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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.
The residual stresses and load transfer in multiphase metal alloys and their composites (with both random planar-oriented short fibers and particles) will be shown, as studied by neutron diffraction, by X-ray computed tomography, and by a model based on the reformulation of classic Maxwell’s homogenization method.
Contrary to common understanding and state-of-the-art models, we experimentally observe that randomly oriented phases possess non-hydrostatic residual stress. Moreover, we disclose that the unreinforced matrix alloy stays under hydrostatic compression even under external uniaxial compression.
The recently developed modeling approach allows calculating the residual stress in all phases of the composites. It rationalizes the presence of deviatoric stresses accounting for the interaction of random oriented phases with fibers having preferential orientation. It also allows the explanation of the unconventional in-situ behavior of the unreinforced alloy and the prediction of the micromechanical behavior of other similar alloys.
Additiv gefertigte (AM) dreifach periodische metallische minimale Oberflächenstrukturen (TPMSS, aus dem Englischen Triply Periodic Minimum Surface Structures) erfüllen mehrere Anforderungen sowohl im biomedizinischen als auch im technischen Bereich: Abstimmbare mechanische Eigenschaften, geringe Empfindlichkeit gegenüber Herstellungsfehlern, mechanische Stabilität und hohe Energieabsorption. Allerdings stellen sie auch einige Herausforderungen in Bezug auf die Qualitätskontrolle dar, die ihre erfolgreiche Anwendung verhindern können. Tatsächlich ist die Optimierung des AM-Prozesses ohne die Berücksichtigung struktureller Merkmale wie Fertigungsgenauigkeit, interne Defekte sowie Oberflächentopographie und -rauheit unmöglich. In dieser Studie wurde die quantitative zerstörungsfreie Analyse von Ti-6Al-4V-Legierung TPMSS mit Hilfe der Röntgen-Computertomographie (XCT) durchgeführt. Es werden mehrere neue Bildanalyse-Workflows vorgestellt, um die Auswirkungen der Aufbaurichtung auf die Wanddickenverteilung, die Wanddegradation und die Verringerung der Oberflächenrauheit aufgrund des chemischen Ätzens von TPMSS zu bewerten. Es wird gezeigt, dass die Herstellungsgenauigkeit für die Strukturelemente, die parallel und orthogonal zu den hergestellten Schichten gedruckt werden, unterschiedlich ist. Verschiedene Strategien für das chemische Ätzen zeigten unterschiedliche Pulverabtragsfähigkeiten und damit ein Gradient der Wanddicke. Dies wirkte sich auf die mechanische Leistung unter Druck durch die Verringerung der Streckspannung aus. Eine positive Auswirkung des chemischen Ätzens ist die Verringerung der Oberflächenrauhigkeit, die möglicherweise die Ermüdungseigenschaften der Bauteile verbessern kann. Schließlich wurde XCT eingesetzt, um die Menge des zurückgehaltenen Pulvers mit der Porengröße des TPMSS zu korrelieren, wodurch der Herstellungsprozess weiter verbessert werden kann.
Additively manufactured (AM) metallic sheet-based Triply Periodic Minimal Surface Structures (TPMSS) meet several requirements in both bio-medical and engineering fields: Tunable mechanical properties, low sensitivity to manufacturing defects, mechanical stability, and high energy absorption. However, they also present some challenges related to quality control. In fact, the optimization of both the AM process and the properties of TPMSS is impossible without considering structural characteristics as manufacturing accuracy, internal defects, and as well as surface topography and roughness. In this study, the quantitative non-destructive analysis of TPMSS manufactured from Ti-6Al-4V alloy by electron beam melting was performed by means of laboratory X-ray computed tomography (XCT).
Additively manufactured (AM) triply periodic metallic minimum surface structures (TPMSS, from the English Triply Periodic Minimum Surface Structures) fulfill several requirements in both biomedical and engineering fields: tunable mechanical properties, low sensitivity to manufacturing defects, mechanical stability, and high energy absorption. However, they also present some quality control challenges that may prevent their successful application. In fact, optimization of the AM process is impossible without considering structural features such as manufacturing accuracy, internal defects, and surface topography and roughness. In this study, quantitative nondestructive analysis of Ti-6Al-4V alloy TPMSS was performed using X-ray computed tomography (XCT). Several new image analysis workflows are presented to evaluate the effects of buildup direction on wall thickness distribution, wall degradation, and surface roughness reduction due to chemical etching of TPMSS. It is shown that the fabrication accuracy is different for the structural elements printed parallel and orthogonal to the fabricated layers. Different strategies for chemical etching showed different powder removal capabilities and thus a gradient in wall thickness. This affected the mechanical performance under compression by reducing the yield stress. A positive effect of chemical etching is the reduction of surface roughness, which can potentially improve the fatigue properties of the components. Finally, XCT was used to correlate the amount of powder retained with the pore size of the TPMSS, which can further improve the manufacturing process.
A paradigm shift in the description of creep in metals can only occur through multi-scale imaging
(2022)
The description of creep in metals has reached a high level of complexity; fine details are revealed by all sorts of characterization techniques and different theoretical models. However, to date virtually no fully microstructure-driven quantitative description of the phenomenon is available. This has brought to interesting inconsistencies; the classic description of (secondary) creep rests on the so-called power law, which however: a- has a pre-factor spanning over 10 orders of magnitude; b- has different reported exponents for the same material; c- has no explanation for the values of such exponents.
Recently, a novel description (the so-called Solid State Transformation Creep (SSTC) Model) has been proposed to tackle the problem under a different light. The model has two remarkable features: 1- it describes creep as the accumulation of elementary strains due to dislocation motion; 2- it predicates that creep is proceeding by the evolution of a fractal arrangement of dislocations. Such description, however, needs a great deal of corroborating evidence, and indeed, is still incomplete.
To date, we have been able to observe and somehow quantify the fractal arrangement of microstructures through Transmission Electron Microscopy (TEM), observe the accumulation of dislocations at grain boundaries by EBSD-KAM (Electron Back-Scattered Diffraction-Kernel Angular Misorientation) analysis, quantify the kinetic character (solid state transformation) of experimental creep curves, and estimate the sub-grain size of the fractal microstructure through X-ray refraction techniques. All pieces of the mosaic seem to yield a consistent picture: we seem being on the right path to reconstruct the whole elephant by probing single parts of it. What is still missing is the bond between the various scales of investigation.
In this work, synchrotron X-ray refraction radiography (SXRR) was combined with in-situ heat treatment to monitor microstructure and porosity evolution as a function of temperature. The investigated material was a laser powder bed fusion (LPBF) manufactured AlSi10Mg, where the initial eutectic Si network is known to break down into larger particles with increasing temperature. Such alloy is also prone to thermally induced porosity (TIP). We show that SXRR allows detecting the changes in the Si-phase morphology upon heating, while this is currently possible only using scanning electron microscopy. SXRR also allows observing the growth of pores, usually studied via X-ray computed tomography, but on much smaller fields-of-view. Our results show the great potential of in-situ SXRR as a tool to gain in-depth knowledge of the susceptibility of any material to thermally induced damage and/or microstructure evolution over statistically relevant volumes.
The availability of high-performance Al alloys in AM is limited due to difficulties in printability, requiring both the development of synergetic material and AM process to mitigate problems such as solidification cracking during laser powder bed fusion (LPBF). The goal of this work was to investigate the failure mechanism in a LPBF 7017 Aluminium alloy + 3 wt% Zr + 0.5 wt% TiC. The processing leads to different categories of Zr-rich inclusions, precipitates and defects.
The micromechanical behavior of an annealed Ti-6Al-4V material produced by Laser Powder Bed Fusion was characterized by means of in-situ synchrotron X-ray diffraction during a tensile test. The lattice strain evolution was obtained parallel and transversal to the loading direction. The elastic constants were determined and compared with the conventionally manufactured alloy. In the plastic regime, a lower plastic anisotropy exhibited by the lattice planes was observed along the load axis (parallel to the building direction) than in the transverse direction.
Also, the load transfer from α to β phase was observed, increasing global ductility of the material. The material seems to accumulate a significant amount of intergranular strain in the transverse direction.
Additively manufactured (and in particular laser powder bed fused) materials represent a manyfold challenge for the materials scientist and engineer because of their distinctive microstructure. If laser powder bed fusion is used to produce components, the complexity level increases because meso-structures (e.g., overhanging features, surface and internal defects) gain importance. Furthermore, if the main advantage of additive manufacturing, i.e., the freedom of design, is to be fully exploited, and geometrically complex structures, such as lattices, are manufactured, then such structures become meta-materials. This means that the geometry and the materials properties become equally important.
This matryoshka-like (more literary than the dry “multi-scale”) complexity makes the characterization of the residual stress fields by means of diffraction methods so difficult with the current means, that new paradigms are necessary to tackle the challenge.
Indeed, classic open problems acquire an extra layer of difficulty, such that new solutions need to be found and the sometimes-dormant debate needs to be re-opened. Examples include the determination of: a- the unstrained reference: this reference can become location-dependent and needs to be carefully determined; b- the so-called diffraction elastic constants, which becomes immensely challenging since even the single-crystal elastic constants are not known for additively manufactured materials.
On top of this, other problems arise. The determination of the principal axes of stress becomes non-trivial because the hatching strategy sometimes dominates over the sample geometry. Even further, in complex structures, such as lattices, the textbook statement that the strain measurement in six independent directions uniquely identifies the strain tensor becomes simply invalid. The peculiar surface features of additively manufactured materials transform trivial tasks into formidable challenges: the precise alignment of a specimen in a beam or the determination of surface stresses with laboratory X-rays need to be thoroughly re-discussed and lay far from being routine tasks.
In this paper, we will show a few examples of the cases mentioned above. We will demonstrate that sometimes the classic approach works very well, but other times surprising conclusions can be drawn from in-depth studies of the residual stress in additively manufactured materials. In short, we predicate that classic methods cannot be used on additively manufactured materials and structures without a critical evaluation of their validity and application range.
Alternative to conventional transmission-based radiography and computed tomography, X-ray refraction techniques are being increasingly used to detect damage in light materials. In fact, their range of application has been recently extended even to metals. The big advantage of X-ray refraction techniques is that they are able to detect nanometric defects, whose size would lie below the resolution of even state-of-the-art synchrotron-based X-ray computed tomography (SXCT). The superiority of synchrotron X-ray refraction radiography and tomography (SXRR and SXRCT) has been shown in the case of light materials, in particular composites. X-ray refraction techniques also yield a quantitifaction of the amount of damage (the so-called relative internal specific surface) and can well be compared with damage models. At the same time, it is impossible for SXRR and SXRCT to image single defects. We show that the combination of refraction- and transmission-based imaging techniques yields an impressive amount of additional information about the type and amount of defects in microstructured materials such as additively manufactured metals or metal matrix composites. We also show that the use of data fusion techniques allows the classification of defects in statistically significant representative volume elements.
Alternative to conventional transmission-based radiography and computed tomography, X-ray refraction techniques are being increasingly used to detect damage in light materials. In fact, their range of application has been recently extended even to metals. The big advantage of X-ray refraction techniques is that they are able to detect nanometric defects, whose size would lie below the resolution of even state-of-the-art synchrotron-based X-ray computed tomography (SXCT). The superiority of synchrotron X-ray refraction radiography and tomography (SXRR and SXRCT) has been shown in the case of light materials, in particular composites. X-ray refraction techniques also yield a quantitifaction of the amount of damage (the so-called relative internal specific surface) and can well be compared with damage models. At the same time, it is impossible for SXRR and SXRCT to image single defects. We show that the combination of refraction- and transmission-based imaging techniques yields an impressive amount of additional information about the type and amount of defects in microstructured materials such as additively manufactured metals or metal matrix composites. We also show that the use of data fusion techniques allows the classification of defects in statistically significant representative volume elements.
Wir präsentieren Labor- und Synchrotron-Röntgenrefraktionstechniken, wie sie an der BAM implementiert sind.
Wir zeigen, dass die Labor-Röntgenrefraktionstopographie (XRRT) und die Synchrotron-Röntgenrefraktionsradiographie (SRRR) außergewöhnliche Werkzeuge zur Untersuchung von Schädigungen und inneren Defekten (Poren, Mikrorisse) in leichten Materialien wie Keramiken und Kompositen sind. Tatsächlich nutzen diese Techniken den an Grenzflächen auftretenden Röntgenbrechungseffekt aus, um den Kontrast zwischen dem (schwach absorbierenden) Objekt und dem Hintergrund zu erhöhen. Dies ermöglicht die Erkennung sehr kleiner Objekte (sogar bis zu 1 nm Rissöffnung) und die Quantifizierung ihrer spezifischen Oberfläche, die mit ihrem Einfluss auf die Materialeigenschaften korreliert. Wir zeigen die folgenden Anwendungen: a) Quantifizierung der Faserentbindung in laminaten Epoxid-Kohlenstoff-Verbundwerkstoffen; b) Mapping der Porengröße in gesinterten Keramiken; c) Eindringstiefe von Aschen in Keramikschutzschichten; d) Quantifizierung der Porenorientierung in Diesel Partikelfiltern; e) 3D-Darstellung von Makrorissen und Faserentbindung in Verbundwerkstoffen auf Ti-Basis für Anwendungen in der Luft- und Raumfahrt (unter Verwendung von Röntgenrefraktionstomographie).
Die Degradation von Wärmedämmschichten(thermal barrier coatings - TBCs) in Gasturbinen durch glasartige Calcium-Magnesium-Aluminiumsilikat (CMAS)Ablagerungen aus verschiedenen Quellen istseit vielen Jahren ein anhaltendes Problem. In dieser Studie wurde mit Hilfe derSynchrotron-Röntgen-Refraktions-Radiographie (SXRR), und vergleichend mit der Elektronenmikroskopie, das Eindringen von CMAS in die poröse Struktur von atmosphärisch plasmagespritzten (APS)TBCs sowie die Bildung und das Wachstum von Rissen unter thermisch zyklischer Belastung untersucht. Die Ergebnisse deuten darauf hin, dass die Infiltration sowie deren Kinetik im Brenner-Teststand wesentlich vom Benetzungsverhalten des CMAS beeinflusst werden. Trotz desoffensichtlichen Angriffs von CMAS auf die Korngrenzen hat die Wechselwirkung von Yttriumdioxid-stabilisiertem Zirkoniumdioxid (YSZ) mit intrudiertem CMAS keinen unmittelbaren Einfluss auf die Struktur und Dichte der innen Oberflächen(Risse, Poren). In einem späteren Stadium wird die Bildung von Rissen senkrecht zur äußeren Oberfläche in einer breiteren Zone der TBC-Schicht beobachtet.
In this talk the basics of X-ray computed tomography (XCT) are presented, together with a description of complementary techniques such as Laminography and Stereoradiography.
A overview of the common reconstruction approach and of the artifacts that can occur during reconstruction or acquisition of XCT images is also given.
Finally, application examples in the field of construction materials are given, whereby several experimental techniques (Region of Interest Approach) and data analysis methods (e.g. Digital volume correlation) are explained. Such techniques and algorithms are used to extract quantitative information from ex- and in-situ experiments.
In this seminar I present the microstructure and micromechanical properties of diesel particulate filter materials, and then particularize them to porous microcracked aluminum titanate.
I show that neutron diffraction is particularly suited for bulk studies, especially under applied load or at high temperatures. The combination of macroscopic and microscopic tests with modeling and simulation yields great added value to understand the mechanics of microcracking.
In Additive Manufacturing everybody is talking about Free Form, Unconventional Design, Re-thinking Components, “Think out of the box”.
However, there are a few outstanding question: a) What are the material properties ? They certainly differ from literature values for conventional materials; b) How about the microstructure? It is different from conventional materials. Does it stay so with ageing? How does it form? c) Do we properly take residual stress into account? We often blame them for our ignorance about failure scenarios. d) Do we apply tailored heat treatments? Very often, we follow conventional schedules…
This talk describes the summary of the efforts carried out within the BAM Project AGIL.
At BAM, we aimed to thoroughly investigate the microstructure and how it evolves as a function of load and temperature (service), to determine the material properties after different process and service conditions, to properly determine residual stress and the way it impacts mechanical properties and component performance, to properly quantify the impact of (unavoidable?) defects, and to determine heat treatments tailored to the process-specific material (stress relieve, microstructure homogenization etc.).
The Project AGIL was and is intimately coupled with the project ProMoAM, dealing with online monitoring of AM processes.
Um das Material- und Schädigungsverhalten von additiv gefertigtem Polyamid 12 (PA12) unter quasistatischer Belastung zu charakterisieren, wurden mechanische Tests und Röntgenverfahren zur Bestimmung der Mikrostruktur eingesetzt. Die Proben wurden nach dem Prinzip des Selektiven Lasersinterns (SLS) hergestellt. Unter quasistatischer Belastung mit Haltezeiten ergab sich ein viskoplastisches Materialverhalten. Im Zugversuch wurde eine maximale Zugfestigkeit von 40.6 MPa und eine Bruchdehnung von 7.4% beobachtet. Mittels Röntgenrefraktion wurde eine Erhöhung von inneren Oberflächen beobachtet, die senkrecht zur Zugrichtung orientiert sind. Die Analyse der Gesamtporosität aus Computertomographie-Messungen ergab keine Änderung infolge der Zugbelastung. Jedoch wurde eine bimodale Porengrößenverteilung und eine steigende Sphärizität festgestellt. Das Materialverhalten wurde mit dem Chaboche-Modell simuliert und ergab eine sehr gute Übereinstimmung mit den experimentellen Ergebnissen. Allerdings gestattet dieses Modell nicht, das Schädigungsverhalten abzubilden. Daher wurde zur Simulation des Schädigungsverhaltens das Modell gemäß dem Ansatz von Gurson, Tvergaard und Needleman unter Berücksichtigung der mikrostrukturellen Parameter erweitert. Der Schwerpunkt des Beitrags liegt auf den Röntgenverfahren zur experimentellen Bestimmung der Mikrostruktur.
Wir präsentieren Labor- und Synchrotron-Röntgenrefraktionstechniken, wie sie an der BAM implementiert sind.
Wir zeigen, dass die Labor-Röntgenrefraktionstopographie (XRRT) und die Synchrotron-Röntgenrefraktionsradiographie (SRRR) außergewöhnliche Werkzeuge zur Untersuchung von Schädigungen und inneren Defekten (Poren, Mikrorisse) in leichten Materialien sind. Tatsächlich nutzen diese Techniken den an Grenzflächen auftretenden Röntgenbrechungseffekt aus, um den Kontrast zwischen dem (schwach absorbierenden) Objekt und dem Hintergrund zu erhöhen. Dies ermöglicht die Erkennung sehr kleiner Objekte (z. B. bis zu 1 nm Rissöffnung) und die Quantifizierung ihrer spezifischen Oberfläche, die mit ihrem Einfluss auf die Materialeigenschaften korreliert. Wir zeigen die folgenden Anwendungen: a) Quantifizierung der Faserentbindung in laminaten Epoxid-Kohlenstoff-Verbundwerkstoffen; b) Mapping der Porengröße in gesinterten Keramiken; c) Klassifizierung von Defekttypen in additiv gefertigter Ti6Al4V-Legierung; d) Früherkennung des Versagens in Aluminium-Keramik-Verbundwerkstoffen (unter Verwendung von In-situ-Experimenten); e) 3D-Darstellung von Makrorissen und Faserentbindung in Verbundwerkstoffen auf Ti-Basis für Anwendungen in der Luft- und Raumfahrt (unter Verwendung von Röntgenbeugungstomographie).
While there is a extensive literature on the micro-mechanical behavior of metal matrix composites (MMCs) under uniaxial applied stress, very little is available on multi-phase MMCs. In order to cast light on the reinforcement and damage processes in such multi-phase composites, an Al alloy with one and two ceramic reinforcements (planar-random oriented alumina fibers and SiC particles) were studied. In-situ compression tests during neutron diffraction experiments were used to track the load transfer among phases, while X-ray computed tomography was used to investigate pre-strained samples, in order to monitor and quantify damage. We found that damage progresses differently in composites with different orientations of the fiber mat. Because of the presence of the intermetallic network, it was observed that the second ceramic reinforcement changes the load transfer scenario only at very high applied load, when also intermetallic particles break. We rationalized the experimental results by means of a micromechanical model based on Maxwell’s homogenization scheme, and we could explain why no damage is observed in the ductile matrix under compression: the matrix finds itself in hydrostatic compression, and the Poisson’s tensile strain is totally carried by the reinforcement phases
The residual stresses and load transfer in multiphase metal alloys and their composites (with both random planar-oriented short fibers and particles) will be shown, as studied by neutron diffraction, by X-ray computed tomography, and by a model based on the reformulation of classic Maxwell’s homogenization method.
Contrary to common understanding and state-of-the-art models, we experimentally observe that randomly oriented phases possess non-hydrostatic residual stress. Moreover, we disclose that the unreinforced matrix alloy stays under hydrostatic compression even under external uniaxial compression.
The recently developed modeling approach allows calculating the residual stress in all phases of the composites. It rationalizes the presence of deviatoric stresses accounting for the interaction of random oriented phases with fibers having preferential orientation. It also allows the explanation of the unconventional in-situ behavior of the unreinforced alloy and the prediction of the micromechanical behavior of other similar alloys.
The residual stresses and load transfer in multiphase metal alloys and their composites (with both random planar-oriented short fibers and particles) will be shown, as studied by neutron diffraction, by X-ray computed tomography, and by a model based on the reformulation of classic Maxwell’s homogenization method.
Contrary to common understanding and state-of-the-art models, we experimentally observe that randomly oriented phases possess non-hydrostatic residual stress. Moreover, we disclose that the unreinforced matrix alloy stays under hydrostatic compression even under external uniaxial compression.
The recently developed modeling approach allows calculating the residual stress in all phases of the composites. It rationalizes the presence of deviatoric stresses accounting for the interaction of random oriented phases with fibers having preferential orientation. It also allows the explanation of the unconventional in-situ behavior of the unreinforced alloy and the prediction of the micromechanical behavior of other similar alloys.
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.
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.
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.
The effect of porosity and microcracking on the mechanical properties (strength, fracture toughness,Young’s modulus, and fracture energy) and thermal expansion of diesel particulate filter (DPF) gradecordierite materials has been investigated. A method to deconvolute the effect of porosity and microc-racking on Young’s modulus is proposed. In addition, the microcrack density and the pore morphologyfactor are calculated by applying a micromechanical differential scheme. The values of the investigatedmechanical properties are shown to decrease with an increase in porosity, but the thermal expansionvalues are insensitive to porosity. The variation in mechanical properties as a function of porosity leadsto distinct porosity dependence of thermal shock resistance for crack initiation and crack propagationfor DPF grade synthetic cordierite.
Ein kurzes Blick in die Computertomographie (CT) im Rahmen des RT3 Kurs der DGZfP ist gegeben.
Die Radontransformation ist bildlich erklärt, und die Grundlagen der Technik mit Vergleich zu der Radiographie sind auch erwähnt. Die typische Rekonstruktionsfehler und deren Beseitigung sind behandelt. Am Ende Beispiele der Anwendungen der CT sind gegeben, aus der zerstörungsfreie Prüfung, der Materialwissenschaft und der Metrologie.
Applications of X-ray refraction to non-destructive characterization of ceramics and composites
(2013)
X-ray refraction is analogous to visible light deflection by matter, with two main differences: 1- convex objects cause divergence (i.e., the refraction index n is smaller than 1), and 2- deflection angles are very small, from a few seconds to a few minutes of arc (i.e., n is near to 1). Trivially but importantly, deflection of X-rays is also sensitive to the orientation of the object boundaries. These features make X-ray refraction techniques extremely suitable to a) detect defects such as pores and microcracks, and quantify their densities in bulk (light) materials, and b) evaluate porosity and particle properties such as orientation, size, and spatial distribution (by mapping). While X-ray refraction techniques cannot in general image single defects, their detectability is simply limited by the wavelength of the radiation.
We will thereby show the application of X-ray refraction 2D mapping (topography) and tomography to different sorts of problems in ceramic science and technology: 1) Sintering of SiC green bodies; 2) Porosity analysis in diesel particulate filter silicates; 3) fiber de-bonding in metal and polymer matrix composites; 4) micro-cracking of glass-precursor -eucryptite. We will see that the use of X-ray refraction analysis yields quantitative results, also directly usable in available models.
To better understand the mechanism of hydrogen assisted cracking (HAC), it is important to investigate the 3D structure of the cracks non-destructively. Since, cracks introduced by HAC are usually very small, conventional x-ray imaging methods often lack the required spatial resolution.
However, the detection of those cracks can be enhanced by taking advantage of refraction at interfaces within the sample.
To image this refractive deflection we employ analyser based imaging (ABI). In this work we aim at proving the enhanced crack detection of ABI by investigating an alluminum alloy weld.
Neutronenbeugung hat verschiedenste Anwendungen, die auf die eigenartigen physikalischen Eigenschaften der Neutronen berühen.
Während die Beugungstechniken wie z.B. die klassische Pulverbeugung, die Kleinwinkelstreuung und die Texturanalyse besonders für die Materialcharakterisierung nutzbar sind, setzt sich die Neutronenbeugung als zerstörungsfreies Verfahren für Eigenspannungsanalyse extrem relevant ein.
Allerdings sind nur wenig die Leute, die die Neutronenbeugung in der ZfP Community benutzen. Dieser Vortrag hat das Ziel die Interesse an der Nutzung von einem solchen Grossgerätwerkzeug aufzuwecken und ein Paar impactvolle Anwendungsbeispiele einiger Techniken zu zeigen.
Die Bestimmung mikroskopischer mechanischen Eigenschaften von Kompositen (MMC oder CMC), sowie der Mapping von Eigenspannungsfelder in Komponenten werden bearbeitet.
Es wird gezeigt, dass Neutronenbeugung grundsätzlich eine zerstörungsfreie Methode für beide die Materialcharakterisierung und die Komponentenintegrität ist, die hohes Potentiell hat, zum Verfahrensportfolio der zerstörungsfreier Prüfung zu gehören.
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.
Neutron diffraction: the forgotten non-destructive technique for residual stress analysis … and more
(2016)
3-D Stress Analysis
(Bulk) Stress mapping
Thick (and thin) films & Interfaces
Bulk high temperature
Real time
In-situ testing: Large sample environment (Stress rigs, Furnaces, …)
Neutrons and Synchrotron Radiation allow all this because they are FASTER , DEEPER and MORE PRECISE than lab equipment
(Flux)(Energy)(Parallel Beam)
Hydrogen in metals can cause a degradation of the mechanical properties with possible subsequent hydrogen assisted cracking (HAC). Though, the mechanism of HAC is not completely understood yet and thus suitable methods for in situ investigations to characterise the crack formation are needed. X-ray computed tomography (CT) is a well-known tool for analysing these properties. However, the effective resolution of the detector system limits the detection of small defects by CT. Analyser based imaging (ABI) takes advantage of x-ray refraction at interfaces between volumes of different density, i.e. of cracks, pores, inclusions, etc., within the sample to detect defects smaller than the resolution of the detector system. In this study, measurements on an aluminium alloy weld showed that ABI allows us to resolve the 3D structure of cracks undetected by absorption based CT. Prospective investigations will analyse HAC in steels.
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.
For how trivial or provocative it can sound, the best neutron spectrometer in the world does not produce science by itself. By definition of Materials Science, neutron scattering data on engineering materials must be used as a tool to understand, and even tailor, materials performance. In order for this to happen, it is clear that neutron data need to be acquired under the most relevant condition possible, coupled to other experimental techniques, and capitalized by means of proper simulations and data analysis.
In fact, access to neutron sources is not routine. Consequently, it is imperative to search ways to make neutron data rentable for the material science and industrial research community.
In this presentation, and based on the example of Ceramic Diesel Particulate Filters and Aluminum Matrix Composites, we will show a couple of strategies to combine neutron data with other experiments, and with theoretical models. Their combination allows raising the value of experiments from data production to problem-solving. Obviously, these are only a few among the many combinations possible to help improving materials properties, performance, and safety.
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.
The most substantial innovations in radiographic imaging techniques of the last two decades aim at enhanced image contrast of weakly absorbing micro and nano structures by taking advantage of X-ray refraction effects occurring at outer and inner surfaces. The applications range from fibre reinforced plastics to biological tissues. These techniques comprise, among others, X-ray refraction topography, diffraction enhanced imaging, phase contrast imaging, Talbot-Lau grating interferometry, and refraction enhanced imaging. They all make use of selective beam deflections up to a few minutes of arc: the X-ray refraction effect. In contrast to diffraction, this type of interaction has a 100 % scattering cross section, as shown experimentally. Since X-ray refraction is very sensitive to the orientation of interfaces, it is additionally a tool to detect, e.g., fibre or pore orientation. If the detector resolution exceeds the size of (small) individual features, one detects the integral information (of inner surfaces) within the gauge volume. We describe the above-mentioned techniques, and show their experimental implementation in the lab and at a synchrotron source. We also show strategies for data processing and quantitative analysis.
3D Crack analysis in hydrogen charged lean duplex stainless steel with synchrotron refraction CT
(2016)
Hydrogen in metals can cause a degradation of the mechanical properties, the so-called hydrogen embrittlement. In combination with internal stresses, hydrogen assisted cracking (HAC) can occur. This phenomenon is not completely understood yet. To better characterise the cracking behaviour, it is important to gain information about the evolution of the 3D crack network. For this purpose samples of lean duplex stainless steel were loaded with hydrogen by means of electrochemical charging and investigated by means of synchrotron refraction CT and SEM fractography after uniaxial tensile loading. Synchrotron refraction CT is an analyser-based imaging (ABI) technique. It uses a Si (111) single crystal as analyser, which is placed into the beam path between sample and detector. According to Bragg’s law only incident x-rays within a narrow range around the Bragg-angle are diffracted from the analyser into the detector. Hence, the analyser acts as an angular filter for the transmitted beam. This filtering allows to turn the refraction and scattering of x-rays into image contrast. Refraction occurs at all interfaces, where the density of the material changes and is more sensitive to density changes than the attenuation. Therefore, it is possible to detect smaller cracks than with classical x-ray imaging techniques, like CT, with comparable spacial resolution. It also visualises the 3D structure of the cracks and gains quantitative information about their morphology and distribution. Since cracks introduced by HAC are usually very small and have a small opening displacement, synchrotron refraction CT is expected to be well suited for imaging this cracking mechanism and can be a valuable tool to characterise the formation and the evolution of a 3D crack network.
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 equally holds for industrial and academic research, and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will 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. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Additionally, I will present a new technique in our portfolio, Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load.
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.
I will 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. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
“Neutrons are a powerful tool” say the neutron scientists. However the use of neutrons remains sometimes disconnected from the practical problems of Materials Science, and facilities themselves are seen as ivory towers.
In this presentation, I will give an overview of the modalities of access to Large Scale facilities, and show a couple of examples on how neutron scattering data on engineering materials can be used as a tool to understand, and even tailor, materials performance.
In order for this to happen, it is clear that neutron data need to be
1. Acquired under the most relevant condition possible
2. Coupled to other experimental techniques
3. Capitalized by means of proper simulations and data analysis
Point 1- calls for an intense use and the development of top-notch of in-situ techniques; Point 2- means that the sole use of neutron data will not lead to any solution of a global problem; All points above hint to the fact that access to neutron sources is not routine, and therefore it is imperative to search ways to make neutron data rentable for the material science and industrial research community.
Microstructural changes in porous cordierite for diesel particulate filter applications caused by machining were characterized using microtensile testing and X-ray computed tomography (XCT). Young’s modulus was determined on ~215-380 m thick machined samples by digital image correlation. Results show a decrease of Young’s modulus due to machining of the thin samples. Explanation of this phenomenon was provided by XCT: the presence of debris due to machining and the variation of porosity due to removal of the outer layers were quantified and correlated with the introduction of further microcracking.
3D structural investigations are described by X-ray laminography studies of sandwich shell segments, made of a PVC foam core, covered by non-crimp fabric glass fibre composite lay-ups processed by vacuum assisted resin infusion of epoxy. The specific scope of this study is to image transversal flaws within the foam core (joints) and of single ply overlaps. Test flaws were purposely implemented in order to simulate typical failure under cyclic load. In a dedicated test rig for shell structures, the flaw evolution/propagation is monitored by thermography and optical 3D inspection of deformation. Due to the unfavourable preconditions for classical computed tomography as of large aspect ratio, the samples were investigated by coplanar translational laminography. Its limited range of observation angles of ± 45°, results in anisotropic artefacts about the normal to the sample surface, but the typical flaws are well visualized in the as-prepared state, in a state of early damage, and in the repaired state.
Additive Manufacturing (AM) of metals has become industrially viable for a large variety of applications, including aerospace, automotive and medicine. Powder bed techniques such as Selective Laser Melting (SLM) based on layer-by-layer deposition and laser melt enable numerous degrees of freedom for the geometrical design. Developing during the manufacturing process, residual stresses may limit the application of SLM parts by reducing the load bearing capacity as well as induce unwanted distortion depending on the boundary conditions specified in manufacturing.
The residual stress distribution in the bulk of IN718 elongated prisms produced by SLM was studied non-destructively by means of neutron diffraction. The samples with different scanning strategies, i.e. hatching length, were measured in as-build condition (on a build plate) and after removal from the build plate.
The absolute values of all stress components decreased after removal from the build plate. Together with surface scan utilizing a coordinate-measuring machine (CMM), it is possible to link the stress release to the sample distortion. Obtained results indicated different residual stress states for each of the transversal, longitudinal and normal component depending on the thermal gradient in the respective direction.
Ein Nachteil der klassischen Durchstrahlungstechnik mit Röntgenstrahlen ist die, in der Abbildung des Untersuchungsobjektes, fehlende Tiefeninformation. Die Anwendung von radiografischen Verfahren, die das Objekt unter zwei oder mehreren Winkelpositionen durchstrahlen, erlauben die Rekonstruktion räumlicher Abbildungen. Dazu zählen Stereoradiografie, Translations- und Rotationslaminographie. Bei der Computertomographie erfolgt die Durchstrahlung unter einem Winkelbereich von 180° oder 360°. Die dabei aufgenommenen Projektionen werden anschließend durch Anwendung der Fourier Transformation und der gefilterten Rückprojektion zu einem 3D-Bilddatensatz rekonstruiert. Verschiedene systembedingte Artefakte, die das Ergebnis negativ beeinflussen können, lassen sich durch geeignete Meß- und Rekonstruktionsparameter, sowie einer nachfolgende Bildverarbeitung eliminieren oder reduzieren.
Das selektive Laserschmelzen (SLM) ist eine pulverbasierte, additive Fertigungsmethode, welche die Herstellung von komplex und individuell geformten Bauteilen ermöglicht. Im Laufe der vergangenen Jahre haben verschiedene Branchen, unter anderem die Luft- und Raumfahrt Industrie, begonnen diese Technologie intensiv zu erforschen. Insbesondere die Titanlegierung Ti-6Al-V4, welche aufgrund ihrer Kombination von mechanischen Eigenschaften, geringer Dichte und Korrosionsbeständigkeit häufig in der Luft- und Raumfahrt eingesetzt wird, eignet sich für die Herstellung mittels SLM. Allerdings können durch nicht optimal gewählte Prozessparameter, welche für gewöhnlich in einer Energiedichte zusammengefasst werden, Defekte in den Bauteilen entstehen.
In dieser Studie wurde untersucht, in wie weit Röntgen-Refraktionsradiographie geeignet ist diese Defekte zu detektieren und zu charakterisieren. Bei der Röntgen-Refraktionsradiographie wird die Röntgenstrahlung, nachdem sie die Probe transmittiert hat, über einen Analysatorkristall gemäß der Bragg-Bedingung in den 2D-Detektor reflektiert und dabei nach ihrer Ausbreitungsrichtung gefiltert. Dadurch wird neben der Schwächung auch die Ablenkung der Röntgenstrahlung durch Refraktion im inneren der Probe zur Bildgebung ausgenutzt. Aus den aufgenommen Refraktionsradiogrammen kann der Refraktionswert berechnet werden. Dieser ist ein Maß für die Menge an inneren Oberflächen in der Probe.
Zum einen konnte gezeigt werden, dass die Röntgen-Refraktionsradiographie Defekte detektieren kann, die kleiner sind als die Ortsauflösung des verwendeten 2D-Detektors. Zum anderen können zwei verschiedene Typen von Defekten unterschieden werden. Bei dem ersten Typ handelt es sich um runde Poren mit geringer innerer Oberfläche. Diese, sogenannten „keyhole pores“ sind charakteristisch für eine zu hohe Energiedichte während des SLM Prozesses. Bei dem zweiten Typ handelt es sich um nicht komplett aufgeschmolzenes Pulver. Diese Defekte zeichnen sich durch eine hohe innere Oberfläche aus und sind charakteristisch für eine zu geringe Energiedichte. Vergleichende Messungen mit hochauflösender Synchrotron CT und optischer Mikroskopie bestätigen die charakteristischen Formen der verschiedenen Defekte.
Synchrotron X-ray diffraction is a powerful non-destructive technique for the analysis of the material stress-state. High cooling rates and heterogeneous temperature distributions during additive manufacturing lead to high residual stresses. These high residual stresses play a crucial role in the ability to achieve complex geometries with accuracy since they can promote distortion of parts during manufacturing. Furthermore, residual stresses are critical for the mechanical performance of parts in terms of durability and safety.
In the present study, Ti-6Al-4V bridge-like specimens were manufactured additively by selective laser melting (SLM) under different laser scanning speed conditions in order to compare the effect of process energy density on the residual stress state. Subsurface residual stress analysis was conducted by means of synchrotron X-ray diffraction in energy dispersive mode for three conditions: as-built on base plate, released from base plate, and after heat treatment on the base plate. The quantitative residual stress characterization shows a correlation with the qualitative bridge curvature method. Computed tomography (CT) was carried out to ensure that no stress relief took place owing to the presence of porosity. CT allows obtaining spatial and size pores distribution which helps in optimization of the SLM process.
High tensile residual stresses were found at the lateral surface for samples in the as-built conditions. We observed that higher laser energy density during fabrication leads to lower residual stresses. Samples in released condition showed redistribution of the stresses due to distortion.
Influence of deposition hatch length on residual stress in selective laser melted Inconel 718
(2018)
The present study aims to evaluate the bulk residual stresses in SLM parts by using neutron diffraction measurements performed at E3 line -BER II neutron reactor- of Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. Together with microstructure characterization and distortion measurements, it is possible to describe the stress state throughout the whole sample. The sample was measured in as-build condition (on a build plate) and after releasing from the build plate. The used material is the nickel based superalloy 718. This alloy is widely used in aerospace and chemical industries due to its superior corrosion and heat resistant properties.
Obtained results indicated different residual stress states for each of the transversal, longitudinal and normal component. The normal and transversal component exhibits a rather compressive behavior while the longitudinal was tensile in the center part of the sample and became compressive towards the tip. As expected, the absolute values of all stress components decreased after releasing the sample from the building plate. A surface scan utilizing a coordinate-measuring machine (CMM) allowed us to present top surface distortion before and after releasing. The top surface showed a distortion around ±80µm after releasing. Microstructure evolution in the scanning-building cross-section is largely dominated by columnar grains. In addition, many small random orientated grains are prominent in the regions of a laser overlap during SLM.
In summary, for the sample of superalloy 718 manufactured by SLM, a small distortion occurred when removing the sample from the build plate whereby the residual stress state decreases. Moreover, the observed columnar grains in the building direction could give a reason for the lowest stress values in that normal direction. However, the most important parameter controlling the residual stresses is the temperature gradient. Hence, future investigations are planned for a different scan strategy to distribute the laser impact in a more homogenous manner.
While additive manufacturing (AM) is blossoming in nearly every industrial field, and the most different process are being used to produce components and materials, little attention is paid on the safety concerns around AM materials and processes.
Leveraging on our leading expertise in non-destructive testing (NDT) and materials characterization, we approach AM at BAM under two important viewpoints: first the on-line monitoring of the process and of the product, second the evolution of the (unstable) microstructure of AM materials under external loads.
These two subjects are the core of the two new-born internal projects ProMoAM and AGIL, respectively.
A detailed view of the goals and the organization of these two projects will be given, together with the expected output, and some preliminary results.
The combination of microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on porous material 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. I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of porosity in ceramics.
Moreover, I will show how not-so-novel 2D characterization techniques, based X-ray refraction, can allow a great deal of insights in the damage evolution in microcracked (and porous) ceramics. I will show how X-ray refraction can detect objects (e.g. microcracks) below its own spatial resolution.
Finally, I will discuss the link between the microstructural findings and the mechanical properties of porous microcracked ceramics.
As opposed to reviewing results on experimental determination of residual stress by diffraction, this paper discusses the open issues when dealing with residual stress determination in additive manufactured parts, in particular those manufactured with laser powder bed fusion techniques. Three points are addressed in detail: (a) the proper determination of the strain-free reference d0, (b) the problem of the determination of the principal axes, and (c) the use of the correct diffraction elastic constants. It is shown that all methods to determine the strain-free reference d0 suffer from caveats, and care must be taken in evaluating the most suitable for the problem being tackled. In addition, it is shown that, in some systems, the principal axes do correspond to the geometrical axes of the specimen, but this needs to be systematically checked, especially in the case of uni- or bidirectional hatching strategies. Finally, the need to experimentally determine the proper diffraction elastic constants is underlined, especially in the case of strongly textured specimens, which again depends on the deposition strategy.
The mixture of ammonium nitrate (AN) prills and fuel oil (FO), usually called ANFO, is extensively used in the mining industry as a bulk industrial explosive. One of the major performance predictors of ANFO mixtures is the fuel oil retention, which is itself governed by the porosity of the AN prills. Standardised tests routinely used to assess oil retention face several important limitations; the first being the difficulty to cover the wide range of porosity contents and morphologies from different types of ammonium nitrate prills; the second being the inability to evaluate the closed porosity, which is an important factor regarding the sensitivity of the explosive to detonation. In this study, we present how X-ray computed tomography (XCT), and the associated advanced data processing workflow, can be used to fully characterise the structure and morphology of AN prills. We show that structural parameters such as volume fraction of the different phases and morphological parameters such as specific surface area and shape factor can be reliably extracted from the XCT data, and that there is a good agreement with the measured oil retention values. XCT can therefore be employed to non-destructively and accurately evaluate and characterise porosity in ammonium nitrate prills.
The creep strengthening mechanisms in (age-hardenable) aluminum alloys are analyzed on the basis of a new microstructural study of powder samples, an analysis of a comprehensive revision of creep data from the literature, and a new modeling approach. A strategy based on the strength difference (SD) method to separate the contributions of solid solution atoms and precipitates to creep strengthening is proposed. The new methodology considers the combination of the two contributions avoiding the need of a threshold stress term in the creep equation. The contribution of both precipitates and solid solution is taken into account by means of the analysis of the lattice parameter variation with aging time. For this study, powders of two commercial AA2xxx alloys have been analyzed using diffraction methods. The experimental results are modeled using Lubarda’s approach combined with the SD method.
In this paper we report on the characterization by X-ray computed tomography of calcium phosphate (CaP) and polycaprolactone (PCL) coatings on Ti-6Al-4V alloy scaffolds used as a material for medical implants. The cylindrical scaffold has greater porosity of the inner part than the external part, thus, mimicking trabecular and cortical bone, respectively. The prismatic scaffolds have uniform porosity. Surface of the scaffolds was modified with calcium phosphate (CaP) and polycaprolactone (PCL) by dip-coating to improve biocompatibility and mechanical properties. Computed tomography performed with X-ray and synchrotron radiation revealed the defects of structure and morphology of CaP and PCL coatings showing small platelet-like and spider-web-like structures, respectively.
Porous ceramic diesel particulate filters (DPFs) are extruded products that possess macroscopic anisotropic mechanical and thermal properties. This anisotropy is caused by both morphologic features (mostly the orientation of porosity) and crystallographic texture. We systematically studied those two aspects in a cordierite and two aluminum titanate (AT) ceramic materials of different porosity using mercury porosimetry, gas adsorption, electron microscopy, X-ray diffraction, and X-ray refraction radiography. We found that a lower porosity in AT content implies a larger isotropy of both the crystal texture and the porous space orientation. We also found that, analogous to cordierite, AT crystallites do align with their axis of negative thermal expansion along the extrusion direction. However, unlike what found for cordierite, the aluminium titanate crystallite form is such that a more pronounced (0 0 2) texture along the extrusion direction implies porosity aligned perpendicular to it.
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.
I will 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. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
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.
A few Aspects of the Current Understanding of DPF Materials Thermal and Mechanical Properties
(2016)
Bi-continuous porous ceramics for filtration applications possess a particularly complicated microstructure, whereby porosity and solid matter are intermingled. Moreover, they very often display a microcrack network, resulting from the strong anisotropy of the microscopic coefficient of thermal expansion (CTE). Mechanical, thermal, and filtration properties, they all strongly depend on the morphology of both solid matter and porosity, and on the degree of microcracking (also, the microcrack density), which is in its turn tightened to the grain size.
Recent industrial and academic research has enormously progressed in understanding the microstructure-property-performance relationships existing in these complicated materials:
- Using 3D computed tomography (CT) at different resolutions, and several X-ray refraction-based techniques, porosity and pore orientation could be quantitatively evaluated (in the example of cordierite).
- Neutron and X-ray Diffraction has been instrumental to disclose a) the non-linear character of the stress-strain response, and b) the negative CTE of these materials, and its consequences on the materials properties;
- Analytical and numerical models have been elaborated to rationalize these behaviours in terms of microcracking and microstructural features.
Here these results will be reviewed, and a outlook at (some of the) outstanding problems will be given.
Diffraction-based experimental determination of Residual Stress in AM parts: A critical discussion
(2019)
Additive manufacturing (AM) technologies have experienced an exceedingly rapid growth, not always paralleled by the knowledge about the materials properties and performance. In particular, residual stress (RS) has been soon recognized as an issue in AM parts, so that parts are always post-heat-treated. Moreover, much effort has been spent on simulating RS, especially using finite element methods.
The experimental determination of RS has thereby become increasingly important, and even simple data constitute (to date) a piece of knowledge to fill the above-mentioned gap. In particular, diffraction methods, which are basically non-destructive, offer enormous possibilities to gain knowledge on real components, since neutrons and synchrotron radiation can penetrate even heavy metals up to several millimeters (or even centimeters). Indeed, some success has been obtained, and the knowledge about the origins of the RS fields, as well as their variation as a consequence of heat or mechanical treatments, has been greatly expanded.
In this talk, a few success stories will be outlined. It will be shown how the determination of RS in metallic parts (with focus on those produced by laser powder bed fusion) has even allowed showing that process parameters that were considered unimportant play a major role in the onset of stress.
However, while RS is starting to be considered in the part design, deposition strategy (e.g. build plate temperature), and even in the definition of the relevant metric to assess the quality of a part, much is still to be investigated about the hypotheses underlying its experimental determination. Therefore, some aspects to be aware of, or even to date unclear will also be discussed, such as the determination of the reference unstrained samples and of the principal axes of stress. All these aspects will draw the path towards a comprehensive understanding of the process-structure-performance relationships in AM materials and parts.
Ammonium nitrate (AN) prills are commonly used as an ingredient in industrial explosives and in fertilisers. Conventional techniques (such as BET or mercury intrusion porosimetry) can measure the open porosity and specific surface area of AN prill, but the closed porosity is not obtainable. This work was focused on evaluating X-ray computed tomography (XCT) as a non-destructive technique for the assessment of porosity in AN prills. An advanced data processing workflow was developed so that the segmentation and quantification of the CT data could be performed on the entire 3D volume, yet allowing the measurements (e.g.; volume, area, shape factor…) to be extracted for each individual phase (prill, open porosity, closed porosity) of each individual prill, in order to obtain statistically relevant data. Clear morphological and structural differences were seen and quantified between fertiliser and explosive products. Overall, CT can provide a very wide range of parameters that are not accessible to other techniques, destructive or non-destructive, and thus offers new insights and complementary information.
In this talk, the evolution of the demand for engineering applications of neutrons at the ILL in the last 10 years is presented. It is shown that small angle neutron scattering and diffraction are highly demanded by the materials science community. Further development in the field is foreseen, with the use of in-situ (furnace, tension/compression rig, humidity cells, etc.) techniques to associate to the neutron techniques.
In this Seminar cycle I will present first diffraction methods to determine residual stress and investigate micromechanical properties of complex materials, and then particularize the treatment with applications to porous microcracked ceramics for diesel particulate filter applications.
I will show that neutron diffraction is particularly suited for bulk studies, where 3D stresses are needed. The advantages to use Time-of-Flight or steady state sources will be discussed, together with the problematic of the determination of absolute RS values.
Finally, the behavior of DPF materials under applied load or at high temperatures will be discussed under the combination of macroscopic and microscopic tests.
In this Seminar cycle I will present first diffraction methods to determine residual stress and investigate micromechanical properties of complex materials, and then particularize the treatment with applications to porous microcracked ceramics for diesel particulate filter applications.
I will show that neutron diffraction is particularly suited for bulk studies, where 3D stresses are needed. The advantages to use Time-of-Flight or steady state sources will be discussed, together with the problematic of the determination of absolute RS values.
Finally, the behavior of DPF materials under applied load or at high temperatures will be discussed under the combination of macroscopic and microscopic tests.
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 equally holds for industrial and academic research and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will 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. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Additionally, I will show how Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load, can well be coupled to the microstructural framework gained by CT, allowing understanding the microstructure-property relationships in materials.
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 equally holds for industrial and academic research and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will 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. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Additionally, I will show how Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load, can well be coupled to the microstructural framework gained by CT, allowing understanding the microstructure-property relationships in materials.
Finally, I will show that BAM is very active in standardization and certification, including production of Reference Materials and Methods.
The influence of the support structure on residual stress and distortion in SLM Inconel 718 parts
(2017)
The effect of support structure and of removal from the base plate on the residual stress state in Selective Laser Melted IN718 parts was studied by means of synchrotron X-ray diffraction. The residual stresses in subsurface region of two elongated prisms in as-built condition and after the cutting from the base plate were determined. One sample was directly built on a base plate and another one on a support structure. Also, the distortion on the top surface due to stress release was measured by contact profilometry. High tensile residual stress values were found, with pronounced stress gradient along the hatching direction. In the sample on support stress redistribution took place after removal of the base plate, as opposed to simple stress relaxation for the sample without support. The sample on support structure showed larger distortion compared to sample without support. We conclude that the use of a support decreases stress values but stress relieving heat treatments are still needed.
Ein kurzes Blick in die Computertomographie (CT) im Rahmen des RT3 Kurs der DGZfP ist gegeben.
Die Radontransformation ist bildlich erklärt, und die Grundlagen der Technik mit Vergleich zu der Radiographie sind auch erwähnt. Die typische Rekonstruktionsfehler und deren Beseitigung sind behandelt. Am Ende Beispiele der Anwendungen der CT sind gegeben, aus der zerstörungsfreie Prüfung, der Materialwissenschaft und der Metrologie.
In the present study, Ti-6Al-4V bridge-like specimens were manufactured additively by selective laser melting (SLM) under different laser scanning speed conditions in order to compare the effect of process energy density on the residual stress state. Subsurface residual stress analysis was conducted by means of synchrotron diffraction in energy dispersive mode for three conditions: as-built on base plate, released from base plate, and after heat treatment on the base plate. The quantitative residual stress characterization shows a correlation with the qualitative bridge curvature method. Computed tomography (CT) was carried out to ensure that no stress relief took place owing to the presence of porosity. CT allows obtaining spatial and size pores distribution which helps in optimization of the SLM process.
High tensile residual stresses were found at the lateral surface for samples in the as-built conditions. We observed that higher laser energy density during fabrication leads to lower residual stresses. Samples in released condition showed redistribution of the stresses due to distortion. A method for the calculation of the stress associated to distortion of the parts after cutting from base plate is proposed. The distortion measurements were used as input for FEM simulations.
Im vergangenen Jahrzehnt sind gitterinterferometrische Röntgenabbildungen zunehmend in den Fokus des Interesses gerückt. Sie sind insbesondere dann Vorteil, wenn der in der Standardradiographie erreichbare Kontrast nicht genügt, schwach absorbierende Mikro- und Nanostrukturen abzubilden.
Auf Kosten mehrerer Aufnahmen gestattet die Talbot-Lau Gitterinterferometrie, die Beiträge aus Absorption, Refraktion und (refraktiver) Streuung zu trennen. Dazu werden die Störungen der Interferenzmuster von Phasengittern ausgewertet. Im Gegensatz zu einer Vielzahl anderer refraktionsbasierter Abbildungsmethoden kann diese Technik mit konventionellen Röntgenröhren (mit divergenter, polychromatischer Strahlung) angewendet werden. Damit ist die Technik geeignet, typische ZfP-Fragestellungen zu lösen.
Hier stellen wir Untersuchungen zur Effizienz von Phasengittern vor. Die Visibilität (d.h. die Höhe der Oszillation im Interferenzmuster) wird als Funktion verschiedener geometrischer Parameter verfolgt. Eine Rotation um die Achse parallel zu den Gitterstegen ändert die Form des Gitterprofils (d.h. die Verteilung der Phasenschiebungen). Die kontinuierliche Variation des Winkels und des Detektionsabstandes führt zur Identifikation von ausgezeichneten Kombinationen mit maximaler Visibilität, wobei die Abstände deutlich geringer sind als im Standardaufbau mit senkrechter Gitterbestrahlung.
Unsere Studie umfasst Simulationen für monochromatische Quelle und den Vergleich zu experimentellen Ergebnissen mit der Synchrotronstrahlung.
In der Literatur wurden die Vorteile der Talbot-Lau Interferometrie für die zerstörungsfreie Prüfung von Faserkompositen und Verbundwerkstoffen demonstriert. Hier werden als Beispiele Messungen an Aluminiumtitanat (Al2TiO5) Pulver gezeigt.
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. I will 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, with particular focus on additively manufactured materials. I will also show how X-ray refraction computed tomography (CT) and Neutron diffraction can be highly complementary to classic absorption CT, being sensitive to internal interfaces and residual stress analysis, respectively.
Shock tube systems are non-electric explosive fuses employed in blasting and demolition applications to trigger the detonation of explosive charges. Their working principle is based on the explosive reaction of a fine explosive powder on the tubing's inner surface, generating a shock wave traveling at a velocity of 2,100 m/s along the length of the tube, without destroying it. One of
the key aspects of the manufacturing process of these shock tubes is the size and morphology of the explosive powder grains and their distribution on the inner wall of the tube, in order to propagate the shockwave efficiently and reliably. For the first time, synchrotron X-ray computed tomography has been used to characterize non-destructively the explosive powder grains, typically Al/HMX between 10 and 20 μm in size, in terms of morphology and 3D distribution but also to characterise the presence and location of defects
within the shock tube walls.
The porosity and the surface roughness are recently discussed problems for SLM parts. The influence of SLM process parameters on porosity is well studied for different materials. Nevertheless, the build angle (i.e. the angle between part orientation and build plate) needs to be understood as an additional SLM process parameter, as it has been shown, that the microstructure and hence the mechanical performance of various materials depend on the build angle. The inherent build angle of each strut as a part of a lattice structure is the motivation to investigate the influence of the build angle on the porosity and roughness on round-shaped (1 mm diameter) struts by means of CT. Conventional Coordinate Measuring Machine (CMM) has the limitation towards small and round shaped samples. The need for Computed Tomography (CT) regarding investigations of SLM parts will increase because no other non-destructive technique allows the assessment of complex geometries with inner laying surfaces. We used CT to assess the pores and the strut surface. Seven struts out of the nickel alloy Inconel 625 with build angles from 30° to 90° were studied. It was found that the number of pores is smaller, and the size of pores is larger for the 90° strut. In case of 30° strut, the number of pores is increased towards down-skin side, additionally, this strut orientation showed to have the largest number of attached powder particles. The elongated pores exist exclusively near the strut surface. While the roughness at the down-skin surface is highly depending of the biud angle, the roughness at the up-skin surface is the same for all struts. The mechanisms of pore and surface roughness formation is not mainly driven by gravity.
Avoid living dangerously: non-destructive characterization of AM parts from powder to end-of-life
(2019)
The freeform and the revolutionary design possibilities offered by additive manufacturing have skyrocketed the amount of optimization studies in the realm of engineering, and metallic additive manufactured parts are becoming a reality in industry.
Not surprisingly, this has not been paralleled by a similar enthusiastic wave in the realm of materials science, and still very little is known about AM materials properties. This has the consequence that, typically, conventional materials properties are still used in design and even in simulations.
lt is necessary to dig a lot deeper than at present, in order to understand these new materials classes, and in particular their microstructure and their intemal stresses, largely different from their cast or wrought companions.
In this paper we report on the characterization by X-ray computed tomography of calcium phosphate (CaP) and polycaprolactone (PCL) coatings on Ti-6Al-4V alloy scaffolds used as a material for medical implants. The cylindrical scaffold has greater porosity of the inner part than the external part, thus, mimicking trabecular and cortical bone, respectively. The prismatic scaffolds have uniform porosity. Surface of the scaffolds was modified with calcium phosphate (CaP) and polycaprolactone (PCL) by dip-coating to improve biocompatibility and mechanical properties. Computed tomography performed with X-ray and synchrotron radiation revealed the defects of structure and morphology of CaP and PCL coatings showing small platelet-like and spider-web-like structures, respectively.
The quality of components made by laser beam melting (LBM) additive manufacturing is naturally influenced by the quality of the powder bed. A packing density <1 and porosity inside the powder particles lead to intrinsic voids in the powder bed. Since the packing density is determined by the particle size and shape distribution, the determination of these properties is of significant interest to assess the printing process. In this work, the size and shape distribution, the amount of the particle’s intrinsic porosity, as well as the packing density of micrometric powder used for LBM, have been investigated by means of synchrotron X-ray computed tomography (CT). Two different powder batches were investigated: Ti–6Al–4V produced by plasma atomization and stainless steel 316L produced by gas atomization. Plasma atomization particles were observed to be more spherical in terms of the mean anisotropy compared to particles produced by gas atomization. The two kinds of particles were comparable in size according to the equivalent diameter. The packing density was lower (i.e., the powder bed contained more voids in between particles) for the Ti–6Al–4V particles. The comparison of the tomographic results with laser diffraction, as another particle size measurement technique, proved to be in agreement.
Applications of X-ray refraction to non-destructive characterization of ceramics and composites
(2017)
X-ray refraction is analogous to visible light deflection by matter, with two main differences: 1- convex objects cause divergence (i.e., the refraction index n is smaller than 1), and 2- deflection angles are very small, from a few seconds to a few minutes of arc (i.e., n is near to 1). Trivially but importantly, deflection of X-rays is also sensitive to the orientation of the object boundaries. These features make X-ray refraction techniques extremely suitable to a) detect defects such as pores and microcracks, and quantify their densities in bulk (light) materials, and b) evaluate porosity and particle properties such as orientation, size, and spatial distribution (by mapping). While X-ray refraction techniques cannot in general image single defects, their detectability is simply limited by the wavelength of the radiation.
We will thereby show the application of X-ray refraction 2D mapping (topography) and tomography to different sorts of problems in ceramic science and technology: 1) Sintering of SiC green bodies; 2) Porosity analysis in diesel particulate filter silicates; 3) fiber de-bonding in metal and polymer matrix composites; 4) micro-cracking of glass-precursor -eucryptite. We will see that the use of X-ray refraction analysis yields quantitative results, also directly usable in available models.
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 equally holds for industrial and academic research, and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will 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. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Additionally, I will present a new technique in our portfolio, Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load.
X-ray refraction techniques represent a very promising, yet not so wide-spread, set of X-ray techniques
based on refraction effects. They allow determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with nanometric detectability. While they are limited by the X-ray absorption of the material under investigation, we demonstrate showcases of ceramics and composite materials, where understanding of microstructural features could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography.
Complex materials (e.g., porous ceramics) need high resolution techniques at multi-scale levels. Microstructure is intimately linked to properties and performance. One technique (or even a few techniques) is not enough. X-ray refraction and CT are very powerful tools. Non-destructive characterisation and quantitative image analysis techniques (2D and 3D) are necessary to understand the anisotropy.
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 equally holds for industrial and academic research, and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will 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. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Additionally, I will present a new technique in our portfolio, Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load.