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The quantification of experimental and data analysis errors is most of the times jeopardised by the presence of surface roughness, waviness, as well as by typical measurement artefacts of the XCT technique (for instance refraction at sharp edges). One way to at least estimate the influence of those factors on dimensional measurements and on tolerances is to simulate them using Monte-Carlo method. An alternative strategy is to use independent knowledge (e.g. CMM data) to smoothen/calibrate/correct XCT data.
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.
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.
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.
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.
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 BAMline at the synchrotron X-ray source BESSY II (Berlin, Germany) is supporting researchers especially in materials science. As a non-destructive characterization method, synchrotron X-ray imaging, especially tomography with hard X-Rays, plays an important role in structural 3D characterization. The imaging capabilities allow for in-situ and operando experiments. In this presentation the data handling pipeline is presented.
After a general presentation of the beamline, specifically the workflow for ex-situ CT at BAMline is presented. Although being used in a broad variety of research fields the usual workflow for CT experiments is in most cases similar in terms of sample mounting, tomographic scan and reconstruction. Specific scanning schemes allow for a preview reconstruction carried out during the scan. A detailed description of the used hardware as well as the self-coded programs applied in the data pipeline will be given. This will be accompanied by a practical demonstration of the software involved in the entire process.
After a general presentation of the beamline, specifically the workflow for ex-situ CT at BAMline is presented. Although being used in a broad variety of research fields the usual workflow for CT experiments is in most cases similar in terms of sample mounting, tomographic scan and reconstruction. Specific scanning schemes allow for a preview reconstruction carried out during the scan. A detailed description of the used hardware as well as the self-coded programs applied in the data pipeline will be given. This will be accompanied by a practical demonstration of the software involved in the entire process.
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.
Die Entwicklung von Werkzeugen zur realitätsnahen Nachbildung eines industriellen CT-Systems in einer Simulationssoftware ist derzeit Hauptaufgabe des WIPANO Forschungsprojektes CTSimU2 Realistische Simulation realer Röntgencomputertomografie - Systeme mit basisqualifizierter Simulationssoftware. Als Voraussetzung dienen dabei Simulationssoftwares, die durch das Testframework aus dem Vorprojekt CTSimU1 basisqualifiziert wurden. Das Testframework testet die hinreichende physikalische Korrektheit und Funktionalität einer Simulationssoftware (Basisqualifizierung der Software). Für eine realitätsnahe Nachbildung ist nicht nur die Güte der Simulationssoftware, sondern insbesondere die Güte der Parametrisierung des realen CT-Systems in der Simulationssoftware ausschlaggebend. Dabei kann das Vorgehen der Parametrisierung in vier Schritte unterteilt werden: die Datenaufnahme am realen CT-System (Schritt 1), die Auswertung der aufgenommenen Daten für die Generierung allgemeiner Parameterangaben (Schritt 2), die Übertragung der Parameter in die spezifischen Simulationssoftwares (Schritt 3) und die Validierung der resultierenden Simulationsparameter durch einen geeigneten Test (Schritt 4). Ziel des Projektes ist es daher neben der Erarbeitung eines Werkzeugkastens mit allgemeinen Methoden zur Datenaufnahme und Auswertung der Daten, die Entwicklung eines Tests, auf dessen Basis die ausreichend korrekte Simulation einer realen Anlage beurteilt werden kann. Die erarbeiteten Ergebnisse sollen wie bereits im Vorprojekt CTSimU1 in einen Richtlinienentwurf für die Richtlinienreihe VDI/VDE 2630 übertragen werden. Dieser Beitrag soll einen Überblick über das Projekt und die ersten Ergebnisse geben.
The simulator aRTist combines analytical and Monte Carlo methods to efficiently model the radiographic process of industrial radiology. In this contribution we focus on virtual computer tomography, the simulation of tomographic scans. The possibilities to simulate complex scanning trajectories are shown in combination with the tomographic reconstruction using individual projection matrices.
Virtual CT with aRTist
(2021)
Simulation becomes more and more important in modern CT imaging. It is increasingly used to optimize techniques for complex applications, to support the preparation of written procedures, and for educational purposes. The radiographic simulator aRTist is a modelling tool which simulates X-ray imaging using a hybrid analytical and Monte Carlo method to efficiently model the radiation transport. In addition to the relevant physical effects such as absorption, scattering and fluorescence, simplified fast models are employed to describe the characteristics of the X-ray source and the detector. aRTist is well equipped to model realistic X-ray imaging setups due to the ability to load exported CAD object descriptions. A simple CT scan module is contained in aRTist which allows the simulation of standard (circular cone beam) scanning trajectories.
This training session starts with a general introduction to aRTist and will highlight its basic usage. Furthermore, the focus is on the configuration of scan trajectories and batch simulations for virtual CT. The aim is to enable the audience to use the aRTist software for their own experiments in virtual CT.
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.
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.
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 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 BAMline at the synchrotron X-ray source BESSY II (Berlin, Germany) is supporting researchers especially in materials science. As a non-destructive characterization method, synchrotron X-ray imaging, especially tomography with hard X-Rays, plays an important role in structural 3D characterization. The imaging capabilities allow for in-situ and operando experiments. In this presentation the equipment, data handling pipeline as well as various examples from material science are presented.
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.
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.
The relaxation of macroscopic residual stresses in laser powder bed fused stainless steel 316L
(2021)
The processing of stainless steel 316L using the additive manufacturing process Laser Powder Bed Fusion (LPBF) can widen its field of application due to a strong increase in Yield strength, without making major compromises on the ductility nor its outstanding corrosion and oxidation properties. Furthermore, improved designs that either reduce the weight or optimise the function of a part can be obtained using LPBF. These benefits are however counterbalanced by the proneness of LPBF to inducing high Residual Stresses (RS) during manufacturing. The characterisation and monitoring of these RS are of paramount importance for the wider acceptance of the LPBF process. This study focuses on the relaxation of the initial macroscopic RS present in an LPBF 316L as-built prism that undergoes various routes of manufacturing steps to achieve different specimen geometries and stress relieving treatments. The RS are determined using Angle-Dispersive (AD) and Time-of-Flight (TOF) neutron diffraction. The results reveal high tensile RS close to the surfaces and compressive RS near the centre of the as-built parts. The reduction in size and change of geometry heavily impact the stress ranges of the remaining RS, with lower stress ranges in cylindrical shaped compared to rectangular shaped specimens. Also, the application of different stress relieving heat treatments showed that heat-treating temperatures above 800 °C are necessary to obtain a strong relaxation in LPBF 316L.
Advanced Manufacturing and Advanced Materials have been identified by the European Commission as one of six Key Enabling Technologies (KETs), the full exploitation of which will create advanced and sustainable economies. Metrology is a key enabler for progress of these KETs. EURAMET, which is the association of metrology institutes in Europe, has addressed the vital importance of Metrology for these KETs through the support for the creation of a European Metrology Network for Advanced Manufacturing. The EMN for Advanced Manufacturing (AdvanceManu) was approved in June 2021 and held the formal kick-of meeting in October 2022. The EMN comprises both National Metrology Institutes (NMIs) from across Europe and other designated Institutes (Dis). The EMN is organized in three sections; Advanced Materials, Smart Manufacturing Systems and Manufactured components and products. The aim of the EMN is to engage with stakeholders in the field of Advanced Manufacturing and Advanced Materials (Large & SMEs, industry organisations, existing networks and academia) with the aim to prepare a Strategic Research Agenda (SRA) for Metrology for Advanced Manufacturing. In the shorter term, an orientation paper is aimed to be produce to in the context of the European Partnership for Metrology. In addition to the SRA, the EMN will establish knowledge and technology transfer and promotion plan. This includes leveraging the existing research results from the completed and running EMPIR JRP projects funded through EURAMET.
This presentation will outline the EMN for Advanced Manufacturing, describing the structures and goals, the route to the production of the SRA and the progress made to date identifying the key metrology challenges across the related Key Industrial Sectors (KICs). In particular, the presentation aims to inform the community on how to be involved in the shaping of the strategic research agenda for the future of Metrology for Advanced Manufacturing and Advanced Materials.
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.
Additive manufacturing methods such as laser powder bed fusion (LPBF) allow geometrically complex parts to be manufactured within a single step. However, as an aftereffect of the localized heat input, the rapid cooling rates are the origin of the large residual stress (RS) retained in as-manufactured parts. With a view on the microstructure, the rapid directional cooling leads to a cellular solidification mode which is accompanied by columnar grown grains possessing crystallographic texture. The solidification conditions can be controlled by the processing parameters and the scanning strategy. Thus, the process allows one to tailor the microstructure and the texture to the specific needs. Yet, such microstructures are not only the origin of the mechanical anisotropy but also pose metrological challenges for the diffraction-based RS determination. In that context the micromechanical elastic anisotropy plays an important role: it translates the measured microscopic strain to macroscopic stress. Therefore, it is of uttermost importance to understand the influence of the hierarchical microstructures and the texture on the elastic anisotropy of LPBF manufactured materials.
This study reveals the influence of the build orientation and the texture on the micro-mechanical anisotropy of as-built Inconel 718. Through variations of the build orientation and the scanning strategy, we manufactured specimens possessing [001]/[011]-, [001]-, and [011]/[111]-type textures. The resulting microstructures lead to differences in the macroscopic mechanical properties. Even further, tensile in-situ loading experiments during neutron diffraction measurements along the different texture components revealed differences in the microstrain response of multiple crystal lattice planes. In particular, the load partitioning and the residual strain accumulation among the [011]/[111] textured specimen displayed distinct differences measured up to a macroscopic strain of 10 %. However, the behavior of the specimens possessing [001]/[011]-and [001]-type texture was only minorly affected. The consequences on the metrology of RS analysis by diffraction-based methods are discussed.
An unusual microstructure, inherent residual stresses and void formation are the three key aspects to control when assessing metallic parts made by LPBF. This talk explains an experiment to unravel the interlinked influence of the two mechanisms for the formation of residual stresses in LPBF: the temperature gradient mechanism and constricted solidification shrinkage. The impact of each mechanism on the shape and magnitudes of the residual stress distribution is described. Combined results from neutron diffraction, X-ray diffraction, computed tomography and in-situ thermography are presented.
Also, influence of scan strategies as well as surface roughness of subjacent layers on void formation is shown. Results from computed tomography and in-situ thermography of a specimen dedicated to study the interaction of the melt pool with layers of powder underneath the currently illuminated surface are presented.
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 complexity of any microstructural characterization significantly increases when there is a need to evaluate the icrostructural evolution as a function of temperature. To date, this characterization is primarily performed by undertaking elaborative ex-situ experiments where the material’s heating procedure is interrupted at different temperatures or times. Moreover, these studies are often limited to a region smaller than the representative elementary volume, which can lead to partial or even biased interpretations of the collected data. This limitation can be greatly overcome by using in-situ synchrotron X-ray refraction (SXRR).
Absorption edge tomography is a method which exploits the sudden change of the attenuation coefficient, when the photon energy crosses the absorption edge of an element. The beamline BAM line at BESSY II, which is operated by the Federal Institute for Materials Research and Testing, can provide a monochromatized beam in a photon energy range from 5 keV up to 80 keV with a bandwidth of 2%. Together with the microtomography setup, this enables differential tomography sensitive to any element with N >= 24 (Cr) by using an appropriate K- or L-edge in this range. Here, a polymer filament embedding metal organic framework (MOF) was prepared and used for 3D printing. Absorption edge tomography at the copper K edge was employed to perform a non-destructive 3D characterization of the microstructure of the embedded MOF. Data fusion was then used to determine the size distribution of the embedded MOF.
Absorption edge tomography, also known as differential tomography at absorption edges, is a method which exploits the sudden change of the attenuation coefficient, when the photon energy crosses the absorption edge of an element. Synchrotron radiation is the best source for absorption edge tomography, because of its small bandwidth, high intensity and easily adjustable photon energy. The synchrotron beamline BAMline at the synchrotron radiation facility BESSY II in Berlin, which is operated by the BundesanstaltfürMaterialforschung und -prüfung (BAM), provides a monochromatized beam in a photon energy range from 5 keV up to 80 keV with a bandwidth of 2%, when the double multilayer monochromator is used. Together with the microtomography setup, this enables differential tomography at the K edge of the elements from chromium up to the lanthanides, and up to uranium, when the L edges are used as well.
In this work, the absorption edge tomography is employed to perform a non-destructive, three-dimensional characterization of the microstructure of metallic alloys. As an example, a high strength Mg-Y-Zn alloy containing long period stacking ordered (LPSO) phases is analysed. The alloy with a nominal composition of Mg97Y2Zn1 was synthesized by melting highly pure magnesium, zinc and a Mg-22%Y master alloy and casting an ingot, which was homogenised at 350 °C and then extruded using an extrusion ratio of 18:1.
The results demonstrate that synchrotron based absorption edge tomography is a promising technique to perform a 3D characterization of the microstructure of metallic alloys.
The influence of the inter-layer-time and the scanning velocity on the surface and bulk residual stress in laser powder bed fused 316L specimens was investigated. This study combines X-ray and neutron diffraction results with the thermal history of the specimens acquired through in-situ process monitoring. The process parameter variations were observed to directly influence the thermal history, which gave new insights in the assessment of the residual stress results.
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.
Near eutectic cast Al–Si alloys are the basis of all Al-alloys used for pistons due to their high fluidity and relatively high strength-to-weight ratio. Their microstructure is characterized by the presence of eutectic-Si embedded in an age hardenable -Al matrix. During solution heat treatment, the eutectic Si network undergoes a process of gradual disintegration, reducing the load bearing capability and the strength of the alloy. The improvement of the high temperature strength is achieved by addition of transition elements such as Cu, Mg or Ni through the formation of stiff intermetallic (IM) phases.
In present study a near-eutectic AlSi12CuMgNi alloy produced by squeeze casting was investigated in as-cast condition. The in-situ neutron diffraction compression tests revealed the stress partitioning mechanism between phases of the alloy. Large stresses were found in IMs, showing their significant role as a reinforcement elements. After the failure of IM and Si phases the load is transferred back to the Al matrix, inducing further plastic deformation in it, yet without creating microcracking. The neutron diffraction experiments were coupled with assessment of internal damage after ex-situ compression tests by synchrotron radiation computed tomography. The quantitative analysis of CT data revealed that local tensile stresses in IM and Si phases induce microcracks with preferential orientation, parallel to the axis of applied load.
Altogether, present experimental data was used as an input for the developed micromechanical model based on Maxwell homogenization scheme. In contrast to the neutron diffraction experiment, which can only determine stress differences between the axial and radial sample directions, the model allows predicting the principal stresses in each phase of the alloy.
For how trivial or provocative it can sound, the best neutron spectrometer in the world does not produce science and technology 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, 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 and sustainable for the material science and industrial research community.
In this presentation, and based on two examples, we will show a couple of strategies to combine neutron data with other experiments, and with theoretical models to raise the validity of experiments to the level of problem-solving. As one might imagine, these are only a few among the almost infinite combinations possible to help improving material properties, performance, and safety, i.e., ripe for everyday use.
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.
Ti-6Al-4V alloy is intensively used in the aerospace industry because of its high specific strength. However, the application of Laser Powder Bed Fusion (LPBF) Ti-6Al-4V alloy for structurally critical load-bearing components is limited. One of the main limiting factors affecting the structural integrity, are manufacturing defects. Additionally, the high cooling rates associated with LPBF process result in the formation of large residual stress (RS) with complex fields. Such RS can cause cracking and geometrical distortions of the part even right after production. Also, the microstructure of LPBF Ti-6Al-4V in the as-built condition is significantly different from that of the conventionally produced alloy. All these factors affect the mechanical behavior of the material. Therefore, to improve the material performance it is important to evaluate the individual effect of RS, defects, and microstructure on fatigue life. To this aim Ti-6Al-4V LPBF material in as-built condition and subjected to different post-processing, including two heat treatments (for stress relief and microstructural modification) and Hot Isostatic Pressing (HIP, for densification), were investigated.
Prior to fatigue tests at elevated temperature, the microstructure, the mesostructure, and subsurface RS on the fatigue samples were investigated. It was found that the fatigue performance of HIPped samples is similar to that of conventionally produced Ti-6Al-4V. The tensile RS found at the surface of as-built samples decreased the fatigue life compared to heat-treated samples. Additionally, the modification of the microstructure (by heat treatment) did not affect the fatigue performance in the regime of mostly elastic strain. This shows that in the absence of tensile RS the manufacturing defects solely control the failure of LPBF components and densification has the strongest effect on the improvement of the mechanical performance.
Beton ist das meistbenutzte Baumaterial der Welt. Sein Herstellungsprozess ist auch für schätzungsweise 5% der globalen Kohlenstoffemissionen verantwortlich. Daher können selbst kleine Verbesserungen in der Festigkeit oder Haltbarkeit zu einer erheblichen Verringerung der Bau- und Wartungskosten, der Umweltschäden und der Gefahr für die Menschen führen. Um das grundlegende Verhalten dieses Materials zu verstehen, ist es notwendig, seine Leistung während thermischer, chemischer und mechanischer Prozesse (d. h. in-situ) zu beobachten. Es wird eine zerstörungsfreie Messmethode benötigt, die in der Lage ist, nicht nur Änderungen des Materials wie Feuchtigkeitsumverteilung, Korrosion und Dehnung zu messen, sondern auch die innere Struktur des Materials im Dreidimensionalen aufzulösen, so dass Versagensmechanismen und Transportphänomene direkt auf bestimmte Eigenschaften der heterogenen Materialstruktur bezogen werden können (wie z.B. die Übergangszone zwischen Gesteinskörnungen und Zementstein oder die Orientierung von eingebetteten Fasern).
Die Röntgencomputertomographie (CT) hat sich als ideal für solche Zwecke erwiesen. Neuere Forschungen an der BAM werden vorgetragen, die die Fähigkeiten der CT zur Identifizierung quantitativer Materialeigenschaften wie Faserorientierung, Rissoberfläche, Korrosionsverteilung und Änderungen des volumetrischen Feuchtigkeitsanteils demonstrieren. Der Nutzen dieser leistungsstarken Analysewerkzeuge wird dann anhand der Ergebnisse einer Reihe von Ex-situ und In-situ Testprogrammen für Bedingungen wie mechanische Belastung, Wassertransport und thermische Exposition gezeigt. Speziell entwickelte In-situ Testmaschinen für diese verschiedenen Testprogramme werden ebenfalls beschrieben. Die von der CT gelieferten quantitativen Charakterisierungsinformationen haben sich als ideale Grundlage für die Kalibrierung bzw. Validierung von numerischen Simulationen erwiesen. CT ist auch wesentlich für die Beantwortung von vielen anwendungsspezifischen Fragen, u.a. wie sich verschiedene Gießverfahren auf die Materialleistung auswirken, welche Mineralien sich als Zuschlagstoffe anfällig für langfristige chemische und hydraulische Prozesse erweisen und wie Polymerfasern den Druckaufbau in Beton während der thermischen Belastung beeinflussen.
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.
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).
In Leichtbauanwendungen sind Materialien mit geringen Dichten und hohen Festigkeiten gefragt. Insbesondere Faser-Kunststoff-Verbunde (FKV) erfüllen diese Anforderungen und werden zunehmend für Strukturbauteile eingesetzt. Die Oberflächen moderner Rotorblätter von Windkraftanlagen werden aus FKV gefertigt. Das Versagen dieser Materialien hat massiven Einfluss auf die Einsatzfähigkeit der gesamten Windkraftanlage. Daher ist die Kenntnis des Versagensverhaltens dieser Komponenten unter statischer und zyklischer Belastung von großem Interesse, um die Betriebsbeanspruchung abzuschätzen. Im Idealfall wird die Schadensentwicklung unter Betriebslast mit zerstörungsfreien in-situ-Prüfverfahren ermittelt. Hier berichten wir über die Beobachtung der Rissentwicklung in Carbon-Faserverstärkten Kunststoffen (CFK) unter kontinuierlicher Zugbelastung durch in-situ Synchrotron-Röntgenrefraktionsradiographie. Eine selbst entwickelte elektromechanische Zugprüfmaschine mit einem Kraftbereich bis zu 15 kN wurde in den Strahlengang an der BAMline (BESSY II) integriert. Da in herkömmlichen (Absorptions-) Radiographien Defekte wie Zwischenfaserbrüche oder Faser-Matrix-Enthaftung keinen ausreichenden Kontrast verursachen, wird zur Kontrastanhebung die Röntgenrefraktion benutzt. Hier wird das sogenannte Diffraction Enhanced Imaging (DEI) angewandt, um Primär- und gebrochene Strahlung mit Hilfe eines Analysatorkristalls zu trennen. Diese Technik ermöglicht schnelle Messungen mit einem Gesichtsfeld von einigen Quadratmillimetern (hier: 14 mm × 7.2 mm) und ist ideal für in-situ Untersuchungen. Die Bildgebung und der Zugversuch erfolgen mit einer Bildfrequenz von 0.7 / s und einer Dehnrate von 0.00055 / s . Bei 0°/90° Fasergelegen treten die ersten Zwischenfaserrisse bei 380 MPa (Dehnung 0.8 %) auf. Vor dem Versagen bei ca. 760 MPa (Dehnung 2.0 %) beobachten wir die Ausbildung eines nahezu äquidistanten Rissmusters (Risse in ca. 1 mm Abstand), das sich im geschädigten Zustand über die gesamte Probe erstreckt.
Residual stresses in Laser Beam Melting (LBM) – Critical Review and outlook of activities at BAM
(2019)
Additive manufacturing (AM) technologies have experienced an exceedingly rapid growth, which is coupled with the knowledge about the resulting material properties and performance. In particular, residual stress (RS) was soon recognized as an important issue in AM parts, such that parts are usually subjected to a post build-heat-treated. Significant effort has been spent on simulations of RS in AM, especially using finite element methods. As a consequence, the experimental determination of RS has thereby become increasingly important as a validation tool for simulations, as well as a method for assessing the influence of process parameters. In particular, diffraction methods, which are fundamentally non-destructive, offer enormous possibilities to gain knowledge on the residual stress state in real components, since synchrotron radiation and neutrons can penetrate even heavy metals up to several millimeters or centimeters, respectively. Indeed, significant progress has been achieved, in the understanding of the origins of the RS fields as a function of process parameters, as well as their stability under thermal and/or mechanical exposure.
In this paper, a few success stories will be outlined. It will be shown how the determination of RS in metallic parts (with the focus on those produced by laser powder bed fusion) has even revealed that process parameters that were previously considered unimportant (e.g. the position and orientation on the base plate) play a major role in the onset of residual stress accumulation.
However, while RS characterization is starting to be considered in the component 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 investigates about the hypotheses underlying its experimental determination. Therefore, some aspects to be aware of, or even those which to date are unclear, will also be discussed. These include the determination of the stress-free reference and of the principal axes of stress. All of these aspects will lead towards a comprehensive understanding of the process-structure-performance relationships in AM materials and parts.
Residual stresses in Laser Beam Melting (LBM) – Critical Review and outlook of activities at BAM
(2019)
Additive manufacturing (AM) technologies have experienced an exceedingly rapid growth, which is coupled with the knowledge about the resulting material properties and performance. In particular, residual stress (RS) was soon recognized as an important issue in AM parts, such that parts are usually subjected to a post build-heat-treated. Significant effort has been spent on simulations of RS in AM, especially using finite element methods. As a consequence, the experimental determination of RS has thereby become increasingly important as a validation tool for simulations, as well as a method for assessing the influence of process parameters. In particular, diffraction methods, which are fundamentally non-destructive, offer enormous possibilities to gain knowledge on the residual stress state in real components, since synchrotron radiation and neutrons can penetrate even heavy metals up to several millimeters or centimeters, respectively. Indeed, significant progress has been achieved, in the understanding of the origins of the RS fields as a function of process parameters, as well as their stability under thermal and/or mechanical exposure.
In this paper, a few success stories will be outlined. It will be shown how the determination of RS in metallic parts (with the focus on those produced by laser powder bed fusion) has even revealed that process parameters that were previously considered unimportant (e.g. the position and orientation on the base plate) play a major role in the onset of residual stress accumulation.
However, while RS characterization is starting to be considered in the component 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 investigates about the hypotheses underlying its experimental determination. Therefore, some aspects to be aware of, or even those which to date are unclear, will also be discussed. These include the determination of the stress-free reference and of the principal axes of stress. All of these aspects will lead towards a comprehensive understanding of the process-structure-performance relationships in AM materials and parts.
Additive manufacturing (AM) technologies are experiencing an exceedingly rapid growth, driven by their potential through layer wise deposition for transformational improvements of engineering design, leading to efficiency and performance improvements. Laser Powder Bed Fusion (LPBF) is an Additive Manufacturing (AM) method which permits the fabrication of complex structures that cannot otherwise be produced via conventional subtractive manufacturing methods. Nevertheless, the rapid cooling rates associated with this process results in the formation of significant and complex residual stress (RS) fields. A large body of both experimental and simulation research has been dedicated in recent years to the control and mitigation of RS in AM. In order to validate simulations with the end goal of being able to model the residual stress state in AM components and to devise strategies for their reduction during manufacturing, experimental methods need to be able to accurately determine 3D residual stresses fields in complex geometries. Several destructive and non-destructive methods can be used to analyze the RS state, the choice of which depends on the geometry and the information required. Diffraction-based methods using penetrating neutron and synchrotron X-rays at large scale facilities offer the possibility to non-destructively spatially resolve both surface and bulk residual stresses in complex components and track their changes following applied thermal or mechanical loads. This presentation will overview the success stories of using large scale facilities by the BAM for the characterization of residual stresses in additively manufactured metallic alloys. In particular, the study of the influence of process parameters on the residual stress state and the relaxation of these stresses through heat treatment will be presented. However there remains challenges to overcome particularly of the hypotheses underlying the experimental determination of residual stresses, which will be discussed.
Metal Additive manufacturing (AM) technologies such as Laser Powder Bed Fusion (LPBF) enable the fabrication of complex structures, giving rise to potential improvements in component and manufacturing efficiency. However, the processes are typically characterized by the generation of high magnitude residual stress (RS) which can have detrimental consequences for subsequent applications. Therefore, the characterization of these RS fields and the understanding of their formation and mitigation through optimized processing is crucial for the wider uptake of the technology. Due to the potential complex nature and high value of components manufactured by LPBF, it is important to have suitable characterisation methods which can determine the spatial variations of RS in a non-destructive manner. Neutron diffraction is considered to be the best suited for these requirements. However, the microstructures developed in the complex thermal cycles experience in the production can pose challenges to the ND method for RS analysis. The BAM has conducted significant research over the past years to overcome these obstacles, enabling higher confidence in the RS determined in LPBF materials by neutron diffraction. This contribution will overview some of these advancements made recently at European neutron sources including on Stress-Spec at FRM2/MLZ.
Residual stresses Analysis in Additively Manufactured alloys using neutron diffraction (L-PBF)
(2023)
An overview of recent progress at BAM of residual stress analysis in additively manufactured, in particular Laser Powder Bed Fusion of metallics materials, using neutron diffraction will be presented. This will cover important topics of the stress-free reference, the diffraction elastic moduli and principal stress determination.
Design of freedom, performance improvement, cost reduction and lead time reduction are key targets when manufacturing parts in a layer-by-layer fashion using the laser powder bed fusion process (LPBF). Many research groups are focussed on improving the LPBF process to achieve the manufacturing of sound parts from a structural integrity perspective. In particular, the formation and distribution of residual stress (RS) remains a critical aspect of LPBF. The determination of the RS in LPBF benefits from the use of neutron diffraction (ND), as it allows the non-destructive mapping of the triaxial RS with a good spatial resolution. Two case studies are presented based on experiments carried out on the angular-dispersive neutron diffractometers Strain Analyser for Large Scale Engineering Applications (SALSA) (Institut Laue Langevin, Grenoble) and STRESS-Spec (FRM II, Garching). The RS in LPBF parts having a rectangular and more complex geometry (lattice structure) is analysed. The former example discusses the mapping of the RS in a rectangular body manufactured from stainless steel 316L. The manufacturing of these parts was monitored using an in-situ thermography set-up to link the RS to the thermal history. The latter discusses the RS in a lattice structure manufactured from the nickel base superalloy IN625. This geometry is challenging to characterise, and the use of a X-ray computed tomography twin is presented as tool to support the alignment of the ND experiment. The results from these case studies show a clear link between the thermal history and the RS magnitudes, as well as giving insights on the RS formation.
Additive Manufacturing (AM) through the Selective Laser Melting (SLM) route offers ample scope for producing geometrically complex parts compared to the conventional subtractive manufacturing strategies. Nevertheless, the residual stresses which develop during the fabrication can limit application of the SLM components by reducing the load bearing capacity and by inducing unwanted distortion, depending on the boundary conditions specified during manufacturing.
The present study aims at characterizing the residual stress states in the SLM parts using different diffraction methods. The material used is the nickel based superalloy Inconel 718. Microstructure as well as the surface and bulk residual stresses were characterized. For the residual stress analysis, X-ray, synchrotron and neutron diffraction methods were used. The measurements were performed at BAM, at the EDDI beamline of -BESSY II synchrotron- and the E3 line -BER II neutron reactor- of the Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin.
The results reveal significant differences in the residual stress states for the different characterization techniques employed, which indicates a dependence of the residual state on the penetration depth in the sample. For the surface residual stresses, longitudinal and transverse stress components from both X-ray and synchrotron agree well and the obtained values were around the yield strength of the material. Furthermore, synchrotron mapping disclosed gradients along the width and length of the sample for the longitudinal and transverse stress components. On the other hand, lower residual stresses were found in the bulk of the material measured using neutron diffraction. The longitudinal component was tensile and decreased towards the boundary of the sample. In contrast, the normal component was nearly constant and compressive in nature. The transversal component was almost negligible. The results indicate that a stress re-distribution takes place during the deposition of the consecutive layers. Further investigations are planned to study the phenomenon in detail.
Additive Manufacturing (AM) through the Selective Laser Melting (SLM) route offers ample scope for producing geometrically complex parts compared to the conventional subtractive manufacturing strategies. Nevertheless, the residual stresses which develop during the fabrication can limit application of the SLM components by reducing the load bearing capacity and by inducing unwanted distortion, depending on the boundary conditions specified during manufacturing. The present study aims at characterizing the residual stress states in the SLM parts using different diffraction methods. The material used is the nickel based superalloy Inconel 718. Microstructure as well as the surface and bulk residual stresses were characterized.
For the residual stress analysis, X-ray, synchrotron and neutron diffraction methods were used. The measurements were performed at BAM, at the EDDI beamline of -BESSY II synchrotronand the E3 line -BER II neutron reactor- of the Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. The results reveal significant differences in the residual stress states for the different characterization techniques employed, which indicates the dependence of the residual state on the penetration depth in the sample. For the surface residual stresses, longitudinal and transverse stress components from X-ray and synchrotron agree well and the obtained values were around the yield strength of the material. Furthermore, synchrotron mapping disclosed gradients along the width and length of the sample for the longitudinal and transverse stress components. On the other hand, lower residual stresses were found in the bulk of the material measured using neutron diffraction. The longitudinal component was tensile and decreased towards the boundary of the sample. In contrast, the normal component was nearly constant and compressive in nature. The transversal component was almost negligible. The results indicate that a stress re-distribution takes place during the deposition of the consecutive layers. Further investigations are planned to study the phenomenon in detail.
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.
The project series CTSimU was initiated with the goal to develop a set of procedures to enable the determination of the task-specific measurement uncertainty of a CT system numerically by radiographic simulation. The first project (2019-2022) “Radiographic Computed Tomography Simulation for Measurement Uncertainty Evaluation - CTSimU” was focused on the sufficient physical correctness of the radiographic simulation and created as a result a test framework for simulation softwares and a draft of a VDI standard in the series VDI/VDE 2630 for this application. However, for the realistic simulation of a CT system in a simulation software (i.e. a digital twin), not only the correctness of the simulation software itself is crucial, but also the quality of the parameterization of the CT system in the simulation software - this represents the starting point of the 2nd project “Realistic Simulation of real CT systems with a basic-qualified Simulation Software - CTSimU2” (2022-2024).
The parameterization of a CT system in a simulation software can be divided into four steps: after the data acquisition at the real CT system (step 1) follows the evaluation of the acquired data for the generation of general parameter specifications (step 2). It follows the transfer of the parameters into the specific simulation software (step 3) and the validation of the resulting simulation parameters by a suitable test (step 4). The intended result of the project CTSimU2 is a draft VDI standard (for VDI/VDE 2630) for this test, which contains an informative annex on the state of the art regarding the possibilities for parameter determination.
Das Prozessmonitoring stellt einen wichtigen Baustein für eine Qualitätssicherung additiv gefertigter Bauteile dar, insbesondere bei kleinen Losgrößen. Der Vortrag zeigt einen Überblick aktueller Entwicklungen der BAM im Bereich des Prozessmonitorings für das Laserstrahlschmelzen (laser powder bed fusion) metallischer Werkstoffe. Durch Vergleich mit der Referenzmethode Computertomografie wird am Beispiel der thermografischen Verfahren gezeigt, wie relevante Defekte in Bauteilen detektiert werden können und Einsatzpotenziale sowie Limitierungen aufgezeigt.
The project ProMoAM is presented. The goal of the project is to evaluate which NDT techniques or combination of techniques is suited for in-situ quality assurance in additive manufacturing of metals. To this end, also 3d-data fusion and visualization techniques are applied. Additional ex-situ NDT-techniques are used as references for defect detection and quantification. Feasability studies for NDT-techniques that are presently not applicable for in-situ use are performed as well.
The presentation gives a brief overview of the whole project and the different involved NDT-techniques.
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.
Structural alloys are largely employed in key industrial sectors and their demand is predicted to rise rapidly for the next decades. Most of these materials require a large amount of energy for extraction and manufacturing, which causes the emission of greenhouse gases and other pollutants. Therefore, strategies for improving the sustainability of structural metallic alloys are urgently needed.
Additive Manufacturing (AM), in particular Laser Powder Bed Fusion (PBF-LB/M), aims to be a sustainable manufacturing process, as it allows the build-up of complex geometry in near net-shape from 3D models, while minimizing material waste and the energy required for the process and post-process treatments.
Nevertheless, the application of additively manufactured parts in structural safety-relevant applications is still hindered by the poor fatigue performance. The cause of this has been mainly attributed to the presence of manufacturing defects and surface roughness. Therefore, a huge effort has been made to optimize the process parameters and to introduce post-process treatments to minimize the defect content. However, material flaws cannot be fully eliminated, but these can be considered in a damage tolerance framework for the prediction of the fatigue performance of additively manufactured metallic materials, which is essential for part design and qualification.
This work aims at presenting different modelling strategies for the prediction of the fatigue limit of AM metals. Simple empirical models and more complex models based on fatigue short crack propagation are proposed. The investigated material is an AlSi10Mg alloy fabricated by PBF-LB/M and subjected to two different low-temperature heat-treatments (265°C for 1 h and 300°C for 2h). The results show that the models can provide good approximation of the fatigue limits and help in the interpretation of the scatter of fatigue data.
Laser powder bed fusion is one of the most promising additive manufacturing techniques for printing complex-shaped metal components. However, the formation of subsurface porosity poses a significant risk to the service lifetime of the printed parts. In-situ monitoring offers the possibility to detect porosity already during manufacturing. Thereby, process feedback control or a manual process interruption to cut financial losses is enabled.
Short-wave infrared thermography can monitor the thermal history of manufactured parts which is closely connected to the probability of porosity formation. Artificial intelligence methods are increasingly used for porosity prediction from the obtained large amounts of complex monitoring data. In this study, we aim to identify the potential and the challenges of deep-learning-assisted porosity prediction based on thermographic in-situ monitoring.
Therefore, the porosity prediction task is studied in detail using an exemplary dataset from the manufacturing of two Haynes282 cuboid components. Our trained 1D convolutional neural network model shows high performance (R2 score of 0.90) for the prediction of local porosity in discrete sub-volumes with dimensions of (700 x 700 x 40) μm³.
It could be demonstrated that the regressor correctly predicts layer-wise porosity changes but presumably has limited capability to predict differences in local porosity. Furthermore, there is a need to study the significance of the used thermogram feature inputs to streamline the model and to adjust the monitoring hardware. Moreover, we identified multiple sources of data uncertainty resulting from the in-situ monitoring setup, the registration with the ground truth X-ray-computed tomography data and the used pre-processing workflow that might influence the model’s performance detrimentally.
Due to the many possible applications, the uncomplicated production and the high application range, reinforced concrete is a widely used building material. This large range of physical material properties still poses an engineering challenge in determining all necessary requirements for predicting dynamic effects under impact load.
Many aspects of impact have already been examined and some correlations have been studied intensively. Examples are the work of Lastunen and Booker, who studied the influence of projectile properties on the impact form. Li has also investigated the local effects of an impact. The field of detailed damage analysis has not been in focus so far.
This presentation shows some studies in medium-velocity impact with the focus on post-impact damage evaluation. The impactor is modified so that the test plates show low penetration on the top and scabbing on the bottom. With the unique tomography lab test stand at BAM the plate is scanned after the impact and the damage is analyzed. Cracks and scabbing are made visible with a reconstruction. The comparison of simulation and tomography allows to create prognosis models for damage characterization.
3D images such as those produces by X-ray tomography can provide a wealth of information on the internal structure of materials, but quantification of specific geometrical or topological characteristics linked to some bulk physical property is far from being straightforward. This study focuses on methods to quantify the differences in physical properties as a function of direction, i.e. their anisotropy, and how it can be linked to measures of anisotropy of the internal structure of the material. The auto-correlation function gives a similarity measure in the volume as a function of distance and direction. This is a cross-correlation of the image with itself fast to compute and relatively insensitive to noise. It is why we focus on this method to compare with the physical property of our DPF material. Diesel Particulate Filter (DPF) materials are porous ceramics that; a) can be used at very high temperatures; b) have very good thermal shock resistance; c) are inert; d) can be manufactured with tailored porosity. Their usual way of production consists of the extrusion of a slurry into the desired filter shape, with successive ceramming at high temperature. This process causes anisotropy at both microscopic and macroscopic levels.
Since additive manufacturing processes typically introduce heterogeneous microstructures and residual stresses, the applicability of parts produced in an as-built state is limited. Therefore, often different post-processing treatments are necessary to obtain the desired stress state and properties.
For additively manufactured Inconel 718, the recently developed standard ASTM F3301 provides guidance for the heat treatment of powder bed fusion specimens. Although this standard is based on standards developed for wrought Inconel 718, it does not include the direct aging variant. In this study, we characterized the microstructure and tensile behavior of Inconel 718 specimens produced by a laser powder bed fusion process. The specimens were heat-treated according to two different routines after stress relieving: a full heat treatment cycle versus a one-step aging process. Differences in the resulting texture and grain morphology were observed. Although these differences prevail, the ex-situ tensile behavior was broadly similar. Minor differences were observed in yield strength and work hardening rate for the direct aged specimen. In order to understand this behavior, investigations with in-situ tensile testing during synchrotron energy-dispersive X-ray diffraction measurements revealed differences in the load partitioning among different crystal directions. This was attributed to microstructural differences between the heat treatment variants. Further analysis emphasized that the various strengthening mechanisms are present to a different extent depending on the heat-treatment cycle applied. In addition, the elastic anisotropy expressed by the differences in the diffraction elastic constants displayed a dependence on the microstructure. Importantly, a precise knowledge of such constants is indispensable to reliably determine residual stresses in parts.
Nominal-actual comparisons are routinely performed to compare a manufactured specimen to a reference specimen. X-ray Computed Tomography (CT) has brought a profound change in the way that tolerance verifications are performed in industry, by allowing the inner and outer geometries of an object to be measured, without the need for external access or destructive testing. As a results, CT is increasingly used in additive manufacturing applications, where a nominal-actual comparison performed between the digital model (CAD file), used as an input for the 3D printer, and the CT volume from the printed part, can provide invaluable information as to the accuracy of the printing process. However, the nominal-actual comparison process is somewhat different when applied to additively manufactured specimens by comparison to conventionally manufactured specimens.
Um die Gültigkeit der Vorhersagen des aktuellen Solid-State-Transformation-Creep (SSTC)-Modells zu verifizieren, wurde die Schadensakkumulation während eines Kriecheversuchs an einer Al-3,85Mg Legierung mittels Synchrotron Röntgenrefraktionstechnik untersucht. Das Röntgenrefraktionsverfahren erfasst die innere spezifische Oberfläche (d.h. Oberfläche pro Volumeneinheit) im durchstrahlten Volumen. Dabei liegt die Detektierbarkeit von Rissen und Poren in der Größenordnung von wenigen Nano- bis Mikrometern. Im Vergleich zu CT-Messungen mit vergleichbarer Sensitivität ist das untersuchte Probenvolumen jedoch um den Faktor 10 größer. Ein signifikanter Anstieg der inneren spezifischen Oberfläche mit zunehmender Kriechzeit wurde beobachtet, was den Nachweis für die Entstehung einer feinkörnigen Substruktur liefert, wie sie im SSTC-Modell vorhergesagt wird. Diese feinkörnige Substruktur wurde auch mittels Rasterelektronenmikroskopie beobachtet.
The overview of the activity of group 8.5 Micro-NDT (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The challenges in the residual stress analysis of AM components are discussed on the basis on the show studies performed in BAM. Also, the synchrotron X-ray refraction technique, available in BAM, is presented, showing example of in-situ heating test of Al10SiMg AM material.
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 presentation we discuss the online monitoring of metallic AM parts produced by the Laser Powder Bed Fusion (LPBF) process by using optical, thermographic and electromagnetic methods. In a first approach we present the detection of defects generated during the process and discuss how to improve these methods for the optimization of design and production of metallic AM parts.
Within polycrystalline porous ceramics used in automotive applications as diesel particulate filters, it is evidenced that during cooling from firing temperature micro cracks are gradually formed. The cracks are formed as a consequence of strong thermal anisotropy of grains. Typically these micro cracks are granting better thermal shock resistance, with respect to dense materials, but reduce stiffness. The reduction can be quantified by measuring the drop in elastic properties of bulk material which, depending on the level of porosity, can decrease even by 50% with respect to its value at high temperature. It is further observed that upon subsequent heating these cracks are closing and partially or totally healing at very high temperatures. Such peculiar behavior results in partial or complete recovery of the elastic properties of bulk material upon completing one thermal cycle. Despite its evident practical application, still there is no constitutive description of this phenomenon, capable of predicting the evolution of Young's modulus as a function of temperature history. For reliable numerical simulation of this phenomenon, it is required to model fracture. To model inter-crystalline fracture, an effective strategy is to use cohesive elements, since crack patterns are a priori known. Major limitation of this approach is that the cohesive elements already implemented within commercial codes cannot take into account crack healing upon subsequent heating. In this study new cohesive element is developed and numerically implemented within ABAQUS commercial finite element code, capable to model crack opening, closing and healing. Further on, a computer code is generated to build numerical model of porous ceramic specimens that takes into account experimentally measured crystallographic orientation and porosity, and models the microstructure by using Voronoi polygons. The developed numerical tools serve as a framework for more realistic simulations, required to study the hysteresis in elastic properties within porous ceramics provoked by thermal cyclic. In a subsequent phase, an inverse analysis procedure is developed, in which macroscopic properties are used to calibrate parameters entering into micro crack model. The approach is centered on a minimization of a discrepancy function designed to quantify the difference between experimentally measured quantities and their computed counterpart. The model is calibrated on the basis of experimental data regarding the drop of bulk Young's modulus with decrease of temperature. Developed procedure is tested with porous cordierite sample, and obtained results are quit promising despite the current limitation of using only two-dimensional model.
The global demand for concrete is growing, and with it, its carbon footprint. Current literature proposes biochar, a product of pyrolysis, as a possible car-bon sink to reduce the carbon footprint of concrete. This work investigates the microstructure of Portland cement pastes with 0%, 5%, and 25% of the cement replaced with wood biochar, since this should influence its macro-scopic mechanical properties. MIP, gas sorption, NMR, and µ-CT were used to analyze the pore space of the three materials. The combination of these methods, each with different resolution, enables a multi-scale investigation of biochar impact on the microstructure of cement pastes. NMR confirmed that biochar can absorb moisture and, thus, reduces the effective water-to-cement ratio. MIP and gas sorption results show 0% and 5% volume re-placement have similar gel pore structure. The results from µ-CT investiga-tions suggest that biochar may reduce the formation of larger pores. The in-clusion of non-reactive porous particles such as biochar increase the porosity of the material and should act as a weakness in terms of mechanical proper-ties. Overall, this study highlights the need to carefully tailor replacement rates to control the impact of biochar on the microstructure concrete mixtures and sees a strong need for further studies on mechanical properties.
X-ray refraction is an excellent tool for the characterization of the microstructure of materials. However, there are only a few (synchrotron) laboratories in the world that use this technique for material characterisation. Therefore, the seminar will first explain the basic principles of X-ray refraction and the measurement techniques installed at the hard X-ray beamline BAMline at BESSY II (Berlin, Germany). This is followed by examples of investigations on fibre-reinforced plastic composites (CFRP) as well as ceramic (Cordierite, ZrO2-SiO2) and metallic materials (Ti-6Al-4V, Inconel). Some of the investigations were carried out both ex-situ and in-situ under mechanical and thermal load. The results are correlated with the mechanical properties of the materials.
X-ray imaging techniques have an enormous potential to understand the microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this lecture we report the use of a powerful, yet not so wide-spread, set of X-ray techniques based on refraction effects. X-ray refraction allows determining the internal specific surface of materials (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with a nanometric detectability. We demonstrate showcases of ceramics and composite materials, where microstructural parameters could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography. We present in situ analysis of the damage evolution during tensile load and the identification of void formation in parts produced by selective laser melting.
Microstructure characterisation of advanced materials via 2D and 3D X-ray refraction techniques
(2018)
3D imaging techniques have an enormous potential to understand the microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this conference paper we report the use of a powerful, yet not so wide-spread, set of X-ray techniques based on refraction effects. X-ray refraction allows determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with a nanometric detectability. We demonstrate showcases of ceramics and composite materials, where microstructural parameters could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography. We present in situ analysis of the damage evolution in an Al/Al2O3 metal matrix composite during tensile load and the identification of void formation (different kinds of defects, particularly unsintered powder hidden in pores, and small inhomogeneity’s like cracks) in Ti64 parts produced by selective laser melting using synchrotron X-ray refraction radiography and tomography.
Inconel 718 (IN718) is a traditional age-hardenable nickel-based alloy that has been increasingly processed by additive manufacturing (AM) in recent years. In the as-solidified condition, IN718 exhibits chemical segregation and the undesired Laves phase, requiring a solution annealing (SA) prior to aging. The material produced by AM does not respond to the established thermal routines in the same way as conventionally produced IN718, and there is still no consensus on which routine yields optimal results. This work aims to provide a fundamental understanding of the heat treatment (HT) response by continuously monitoring the microstructural evolution during SA via time-resolved synchrotron x-ray diffraction, complemented by ex-situ scanning electron microscopy (SEM). The samples were produced by laser powder bed fusion to a geometry of 10x20x90 mm³, from which Ø1x5 mm³ cylindric specimens were extracted. Two different scanning strategies – incremental 67° rotations, Rot, and alternating 0°/67° tracks, Alt – were used, leading to two different as-built conditions. 1-hour SAs were carried out in the beamline ID22 of the ESRF at 50 KeV. Two SA temperatures, SA1 = 1020 °C, and SA2 = 1080 °C were tested for each scanning strategy. Data were processed using the software PDIndexer. In the as-built state, all samples showed typical subgrain columnar cell structures with predominant Nb/Mo segregation and Laves phase at the cell walls, as seen by SEM. The Alt scan induced higher intensity on the Laves peaks than the Rot scan, suggesting a greater content of Laves. Chemical homogenization in the SA was largely achieved during the heating ramp (Fig. 1). SA2 eliminated the Laves peaks just before reaching 1080 °C, and mitigated differences between Rot and Alt samples. On the other hand, SA1 induced the precipitation of the generally detrimental δ phase, also observed by SEM. Furthermore, the Rot scan showed higher δ peak intensities than the Alt scan, indicating a higher content of δ in the latter. No signs of recrystallization were observed in any of the investigated SAs.
An overview of the main Non-Destructive activities conducted at BAM for the microstructural characterization of Additive Manufacturing (AM) materials will be presented. Focus is made on the study of the influence of Selective Laser Melted (SLM) scan strategies on the defect population of a Ti-6Al-4V alloy using the Analyzer Based Imaging (ABI) technique available at the BAMline (BESSY II synchrotron facility). ABI technique takes advantage of X Ray refraction at interfaces to enable the determination of porosity features (orientation, homogeneity, etc.) within large volumes, otherwise not possible to image by means X ray micro Computed Tomography.
Additionally, for a SLM IN718 material, Energy Dispersive X Ray Diffraction (subsurface measurements at 100 µm depth) and neutrons diffraction (internal measurements at 3 mm depth) are combined with distortion measurements to produce a 3D description of the Residual Stress distribution throughout the entire sample.
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.
Untersuchungen haben gezeigt, dass sich ältere Schafe gut als Modell für die mi-nimalinvasive Behandlung von Osteoporose eignen [1]. Um einen Behandlungs-effekt nachzuweisen, wird dabei unter anderem die Belastungsfähigkeit des Kno-chens durch Druckversuche an kleinen Zylindern aus den behandelten und unbe-handelten Knochen bestimmt. Diese hatten hier einen Durchmesser von 10 mm und eine Höhe von 13 mm. Für den in-situ Druckversuch wurde eine Deben CT5000 verwendet. In einer Serie von Druckerhöhungen wurden die Proben je-weils tomographiert. Dabei ergab sich zunächst, dass mit der µCT innerhalb der Knochen im oberen und unteren Bereich schon Brüche nachgewiesen werden können, obwohl die gemessene Kraftaufnahmekurve keine Unstetigkeit zeigt. Deswegen wurden die starren Probenaufnehmer der Deben Anordnung durch bewegliche Aufnehmer ergänzt, die eine leichte Verkippung der belasteten Ober-flächen ausgleichen können. Ein Vergleich der gemessenen und der aus den µCT-Daten berechneten Verschiebungsfelder ergab trotz der komplexen Struktur der Knochen gute Übereinstimmungen. Diese Verschiebungen wurden dann mit den aus den µCT Daten simulierten mechanischen Druckversuchen, Von-Mise-Spannungen und daraus berechneten Verschiebungen verglichen. (VGStudioMax Simulation).
Seit der Antike gehört die Medea-Sage zu den bekanntesten Geschichten der Weltliteratur. Der berühmte französische Künstler Carle Van Loo hat sich dieses Epos um 1759 angenommen und ein beeindruckendes Ölgemälde mit Abmessungen von 2,30x3,28m² erschaffen. Mit Mademoiselle Clairon als Medea und Henri Louis Le Kain als Jason ist ein Kunstwerk entstanden, das seitdem einige Veränderungen und Restaurierungen erfahren hat.
Die Bundesanstalt für Materialforschung und -prüfung (BAM) hatte 2020 die Möglichkeit, dieses und ein zweites Kunstwerk, im Neuen Palais in Potsdam, für die Stiftung Preußische Schlösser und Gärten Berlin-Brandenburg, radiografisch zu untersuchen. Hierbei wurden sowohl technologisch als auch kunsthistorisch einige interessante Entdeckungen gemacht, die im vorliegenden Beitrag vorgestellt werden.
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.
Die herkömmliche Bildgebung mit Röntgenstrahlung beruht auf unterschiedlicher Absorption durch verschiedene Materialien im Volumen eines Körpers. Es entsteht ein "Massebild". Die hier vorgestellten Verfahren benutzen die Brechung und Beugung von Röntgenstrahlen, um innere Oberflächen oder die Molekulartextur von Materialien und Bauteilen abzubilden. Im Vortrag werden die entsprechenden Messtechniken an der BAM im Labormaßstab sowie an Großforschungseinrichtungen vorgestellt und anhand einiger Anwendungsbeispiele die zusätzlichen Informationen zur herkömmlichen Durchstrahlung diskutiert.
The material and damage behaviour of additively manufactured polyamide 12 (PA12) under dynamic loading was characterized by cyclic tests and microstructure analysis. The results were used to develop a numerical material and damage model. In a recent study, it was shown that the material and damage behaviour of 3D printed PA12 under quasistatic loading is simulated in a realistic way by coupling the
material model by Chaboche and the damage model by Gurson-Tvergaard-Needleman (GTN).
Using microscopy, X-ray refraction, and computed tomography, a porosity of about 5% was evaluated. These results served as a starting point for the present work. For the dynamic load, both the previously used Chaboche model and the GTN model were extended. Furthermore, the temperature was measured during the experiment and the self-heating effect was observed. Therefore, a temperaturedependent material parameters for the simulation were introduced. Considering the results of mechanical experiments, microstructural investigations, and self-heating effects, a good agreement between Experiment and numerical simulation could be achieved.
Metal Additive Manufacturing (AM) technologies such as Laser Powder Bed Fusion (LPBF) are characterized by layer wise construction, which enable advancements of component design, with associated potential gains in performance and efficiency. However, high magnitude residual stresses (RS) are often a product of the rapid thermal cycles typical of the layerwise process. Therefore, a deep understanding of the formation of RS, the influence of process parameters on their magnitude and the impact on mechanical performance is crucial for widespread application. The experimental characterisation of these RS is essential for safety related engineering application and supports the development of reliable numerical models. Diffraction-based methods for RS analysis using neutrons and high energy X-rays enable non-destructive spatially resolved characterisation of both surface and bulk residual stresses in complex components. This presentation will provide an overview of recent research by the BAM at large scale facilities for the characterization of residual stresses in LPBF metallic alloys as a function of process parameters. In addition, the challenges posed by the textured and hierarchical microstructures of LPBF materials on diffraction-based RS analysis in AM materials will be discussed. This will include the question of the d0 reference lattice spacing and the appropriate choice of the diffraction elastic constants (DECs) to calculate the level of RS in LPBF manufactured alloys.
Laser powder-based directed energy deposition (DED-L) is a technology that offers the possibility for 3D material deposition over hundreds of layers and has thus the potential for application in additive manufacturing (AM). However, to achieve broad industrial application as AM technology, more data and knowledge about the fabricated materials regarding the achieved properties and their relationship to the manufacturing process and the resulting microstructure is still needed. In this work, we present data regarding the low-cycle fatigue (LCF) behavior of Ti-6Al-4V. The material was fabricated using an optimized DED-L process. It features a low defect population and excellent tensile properties. To assess its LCF behavior two conventionally manufactured variants of the same alloy featuring different microstructures were additionally tested. The strain-controlled LCF tests were carried out in fully reversed mode with 0.3 % to 1.0 % axial strain amplitude from room temperature up to 400°C. The LCF behavior and failure mechanisms are described. For characterization, optical microscopy (OM), scanning electron microscopy (SEM), and micro-computed tomography (µCT) were used. The low defect population allows for a better understanding of the intrinsic material’s properties and enables a fairer comparison against the conventional variants. The fatigue lifetimes of the DED-L material are nearly independent of the test temperature. At elevated test temperatures, they are similar or higher than the lifetimes of the conventional counterparts. At room temperature, they are only surpassed by the lifetimes of one of them. The principal failure mechanism involves multiple crack initiation sites.
Despite of the significant advances in AM process optimization there is still a lack of experimental results and understanding regarding the mechanical behavior and microstructural evolution of AMparts, especially in loading conditions typical for safety-relevant applications e.g. in the aerospace or power engineering. Within the scope of the presented investigations, a characterization of the fatigue behavior of additively manufactured Ti-6Al-4V in the low cycle fatigue regime was carried out in the range of 0.3 to 1.0 % strain amplitude at room temperature, 250°C and 400°C. The Ti-6Al-4V specimens are machined out of lean cylindrical rods, which were fabricated using powder laser metal deposition (LMD) with an improved build-up strategy. The improved strategy incorporates variable track overlap ratios to achieve a constant growth in the shell and core area. The low-cycle-fatigue behavior is described based on cyclic deformation curves and strain-based fatigue life curves. The lifetimes are fitted based on the Manson-Coffin-Basquin relationship. A characterization of the microstructure and the Lack-of-Fusion (LoF)-defect-structure in the as-built state is performed using optical light microscopy and high-resolution computed tomography (CT) respectively. The failure mechanism under loading is described in terms of LoF-defects-evolution and crack growth mechanism based on an interrupted LCF test with selected test parameters. After failure, scanning electron microscopy, digital and optical light microscopy and CT are used to describe the failure mechanisms both in the longitudinal direction and in the cross section of the specimens. The fatigue lives obtained are comparable with results from previous related studies and are shorter than those of traditionally manufactured (wrought) Ti-6Al-4V. In this study new experimental data and understanding of the mechanical behavior under application-relevant loading conditions (high temperature, cyclic plasticity) is gained. Furthermore, a better understanding of the role of LoFdefects and AM-typical microstructural features on the failure mechanism of LMD Ti-6Al-4V is achieved.
Aluminum alloys are extensively used in the automotive industry. Particularly, squeeze casting production of Al-Si alloys is employed in the conception of metal matrix composites (MMC) for combustion engines. Such materials are of a high interest since they allow combining improved mechanical properties and reduced weight and hence improve efficiency. We investigate two types of MMCs, which can be potentially used for production of combustion engine pistons: 1) a near-eutectic cast AlSi12CuMgNi alloy reinforced with 15%vol. Al2O3 random planar oriented short fibers and 2) the same alloy reinforced with 7%vol. Al2O3 random planar oriented short fibers + 15%vol. SiC particles.
Complex 3D microstructure of the samples in as-cast condition, consisting of four and five phases (Al matrix, eutectic Si, intermetallics, Al2O3 fibers and SiC particles) was investigated by synchrotron computed tomography (CT). Advanced methods based on machine learning were applied for segmentation of all phases. This allowed extracting quantitative information such as volume fraction, shape and interconnectivity of every phase.
In-situ compression tests during neutron diffraction experiments were used to track the load transfer among phases, while CT on pre-strained samples to monitor and quantify damage. A micromechanical model was developed to simulate the evolution of the internal stress of each phase during uniaxial compression. We showed that in composites with the Al2O3 fiber mat plane perpendicular to the load axis the Al-alloy matrix presents a large hydrostatic stress component, i.e. undergoes compression also in the direction transverse to the external load. This feature holds with and without the addition of SiC ceramic reinforcement and is absent in the case when the Al2O3 fiber mat plane is parallel to the load axis. We show, that the intermetallics play a decisive role at very high loads, when all other reinforcement phases suffer (extensive) damage. The addition of SiC particles does alleviate the load on the Al2O3 fibers, on the eutectic Si, and on the intermetallic phases in both cases of parallel and orthogonal (to the load axis) Al2O3 fiber orientation. Apart from the beneficial addition of ceramic reinforcement, the presence of intermetallic phase and eutectic silicon, forming an interconnected network even at high loads, when single particles break, confers peculiar properties to these multi-phase composites.
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).
Eine kritische Aufgabe im Rahmen der Etablierung von Prozess-Struktur-Eigenschafts-Performance-Beziehungen bei der additiven Fertigung (AM) von Metallen ist die Ermittlung von zuverlässigen und gut dokumentierten Kennwerten zum Materialverhalten sowie das Schaffen von Wissen über die Struktur-Eigenschafts-Korrelation. Schließlich ist dies die Grundlage für die Entwicklung gezielterer Prozessoptimierungen und zuverlässigerer Lebensdauer-Vorhersagen. In diesem Zusammenhang zielt dieser Beitrag darauf ab, Daten und Erkenntnisse über das Kriechverhalten des austenitischen Edelstahls 316L zu liefern, der mittels Laser-Powder-Bed-Fusion (L-PBF) hergestellt wird. Um dieses Ziel zu erreichen, wurden Proben aus konventionellem warmgewalztem sowie AM-Material gemäß den bestehenden Normen für konventionelles Material geprüft und vor und nach dem Versagen mikrostrukturell charakterisiert. Die Probekörper wurden aus einzelnen Blöcken des AM-Materials gefertigt. Die Blöcke wurden mit einer Standard-Scan- und Aufbaustrategie hergestellt und anschließend wärmebehandelt. Das Kriechverhalten wird anhand der Kriechlebensdauer und ausgewählter Kriechkurven und Kennwerte beschrieben und vergleichend bewertet. Der Einfluss von Defekten und Mikrostruktur auf das Materialverhalten wird anhand von zerstörenden und zerstörungsfreien Auswertungen an ausgewählten Proben analysiert. Der AM-Werkstoff zeigt kürzere Kriechlebensdauern, erreicht das sekundäre Kriechstadium deutlich schneller und bei geringerer Dehnung und weist eine geringere Kriechduktilität im Vergleich zu seinem konventionellen Gegenstück auf. Das Kriechschädigungsverhalten des AM-Werkstoffs ist eher mikrostruktur- als defektgesteuert und ist durch die Bildung intergranularer Kriechrisse gekennzeichnet. Als kritische Merkmale werden die Versetzungsdichte sowie die Versprödung der Korngrenzen identifiziert. Die Mikro-Computertomographie (µCT) erweist sich als Alternative zur Metallographie, um die Kriechschädigung zu analysieren.
Laser powder bed fusion is used to create near net shape metal parts with a high degree of freedom in geometry design. When it comes to the production of safety critical components, a strict quality assurance is mandatory. An alternative to cost-intensive non-destructive testing of the produced parts is the utilization of in-situ process monitoring techniques. The formation of defects is linked to deviations of the local thermal history of the part from standard conditions. Therefore, one of the most promising monitoring techniques in additive manufacturing is thermography. In this study, features extracted from thermographic data are utilized to investigate the thermal history of cylindrical metal parts. The influence of process parameters, part geometry and scan strategy on the local heat distribution and on the resulting part porosity are presented. The suitability of the extracted features for in-situ process monitoring is discussed.
Laser Powder Bed Fusion (L-PBF) allow the fabrication of lightweight near net shape AlSi10Mg components attractive to the aerospace, automotive, biomedical and military industries. During the build-up process, high cooling rates occur. Thus, L-PBF AlSi10Mg alloys exhibit a Si-nanostructure in the as-built condition, which leads to superior mechanical properties compared to conventional cast materials. At the same time, such high thermal gradients generally involve a deleterious residual stress (RS) state that needs to be assessed during the design process, before placing a component in service. To this purpose post-process heat treatments are commonly performed to relieve detrimental RS. In this contribution two low-temperature stress-relief heat treatments (SRHT) are studied and compared with the as-built state: a SRHT at 265°C for 1 hour and a SRHT at 300°C for 2 hours. At these temperatures microstructural changes occur. In the as-built state, Si atoms are supersaturated in the α-aluminium matrix, which is enveloped by a eutectic Si-network. At 265°C the Si precipitation from the matrix to the pre-existing network is triggered. Thereafter, above 295°C the fragmentation and spheroidization of the Si branches takes place, presumably by Al–Si interdiffusion. After 2 hours the original eutectic network is completely replaced by uniformly distributed blocky particles. The effect of the heat and the microstructure modification on the RS state and the fatigue properties is investigated. Energy dispersive x-ray and neutron diffraction are combined to investigate the near-surface and bulk RS state of a L-PBF AlSi10Mg material. Differences in the endurance limit are evaluated experimentally by high cycle fatigue (HCF) tests and cyclic R-curve determination.
Introduction to AGIL
(2021)
For metal-based additive manufacturing (AM) to achieve leaner designs and enable longer life predictions, it is imperative to gain a detailed knowledge of the residual stress (RS) built-up. Laser powder bed fusion (LPBF) is an AM technique particularly prone to RS because of the highly localized heat source, extremely high cooling rates (in the order of 103-107 K/s), and successive cooling and heating cycles of the solidified material. Furthermore, RS analysis of LPBF materials by diffraction methods is peculiar because of the complexity of the thermal history, the possibility of encountering high levels of surface roughness, spatial textural variations and/or changes in solute concentrations at the component scale.
Diverse aspects of the influence of scanning strategies on the as-built residual stress state of a LPBF IN718 alloy will be presented, with particular focus on the challenges that AM microstructures pose for a reliable RS determination.