergleich mit gefilterten Rückprojektionen bewertet. Dazu wird die Rekonstruktionsqualität mittels einer zirkular erweiterten Modulations-Transfer-Funktion (MTF) und mit integralen Kenngrößen im Radon- und im Ortsraum verglichen. Zur Überprüfung der Rekonstruktionsgenauigkeit experimenteller Daten werden Mustermessungen einfacher Probengeometrien unter definierten physikalischen Bedingungen durchgeführt. Diese beinhalten die Monochromasie, die Unterdrückung von Kantenartefakten und die radiometrische Intensitätsbestimmung. Für die Qualität der Rekonstruktionen mittels DIRECTT erweisen sich sowohl unterschiedliche Rekonstruktionsfilter als auch der Verzicht auf jede Filterung als unerheblich, im Gegensatz zur gefilterten Rückprojektion.
The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread holds equally for industrial and academic research, and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated. We shall show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. We will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Die durch Brechung an Mikrostrukturen abgelenkte Röntgenstrahlung wird direkt zweidimensional abgebildet. Dazu werden Modellproben einfacher Geometrie (Fasern, Kapillaren, monodisperse Nano- und Mikropartikel) mit einem auf 50 µm kollimierten Synchrotronstrahl (20 keV) gescannt. Die nach den Regeln der geometrischen Optik an prismatischen und linsenartigen Grenzflächen abgelenkte Strahlung wird in etwa 3 Metern Entfernung von einem Flächendetektor mit 7 µm Ortsauflösung zusätzlich zu der ungestörten Resttransmission des Primärstrahls registriert. In der Abfolge der Radiogramme werden die lokalen Orientierungsänderungen der Probekörper-Grenzflächen bei deren Abtastung mit wenigen Mikrometern Schrittweite bildhaft verfolgt. Mit der hier erreichten Winkelauflösung von etwa 3 Bogensekunden (Streuvektor-Inkremente Δk = 10-3nm-1) kann bei 50 µm Ortsauflösung das Materialvolumen bezüglich innerer Grenzflächen mit Nanometer-Separation auch bei hohen Abtastraten unterhalb einer Sekunde pro Bild charakterisiert werden.
Bikontinuierliche poröse Keramiken für Filteranwendungen weisen eine komplizierte Mikrostruktur auf, in der Poren und Festkörperphase 'vermischt' sind. Mechanische, thermische sowie Filtereigenschaften können nur präzise bestimmt werden, wenn die Morphologie beider Phasen quantitativ angegeben werden kann. Hier werden unter Anwendung von 3D Computertomographie (CT) und verschiedenen Techniken, die auf der Röntgenrefraktion basieren, die Porosität und die Porenorientierung in keramischen Cordierit-Dieselpartikelfiltern bewertet. Dabei werden zur Auswertung der Tomogramme die Fouriertransformierten sowie eine neu entwickelte richtungssensitive Bildanalyse (DIVA, directional interface variance analysis) angewandt. Sowohl die genannten Messtechniken als auch der statistische Ansatz gestatten die Extraktion optional ortsaufgelöster oder gemittelter Werte. Es ergeben sich sehr gute Übereinstimmungen der experimentell ermittelten Porositätswerte mit Ergebnissen aus Quecksilberintrusionsversuchen als auch der ermittelten Porenorientierung im Vergleich zu publizierten Angaben zur kristallographischen Textur. Dies legt den Schluss nahe, dass die Kenntnis der Grenzflächen (zwischen Poren und Materie) genügt, die morphologischen Eigenschaften solcher Materialien hinreichend zu beschreiben.
Wir stellen eine Prozedur vor, mit der typische 'Missing Wedge' (MW)-Artefakte in CT-Rekonstruktionen effektiv unterdrückt werden können. Dazu wird der iterative DIRECTT-Algorithmus (Direkte Iterative Rekonstruktion Computertomographischer Trajektorien) mit einigen Zyklen diskreter Rekonstruktion eingesetzt. Die Kernfunktionen des Algorithmus', die wiederholte Auswahl und Gewichtung von Elementen einer Zwischenkonstruktion, werden beibehalten. Abgesehen von Sonderfällen der Röntgen- und Neutronentomographie tritt die MW-Restriktion (neben einer Vielzahl anderer) in Standardkonfigurationen der Elektronentomographie auf. Um den MW-Effekt isoliert zu untersuchen und beurteilen zu können, werden hier vollständige experimentelle Datensätze einer bekannten Porenstruktur um einen Sektor beschnitten sowie MW-Rekonstruktionen von Porenmodellen erzeugt. Die Ergebnisse werden mit zurzeit verbreiteten Algorithmen (Gefilterte Rückprojektion (FBP) und ART-Varianten) verglichen. Die Bewertung im Fourierraum zeigt, dass DIRECTT die fehlende Information im MW erfolgreich ergänzt. Zur quantitativen Bewertung der lokalen Rekonstruktionsqualität werden Methoden der räumlichen Statistik eingesetzt.
Bi-continuous porous ceramics for filtration applications possess a particularly complicated microstructure, whereby porosity and solid matter are 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 3D computed tomography (CT) at different resolutions, and several X-ray refraction-based techniques, we quantitatively evaluated porosity and pore orientation in cordierite diesel particulate filter ceramics.Moreover, applying both Fast Fourier Transform (FFT) and a newly developed image analysis algorithm (directional interface variance analysis, DIVA), we quantitatively evaluated porosity and pore orientation. Both the experimental techniques and the statistical approach allow extraction of spatially resolved or average values.Porosity values from synchrotron computed tomography used turn out to agree with mercury intrusion measurements, while pore orientation factors agree with published crystallographic texture data. This latter point also implies that the study of the pore/matter interface is sufficient to describe the morphological properties of these materials.
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.
For the first time we present direct 2D imaging of refracted X-rays without any discrimination of the Primary radiation. X-refraction works in analogy to visible light optics: X-rays are entirely deflected at interfaces where discontinuities of (electron) density occur. This is demonstrated at the example of inner and outer surfaces of model samples of well-defined geometry (fibres, capillaries, and monodisperse micro particles). The samples are scanned through a 50 μm monochromatic (20 keV) pencil beam. In order to warrant a sufficient angular resolution a 2D detector (pixel size 7 μm) is placed 3 m downstream of the sample. Scanning the sample in micron steps allows for detecting local changes of interface / surface orientation directly in two dimensions. At the actual angular resolution of about 3 seconds of arc (scattering vector increments Δk = 10-3 nm-1) and 50 μm spatial resolution (scanning) the material’s inner surfaces (with nanometer separation) can be characterized even at sampling rates below 1 second per frame. Moreover, our technique is suited to directly determine particle diameters of up to 250 nm by means of diffraction fringes. Some potential applications to technical submicron structures are discussed.
X-ray dark field imaging
(2014)
A new kind of enhanced contrast X-ray imaging of weakly absorbing materials in dark field mode is presented.
Samples such as plastics and biological tissue are a perpetual challenge for radiographic imaging. Recent innovative approaches such as Diffraction Enhanced Imaging (DEI), “phase contrast”, grating interferometry (Talbot-Lau), or Refraction Enhanced Imaging (REI) have in common that they yield enhanced contrast based on deflected X-rays.
Here, we introduce a REI modification, which works with a slightly bent single crystal reflecting in Bragg geometry. The samples are placed upstream of the thin crystal within a parallel synchrotron beam. The crystal’s curvature creates a dark-field stripe in the transmission image, similar to the inverse of a Darwin-Prins rocking curve of plane crystals. The reflection condition is met better or worse as a steady function of incidence position.
Refracted beam portions of sample interfaces appear bright on black stripes. The entire image is finally synthesized by multiple dark-field stripes. The technique is an alternative to the mentioned techniques. We demonstrate the technique’s advantage by examples of biological and technical microstructures.
Statistical analysis of tomographic reconstruction algorithms by morphological image characteristics
(2010)
We suggest a procedure for quantitative quality control of tomographic reconstruction algorithms. Our task-oriented evaluation focuses on the correct reproduction of phase boundary length and has thus a clear implication for morphological image analysis of tomographic data. Indirectly the method monitors accurate reproduction of a variety of locally defined critical image features within tomograms such as interface positions and microstructures, debonding, cracks and pores. Tomographic errors of such local nature are neglected if only global integral characteristics such as mean squared deviation are considered for the evaluation of an algorithm. The significance of differences in reconstruction quality between algorithms is assessed using a sample of independent random scenes to be reconstructed. These are generated by a Boolean model and thus exhibit a substantial stochastic variability with respect to image morphology. It is demonstrated that phase boundaries in standard reconstructions by filtered backprojection exhibit substantial errors. In the setting of our simulations, these could be significantly reduced by the use of the innovative reconstruction algorithm DIRECTT.
Die mitunter erhebliche Verschmierung von computertomograpischen Projektionen durch ausgedehnte Strahlenquellen wird durch eine neuartige Entschmierungsprozedur erheblich reduziert, um eine verbesserte Ortsauflösung der Rekonstruktion zu erreichen. Da die Breite der Verschmierungsfunktion der detektornahen und -fernen Objektelemente sich erheblich unterscheiden kann, muss die Entschmierung variabel sein. Im Gegensatz zu einer für alle Voxel-Positionen identischen Entfaltung, also einer grundsätzlich falschen Voraussetzung, wurde eine implizite Entschmierung entwickelt. Die vorab bekannte positionsabhängige Verschmierung wird auf die iterativ wiederholten Projektionen der Teilrekonstruktionen des DIRECTT-Algorithmus angewandt. Die variabel entschmierten Rekonstruktionen aus den Sinogrammen eines Pixelmodells mit Verschmierungen von 1 bis 5 Pixel erreichen eine Ortsauflösung von nahezu einem Pixel.
The emerging technology of generation and detection of Terahertz waves (1 THz = 1012
Hz) offers diverse potentials in non-destructive testing (NDT) regarding security as well
as safety aspects. Herein, we focus on the latter with emphasis on imaging techniques.
The THz range (0.1
10 THz, 3mm
30 µm) closes the technological gap between
ultra high frequency electronics and FIR optics in the electro-magnetic (EM) spectrum.
Electro-optical sampling provides straight access to the EM wave including its phase
(rather than intensity). THz waves are well suited to characterize non-metallic materials
since they penetrate paper, plastics, ceramics and certain composites (e.g. GFC).
We employ a commercial fibre-coupled THz time domain spectrometer (TDS) for
scanning the samples laterally through a focal spot. At each position the entire temporal
pulse train is recorded, which offers the opportunity to use various parameters derivable
for imaging.
Topographic measurements are performed as reflection set-up. The achievable spatial
resolution is diffraction limited at about 100 µm -300 µm (which allows for perception
of single defects on a sub-mm scale). In contrast to typical pulse echoed ultrasound
testing THz topography is a non-contact inspection tool without coupling agents.
Several reflections of subsequent concealed layers are detected instead of just the first
encountered one. Comparing to X-ray (radiology) the non-ionizing THz-waves generate
images of similar contrast regarding metal and plastic (organic) components, while
conventional radiography emphasizes one type of material depending on the energy preselected.
Moreover, the full temporal information is exploited to derive spectra in
certain selected time windows, i.e. separated spectral properties of each layer in
multilayered structures.
Tomographic measurements are performed in transmission mode. The sample is
mounted on a rotation stage in order to allow for lateral scanning under the different
projection angles. The reconstruction is typically performed by filtered backprojection,
which is widely used for X-ray CT. The adaption of this technique to the THz range
comes along with several experimental drawbacks such as considerable refraction and
scattering. According to these difficulties we investigate the occurring artefacts. The
THz-TDS provides the opportunity to calculate a separate backprojection of each
frequency interval as obtained by the Fourier transformation of the recorded time
resolved amplitude. This results in a spectrally resolved reconstruction of each voxel,
which is unique in computed tomography technology.
Computed tomography reconstructions of projected data usually assume an ideal point-like
focal spot. However, in practice, the actual finite focus size leads to blurred projections,
unavoidably. The elements (voxels) of the reconstruction array are smeared differently as a
function of their individual position relative to source and detector. Neglecting the focal
smearing generates considerably blurred reconstructions. Previous attempts were based on
directly deconvolving blurred projections from a constant kernel, which yields better results
but still exhibits artefacts. Iterative algorithms can be adopted to take into account focal
smearing as a function of position. However, this requires detailed prior knowledge of
quantitative smear functions. The DIRECTT (Direct Iterative Reconstruction of Computed
Tomography Trajectories) algorithm is a promising candidate to meet these requirements. It
has been demonstrated elsewhere that DIRECTT copes with limited data sets such as
limited view and region-of- interest data by tracing single sinusoidal-like trajectories in
Radon space, which are selected from the set of all possible trajectories by appropriate
criteria. Currently, position-dependent smearing is used in the projection part of iterations.
At the example of model reconstructions we demonstrate the gain of spatial resolution by
iterative variable desmearing according to the DIRECTT algorithm in comparison to the
standard filtered back-projection.
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.
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.
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.
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.
Als Alternative zur Neutronentomographie wird das Potenzial der Computertomographie (CT) mit inkohärenter Röntgen-Streustrahlung (Compton-Streuung) untersucht. Die gleichzeitige Abbildung von Materialien sehr unterschiedlicher Dichten (Ordnungszahlen) ist eine wiederkehrende Herausforderung für die Radiologie und die Computertomographie mit Röntgenstrahlung. Die Messungen ergeben asymmetrische Projektionsprofile für Sinogramme der Streuintensität. Am Beispiel verschiedener Polymere (Polyethylen, Polyamid, PVC), Glas und Holz wird in den Tomogrammen ein hochaufgelöster 'Comptonkontrast' vergleichbarer Dynamik erreicht, während der simultan gemessene 'Absorptionskontrast' ausschließlich die starken Absorber (Glas und PVC) zeigt. Der Vergleich mit ähnlich auflösender Neutronentomographie zeigt ähnliche Kontraste und eröffnet mithin die Möglichkeit, diese künftig durch Compton-Tomographie im Labormaßstab zu ersetzen.
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.
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.
Die Computertomographie (CT) ist in der Medizin als Standardtechnik etabliert, in der zerstörungsfreien Prüfung wird sie zunehmend angewendet, in einzelnen Fällen sogar als Referenzverfahren eingesetzt. Gegenwärtig ist eine starke Zunahme von Anwendungen der CT in der Materialcharakterisierung zu verzeichnen. Zudem werden weitere moderne 3D-Techniken für werkstoffwissenschaftliche Fragestellungen genutzt, um die Mikrostruktur - auch in situ (z.B. Druck, Temperatur) - aufzuklären. Hier werden neben der konventionellen Absorptions-CT auch die Potenziale der Refraktions-CT zur Beantwortung prozesstechnischer sowie werkstofflicher Fragestellungen aufgezeigt, die ein „ganzheitliches Bild“ des jeweiligen Werkstoffs zum Ziel haben.
Grating interferometric set-ups have been established in the last decade. They are promising candidates to obtain enhanced image contrast from weakly absorbing micro and nano structures. They are based on X-ray refraction and near-field diffraction using the Talbot effect.
At the expense of taking multiple images, Talbot-Lau grating interferometry allows separating the absorption, refraction, and scattering contributions by analysing the disturbances of a phase grating interference pattern. Contrary to other refraction enhanced methods, this technique can be applied using conventional X-ray tubes (divergent, polychromatic source). This makes it attractive to solve typical non-destructive testing problems.
We investigated the efficiency of phase gratings, i.e. the visibility (the amplitude of oscillations) upon variation of propagation distance and phase grating rotation around an axis parallel to the grid lines. This grating rotation changes the grating shape (i.e. the distributions of phase shifts). This can yield higher visibilities than derived from rectangular shapes.
Our study includes experimental results obtained from synchrotron radiation, as well as simulations for monochromatic radiation. The advantages of Talbot-Lau interferometry are demonstrated at the example of glass capillaries.
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.
A strategy to mitigate typical reconstruction artefacts in missing wedge computed tomography is presented. These artefacts appear as elongations of reconstructed details along the mean direction (i.e. the symmetry centre of the projections). Although absent in standard computed tomography applications, they are most prominent in advanced electron tomography and also in special topics of X-ray and Neutron tomography under restricted geometric boundary conditions. We investigate the Performance of the DIRECTT (Direct Iterative Reconstruction of Computed Tomography Trajectories) algorithm to reduce the directional artefacts in standard procedures. In order to be sensitive to the anisotropic nature of missing wedge artefacts, we investigate isotropic substructures of metal foam as well as circular disc models. Comparison is drawn to filtered backprojection and algebraic techniques. Reference is made to reconstructions of complete data sets. For the purpose of assessing the reconstruction Quality, Fourier transforms are employed to visualize the missing wedge directly. Deficient reconstructions of disc models are evaluated by a length-weighted boundary orientations. The DIRECTT results are assessd at different signal-to-noise ratios by means of local and integral evaluation Parameters.
The potentials of incoherent X-ray scattering (Compton) computed tomography (CT) are investigated. The imaging of materials of very different atomic number or density at once is generally a perpetual challenge for X-ray tomography or radiography. In a basic laboratory set-up for simultaneous perpendicular Compton scattering and direct beam attenuation tomography are conducted by single channel photon counting line scans. This results in asymmetric distortions of the projection profiles of the scattering CT data set. In 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. Comparison to neutron tomography
reveals astonishing similarities except for the glass component (without hydrogen). Therefore, Compton CT offers the potential to replace neutron tomography, which requires much more efforts.
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.
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.