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In this work, the structural integrity of LBM fabricated IN625 small cylinders (d = 1 mm, h = 6 mm) was investigated regarding the porosity and the surface roughness by means of computed tomography. The measurements were carried out on a GE v|tome|x L 300/180 with a reconstructed voxel size of 2 µm. The pores were analyzed for size, shape and spatial distribution. The correlation between compactness C and spatial distribution showed that elongated pores (C < 0.2) appear exclusively within a distance of 80 µm to the sample surface. The reconstructed surface was digitally meshed and unwrapped to evaluate the mean roughness Ra. Since the gravity correlates linearly with the sine of the build angle, the influence of gravity on porosity and surface roughness was determined.
µCT is used to validate the capability of online monitoring for in-situ detection of defects during the L-PBF build process, which is a focus of the TF project ProMoAM.
Our first experiments show that online monitoring using thermography and optical tomography cameras are able to detect defects in the built part. But further research is needed to understand root cause of the correlation.
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.
This study is shown as an example of the potential of synchrotron X-ray refraction technique to determine the evolution of damage in brittle (microcracked) materials. The strength of X-ray refraction resides in its high detectability of features (e.g., cracks, pores) within large volumes, enabling a macroscopic characterization of the microstructure. The case study is a Zirconia-based cast refractory, which is aimed to function at high temperatures (even in excess of 1700°C) in industrial furnaces to enable the production of special glasses. Therefore, this material must withstand severe in-service conditions (both thermomechanical and chemical). X-ray refraction technique is used to monitor the microcracking evolution of the material, which was previously subjected to thermal cycles (crossing the martensitic phase transformation around 1000°C) at two different stress levels.
Fibre-Matrix-Debonding in glass fibre reinforced dental posts can play an important role for their mechanical performance and long term stability… We show that synchrotron X-ray refraction radiography (SXRR) allows analysis of large samples (up to several millimetres) without compromising the detectability of sub micrometer defects.
X-ray refraction is analogous to visible light deflection by matter; it occurs at boundaries between different media. The main difference between visible light and X-rays is that in the latter case deflection angles are very small, from a few seconds to a few minutes of arc (i.e., the refraction index n is near to 1). 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 (not too heavy) 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, they can detect objects with size above a few wavelengths of the radiation.
Such techniques, especially at the Synchrotron BESSY II, Berlin, Germany, can be used in-situ, i.e. when the specimen is subjected to temperatures or external loads.
The use of X-ray refraction analysis yields quantitative information, which can be directly input in kinetics, mechanical and damage models.
We hereby show the application of non-destructive X-ray refraction radiography (SXRR, 2D mapping also called topography) to problems in additive manufacturing:
1) Porosity analysis in PBF-LM-Ti64. Through the use of SXRR, we could not only map the (very sparse) porosity distribution between the layers and quantify it, but also classify, and thereby separate, the filled porosity (unmolten powder) from the keyhole and gas pores (Figure 1).
2) In-situ heat treatment of laser powder bed fusion PBF-LM-AlSi10Mg to monitor microstructure and porosity evolution as a function of temperature (Figure 2). By means of SXRR we indirectly observed the initial eutectic Si network break down into larger particles as a function of increasing temperature. We also could detect the thermally induced porosity (TIP). Such changes in the Si-phase morphology upon heating is currently only possible using scanning electron microscopy, but with a much smaller field-of-view. SXRR also allows observing the growth of some individual pores, usually studied via X-ray computed tomography, but again 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 defect distribution and the susceptibility of any material to thermally induced damage and/or microstructure evolution over statistically relevant volumes.
Using magnetic materials for energy conversion as an example, this lecture shows how X-ray tomography investigations can contribute to structure elucidation in composites and solid samples. The components are tested non-destructively in order to characterize cracks, pores and other defects and their influence on the functional properties three-dimensionally and in good time in the life cycle of the material. If you combine microtomography with other methods of magnetic material characterization, you can make unique statements about the structure and the functional properties.
Using magnetic materials for energy conversion as an example, this lecture shows how X-ray tomography investigations can contribute to structure elucidation in composites and solid samples. The components are tested non-destructively in order to characterize cracks, pores and other defects and their influence on the functional properties three-dimensionally and in good time in the life cycle of the material. If you combine microtomography with other methods of magnetic material characterization, you can make unique statements about the structure and the functional properties.
Functional materials for energy conversion are important technology drivers needed for the implementation of low carbon energy. Therefore, researchers commonly focus on improving the intrinsic properties of a functional material. However, for applications, the extrinsic properties are at least as important as the intrinsic ones. Consequently, it is important to investigate and understand the external and internal structure of semi-finished products and especially defect dependent properties. The extrinsic properties may change during application and the life cycle of the material as well as through processing and molding steps.
Our studies show how X-ray tomographic (XCT) investigations can contribute to structure investigations in composites and massive samples using the example of magnetic materials for energy conversion. The components are tested non-destructively in 3D in order to localize and characterize cracks, pores, inclusions as well as other defects and their influence on the functional properties and also “in-time” during the life cycle of the material. Exsitu and in-situ experiments performed with non-destructive XCT are predestinated to follow damaging mechanisms of materials under certain load conditions, atmospheres or liquids, e.g. went through several working cycles of a functional material. By combining microtomography with other methods of magnetic and classical material characterization, unique statements about the structure and the functional properties can be made.
From the applications point of view, sometimes complex, three-dimensional geometries are needed to fully exploit the functional properties of the materials, e.g. to ensure a high surface area for heat exchange. Since many functional materials are brittle and difficult to form, shaping is often a big challenge. In principle, additive manufacturing processes offer the possibility to produce complex, porous components from poorly formable alloys.
If all stages of additive manufacturing are accompanied by X-ray tomographic imaging, the process of finding the optimal parameters for material processing can be significantly accelerated.
Based on the quality control of the initial powder material used and also investigations of the shape and arrangement of defects within the molten structure and their relationship with the melting path scanning strategy, Xray tomography has proven to be an ideal tool for additive manufacturing, even for functional materials. Overall, tomographic methods are important tools for the development of functional materials to application maturity.
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.
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.
X-Ray computed tomography and traditional analysis of a capillary absorption test in cement pastes
(2020)
Water absorption testing has the attraction of being simple, relatively quick and use water as a fluid which is the key substance in the possible concrete deterioration. However, in spite of the advantages its application has remained empirical, except for the testing of resistance to frost, through the identification of the critical degree of saturation. Rilem TC-116 studied this test, among others, for the characterization of concrete resistance against transport through the concrete pore network. Results indicated a low discriminating ability of the absorbency for qualifying concrete resistance and then, it seemed necessary to try to move forward by making the link between the absorption testing and the concrete pore microstructure. In the present work, thanks to the X-Ray computed tomography, it is described the evolution of the water front in three paste-specimen with different w/c ratios (different pore radius distributions). The observations allowed us to deduce that all the pores start to fill simultaneously, but the bigger ones fill quicker and rise less. The saturation degree is measured along the height of the sample, showing that each pore size has a different rate which becomes constant after the first hour. Washburn’s equation was applied to the progressive advance of the water front, resulting in a pore radius much smaller than the one expected.
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.
Water migration in one-side heated concrete: 4D in-situ CT monitoring of the moisture-clog-effect
(2019)
Explosive spalling due to fire exposure in concrete structures can lead severe damage and, in the worst case, to premature component failure. For this reason, an in situ investigation of water Migration in concrete due to surface heating was undertaken.
During these experiments, a miniaturized concrete specimen within a confining and insulating double-hull was subjected to surface heating during simultaneous X-ray computed tomography (CT) scanning. Through the use of subtraction-based Image analysis techniques, it was possible to observe and quantify not only drying within areas of the concrete matrix close to the heated surface, but also the migration of moisture to both pore and matrix regions deeper within the specimen. It was also discovered that the correction of CT images for specimen deformation using DVC and variable detector performance using calibrated image filters significantly improved the quality of the results. This clearly demonstrates the potential of X-ray CT for evaluation of other rapid-density-change phenomena in concrete and other building materials.
Water Migration in One-Side Heated Concrete: 4D In-Situ CT Monitoring of the Moisture-Clog-Effect
(2018)
In order to study damage in concrete exposed to fire, a series of continuous X-ray computed tomography (CT) measurements were performed on a concrete sample heated, in-situ, on one side. The water migration relative to time and 3D space and, in particular, the dynamic condensation and vaporization of water droplets in the pores was quantified. This approach shows significant potential for further investigation of fire-related concrete damage.
Behälter aus hochdichtem Polyethylen (PE-HD) werden zur Lagerung und für den Transport von Kraftstoffen eingesetzt. Beim Kontakt beider Medien diffundiert der Kraftstoff in das Polymer, erhöht dessen Volumen und Duktilität und ändert damit das Fließverhalten des Polymers unter Zugbelastung. Zudem weist PE-HD in Luft im verstreckten Bereich das sogenannte strain-whitening (Lichtstreuung) auf, während in Diesel gelagertes PE-HD optisch transparent wird. Zur Untersuchung dieses Phänomens wurden ortsaufgelöste Röntgenrefraktion und –diffraktion (Topographie) eingesetzt. Aus Sicht der molekularen Struktur (Diffraktion) weisen die beiden Probentypen keine Unterschiede auf: im verstreckten Bereich liegt eine „Fasertextur“ der Polymerketten in Belastungsrichtung vor, im unverstreckten Bereich nahezu ideale Isotropie. Die für mikroskopische Strukturen empfindliche Röntgenrefraktion zeigt außerdem für die Probe in Luft im verstreckten Bereich eine ausgeprägte Orientierung von Grenzflächen in Zugrichtung, während die in Diesel gelagerte Probe keine Grenzflächen zeigt. In Analogie zum optischen Verhalten bewirken die ähnlichen Brechungsindizes beider Medien im Röntgenbereich, dass eindiffundierter Diesel als Immersionsflüssigkeit die Brechungseigenschaften herabsetzt.
Behälter aus hochdichtem Polyethylen (PE-HD) werden zur Lagerung und für den Transport von Kraftstoffen eingesetzt. Beim Kontakt beider Medien diffundiert der Kraftstoff in das Polymer, erhöht dessen Volumen und Duktilität und ändert damit das Fließverhalten des Polymers unter Zugbelastung. Zudem weist PE-HD in Luft im verstreckten Bereich das sogenannte strain-whitening (Lichtstreuung) auf, während in Diesel gelagertes PE-HD optisch transparent wird. Zur Untersuchung dieses Phänomens wurden ortsaufgelöste Röntgenrefraktion und –diffraktion (Topographie) eingesetzt. Aus Sicht der molekularen Struktur (Diffraktion) weisen die beiden Probentypen keine Unterschiede auf: im verstreckten Bereich liegt eine „Fasertextur“ der Polymerketten in Belastungsrichtung vor, im unverstreckten Bereich nahezu ideale Isotropie. Die für mikroskopische Strukturen empfindliche Röntgenrefraktion zeigt außerdem für die Probe in Luft im verstreckten Bereich eine ausgeprägte Orientierung von Grenzflächen in Zugrichtung, während die in Diesel gelagerte Probe keine Grenzflächen zeigt. In Analogie zum optischen Verhalten bewirken die ähnlichen Brechungsindizes beider Medien im Röntgenbereich, dass eindiffundierter Diesel als Immersionsflüssigkeit die Brechungseigenschaften herabsetzt.
Abstract While classically used to visualise the magnetic microstructure of functional materials (e.g., for magnetic applications), in this study, the Bitter technique was applied for the first time to visualise macroscopic deformation gradients in a polycrystalline low-carbon steel. Spherical indentation was chosen to produce a multiaxial elastic–plastic deformation state. After removing the residual imprint, the Bitter technique was applied, and macroscopic contrast differences were captured in optical microscopy. To verify this novel characterisation technique, characteristic “hemispherical” deformation zones evolving during indentation were identified using an analytical model from the field of contact mechanics. In addition, near-surface residual stresses were determined experimentally using synchrotron radiation diffraction. It is established that the magnetic domain distribution contrast provides deformation-related information: regions of different domain wall densities correspond to different “hemispherical” deformation zones (i.e., to hydrostatic core, plastic zone and elastic zone, respectively). Moreover, the transitions between these three zones correlate with characteristic features of the residual stress profiles (sign changes in the radial and local extrema in the hoop stress). These results indicate the potential of magnetic domain distribution imaging: visualising macroscopic deformation gradients in fine-grained ferromagnetic material with a significantly improved spatial resolution as compared to integral, mean value-based measurement methods.
Virtual CT acquisition and reconstruction of complex and noisy scanning trajectories in aRTist
(2019)
In modern CT imaging, simulation has become an important tool to minimize cost- and time-intensive measurements. It is increasingly used to optimize techniques for complex applications, to support the preparation of written procedures, and for educational purposes. We extended the CT simulation software ‘aRTist’ with a module to set-up arbitrary trajectories including disturbing influences during the scan. Moreover, such geometric deviations can be compensated by the internal reconstruction tool.
Using SXRR to Probe the Nature of Discontinuities in SLM Additive Manufactured Inconel 718 Specimens
(2020)
The utilization of additive manufacturing (AM) to fabricate robust structural components relies on understanding the nature of internal anomalies or discontinuities, which can compromise the structural integrity. While some discontinuities in AM microstructures stem from similar mechanisms as observed in more traditional processes such as casting, others are unique to the AM process. Discontinuities in AM are challenging to detect, due to their submicron size and orientation dependency. Toward the goal of improving structural integrity, minimizing discontinuities in an AM build requires an understanding of the mechanisms of formation to mitigate their occurrence. This study utilizes various techniques to evaluate the shape, size, nature and distribution of discontinuities in AM Inconel 718, in a non-hot isostatic pressed (HIPed) as-built, non-HIPed and direct age, and HIPed with two step age samples. Non-destructive synchrotron radiation refraction and transmission radiography (SXRR) provides additional information beyond that obtained with destructive optical microscopy. SXRR was able to distinguish between voids, cracks and lack of melt in, due to its sensitivity to the orientation of the discontinuity.
Die Integrität der Verstärkungsfasern in Komposit-Zahnstiften ist entscheidend für die Biegefestigkeit und die langfristige Haftung am Zement in den Wurzelkanälen. Es wurde vermutet, dass die Integrität von glasfaserverstärkten Zahnstiften durch das Beschleifen während der zahnmedizinischen Behandlung beeinträchtigt wird. Eine Beschädigung der Fasern führt zu einer erheblichen strukturellen Schwächung über den gesamten Stiftdurchmesser. Glasfragmente, die durch den Kontakt mit dem Zahnbohrer entstehen, können sich vom Stift lösen und die Haftfähigkeit erheblich verringern. Mit Hilfe hochauflösender Synchrotron-Röntgen-Refraktions-Radiographie (SXRR) konnte das Ausmaß der Schäden zuverlässig identifiziert und charakterisiert werden.
Dazu wurden die Glasfaserstifte sowohl im Herstellungszustand als auch nach der Bearbeitung mit einem Diamantbohrer untersucht. Die Datensätze wurden zur Visualisierung und Quantifizierung der morphologischen Charakteristika intakter und durch das Beschleifen beschädigter Regionen analysiert. Sie zeigen Schäden im bearbeiteten Bereich (z. B. Brüche, Splitter und Risse) sowie herstellungsbedingte Inhomogenitäten der Fasern mit einer signifikanten Zunahme der inneren Oberflächen in Probenregionen, die durch das Beschleifen beschädigt wurden.
Die Integrität der Verstärkungsfasern in Komposit-Zahnstiften ist entscheidend für die Biegefestigkeit und die langfristige Haftung am Zement in den Wurzelkanälen. Es wurde vermutet, dass die Integrität von glasfaserverstärkten Zahnstiften durch das Beschleifen während der zahnmedizinischen Behandlung beeinträchtigt wird. Eine Beschädigung der Fasern führt zu einer erheblichen strukturellen Schwächung über den gesamten Stiftdurchmesser. Glasfragmente, die durch den Kontakt mit dem Zahnbohrer entstehen, können sich vom Stift lösen und die Haftfähigkeit erheblich verringern. Mit Hilfe hochauflösender Synchrotron-Röntgen-Refraktions-Radiographie (SXRR) konnte das Ausmaß der Schäden zuverlässig identifiziert und charakterisiert werden.
Dazu wurden die Glasfaserstifte sowohl im Herstellungszustand als auch nach der Bearbeitung mit einem Diamantbohrer untersucht. Die Datensätze wurden zur Visualisierung und Quantifizierung der morphologischen Charakteristika intakter und durch das Beschleifen beschädigter Regionen analysiert. Sie zeigen Schäden im bearbeiteten Bereich (z. B. Brüche, Splitter und Risse) sowie herstellungsbedingte Inhomogenitäten der Fasern mit einer signifikanten Zunahme der inneren Oberflächen in Probenregionen, die durch das Beschleifen beschädigt wurden.
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.
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.
The manufacturability of metallic alloys using laser-based additive manufacturing methods such as laser powder bed fusion has substantially improved within the last decade. However, local melting and solidification cause hierarchically structured and crystallographically textured microstructures possessing large residual stress. Such microstructures are not only the origin of mechanical anisotropy but also pose metrological challenges for the diffraction-based residual stress determination. Here we demonstrate the influence of the build orientation and the texture on the microstructure and consequently the mechanical anisotropy of as-built Inconel 718. For this purpose, we manufactured specimens with [001]/[011]-, [001]- and [011]/[111]-type textures along their loading direction. In addition to changes in the Young’s moduli, the differences in the crystallographic textures result in variations of the yield and ultimate tensile strengths. With this in mind, we studied the anisotropy on the micromechanical scale by subjecting the specimens to tensile loads along the different texture directions during in situ neutron diffraction experiments. In this context, the response of multiple lattice planes up to a tensile strain of 10% displayed differences in the load partitioning and the residual strain accumulation for the specimen with [011]/[111]-type texture. However, the relative behavior of the specimens possessing an [001]/[011]- and [001]-type texture remained qualitatively similar. The consequences on the metrology of residual stress determination methods are discussed.
In the present study, in-situ observation of Hot Isostatic Pressure (HIP) procedure of laser powder bed fusion manufactured Ti-6Al-4V parts was performed to quantitatively estimate the densifcation rate of the material and the infuence of the defect initial size and shape on such rate. The observations were performed in-situ using the Ultrafast Tomography Paris-Edinburgh Cell and the combination of fast phase-contrast synchrotron X-ray tomography and energy dispersive difraction. With this strategy, we could quantify how the efectiveness of HIP depends on the characteristics of a defect. Smaller defects showed a higher densifcation rate, while the defect shape did not have signifcant efect on such rate.
Most knowledge about the structure, function, and evolution of early compound eyes is based on investigations in trilobites. However, these studies dealt mainly with the cuticular lenses and little was known about internal anatomy. Only recently some data on crystalline cones and retinula cells were reported for a Cambrian trilobite species. Here, we describe internal eye structures of two other trilobite genera. The Ordovician Asaphus sp. reveals preserved crystalline cones situated underneath the cuticular lenses. The same is true for the Devonian species Archegonus (Waribole) warsteinensis, which in addition shows the fine structure of the rhabdom in the retinula cells. These results suggest that an apposition eye with a crystalline cone is ancestral for Trilobita. The overall similarity of trilobite eyes to those of myriapods, crustaceans, and hexapods corroborates views of a phylogenetic position of trilobites in the stem lineage of Mandibulata.
Most knowledge about the structure, function, and evolution of early compound eyes is based on investigations in trilobites. However, these studies dealt mainly with the cuticular lenses and little was known about internal anatomy. Only recently some data on crystalline cones and retinula cells were reported for a Cambrian trilobite species. Here, we describe internal eye structures of two other trilobite genera. The Ordovician Asaphus sp. reveals preserved crystalline cones situated underneath the cuticular lenses. The same is true for the Devonian species Archegonus (Waribole) warsteinensis, which in addition shows the fine structure of the rhabdom in the retinula cells. These results suggest that an apposition eye with a crystalline cone is ancestral for Trilobita. The overall similarity of trilobite eyes to those of myriapods, crustaceans, and hexapods corroborates views of a phylogenetic position of trilobites in the stem lineage of Mandibulata.
The triaxial distribution of the residual stress in laser powder bed fused austenitic steel 316L was determined by X-ray and neutron diffraction. The residual stress analysis results were linked to the thermal history of the specimens, which were manufactured with varying inter-layer-times and scanning velocities. A clear link between the in-process temperature of the specimens and the residual stress was found, based on in-situ monitoring data.
Electron Beam Powder Bed Fusion-manufactured (E-PBF) porous components with narrow pores or channels and rough walls or struts can be filled with trapped powder after the manufacturing process. Adequate powder removal procedures are required, especially for high-density porous structures. In the present research, sheetbased porous structures with different thicknesses based on triply periodic minimal surfaces fabricated by EPBF were subjected to different post-processing methods, including a traditional powder recovery system for EPBF, chemical etching and ultrasound vibration-assisted powder removal. Wall thickness, internal defects, microstructure and morphology features, powder distribution inside the specimens, mechanical properties and deformation modes were investigated. A powder recovery system could not remove all residual powder from dense structures. In turn, chemical etching was effective for surface morphology changes and subsurface layers elimination but not for powder removal, as it affected the wall thickness, considerably influencing the mechanical properties of the whole structure. The ultrasound vibration method was quite effective for the removal of residual powder from sheet-based TMPS structures and without a severe degradation of mechanical properties. 10.1016/j.msea.2022.144479 Ultrasound vibration also caused grain refinement.
Explosive spalling is caused by, among others, the thermohydraulic spalling mechanism. During this process, vaporization, dehydration, moisture-transport and condensation processes interact. As a result, a drying and dehydration zone as well as a saturated zone, known as a moisture clog, are observed inside the unilaterally-heated concrete. The presented research is focused on the experimental investigation of the underlying thermohydraulic processes.
To investigate these, a test methodology based on X-ray computed tomography (CT) and nuclear magnetic resonance (NMR) was developed. Thereby, the X-ray CT scans are carried out simultaneously during the application of a defined unilateral-heating regime on a specially-constructed specimen. This miniaturized specimen, equipped with a double-layer casing, reproduces the condition within a planar, unilaterally-heated building component.
A preliminary test methodology and the first experimental results were presented at the 5th International Workshop on Concrete Spalling in Borås, Sweden (2017). The contribution for the upcoming workshop presents an improved version of this test methodology and new results for a high-performance concrete (HPC) mixture exposed to temperatures up to 500 °C. Regarding the CT measurements, a higher time-resolution of 15 min was achieved and a quantification of the moisture changes was implemented. Due to an increase in signal quality of the NMR measurements, a pore-size specific moisture distribution can now be resolved. This allows to conclude about the moisture reconfiguration between small gel pores and larger interhydrate pores. Additionally, the NMR measurement are no longer limited to first 2.5 cm below the heated surface but a one-dimensional moisture distribution can now be estimated over the whole 10 cm long specimen.
The presented results demonstrate that the combination of X-ray CT and NMR measurements enables to image and quantify the thermally-induced moisture transport and reconfiguration from small gel pores up to macro pores. This provides important insights into the thermohydraulic damage mechanism and leads to a better understanding of spalling avoidance strategies, like the addition of polypropylene fibres.
Explosive spalling is caused by, among others, the thermohydraulic spalling mechanism. During this process, vaporization, dehydration, moisture-transport and condensation processes interact. As a result, a drying and dehydration zone as well as a saturated zone, known as a moisture clog, are observed inside the unilaterally-heated concrete. The presented research is focused on the experimental investigation of the underlying thermohydraulic processes.
To investigate these, a test methodology based on X-ray computed tomography (CT) and nuclear magnetic resonance (NMR) was developed. Thereby, the X-ray CT scans are carried out simultaneously during the application of a defined unilateral-heating regime on a specially-constructed specimen. This miniaturized specimen, equipped with a double-layer casing, reproduces the condition within a planar, unilaterally-heated building component.
A preliminary test methodology and the first experimental results were presented at the 5th International Workshop on Concrete Spalling in Borås, Sweden (2017). The contribution for the upcoming workshop presents an improved version of this test methodology and new results for a high-performance concrete (HPC) mixture exposed to temperatures up to 500 °C. Regarding the CT measurements, a higher time-resolution of 15 min was achieved and a quantification of the moisture changes was implemented. Due to an increase in signal quality of the NMR measurements, a pore-size specific moisture distribution can now be resolved. This allows to conclude about the moisture reconfiguration between small gel pores and larger interhydrate pores. Additionally, the NMR measurement are no longer limited to first 2.5 cm below the heated surface but a one-dimensional moisture distribution can now be estimated over the whole 10 cm long specimen.
The presented results demonstrate that the combination of X-ray CT and NMR measurements enables to image and quantify the thermally-induced moisture transport and reconfiguration from small gel pores up to macro pores. This provides important insights into the thermohydraulic damage mechanism and leads to a better understanding of spalling avoidance strategies, like the addition of polypropylene fibres.
The water management in proton exchange membrane fuel cells (PEMFC) is strongly influenced by the design of the gas diffusion layers (GDL). Limiting current measurements in small-scale cells operating at high stoichiometries are useful to determine the oxygen transport resistance. The oxygen transport resistance increases, once water condenses inside the GDL. In this study a new electrochemical method for voltage loss estimation of GDL induced oxygen transport losses are presented. This new method, referred to as “transient limiting current” (TLC), is compared with the literature method. TLC allows a direct estimation of oxygen transport resistance at an arbitrarily conditioned state. This study also presents a case study of liquid water visualization of a PEM fuel cell with varying GDLs types.
With the help of quasi in-situ synchrotron X-ray computed tomography and time resolved radiography measurements we investigate appearance and distribution of liquid water inside the GDLs under limiting current conditions.
The stress-induced tetragonal to monoclinic (t-m) zirconia phase transformation can provide a certain degree of plasticity to Ceria-stabilized (Ce-TZP) zirconia-based composites. Characterizing and monitoring this phase transition on a millimeter-size range, within the bulk and in-situ remains a challenge. In this work, the mechanical behavior of Ce-TZP based composite was studied in tension, combining microscopy and synchrotron Xray refraction techniques. In contrast with microscopy methods, which only provide surface information, X-ray refraction radiography (SXRR) allowed the visualization of all the transformation bands, over the entire length and thickness of tested specimens, opening up new avenues for in-situ stress-induced t-m transformation studies.
This study reports on the stress relaxation potential of stress-relieving heat treatments for laser powder bed fused 316L. The residual stress is monitored non-destructively using neutron diffraction before and after the heat treatment. Moreover, the evolution of the microstructure is analysed using scanning electron microscopy. The results show, that a strong relaxation of the residual stress is obtained when applying a heat treatment temperature at 900°C. However, the loss of the cellular substructure needs to be considered when applying this heat treatment strategy.
The laser powder bed fusion of 316L leads to the formation of large residual stress. In this presentation, different stress relieve treatments were employed to assess their potential to relax the residual stress. The residual stress was determined by X-ray and neutron diffraction. The results give insights on the range of relaxation one can obtain by employing low and high temperature heat treatments and relates the relaxation to changes in the microstructure.
The formation of high magnitude residual stresses is inherent in laser powder bed fused processed austenitic steel 316L. Post-process heat treatments to relieve these stresses are necessary. In this study, heat treatment temperatures of 450°C, 800°C and 900°C were applied in order to avoid excessive sensitization. This temperature range thereby encompassed the upper and lower bounds for stress relieving treatment of this material. The residual stresses were determined by neutron diffraction and the evolution of the microstructure was monitored using scanning electron microscopy and electron backscattered diffraction. The results show that a full relaxation of the residual stresses is achieved when applying 900°C for 1 hour, which seems to be closely related to the dissolution of the subgrain solidification cellular structure.
The safe fatigue design of metallic components fabricated by additive manufacturing (AM) is still a largely unsolved problem. This is primarily due to (a) a significant inhomogeneity of the material properties across the component; (b) defects such as porosity and lack of fusion as well as pronounced surface roughness of the asuilt components; and (c) residual stresses, which are very often present in the as‐built parts and need to be removed by post‐fabrication treatments. Such morphological and microstructural features are very different than in conventionally manufactured parts and play a much bigger role in determining the fatigue life. The above problems require specific solutions with respect to the identification of the critical (failure) sites in AM fabricated components. Moreover, the generation of representative test specimens characterized by similar temperature cycles needs to be guaranteed if one wants to reproducibly identify the critical sites and establish fatigue assessment methods taking into account the effect of defects on crack initiation and early propagation. The latter requires fracture mechanics‐based approaches which, unlike common methodologies, cover the specific characteristics of so‐called short fatigue cracks. This paper provides a discussion of all these aspects with special focus on components manufactured by laser powder bed fusion (L‐PBF). It shows how to adapt existing solutions, identifies fields where there are still gaps, and discusses proposals for potential improvement of the damage tolerance design of L‐PBF components
We show that the equation proposed by Takeuchi and Argon to explain the creep behavior of Al–Mg solid solution can be used to describe also the creep behavior of pure aluminum. In this frame, it is possible to avoid the use of the classic pre-exponential fitting parameter in the power law equation to predict the minimum creep strain rate. The effect of the fractal arrangement of dislocations, developed at the mesoscale, must be considered to fully explain the experimental data. These ideas allow improving the recently introduced SSTC model, fully describing the primary and secondary creep regimes of aluminum alloys without the need for fitting. Creep data from commercially pure Al99.8% and Al–Mg alloys tested at different temperatures and stresses are used to validate the proposed ideas.
Toughening mechanisms and enhanced damage tolerant fatigue behaviour in laminated metal composites
(2022)
In the present study, fatigue crack growth (FCG) in a laminated metal composite (LMC) consisting of Al-based constituents with dissimilar strength was studied. Additionally, the FCG in both monolithic constituent materials was determined and a linear elastic rule of mixture (ROM) concept was calculated as a reference for the FCG of the laminated composite. Crack networks in the laminates were analyzed post-mortem by means of light microscopy and synchrotron X-Ray tomography (SXCT). Significantly reduced FCG rates for the LMC were found at elevated stress intensity ranges compared to both the monolithic constituents as well as the ROM concept. This is the result of the formation of a complex 3D crack network in the laminated architecture caused by the appearance of the two different toughening mechanisms a) crack deflection and b) crack bifurcation at the vicinity of the interfaces.
The mechanisms controlling the fatigue response of an A357-T6 cast aluminium alloy under cyclic torsional loading are investigated. Surface crack monitoring coupled with Electron BackScattering Diffraction (EBSD) analysis is used to study crack initiation. Determination of S-N curve combined with interrupted in situ fatigue testing using synchrotron tomography allows the study of the propagation behaviour. It is observed that fractographic morphologies depend on the stress level. At intermediate-low stress levels ( τmax < 100 MPa), the grain structure controls the crack initiation and propagation periods. Cracks are usually nucleated in mode II from slip planes close to the specimen axis or perpendicular to it. Mode II crack growth dominates the early stages of crack propagation as mode III inward crack growth is rapidly decelerated. This behaviour leads to the formation of characteristic shallow surface cracks. Once the crack is long enough for the mode II driving force to be overtaken by mode III, propagation branches into ~45 ◦mode I.
Metastable austenitic stainless steel (304L) samples with a rectangular cross-section were plastically deformed in torsion during which they experienced multiaxial stresses that led to a complex martensitic phase distribution owing to the transformation induced plasticity effect. A three-dimensional characterization of the phase distributions in these cm-sized samples was carried out by wavelength-selective neutron tomography. It was found that quantitatively correct results are obtained as long as the samples do not exhibit any considerable preferential grain orientation. Optical microscopy, electron backscatter diffraction, and finite element modeling were used to verify and explain the results obtained by neutron tomography. Altogether, neutron tomography was shown to extend the range of microstructure characterization methods towards the meso- and macroscale.
Metastable austenitic stainless steel (304L) samples with a rectangular cross-section were plastically deformed in torsion during which they experienced multiaxial stresses that led to a complex martensitic phase distribution owing to the transformation induced plasticity effect. A three-dimensional characterization of the phase distributions in these cm-sized samples was carried out by wavelength-selective neutron tomography. It was found that quantitatively correct results are obtained as long as the samples do not exhibit any considerable preferential grain orientation. Optical microscopy, electron backscatter diffraction, and finite element modeling were used to verify and explain the results obtained by neutron tomography. Altogether, neutron tomography was shown to extend the range of microstructure characterization methods towards the meso- and macroscale.
To see and not to see - Möglichkeiten und Grenzen der Schadensanalyse mit CT an Kompositmaterialien
(2020)
Anhand von drei Beispielen (Datenfusion an CFK; Machine Learning an Metall-Matrix-Kompositen sowie Refraktion an CFK) wird gezeigt, wie die BAM mit neuen Analysemethoden mehr Informationen aus CT-Datensätzen extrahieren kann, sowie mit der Refraktion eine Analysemethode besitzt, die in Fällen eingesetzt werden kann, bei denen klassische Durchstrahlungsmethoden kein Ergebnis liefern.
The synthesis route and thermoelectric characterization of n-type Fe2-xTi1+xO5 (0 ≤ x ≤ 0.5) and Fe1.75(Ti1-yNby)1.25O5 (0 ≤ y ≤ 0.05) are presented. Their electrical conductivity obeys the small polaron model and their Seebeck coefficient is weakly dependent on temperature. The carrier concentration is increased with increasing Ti content in Fe2-xTi1+xO5, thus improving the electrical conductivity and decreasing the absolute values of the Seebeck coefficient. The composition with x = 0.5 shows reduced electrical conductivity contradicting the change in the carrier concentration, as it contains more microcracks than the other compositions. Fe2-xTi1+xO5 exhibits extremely low thermal conductivity. Fe2-xTi1+xO5 with x = 0.25 exhibits the highest ZT, ~ 0.014 at 1000 K. Therefore, a limited extent microcracks are beneficial to thermoelectric properties; however, when they are too extended they can be detrimental. On the contrary to Fe2TiO5, Nb substitution into Fe1.75Ti1.25O5 does not obviously improve its thermoelectric properties.
Thermoelectric properties of doubly substituted La0.95Sr0.05Co1-xCrxO3 (0 ≤ x ≤ 0.5) ceramics
(2018)
Dense La0.95Sr0.05Co1-xCrxO3 (0 ≤ x ≤ 0.5) ceramics were synthesized by solid-state reaction and conventional sintering. Room-temperature crystal structure and microstructure were investigated and the thermoelectric properties were measured in the temperature range 323 K – 1020 K. All compositions are single phase with rhombohedral structure, and the lattice parameter of La0.95Sr0.05Co1-xCrxO3 increases with increasing Cr content.
La0.95Sr0.05Co1-xCrxO3 is a p-type small polaron conductor. The charge carrier concentration is determined by both substitution of La3+ with Sr2+ and thermally-activated charge disproportionation of Co3+ and / or Cr3+. Above 550 K, the substitution of Co with Cr increases the Seebeck coefficient and reduces the electrical conductivity. Below 550 K, the trend of Seebeck coefficient with Cr content is not clear due to the thermally activated charge disproportionation. At low temperature, the electrical conductivity shows a minimum with Cr content of x = 0.4, as a result of trapped polarons in the Cr sites. By substituting Co with Cr, the power factor below 800 K is reduced and that above 800 K is improved.
The thermal conductivity is effectively reduced by doping Cr. The highest ZT value of 0.053 at 373 K is achieved for x = 0, but it decreases rapidly with increasing temperature. Substitution of Co with Cr can effectively improve the ZT values at high temperatures. In the temperature range 700 K – 1000 K, ZT increases with increasing Cr content, the highest being 0.04 at 1000 K for the composition with x = 0.5, more than 4 times the value of the La0.95Sr0.05CoO3 compound.
Thermally-induced moisture transport in high-performance concrete studied by X-ray-CT and 1H-NMR
(2019)
The thermohydraulic damage mechanism is one of the primary causes for explosive spalling of highperformance concrete. This paper presents the spatially- and temporally-resolved analysis of the thermally-induced moisture transport and reconfiguration processes by means of X-ray-CT and 1HNMR.
Thermal testing results for a high-performance concrete, which is sensitive to explosive spalling and which was prepared with and without added polypropylene fibres, are presented in this paper. These results indicate that the addition of fibres leads to a faster and deeper migration of the drying front and, thus, to a lower likelihood of vapour-pressure induced explosive spalling.