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In this presentation, the results of the determination of the diffraction and single-crystal elastic constants of laser powder bed fused Inconel 718 are presented. The analysis is based on high-energy synchrotron diffraction experiments performed at the Deutsches Elektronen-Synchrotron. It is shown that the characteristic microstructure of laser powder bed fused Inconel 718 impacts the elastic anisotropy and therefore the diffraction and single-crystal elastic constants. Finally, the consequences on the diffraction-based residual stress determination of laser powder bed fused Inconel 718 are discussed.
The overview of the activity of Federal Institute for Material Research and Testing (BAM, Belin, Germany) in the field material characterization by X-ray imaging is presented. The principle of X-ray Computed Tomography (XCT) is explained. The multiple examples of application of quantitative analysis by XCT are reported, such as additive manufacturing, Li-ion battery, concrete research.
Die Erzeugung rissschließfreier Anrisse in gekerbten bruchmechanischen Proben für anschließende Ermüdungsversuche kann durch eine zyklische Druckbelastung an der Kerbe erfolgen: Bei der Erstbelastung wird eine plastische Verformung an der Kerbspitze erzeugt, welche Zugeigenspannungen und damit eine risstreibende Kraft bei der folgenden zyklischen Druckbelastung hervorruft. Durch das Risswachstum kommt es zu einer Entspannung, bis der Riss schließlich arretiert, weil die effektive risstreibende Kraft auf den Schwellenwert abgesunken ist. Um Kurzrisswachstum in additiv, mittels pulverbettbasiertem Laserstrahlschmelzen (Laser Powder Bed Fusion - LPBF) gefertigtem AISI 316L Stahl und seinem konventionell erzeugten, warmgewalzten Pendant zu untersuchen, wurde dieses Verfahren im Rahmen der vorliegenden Arbeit genutzt. Im Falle des additiv gefertigten Materials kam es zu unerwartet langem Ermüdungsrisswachstum, bevor der Riss arretierte. Zur Ermittlung der Ursache erfolgte eine Messung der Eigenspannungsverteilungen mittels Neutronendiffraktion in der Kerbebene der additiv gefertigten Proben. Anschließend wurde ein Finite-Elemente-Modell zur Simulation des Ermüdungsrisswachstums in konventionellem und additiv gefertigtem Material implementiert. Im Rahmen dieses Vortrages wird insbesondere auf das Vorgehen bei der Simulation und auf die getroffenen Annahmen und Vereinfachungen eingegangen. Die Resultate werden mit den experimentellen Ergebnissen verglichen und das für die Simulation von Risswachstum genutzte Knoten-Freigabe-Verfahren (Node-Release), das Einbringen von Eigenspannungen als initiale Spannungen in der Simulation, und die Rechengrößen zur Quantifizierung der risstreibenden Kraft kritisch diskutiert.
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.
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.
The European Commission has identified Advanced Manufacturing and Advanced Materials as two of six Key Enabling Technologies (KETs). It is considered that Metrology is a key enabler for the advancement of these KETs. Consequently, EURAMET, the association of metrology institutes in Europe, has strengthened the role of Metrology for these KETs by enabling the creation of a European Metrology Network (EMN) for Advanced Manufacturing. The EMN is comprised of National Metrology Institutes (NMIs) and Designated Institutes (DIs) from across Europe and was formally established in October 2021. The aim of the EMN is to provide a high-level coordination of European metrology activities for the Advanced Manufacturing community.
The EMN itself is organized in three sections representing the major stages of the manufacturing chain: 1) Advanced Materials, 2) Smart Manufacturing Systems, and 3) Manufactured Components & Products. The EMN for Advanced Manufacturing is engaging with stakeholders in the field of Advanced Manufacturing (large companies & SMEs, industry organisations, existing networks, and academia), as well as the wider Metrology community, including Technical Committees, to provide input for the Strategic Research Agenda (SRA) on Metrology for Advanced Manufacturing.
This contribution will give an overview about the first version of the SRA prepared by the EMN for Advanced Manufacturing.
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.
The overview of the activity of Federal Institute for Material Research and Testing (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The research of our group is focused on the 3D imaging of AM materials by means of X-ray Computed Tomography at the lab and at synchrotron, and the residual stress characterization by diffraction (nondestructive technique). Also, two successful research project in collaboration with CAM2, Sweden are presented.
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.
Hot Isostatic Pressing (HIP) is often introduced to tackle the porosity issue in additively manufactured (AM) materials. For instance, HIP post-processing is recommended to improve fatigue resistance of Laser powder bed fusion (PBF-LB) manufactured parts [1, 2]. Even though HIP cannot completely remove porosity, it significantly decreases the defect population and its average size below the critical threshold value leading to early crack initiation.
In the present study, in-situ investigation of HIP procedure of PBF-LB Ti-6Al-4V parts was carried out to gain further insights into the densification mechanism occurring during HIP. The in-situ observations at high pressure and high temperature are uniquely possible at the PSICHE beamline of the Soleil synchrotron (France), thanks to the Ultrafast Tomography on a Paris-Edinburgh Cell (UToPEC) and the combination of the fast phase-contrast tomography and energy-dispersive diffraction [3, 4]. A detailed methodology was developed to ensure that the correct pressure and temperature were maintained during the experiments.
The results allowed an estimation of the global dentification rate during HIP of PBF-LB Ti-Al-4V material, as well as a detailed quantitative characterization of the influence of pore size and shape on the densification process, thereby understanding the effectiveness of HIP process on different pore categories. After 20 mins, 75% of porosity can be considered as closed or has size below the resolution of the XCT reconstruction. We also observed that the smallest defects showed higher densification rate, while the defect shape did not have significant effect on such rate. The current development of in-situ HIP experiment allows experimental quantification and validation of the simulation work. Ultimately it paves the road to tailoring the HIP procedure for different materials depending on the porosity and microstructure.
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.
The damage mechanisms of metallic components produced by process laser powder bed fusion differ significantly from those typically observed in conventionally manufactured variants of the same alloy. This is due to the unique microstructures of additively manufactured materials. Herein, the focus is on the study of the evolution of creep damage in stainless steel 316L specimens produced by laser powder bed fusion. X-ray computed tomography is used to unravel the influence of the process-specific microstructure from the influence of the initial void distribution on creep damage mechanisms. The void distribution of two specimens tested at 600 °C and 650 °C is analyzed before a creep test, after an interruption, and after fracture. The results indicate that the formation of damage is not connected to the initial void distribution. Instead, damage accumulation at grain boundaries resulting from intergranular cracking is observed.
The focus of the presentation focus will be on 3D imaging by means of X-ray Computed Tomography (XCT) at the lab and at synchrotron, and the non-destructive residual stress (RS) characterization by diffraction of additively manufactured (AM) materials in BAM (Berlin, Germany). The manufacturing defects and high RS are inherent of AM techniques and affect structural integrity of the components. Using XCT the defects size and shape distribution as well as geometrical deviations can be characterized, allowing the further optimization of the manufacturing process. Diffraction-based RS analysis methods using neutron and synchrotron X-rays at large scale facilities offer the possibility to non-destructively spatially resolve both surface and bulk RS in complex components and track their changes following applied thermal or mechanical loads.
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.
Metal Additive Manufacturing (AM) technologies such as Laser Powder Bed Fusion (LPBF) are characterized by layer wise construction, which enable advancements of component design, leading to potential efficiency and performance improvements. However, the rapid cooling rates associated with the process consequently leads to the generation of high magnitude residual stresses (RS). 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 characterization of these RS is essential for safety related engineering application and supporting the development of reliable numerical models. Diffraction-based methods for RS analysis using high energy synchrotron X-rays and neutrons enable non-destructive spatially resolved characterization of both surface and bulk residual stresses in complex components. This presentation will provide an overview of recent research conducted by the BAM at large scale facilities for the characterization of residual stresses in LPBF metallic alloys. Special focus will be given to the challenges posed by textured LPBF materials for the reliable choice of the diffraction elastic constants (DECs), which is crucial to the accurate calculation of the level of RS.
The high cooling rates (~106 K/s) occurring during Laser Powder Bed Fusion (PBF-LB/M) of AlSi10Mg induce to the formation of a fine nanometric silicon network in the as-built condition. Such unprecedented microstructure enhances the mechanical strength when compared to equivalent as-cast materials. Nevertheless, PBF-LB/M also leads to high magnitude residual stress (RS) due to the extreme localized temperature gradients. The presence of RS can be detrimental to the fatigue life of engineering components, and great efforts are focused on understanding their generation and evolution after post-process heat treatments. Typically, T6 heat treatments are used to mitigate RS and improve mechanical performances by Mg2Si precipitation during ageing at 160-180°C. Nevertheless, the solutionizing at 500-540°C vanishes the fine silicon network, leading to the formation of micrometric (average of ~2-5 µm) polygonal Si particles, similar to those observed in T6 heat-treated Al-Si cast materials. Therefore, the aim of this work is to evaluate the ability of two so-called low temperature heat treatments (i.e., at 265°C and 300°C) to mitigate RS while retaining the fine as-built microstructure inherent to PBF-LB/M AlSi10Mg. The fatigue behavior of the as-built material is subsequently compared to the two low temperature conditions.
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.
In this study, we present an enhanced deep learning framework for the prediction of porosity based on thermographic in-situ monitoring data of laser powder bed fusion processes. The manufacturing of two cuboid specimens from Haynes 282 (Ni-based alloy) powder was monitored by a short-wave infrared camera. We use thermogram feature data and x-ray computed tomography data to train a convolutional neural network classifier. The classifier is used to perform a multi-class prediction of the spatially resolved porosity level in small sub-volumes of the specimen bulk.
The overview of the activity of Federal Institute for Material Research and Testing (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The research of our group is focused on the 3D imaging of AM materials by means of X-ray Computed Tomography at the lab and at synchrotron, and the residual stress characterization by diffraction (nondestructive technique).
Laser powder bed fusion (PBF-LB/M) of metallic alloys is a layer wise additive manufacturing process which provides significant scope for more efficient designs of components, benefiting performance and weight, leading to efficiency improvements for various sectors of industry. However, to benefit from these design freedoms, knowledge of the high produced induced residual stress and mechanical property anisotropy associated with the unique microstructures is critical. X-ray and neutron diffraction are considered the benchmark for non-destructive characterization of surface and bulk internal residual stress. The latter, characterized by the high penetration power in most engineering alloys, allows for the use of diffraction angle close to 90° enabling a near cubic sampling volume to be specified. However, the complex microstructures of columnar growth with inherent crystallographic texture typically produced during PBF-LB/M of metallics present significant challenges to the assumptions typically required for time efficient determination of residual stress. These challenges include the selection of an appropriate set of diffraction elastic constants and a representative strain-free reference for the material of interest. In this presentation advancements in the field of diffraction-based residual stress analysis of L-PBF Inconel 718 will be presented. The choice of an appropriate set of diffraction-elastic constants depending on the underlying microstructure will be described.
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.
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.
The appearance of irregularities such as keyhole porosity is a major challenge for the production of metal parts by laser powder bed fusion (PBF-LB/M). The utilization of thermographic in-situ monitoring is a promising approach to extract the thermal history which is closely related to the formation of irregularities. In this study, we investigate the utilization of convolutional neural networks to predict keyhole porosity based on thermographic features. Here, the porosity information calculated from an x-ray micro computed tomography scan is used as reference. Feature engineering is performed to enable the model to learn the complex physical characteristics of the porosity formation. The model is examined with regard to the choice of hyperparameters, the significance of thermal features and characteristics of the data acquisition. Based on the results, future demands on irregularity prediction in PBF-LB/M are derived.
Additively manufactured (AM) triply periodic metallic minimum surface structures (TPMSS, from the English Triply Periodic Minimum Surface Structures) fulfill several requirements in both biomedical and engineering fields: tunable mechanical properties, low sensitivity to manufacturing defects, mechanical stability, and high energy absorption. However, they also present some quality control challenges that may prevent their successful application. In fact, optimization of the AM process is impossible without considering structural features such as manufacturing accuracy, internal defects, and surface topography and roughness. In this study, quantitative nondestructive analysis of Ti-6Al-4V alloy TPMSS was performed using X-ray computed tomography (XCT). Several new image analysis workflows are presented to evaluate the effects of buildup direction on wall thickness distribution, wall degradation, and surface roughness reduction due to chemical etching of TPMSS. It is shown that the fabrication accuracy is different for the structural elements printed parallel and orthogonal to the fabricated layers. Different strategies for chemical etching showed different powder removal capabilities and thus a gradient in wall thickness. This affected the mechanical performance under compression by reducing the yield stress. A positive effect of chemical etching is the reduction of surface roughness, which can potentially improve the fatigue properties of the components. Finally, XCT was used to correlate the amount of powder retained with the pore size of the TPMSS, which can further improve the manufacturing process.
A paradigm shift in the description of creep in metals can only occur through multi-scale imaging
(2022)
The description of creep in metals has reached a high level of complexity; fine details are revealed by all sorts of characterization techniques and different theoretical models. However, to date virtually no fully microstructure-driven quantitative description of the phenomenon is available. This has brought to interesting inconsistencies; the classic description of (secondary) creep rests on the so-called power law, which however: a- has a pre-factor spanning over 10 orders of magnitude; b- has different reported exponents for the same material; c- has no explanation for the values of such exponents.
Recently, a novel description (the so-called Solid State Transformation Creep (SSTC) Model) has been proposed to tackle the problem under a different light. The model has two remarkable features: 1- it describes creep as the accumulation of elementary strains due to dislocation motion; 2- it predicates that creep is proceeding by the evolution of a fractal arrangement of dislocations. Such description, however, needs a great deal of corroborating evidence, and indeed, is still incomplete.
To date, we have been able to observe and somehow quantify the fractal arrangement of microstructures through Transmission Electron Microscopy (TEM), observe the accumulation of dislocations at grain boundaries by EBSD-KAM (Electron Back-Scattered Diffraction-Kernel Angular Misorientation) analysis, quantify the kinetic character (solid state transformation) of experimental creep curves, and estimate the sub-grain size of the fractal microstructure through X-ray refraction techniques. All pieces of the mosaic seem to yield a consistent picture: we seem being on the right path to reconstruct the whole elephant by probing single parts of it. What is still missing is the bond between the various scales of investigation.
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.
Entwicklung der Mikrostruktur der mechanischen Eigenschaften und der Eigenspannungen in L-PBF 316L
(2022)
Die additive Fertigung (AM) metallischer Werkstoffe mittels Laser Powder Bed Fusion (L-PBF) ermöglicht einzigartige hierarchische Mikrostrukturen, die zu Verbesserungen bestimmter mechanischer Eigenschaften gegenüber konventionell hergestellten Varianten derselben Legierung führen können. Allerdings ist das L-PBF-Verfahren häufig durch das Vorhandensein hoher Eigenspannungen gekennzeichnet, die es zu verstehen und zu mindern gilt. Daher ist das Verständnis der Mikrostrukturen, der Eigenspannungen und der daraus resultierenden mechanischen Eigenschaften entscheidend für eine breite Akzeptanz bei sicherheitskritischen Anwendungen. Die BAM hat ein multidisziplinäres Forschungsprogramm gestartet, um diese Aspekte bei LPBF 316L zu untersuchen. Der vorliegende Beitrag stellt einige der wichtigsten Ergebnisse vor: der Einfluss von Prozessparametern auf die Mikrostruktur, der Einfluss von Mikrostruktur und Textur auf die Festigkeit, Kriechverhalten und Schädigung und die Stabilität von Eigenspannungen und Mikrostruktur unter Wärmebehandlungsbedingungen.
Avoiding the formation of defects such as keyhole pores is a major challenge for the production of metal parts by Laser Powder Bed Fusion (LPBF). The use of in-situ monitoring by thermographic cameras is a promising approach to detect defects, however the data is hard to analyze by conventional algorithms. Therefore, we investigate the use of Machine Learning (ML) in this study, as it is a suitable tool to model complex processes with many influencing factors. A ML model for defect prediction is created based on features extracted from process thermograms. The porosity information calculated from an x-ray Micro Computed Tomography (µCT) scan is used as reference. Physical characteristics of the keyhole pore formation are incorporated into the model to increase the prediction accuracy. Based on the prediction result, the quality of the input data is inferred and future demands on in-situ monitoring of LPBF processes are derived.
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.
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).
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.
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.
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.
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 research of our group is focused on the 3D imaging of AM materials by means of X-ray Computed Tomography at the lab and at synchrotron, and the residual stress characterization by diffraction (nondestructive technique).
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.
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.
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.
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.
Laser powder bed fusion (LPBF) is an additive manufacturing process for materials which inherently tends to yield various degrees of metastable hierarchical microstructures, defects and high residual stresses in the as-built condition depending on the process parameters. The understanding of the evolution of these typical features during heat treatment and subsequent thermal and mechanical ageing is crucial for the wider acceptance for safety critical structures. A multi-disciplinary research project at BAM studying the development of the microstructure, defects, residual stresses typical of LPBF 316L and their evolution during thermal and mechanical ageing has led to insights into the stability of these inherent features. This presentation aims to give a broad overview of the project with a few specific cases of investigation. Firstly, the formation of residual stresses, the nature of the initial microstructure, the tensile properties and a modelling approach to understand the anisotropy will be presented. This will be followed by examples of studies of their evolution during heat treatment, long term thermal exposure, and room temperature and high temperature mechanical testing compared to a baseline of conventional wrought variant of the same alloy.
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.
The progress of Advanced Manufacturing, which has been identified by the European Commission as a Key Enabling Technology (KET) for future economic and societal progress is strongly reliant on the development of metrology capabilities. EURAMET, the association of metrology institutes in Europe, has established metrology research programs to address the metrology requirements across a spectrum of different thematic areas. In order to leverage the benefits of these developments on the wider industrial landscape, a high-level coordination of the metrology community supporting the Advanced Manufacturing landscape is required. This coordination is aimed to be achieved by the establishment of European Metrology Networks (EMNs), which are intended by EURAMET to provide a sustainable structure for stakeholder engagement and support. The joint networking project 19NET01 AdvManuNet funded by EMPIR for 4 years, started in June 2020 and aims to accelerate the process of establishing an EMN to strengthen Europe’s position in Advanced Manufacturing. The AdvManuNet project aims to support the establishment of an EMN on Advanced Manufacturing via the following specific aims:
1. Creation of a single hub for stakeholder engagement across the landscape of various industrial sectors including relevant societies and standardization bodies.
2. Development of a Strategic Research Agenda (SRA) and roadmaps for Advanced Manufacturing metrology based on the stakeholder engagement activities, considering current gaps in metrological capabilities existing networks and roadmaps.
3. Establish a knowledge-sharing program for Advanced Manufacturing stakeholders, promoting the dissemination and exploitation of the results of the project, including those from previous EU funded research projects.
4. Development of a sustainable web-based platform and service desk for Advanced Manufacturing stakeholders to allow for easy access to European metrology capabilities and support the wider advanced manufacturing community with metrology-based requirements.
5. Develop a plan for a coordinated and sustainable European metrology infrastructure for Advanced Manufacturing via a European Metrology Network.
The project concept followed by the scope and definition of Advanced Manufacturing will be described. The analysis of the current capability of metrology for Advanced Manufacturing and the preliminary concepts for the strategic research agenda will be presented with a focus on dimensional metrology.
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.
Introduction to AGIL
(2021)
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).
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.
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.
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.