Filtern
Erscheinungsjahr
Dokumenttyp
Schlagworte
- Computed tomography (8)
- Electron tomography (8)
- DIRECTT (5)
- Reconstruction algorithm (5)
- Catalyst (4)
- Fuel cell (4)
- Neutron tomography (4)
- Tomography (4)
- Computer-Tomographie (3)
- Elektronen-Tomographie (3)
Organisationseinheit der BAM
In-situ-Neutronenradiografie wird erfolgreich eingesetzt, um flüssiges Wasser in Niedertemperatur-PEM-Brennstoffzellen während des Betriebs zerstörungsfrei abzubilden und das sogenannte Wassermanagement eine der größten Herausforderungen der Entwicklung durch Anpassung der Materialeigenschaften zu optimieren. Dabei werden die besonderen Eigenschaften der Neutronen genutzt, die metallische Bauteile relativ leicht durchdringen, während selbst kleine Wassermengen durch ihre starke Streuung leicht nachweisbar sind. Die relativ langen Messzeiten für die Neutronentomografie werden durch den Betrieb der Zelle im angehaltenen Zustand realisierbar, sodass die dreidimensionale Wasserverteilung darstellbar wird.
In this work, the applicability of a new 3D micro X-ray fluorescence (3D Micro-XRF) laboratory spectrometer for the investigation of historical glass objects is demonstrated. The non-destructiveness of the technique and the possibility to measure three-dimensionally resolved fluorescence renders this technique into a suitable tool for the analysis of cultural heritage objects. Although absorption and resolution effects complicate qualitative analysis of the data, layered structures can be distinguished from homogeneous samples without the need for full quantification. Different manufacturing techniques were studied in this work with the help of hand-made reference samples. With the gained knowledge it could be shown for the investigated historical glass object, that black enamel as a stained glass contour colour was used in a cold painting. The object was not fired after the application of the black enamel, but instead the adhesion of the paint was solely provided through organic binding agents and the backing with metal foils. Thus, for the manufacturing of the object, a mixture of cold painting technique with a stained glass color was used. Quantitative measurements with a 3D Micro-XRF setup at the Berlin synchrotron BESSY II confirm the assumptions drawn on the basis of the qualitative investigation with the 3D Micro-XRF spectrometer with X-ray tube excitation.
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.
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.
While X-ray based darkfield imaging with grating interferometers is already widely used, darkfield imaging with neutrons has still a relatively small user community focused mostly on magnetic materials. Here, we demonstrate the application of neutron darkfield imaging byTalbot-Lau type grating interferometry to fiber reinforced plastics. Common carbon and glass fiber composites have been investigated including characteristic damage structures. The darkfield images show a strong signal response caused by fiber delamination, suitable fiber direction, particles, pores and cracks. The basic principles of neutron darkfield imaging applied to fiber composites are highlighted.
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.
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.
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.
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.
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.
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.
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.
In various kinds of radiography, deficient transmission imaging may occur due to backlighting inside the detector itself arising from light or radiation scattering. The related intensity mismatches barely disturb the high resolution contrast, but its long range nature results in reduced attenuation levels which are often disregarded. Based on X-ray observations and an empirical formalism, a procedure is developed for a first order correction of detector backlighting. A backlighting factor is modeled as a function of the relative detector coverage by the sample projection. Different cases of sample transmission are regarded at different backlight factors and detector coverage. The additional intensity of backlighting may strongly affect the values of materials’ attenuation up to a few 10%. The presented scenario provides a comfortable procedure for corrections of X-ray or neutron transmission imaging data.
A general method to carry out the fluorination of metal oxides with poly(tetrafluoroethylene) (PTFE, Teflon) waste by spark plasma sintering (SPS) on a minute scale with Teflon is reported. The potential of this new approach is highlighted by the following results. i) The tantalum oxyfluorides Ta3O7F and TaO2F are obtained from plastic scrap without using toxic or caustic chemicals for fluorination. ii) Short reaction times (minutes rather than days) reduce the process time the energy costs by almost three orders of magnitude. iii) The oxyfluorides Ta3O7F and TaO2F are produced in gram amounts of nanoparticles. Their synthesis can be upscaled to the kg range with industrial sintering equipment. iv) SPS processing changes the catalytic properties: while conventionally prepared Ta3O7F and TaO2F show little catalytic activity, SPS-prepared Ta3O7F and TaO2F exhibit high activity for photocatalytic oxygen evolution, reaching photoconversion efficiencies up to 24.7% and applied bias to photoconversion values of 0.86%. This study shows that the materials properties are dictated by the processing which poses new challenges to understand and predict the underlying factors.
Solid state reactions are slow because the diffusion of atoms or ions through the reactant, intermediate and crystalline product phases is the rate-limiting step. This requires days or even weeks of high temperature treatment, and consumption of large amounts of energy. We employed spark-plasma sintering, an engineering technique that is used for high-speed consolidation of powders with a pulsed Electric current passing through the sample to carry out the fluorination of niobium oxide in minute intervals. The approach saves time and large amounts of waste energy. Moreover, it allows the preparation of fluorinated niobium oxides on a gram scale using poly (tetrafluoroethylene) (®Teflon) scrap and without toxic chemicals.
The synthesis can be upscaled easily to the kg range with appropriate sintering equipment. Finally, NbO2F and Nb3O7F prepared by spark plasma sintering show significant photoelectrocatalytic (PEC) oxygen evolution from water in terms of photocurrent density and incident photon-to-current Efficiency (% IPCE), whereas NbO2F and Nb3O7F prepared by conventional high temperature chemistry show little to no PEC response. Our study is a proof of concept for the quick, clean and energy saving production of valuable photocatalysts from plastic waste.
Ziel des Projektes HARFE (Haftfestigkeit Reproduzierbarkeit Festigkeit) war es, eine Er-höhung der Haft- bzw. Klebfestigkeit auf Niedrigenergie-Polymeren (PE, PP, PTFE) zu erreichen. SENTECH realisierte dazu plasmachemische Oberflächenaktivierungen mit O2 und die Abscheidung von Aluminiumoxidschichten (Al2O3) mittels Atomic Layer Deposition (ALD), wobei die Ellipsometrie zum in-situ Monitoring der ALD-Prozesse diente. Die BAM charakterisierte die modifizierten Oberflächen bezüglich der Oberflächenenergie (OFE) und bestimmte die Verbund- bzw. Klebfestigkeit mittels der Zentrifugentechnologie