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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.
While the problem of the identification of mechanisms of hydrogen assisted damage has and is being thoroughly studied, the quantitative analysis of such damage still lacks suitable tools. In fact, while, for instance, electron microscopy yields excellent characterization, the quantitative analysis of damage requires at the same time large field-of-views and high spatial resolution. Synchrotron X-ray refraction techniques do possess both features. In this work, we show how synchrotron X-ray refraction computed tomography (SXRCT) can quantify damage induced by hydrogen embrittlement in a lean duplex steel, yielding results that overperform even those achievable by synchrotron X-ray absorption computed tomography. As already reported in literature, but this time using a non-destructive technique, we show that the hydrogen charge does not penetrate to the center of tensile specimens. By the comparison between virgin and hydrogen-charged specimens, we deduce that cracks in the specimen bulk are due to the rolling process rather than hydrogen-assisted. We show that (micro)cracks propagate from the surface of tensile specimens to the interior with increasing applied strain, and we deduce that a significant crack propagation can only be observed short before rupture.
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.
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.
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.
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.
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.
Es wird ein Verfahren zur Röntgenabbildung schwach absorbierender Objekte vorgestellt. Als kontrastgebender Effekt wird die Röntgenrefraktion an Ober- und Grenzflächen ausgenutzt. Zur Erzeugung eines sogenannten Dunkelfeldes wird ein schwach gekrümmter Transmissionskristall eingesetzt, der lokal, d.h. in einem kleinen Ausschnitt des Einstrahlquerschnitts, die Bragg-Bedingung erfüllt. Innerhalb dieser Zone erscheinen die durch Refraktion abgelenkten Strahlkomponenten als hell leuchtende Interface-Strukturen. Die Synthese mehrerer Dunkelfeldstreifen ergibt hochaufgelöste 2D Beispiel von biologischen und technischen Mikrostrukturen.
Hinterleuchten stellt eine oft unerkannte Fehlweisung in der radiographischen Abbildung mit Flächendetektoren dar, die durch diffuse Umverteilung der Intensität verursacht wird. Dieser Effekt kann die korrekte Transmissions-Intensität eines Probekörpers gemäß dem Lambert-Beer'schen Gesetz erheblich verfälschen. Hinterleuchten wird sowohl mit Bremsstrahlung von Röntgenröhren als auch mit monochromatischer Synchrotronstrahlung beobachtet. Die fehlerhaft reduzierten Schwächungskoeffizienten von einigen 10 % korrelieren mit der Strahlschwächung und dem direkt bestrahlten Detektorbereich. Für eine einfache numerische Korrektur des Hinterleuchtens werden lediglich integrale Intensitätswerte benötigt.
Modellrechnungen mit dem CT-Algorithmus DIRECTT (Direkte iterative Rekonstruktion computertomographischer Trajektorien) haben die Vorteile gegenüber anderen Ansätzen bezüglich Ortsauflösung und Dichte gezeigt, insbesondere auch für unvollständige Datensätze wie Limited View- und Region of Interest-Szenarien. Entsprechend dem Normalfall werden hier jedoch vollständige Datensätze von Modellen und Messungen und ihre Rekonstruktionen bewertet. Die Qualität von DIRECTT wird mit der Gefilterten Rückprojektion anhand der Modulations-Transfer-Funktion (MTF) sowie integraler Kenngrößen im Radon- und im Ortsraum verglichen. Zur Überprüfung der Rekonstruktionsgenauigkeit experimenteller Daten werden Mustermessungen einfacher Probengeometrien unter definierten physikalischen Bedingungen durchgeführt. Diese betreffen Monochromasie, Unterdrückung von Kantenartefakten und radiometrische Intensitätsbestimmung mit Einkanaldetektor.
We present transmission electron microscope (TEM) tomography investigations of ruthenium-based fuel cell catalyst materials as employed in direct methanol fuel cells (DMFC). The digital three-dimensional representation of the samples not only enables detailed studies on number, size, and shape but also on the local orientation of the ruthenium particles to their support and their freely accessible surface area. The shape analysis shows the ruthenium particles deviate significantly from spherical symmetry which increases their surface to volume ratio. The morphological studies help to understand the structure formation mechanisms during the fabrication as well as the high effectiveness of these catalysts in the oxygen reduction reaction at the cathode side of fuel cells.
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.