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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.
Ziel des FuE-Vorhabens ist die Entwicklung, Aufbau und Validierung eines gasto-mographischen Messsystems basierend auf stationärer und mobiler Sensorik zum Emissionsmonitoring in kommunalen Kläranlagen. Die Gastomographie basiert hierbei im Wesentlichen auf, aus unterschiedlichen Sichtwinkeln aufgenommenen, integralen Konzentrationsmessungen, anhand derer eine Rekonstruktion der Gasverteilung erfolgt. Das FuE-Projekt kombiniert hierfür stationäre Sensornetzwerke mit luftgestützten und bodengebundenen Robotersystemen in einem System. Letztere werden mit Reflektoren und/oder Gasdetektoren ausgestattet. Hierfür werden Open-Path-Gasmesstechnik basierend auf Tunable Diode Laser Ab-sorption Spectroscopy (TDLAS, primär CH4 in ppm·m) und In-situ-Gassensorik (CH4, ppm) auf Basis von z.B. Infrarot eingesetzt. Dies sind zwei komplementäre Methoden der Gasmessung: Die In-situ-Gassensorik ermöglicht Punktmessungen, wohingegen TDLAS-Sensoren Gaskonzentrationen integral über offene Messstre-cken von bis zu 60 m gegen Oberflächen messen. Die In-situ-Gassensorik wird für Referenzmessungen und ggf. zur Erhöhung der Rekonstruktionsqualität zum Ein-satz kommen. Die wesentlichen Neuheiten des Projekts sind:
• 2D-Gastomographie auf Basis eines mit TDLAS-basierter Open-Path-Gasmesstechnik und Reflektoren ausgestatteten heterogenen Messsystems.
• CT-basierte Rekonstruktionsalgorithmen, adaptiert an die komplexen Rahmenbedingungen.
• Validierung des Messsystems anhand realer Messungen auf Kläranlagen.
Automated Wall Thickness Evaluation for Turbine Blades Using Robot-Guided Ultrasonic Array Imaging
(2024)
Nondestructive testing has become an essential part of the maintenance of modern gas turbine blades and vanes since it provides an increase in both safety against critical failure and efficiency of operation. Targeted repairs of the blade’s airfoil require localized wall thickness information. This information, however, is hard to obtain by nondestructive testing due to the complex shapes of surfaces, cavities, and material characteristics. To address this problem, we introduce an automated nondestructive testing system that scans the part using an immersed ultrasonic array probe guided by a robot arm. For imaging, we adopt a two-step, surface-adaptive Total Focusing Method (TFM) approach.
For each test position, the TFM allows us to identify the outer surface, followed by calculating an adaptive image of the interior of the part, where the inner surface’s position and shape are obtained. To handle the large volumes of data, the surface features are automatically extracted from the TFM images using specialized image processing algorithms. Subsequently, the collection of 2D extracted surface data is merged and smoothed in 3D space to form the outer and inner surfaces, facilitating wall thickness evaluation. With this approach, representative zones on two gas turbine vanes were tested, and the reconstructed wall thickness values were evaluated via comparison with reference data from an optical scan. For the test zones on two turbine vanes, average errors ranging from 0.05 mm to 0.1 mm were identified, with a standard deviation of 0.06–0.16 mm.
Ultrasonic guided waves interacting with complex geometrical features are of high interest in the SHM field. For example, investigations into the extent to which a small change in defect geometry affects wave propagation have applications in Probability of Detection and defect reconstruction. These fields have to be supported by numerical tools aiming to retrieve accurate and reliable results and, thus, more realistic modeling.
Due to the short wavelengths of ultrasonic waves and the relatively large domains in which the waves propagate, fine grid resolution for the entire domain is usually not possible due to limited computational resources. One solution is to partition the domain into different subdomains and use a specific, efficient approach for each subdomain.
This contribution shows a combination of methods that aims to study these wave defect interactions in an elastic media. Firstly we introduce high-order 3D meshes that can resolve very fine geometrical details and are based on an Octree discretisation technique that employs special transition shape functions to resolve the hanging nodes that may appear due to the nature of the method. Afterward, the Octree mesh is embedded in a prismatic wave-guide based on the semi-analytical formulation of the SBFEM in 3D. To couple the different domains, we employ the mortar method, which enforces the continuity of the wave field across the internal boundaries of the domains. Examples show the power of the approach especially when it comes to parametric analysis.
For structural health monitoring systems or non-destructive testing, it is crucial to study the interactions of ultrasonic-guided waves with inhomogeneities or damage in structural components. Simulation of these interactions poses a challenge.
After the wave-damage interaction, the numerical model must reproduce features like mode conversion or wave scattering. Mathematically, damages are discontinuities in a computational domain, and each interacts diversely depending on its geometrical features. We propose a quadtree-based meshing in the current contribution to capture these geometrical
characteristics.
This kind of discretisation approach requires special techniques to couple cells of different sizes since, after a quadtree decomposition, the problem of so-called hanging nodes may arise. Transition elements based on high-order transfinite shape functions are used to solve this issue. The advantage is that these elements allow the correct coupling of the cells while retaining a high-order interpolation. Moreover, the reuse of the dynamic stiffness matrices can be exploited based on the similarity of the cells. This procedure renders the approach very efficient.
Examples show the scattering characteristics of different guided wave modes after interacting with inhomogeneities and discontinuities in a plate.
Determination of short carbon fiber orientation in zirconium diboride ceramic matrix composites
(2024)
In fiber-reinforced components, the fiber alignment and orientation have paramount influence on the thermomechanical properties of the resulting composite, for both short and continuous fiber. Here we present the case of an ultra-refractory matrix intended for extreme environment applications, ZrB2, reinforced with 20 vol% and 50 vol% short carbon fibers. In both cases, fibers tend to align perpendicular to the uniaxial pressure applied during shaping and sintering of a pellet, although the fiber tilt across the pellet thickness is difficult to determine. Moreover, for high volume fractions of reinforcement, the spatial distribution of the fibers is heterogeneous and tends to have domains of preferential orientations. We compare the information on the fiber distribution as collected by scanning electron microscopy images, X-ray computed tomography and synchrotron X-ray refraction radiography (SXRR). The three techniques prove to be complementary. Importantly, we demonstrate that SXRR yields the most statistically significant information due to the largest field of view, yet with a sensitivity down to the nanometer, and that can be successfully applied also to heavy matrix materials, such as zirconium boride.
AbstractIn this study, we compare the residual stress state in a laser powder bed fusion (PBF‐LB/M) AlSi10Mg alloy in the as‐built (AB) condition with that after two different heat treatments (265 °C for 1 h, HT1; and 300 °C for 2 h, HT2). The bulk residual stress (RS) is determined using synchrotron X‐ray diffraction (SXRD), and near‐surface profiles are determined using laboratory energy‐dispersive X‐ray diffraction (EDXRD). The EDXRD results do not reveal any notable difference between the conditions at a depth of 350 μm, suggesting that the machining process yields a comparable residual stress state in the near‐surface regions. On the other hand, the SXRD results show that HT1 is more effective in relieving the bulk RS. It is observed that HT1 reduces the RS state in both the aluminium matrix and the silicon network. In addtion, HT2 does not have a significant impact on relaxing the RS as‐built state of the matrix, although it does induce a reduction in the RS magnitudes of the Si phase. It is concluded that the heat treatment stress relieving is effective as long as the Si‐network is not disaggregated.
A new titanium alloy improving the operation of implants additively manufactured and including laterally closed lattice structures is proposed. The new alloy possesses an increased affinity to the bone. The measured bone–interface implant (BII) of less than 10 mm and bone–implant contact (BIC) of 95% demonstrated an excellent osseointegration. Furthermore, since additive manufacturing naturally leads to a high-roughness surface finish, the wettability of the implant is increased. The combination of these factors is pushing ossification beyond its natural limits. In addition, the quality and speed of the ossification and osseointegration in/around laterally closed lattice implants open the possibility of bone spline key of prostheses. This enables the stabilization of the implant into the bone while keeping the possibility of punctual hooks allowing the implant to be removed more easily if required.
Powder Bed Fusion – Laser Beam (PBF-LB) of high γ’ strengthened Ni-base superalloys, such as CM247LC, is of great interest for high temperature applications in gas turbines. However, PBF-LB of CM247LC is challenging due to the high cracking susceptibility during PBF-LB processing (solidification cracking) and heat treatment (strain age cracking, mostly caused by residual stresses). This study focuses on understanding the impact of process parameters on microstructure, residual stresses and solidification cracking. Laser power (P), speed (v) and hatch spacing (h) were varied while the layer thickness (t) was fixed. The melt pool size and shape were found to be key factors in minimizing solidification cracking. Narrower and shallower melt pools, achieved using a low line energy density (LED = P/v ≤ 0.1 J/mm), gave low crack densities (0.7 mm/mm2). A tight hatch spacing (h = 0.03 mm) resulted in reduced lack of fusion porosity. Electron backscatter diffraction investigations revealed that parameters giving finer microstructure with 〈100〉crystallographic texture had low crack densities provided they were processed with a low LED. Atom probe tomography elucidated early stages of spinodal decomposition in the as-built condition, where Cr and Al cluster separately. The extent of spinodal decomposition was found to be affected by the LED and the hatch spacing. Samples with low LED and small hatch spacing showed higher degrees of spinodal decomposition. X-ray diffraction residual stress investigations revealed that the residual stress is proportional to the volumetric energy density (VED = P/(v. h. t)). Although low residual stresses can be achieved by using low VED, there is a high risk of lack of fusion. Hence, other parameters such as modified scan strategy, build plate pre-heating and pulsed laser mode, must be further explored to minimize the residual stresses to reduce the strain age cracking susceptibility.
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.
Bei der zerstörungsfreien Prüfung verlegter Eisenbahnschienen werden die Rohdaten derzeit in proprietären Datenformaten gespeichert und auf Datenträgern zwischen den Prüfzügen und den auswertenden Stellen versendet. Die proprietären Datenformate sind in der Regel nur den Herstellern der Prüfsysteme bekannt und deren Dokumentation nicht allgemein zugänglich.
Das Forschungsprojekt „Artificial Intelligence for Rail Inspection“ (AIFRI) erfordert den Austausch von Prüfdaten in einem offenen Format sowohl zwischen den Projektpartnern als auch die Veröffentlichung anonymisierter Daten ausgewählter Strecken aus dem Offenen Digitalen Testfeld (ODT). Wir haben uns in dem Projekt für die Verwendung der „Standard Practice for Digital Imaging and Communication in Nondestructive Evaluation“ (DICONDE) entschieden. DICONDE basiert auf dem medizinischen Standard „Digital Imaging and Communication in Medicine“ (DICOM) und wurde von ASTM an die ZfP angepasst. DICOM bzw. DICONDE ist nicht nur ein Datenformat, sondern beinhaltet auch Kommunikationsschnittstellen für die Auftragsvergabe, Datenübertragung und Abfrage gespeicherter Datensätze aus einem Archiv.
In dem Vortrag werden DICOM und DICONDE vorgestellt, sowie die Verwendung von DICONDE für die Schienenprüfung im Projekt AIFRI näher erläutert. Es wird gezeigt, wie sich Prüfdaten, Prüfparameter, Streckeninformationen incl. Kilometertafeln und Geokoordinaten und Befunde in DICONDE kodieren lassen.
Die Wirbelstromprüfung ist ein bewährtes Verfahren zur zerstörungsfreien Prüfung elektrisch leitfähiger Objekte im oberflächennahen Bereich. Nach einer Einführung in die Wirkungsweise, Möglichkeiten und Grenzen des Wirbelstromprüfverfahrens wird am Beispiel des Schreins der Heiligen Drei Könige gezeigt, wie sich mit dem Wirbelstromprüfverfahren unterschiedliche Metalllegierungen unter einer Vergoldung zerstörungsfrei identifizieren lassen.
Der Schrein der Heiligen Drei Könige wurde um das Jahr 1200 von Nikolaus von Verdun erschaffen, ca. 1750 von Johann Rohr und 1807 von Wilhelm Pollack restauriert. Die Restaurierungsarbeiten wurden jedoch nur unvollständig dokumentiert. Es ist bekannt, dass zu den unterschiedlichen Zeiten unterschiedliche Metalllegierungen als Grundmaterial unter der Vergoldung verwendet wurden. Mit Hilfe von Vergleichsproben aus einer Sammlung der Kölner Dombauverwaltung ließen sich die Akanthus-Prägungen des Schreins den verschiedenen Restaurierungen zuordnen.
Currently, mandatory requirements and recommendations for the detection of irregularities in laser beam welded joints are based on classic micrographs as set out in the standard ISO 13919-1:2019. Compared to classic micrographs, computed tomography enables a non-destructive, three-dimensional and material-independent mode of operation, which delivers much more profound results. Even in building material testing, methods with limited informative value can be checked and supplemented by CT examinations.
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.
An observation of the fracture process in front of the crack tip inside a dentin sample by means of ex-situ X-ray computed tomography after uniaxial compression at different deformation values was carried out in this work. This ex-situ approach allowed the microstructure and fracturing process of human dentin to be observed during loading. No cracks are observed up to the middle part of the irreversible deformation in the samples at least visible at 0.4μm resolution. First cracks appeared before the mechanical stress reached the compression strength. The growth of the cracks is realized by connecting the main cracks with satellite cracks that lie ahead of the main crack tip and parallel its trajectory. When under the stress load the deformation in the sample exceeds the deformation at the compression strength of dentin, an appearance of micro-cracks in front of the main cracks is observed. The micro-cracks are inclined (~60°) to the trajectory of the main cracks. The further growth of the main cracks is not realized due to the junction with the micro-cracks; we assume that the micro-cracks dissipate the energy of the main crack and suppressed its growth. These micro-cracks serve as additional stress accommodations, therefore the samples do not break apart after the compression test, as it is usually observed under bending and tension tests.
Efficient density evolution during sintering of the as-printed component is vital to reach full densification and required properties of binder jet (BJT) components. However, due to the high porosity and brittle nature of the green compact, analysis of the microstructure development during sintering is very difficult, resulting in lack of understanding of the densification process. Density development from green state (57 ± 1.6 %) up to full density (99 ± 0.3 %) was characterized by high-resolution synchrotron X-Ray computed tomography (SXCT) on BJT 316L samples from ex-situ interrupted sintering tests. Periodicity of density fluctuations along the building direction was revealed for the first time and was related to the layer thickness of ~ 42 μm during printing that decreased down to ~ 33 μm during sintering. Sintering simulations, utilizing a continuum sintering model developed for BJT, allowed to replicate the density evolution during sintering with a mean error of 2 % and its fluctuation evolution from green (1.66 %) to sintered (0.56 %) state. Additionally, simulation of extreme particle size segregation (1 μm to 130 μm) suggested that non-optimized printing could lead to undesirable density fluctuation amplitude rapid increase (~10 %) during sintering. This might trigger the nucleation of defects (e.g., layer delamination, cracking, or excessive residual porosity) during the sintering process.
AbstractHigh-strength aluminum alloys used in aerospace and automotive applications obtain their strength through precipitation hardening. Achieving the desired mechanical properties requires precise control over the nanometer-sized precipitates. However, the microstructure of these alloys changes over time due to aging, leading to a deterioration in strength. Typically, the size, number, and distribution of precipitates for a quantitative assessment of microstructural changes are determined by manual analysis, which is subjective and time-consuming. In our work, we introduce a progressive and automatable approach that enables a more efficient, objective, and reproducible analysis of precipitates. The method involves several sequential steps using an image repository containing dark-field transmission electron microscopy (DF-TEM) images depicting various aging states of an aluminum alloy. During the process, precipitation contours are generated and quantitatively evaluated, and the results are comprehensibly transferred into semantic data structures. The use and deployment of Jupyter Notebooks, along with the beneficial implementation of Semantic Web technologies, significantly enhances the reproducibility and comparability of the findings. This work serves as an exemplar of FAIR image and research data management.
In this work, the thermal properties of ternary Li₃ₓCo₇₋₄ₓSb₂₊ₓO₁₂ solid solutions are studied for different concentrations in the range 0 ≤ x ≤ 0.7. Samples are elaborated at four different sintering temperatures: 1100, 1150, 1200 and 1250 °C. The effect of increasing the content of Li⁺ and Sb⁵⁺, accompanied by the reduction of Co²⁺, on the thermal properties is studied. It is shown that a thermal diffusivity gap, which is more pronounced for low values of x, can be triggered at a certain threshold sintering temperature (around 1150 °C in this study). This effect is explained by the increase of contact area between adjacent grains. Nevertheless, this effect is found to be less pronounced in the thermal conductivity. Moreover, a new framework for heat diffusion in solids is presented that establishes that both the heat flux and the thermal energy (or heat) satisfy a diffusion equation and therefore highlights the importance of thermal diffusivity in transient heat conduction phenomena.
Manufacturing austenitic stainless steels (ASSs) using additive manufacturing is of great interest for cryogenic applications. Here, the mechanical and microstructural responses of a 316L ASS built by laser powder bed fusion were revealed by performing in situ neutron diffraction tensile tests at the low-temperature range (from 373 to 10 K). The stacking fault energy almost linearly decreased from 29.2 ± 3.1 mJm⁻² at 373 K to 7.5 ± 1.7 mJm⁻² at 10 K, with a slope of 0.06 mJm⁻²K⁻¹, leading to the transition of the dominant deformation mechanism from strain-induced twinning to martensite formation. As a result, excellent combinations of strength and ductility were achieved at the low-temperature range.
Laser powder bed fusion of metallic components (PBF-LB/M) is gaining acceptance in industry. However, the high costs and lengthy qualification processes required for printed components create the need for more effective in-situ monitoring and testing methods. This article proposes multispectral Optical Tomography (OT) as a new approach for monitoring the PBF-LB/M process. Compared to other methods, OT is a low-cost process monitoring method that uses long-time exposure imaging to observe the build process. However, it lacks time resolution compared to expensive thermographic sensor systems. Monochromatic OT (1C-OT) is already commercially available and observes the building process layer-wise using a single wavelength window in the NIR range. Multispectral OT (nC-OT) utilizes a similar setup but can measure multiple wavelength ranges per location simultaneously. By comparing the classical 1C-OT and nC-OT approaches, this article examines the advantages of nC-OT (two channel OT and RGB-OT) in reducing the false positive rate for process deviations and approximating maximum temperatures for a better comparison between different build processes and materials. This could ultimately reduce costs and time for part qualification. The main goal of this contribution is to assess the advantages of nC-OT compared to 1C-OT for in-situ process monitoring of PBF-LB/M.
To evaluate the durability of new alternative cement compositions, it is important to examine the internal transport of moisture through these materials. For this purpose, mortars were prepared from different types of cement and capillary suction experiments were carried out. The moisture transport was studied with an NMR tomograph and compared with weight easurements. With the tomograph, the total moisture input could be determined, as well as the moisture content within the samples non-destructively and spatially resolved. This allows precise observation of the moisture fronts. The tomograph was also used to determine the capillary transport
coefficient.
Offshore wind turbines continuously increase in size and weight and demand adequate offshore foundations concepts like monopiles, tripods, or jackets. These components are typically constructed using submerged arc welding (SAW) with high-strength thick steel plates like the S420ML. During welding, the occurrence of delayed hydrogen-assisted cracking (HAC) must be anticipated. HAC is a critical combination of the local hydrogen concentration within a susceptible microstructure under certain mechanical load, i.e., the occurring (welding) residual stresses. The welding sequence of the thick-walled plates complicates the residual stress distribution due to the necessary repeated thermal cycling, i.e., welding seam/layer deposition to fill the joint. For that purpose, SAW with two-wire-technique was used to weld a specially designed and prototype-like mock-up of a real component with a thickness of 50 mm, filled with over 20 passes and a seam length of 1000 mm. Additional welded stiffeners simulated the effect of a high restraint, to achieve critical HAC conditions. The necessity of a minimum waiting time (MWT) before the NDT can be conducted (to exclude HAC) was critically verified by the application of ultrasonic testing of the welded joint at different time-steps of the NDT of up to 48 h after the completion welding. The residual stresses were determined by a robot XRD goniometer. Tensile residual stresses up to the yield limit are found both in the weld metal and in the heat-affected zone. Numerical modeling allowed the qualitative estimation of the hydrogen diffusion in the weld. No noticeable HAC occurrence was identified and confirms the high cracking resistance of the investigated material. Finally, the applicability of the MWT concept should be critically discussed.
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
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.
Ziel der Untersuchung: Evaluation der Eignung der Refraktions-Tomographie zur Analyse von Alterungserscheinungen innerhalb von adhäsiv verankerten Materialien vor und nach künstlicher Probenalterung.
Material und Methode: Vier humane mittlere Oberkieferfrontzähne wurden wurzelkanalbehandelt und ausgedehnte Klasse IV Defekte der Krone mit einer Aufbaufüllung aus dualhärtendem Komposit (Rebilda DC, VOCO) und einem Glasfaserstift (Rebilda Post, VOCO) restauriert. Alle Proben wurden feucht gelagert und in einer Synchrotron-Einrichtung (BAMline, BESSY II, HZB) mit einer Pixelgröße von 4,08 µm gescannt. Für diese Synchrotron-Refraktions-Tomographie (SXRCT) muss zunächst der Analysatorkristall (AK) zu einer Bragg-Reflexion (Beugung) angeregt werden, um eine SXRCT durchzuführen. Die SXRCT wird mit einer Transmissions-Tomographie (ohne AK) verrechnet. Darauf folgte eine künstliche Probenalterung mit 400.000 Kau- und 3.000 Thermozyklen (50N, 5-55°C). Anschließend wurden die Proben ein weiteres Mal gescannt. Die Datensätze beider SXRCT wurden mittels des „filtered back projection“ Algorithmus rekonstruiert, mit einer Bildanalyse-Software aufeinander registriert und ausgewertet. Hierdurch konnten die Veränderungen initialer Schädigungen analysiert werden.
Ergebnisse: Alle 4 Proben zeigten in den Scans Veränderungen des inneren Gefüges und an Grenzflächen nach Belastung. Es zeigten sich Ansammlungen von Wasser innerhalb eingeschlossener Hohlräume, subkritisches Risswachstum, Ausdehnung des Komposit und Quellung des Glasfaserstiftes um 0,4%. In den SXRCT Aufnahmen waren außerdem Dentintubuli, die bei Auflösungen von 4,08 µm sonst nicht deutlich sichtbar sind darstellbar. Dadurch konnte Eindringen von Wasser in die Tubuli im Anschluss an die Alterung belegt werden.
Zusammenfassung: SXRCT bietet die Möglichkeit, trotz einer vergleichbar geringen Auflösung, kleinste Strukturen und Veränderungen abzubilden. Dies ermöglicht unter anderem die detaillierte Analyse relativ großer Proben, wie eines vollständigen Zahnes in einem Scanvorgang.
Large temperature gradients inherent to additive manufacturing (AM) processes induce large residual stress (RS) in the final part. Because RS can influence the tribological properties, this study focuses on the relationship between wear sliding properties and RS in IN718 coatings. Such coatings were deposited with a Laser metal deposition (LMD) machine using two different scanning strategies.
The wear resistance and RS state were investigated after surface milling. RS were measured before and after wear tests on a reciprocating sliding test apparatus.
Two different X-ray diffraction techniques were employed to measure the surface and subsurface state RS: Laboratory Energy Dispersive X-ray Diffraction (LEDXD) and Synchrotron X-ray Energy Dispersive Diffraction (SXEDD). Due to the milling process, the coatings show similar depth distributions of RS from 22 to 92 μm depth, but exhibit different magnitudes depending on the scanning strategy used. Reciprocating sliding wear tests induced high compressive residual stresses that erased the initial RS state, and a similar wear behavior was observed in the two samples. These samples possess similar texture and grain morphology. This demonstrates that the influence of RS on wear resistance is a second-order effect. Nevertheless, it was observed that RS can still impact the wear performance at the early testing stages of the repaired parts.
This data article introduces a dataset comprising 1630 alkali-activated concrete (AAC) mixes, compiled from 106 literature sources. The dataset underwent extensive curation to address feature redundancy, transcription errors, and duplicate data, yielding refined data ready for further data-driven science in the field of AAC, where this effort constitutes a novelty. The carbon footprint associated with each material used in the AAC mixes, as well as the corresponding CO2 footprint of every mix, were approximated using two published articles. Serving as a foundation for future expansions and rigorous data applications, this dataset enables the characterization of AAC properties through machine learning algorithms or as a benchmark for performance comparison among different formulations. In summary, the dataset provides a resource for researchers focusing on AAC and related materials and offers insights into the environmental benefits of substituting traditional Portland concrete with AAC.
In recent decades, the number of components in concrete has grown, particularly in formulations aimed at reducing carbon footprints. Innovations include diverse binders, supplementary cementitious materials, activators, concrete admixtures, and recycled aggregates. These developments target not only the enhancement of material properties but also the mitigation of the ecological and economic impacts of concrete — the most extensively used material by humankind. However, these advancements also introduce a greater variability in the composition of raw materials. The material’s behavior is significantly influenced by its nanoscale properties, which can pose challenges in accurate characterization. Consequently, there’s an increasing need for experimental tuning of formulations. This is accompanied by a more inconsistent composition of raw materials, which makes an experimental tuning of formulations more and more necessary. However, the increased complexity in composition presents a challenge in finding the ideal formulation through trial and error. Inverse design (ID) techniques offer a solution to this challenge by allowing for a comprehensive search of the entire design space to create new and improved concrete formulations. In this publication, we introduce the concept of ID and demonstrate how our open-source app “SLAMD” provides all necessary steps of the workflow to adapt it in the laboratory, lowering the application barriers. The intelligent screening process, guided by a predictive model, leads to a more efficient and effective data-driven material design process resulting in reduced carbon footprint and improved material quality while considering socio-economic factors in the materials design.
Large-language models (LLMs) such as GPT-4 caught the interest of many scientists. Recent studies suggested that these models could be useful in chemistry and materials science. To explore these possibilities, we organized a hackathon. This article chronicles the projects built as part of this hackathon. Participants employed LLMs for various applications, including predicting properties of molecules and materials, designing novel interfaces for tools, extracting knowledge from unstructured data, and developing new educational applications. The diverse topics and the fact that working prototypes could be generated in less than two days highlight that LLMs will profoundly impact the future of our fields. The rich collection of ideas and projects also indicates that the applications of LLMs are not limited to materials science and chemistry but offer potential benefits to a wide range of scientific disciplines.
Offshore-Windenergieanlagen erfordern Gründungskonzepte aus unterpulver-(UP-)geschweißten Dickblechen (bspw. der Güte S420ML). Während der Schweißfertigung kann eine zeitverzögerte wasserstoffunterstützte Kaltrissbildung auftreten, deren Bewertung aufgrund der Bauteilgröße von Offshore-Strukturen sehr komplex ist. Deswegen wurde eine bauteilähnliche Geometrie (Mock-Up) entwickelt, um reale Steifigkeitsverhältnisse auf den Labormaßstab zu übertragen. Zusätzliche Versteifungen simulieren die Wirkung einer Einspannung bzw. Schrumpfbehinderung der Schweißnaht. Über die Verwendung von Schweißpulvern mit definierter Feuchte wurden zudem ein Extremszenario der Wasserstoffaufnahme simuliert. Entsprechend der vorgegebenen Mindestwartezeit für die ZfP von bis zu 48 h wurde die Schweißnaht zerstörungsfrei mit Phased-Array-Ultraschall-Prüfung (PAUT) geprüft und die Eigenspannungen über Röntgendiffraktometrie (XRD) bestimmt. Zusätzlich wurde die Wasserstoffverteilung in der Schweißverbindung numerisch simuliert. Außer zulässigen Defekten (wie Poren), wurde keine verzögerte Kaltrissbildung in den Mock-Ups festgestellt, was auf hohe Rissbeständigkeit hindeutet.
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.
In the present study, in-situ observation of Hot Isostatic Pressure (HIP) procedure of laser powder bed fusion manufactured Ti-6Al-4V parts was performed to quantitatively estimate the densifcation rate of the material and the infuence of the defect initial size and shape on such rate. The observations were performed in-situ using the Ultrafast Tomography Paris-Edinburgh Cell and the combination of fast phase-contrast synchrotron X-ray tomography and energy dispersive difraction. With this strategy, we could quantify how the efectiveness of HIP depends on the characteristics of a defect. Smaller defects showed a higher densifcation rate, while the defect shape did not have signifcant efect on such rate.
The industrial sintering process used to produce metallic matrix pads has been altered to diminish the amount of copper used. Unfortunately, replacing a large part of the copper with iron seems to have reached a limit. In the high-energy, emergency-type rail braking used in this study, the materials are put to the very limit of their usage capacity, allowing us to observe the evolution of the microstructure and mechanical properties of sintered, metallic matrix pads. After the braking test, their compressive behaviour was assessed using digital image correlation (DIC), and their microstructure with scanning electron microscopy (SEM). The worn material has three flat layers with different microstructures and compressive behaviours. The boom layer seems unmodified. Macroscopic and microscopic cracks run through the intermediate layer (2–15 mm depth). The top layer has stiffened thanks to resolidification of copper. The temperature reaches 1000 °C during the braking test, which also explains the carbon diffusion into iron that result in the weakening of iron–graphite interfaces in the pad. Finally, submicronic particles are detected at many open interfaces of the worn and compressed pad. Associated with the predominant role of graphite particles, this explains the weak compressive behaviour of the pads.
Electron backscatter diffraction (EBSD) images of extruded pure aluminum were statistically analyzed to investigate creep-induced subgrain structures after applying two different levels of creep stress, corresponding to the power law (PL) and power-law breakdown (PLB) regimes. Kernel average misorientation analysis of EBSD measurements revealed 2D morphologies, which were subdivided by a multi-step segmentation procedure into subgranular arrangements. Various descriptors were employed to characterize the “subgrains” quantitatively, including their size, shape, spatial arrangement, and crystallographic orientation. In particular, the analysis of the orientations of subgrains was conducted by neglecting rotations around the loading axis. This approach facilitated the individual investigation of the {001} and {111} subgrain families with respect to the loading axis for two investigated stress levels plus a reference specimen. For the PL regime, the statistical analysis of subgrain descriptors computed from segmented image data revealed a similar degree of strain accumulation for {111} and {001} subgrains. In contrast, for the PLB regime, the analyzed descriptors indicate that {111} subgrains tend to accumulate significantly more strain than {001} ones. These observations suggest that the mechanisms leading to PLB may be associated with strain localization dependent on intergranular stress, hindering the recovery process within {111} grains.
Offshore wind turbines (OWT) are a key factor of the sustainable energy generation of tomorrow. The continuously increasing installation depths and weight of the OWTs require suitable foundation concepts like monopiles or tripods. Typically, mild steels like the S420ML are used with plate thicknesses up to several hundreds of mm causing high restraints in the weld joints. Due to the large plate thickness, submerged arc welding (SAW) with multiple wires is the state-of-the-art welding procedure. As a result of the very high stiffness of the construction, a certain susceptibility for time-delayed hydrogen-assisted cracking (HAC) may occur. The evaluation of crack susceptibility is very complex due to the component size and stiffness of real offshore structures. For this purpose, a near-component test geometry was developed to transfer the real stiffness conditions to laboratory (i.e., workshop) scale. The investigated mock-up, weighing 350 kg, comprised heavy plates (thickness 50 mm, seam length 1,000 m) joined by a 22-pass submerged arc weld. Additional stiffeners simulated the effect of high restraint or shrinkage restraint of the weld. Extreme scenarios of hydrogen absorption during welding were simulated via the use of welding fluxes in dry (HD < 5 ml/100g Fe) and moisture condition (HD > 15 ml/100g Fe). The residual stresses were determined by a robot X-ray diffractometer. Areas of critical tensile residual stress (at the level of the yield strength) were found in the weld metal and heat affected zone. To identify possible delayed cracking, the welds were tested by phased array ultrasonic testing (PAUT) after 48 h. Summarized, no significant occurrence of HAC was detected, indicating the high crack resistance of the welded joint, i.e., a suitable combination of base material, welding consumable and welding parameters.
The capability to produce complexly and individually shaped metallic parts is one of the main advantages of the laser powder bed fusion (PBF LB/M) process. Development of material and machine specific process parameters is commonly based on results acquired from small cubic test coupons of about 10 mm edge length. Such cubes are usually used to conduct an optimization of process parameters to produce dense material. The parameters are then taken as the basis for the manufacturing of real part geometries. However, complex geometries go along with complex thermal histories during the manufacturing process, which can significantly differ from thermal conditions prevalent during the production of simply shaped test coupons. This may lead to unexpected and unpredicted local inhomogeneities of the microstructure and defect distribution in the final part and it is a root cause of reservations against the use of additive manufacturing for the production of safety relevant parts. In this study, the influence of changing thermal conditions on the resulting melt pool depth of 316L stainless steel specimens is demonstrated. A variation of thermo-graphically measured intrinsic preheating temperatures was triggered by an alteration of inter layer times and a variation of cross section areas of specimens for three distinct sets of process parameters. Correlations between the preheating temperature, the melt pool depth, and occurring defects were analyzed. The limited expressiveness of the results of small density cubes is revealed throughout the systematic investigation. Finally, a clear recommendation to consider thermal conditions in future process parameter optimizations is given.
Monitoring and maintenance of civil infrastructure are of great importance, as any undetected damage can cause high repair costs, unintended deadtime, or endanger structural integrity. The inspection of large concrete structures such as bridges and parking lots is particularly challenging and time-consuming. Traditional methods are mostly manual and involve mapping a grid of measurement lines to record the position of each measurement. Current semi-automated methods, on the other hand, use GPS or tachymeters for localization but still require trained personnel to operate. An entirely automated approach using mobile robots would be more cost- and time-efficient. While there have been developments in using GPS-enabled mobile robots for bridge inspection, the weak signal strength in indoor areas poses a challenge for the automated inspection of structures such as parking lots. This paper aims to develop a solution for the automated inspection of large indoor concrete structures by addressing the problem of robot localization in indoor spaces and the automated measurement of concrete cover and rebar detection.
The capability to produce complexly and individually shaped metallic parts is one of the main advantages of the laser powder bed fusion (PBF LB/M) process. Development of material and machine specific process parameters is commonly based on results acquired from small cubic test coupons of about 10 mm edge length. Such cubes are usually used to conduct an optimization of process parameters to produce dense material. The parameters are then taken as the basis for the manufacturing of real part geometries. However, complex geometries go along with complex thermal histories during the manufacturing process, which can significantly differ from thermal conditions prevalent during the production of simply shaped test coupons. This may lead to unexpected and unpredicted local inhomogeneities of the microstructure and defect distribution in the final part and it is a root cause of reservations against the use of additive manufacturing for the production of safety relevant parts. In this study, the influence of changing thermal conditions on the resulting melt pool depth of 316L stainless steel specimens is demonstrated. A variation of thermo-graphically measured intrinsic preheating temperatures was triggered by an alteration of inter layer times and a variation of cross section areas of specimens for three distinct sets of process parameters. Correlations between the preheating temperature, the melt pool depth, and occurring defects were analyzed. The limited expressiveness of the results of small density cubes is revealed throughout the systematic investigation. Finally, a clear recommendation to consider thermal conditions in future process parameter optimizations is given.
This study was carried out to investigate the neutron transmission signal as a function of sample temperature during a welding process. A theoretical description that includes the Debye-Waller factor was used to describe the temperature influence on the neutron crosssections. Neutron imaging using a monochromatic beam helps to observe transmission variations related to the material temperature. In-situ neutron imaging of welding experiments show the distribution of the temperature in bulk steel samples. The performed finite element modelling of expected temperature distributions shows good agreement with the obtained experimental data.
In this paper, we demonstrate the value of 1H NMR
relaxometry for studying the hydration of clinker-reduced, more
climate-friendly cementitious binders. The results were obtained
on typical CEM I cements and samples containing two different
reactive agricultural ashes as well as non-reactive biochars as
supplementary cementitious materials. The findings prove that
time-resolved NMR measurements provide valuable additional
information when combined with classical heat flow calorimetry.
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.
We introduce a novel approach that combines the scaled boundary finite element method (SBFEM) with a mortar coupling to enhance the computational modelling of elastic wave propagation and interaction with local features in the ultrasonic range. The key objective is to achieve decoupling between different regions of interest, enabling independent meshes for the zones where waves either propagate or interact with localised discontinuities in the elastic media. This decoupling allows us to exploit the benefits offered by various SBFEM formulations. Thus, we can select the most suitable solution for each specific region. An important concept we emphasise is the differentiation between the near field and far field regions. The near field encompasses zones where the precise representation of small features compared to the wavelength is crucial. At the same time, the far field comprises homogeneous regions where the waves propagate without interactions, eventually radiating towards infinity if the domain is unbounded. By separating these two zones, we can improve the computational performance by employing finer discretisation only where necessary. Furthermore, this decoupling enables the reuse of far field models in parametric analyses, making it highly valuable for scenarios focused particularly on local elastic wave interactions. This approach offers considerable potential in such cases. The modelling technique is validated, and its potential is demonstrated through practical applications.
High energy X-ray synchrotron diffraction is used to investigate the elastic anisotropy of the nickel-based superalloy IN718 produced by laser powder bed fusion (PBF-LB). This material is characterized by a columnar grain morphology with some crystallographic texture. The material is subjected to elastic loading to determine the diffraction elastic constants (DECs). Furthermore, the single-crystal elastic constants (SCEC) are refined from these experiments using different micromechanical models. The results show that each micromechanical model predicts a specific set of SCEC that well describes the elastic anisotropy of PBF-LB/IN718.
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.
For the wide acceptance of the use of additive manufacturing (AM), it is required to provide reliable testing methods to ensure the safety of the additively manufactured parts. A possible solution could be the deployment of in-situ monitoring during the build process. However, for laser powder bed fusion using metal powders (PBF-LB/M) only a few in-situ monitoring techniques are commercially available (optical tomography, melt pool monitoring), which have not been researched to an extent that allows to guarantee the adherence to strict quality and safety standards.
In this contribution, we present results of a study of PBF-LB/M printed parts made of the nickel-based superalloy Haynes 282. The formation of defects was provoked by local variations of the process parameters and monitored by thermography, optical tomography and melt pool monitoring. Afterwards, the defects were characterized by computed tomography (CT) to identify the detection limits of the used in-situ techniques.
This paper presents a novel approach for developing sustainable building materials through Sequential Learning. Data sets with a total of 1367 formulations of different types of alkali-activated building materials, including fly ash and blast furnace slag-based concrete and their respective compressive strength and CO2-footprint, were compiled from the literature to develop and evaluate this approach. Utilizing this data, a comprehensive computational study was undertaken to evaluate the efficacy of the proposed material design methodologies, simulating laboratory conditions reflective of real-world scenarios. The results indicate a significant reduction in development time and lower research costs enabled through predictions with machine learning. This work challenges common practices in data-driven materials development for building materials. Our results show, training data required for data-driven design may be much less than commonly suggested. Further, it is more important to establish a practical design framework than to choose more accurate models. This approach can be immediately implemented into practical applications and can be translated into significant advances in sustainable building materials development.
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.
Fused filament fabrication (FFF) on desktop 3D printers is a material extrusion-based technique often used by educational institutions, small enterprises and private households. Polymeric filaments are melted and extruded through a heated nozzle to form a 3D object in layers. The extrusion temperature is therefore a key parameter for a successful print job, but also one of the main driving factors for the emission of harmful air pollutants, namely ultrafine particles and volatile organic gases, which are formed by thermal stress on the polymeric feedstock. The awareness of potential health risks has increased the number of emission studies in the past years. However, the multiplicity of study designs makes an objective comparison of emission data challenging because printer hardware factors such as the actual extruder temperature (TE) and also feedstockspecific emissions are not considered. We assume that across the market of commercial low- and mid-price FFF printers substantial deviations between actual and set extruder temperatures exist, which have a strong effect on the emissions and hence may bias the findings of exposure studies. In our last publication, we presented a standardized feedstock-specific emission test method and showed that for each investigated feedstock an increase in actual extruder temperature was accompanied by an increase in particle emissions (Tang and Seeger, 2022). Therefore, any systematic discrepancy between set and actual extruder temperature matters. In this study, we used a thermocouple and an infrared camera to measure the actual extruder temperatures at different heights. We found significant under- and overestimation of the actual extruder temperatures by the respective set temperatures in three commercial printers. This caused a broad variation of the measured total numbers of emitted particles (TP), even when the same feedstock was operated. For the determination of TP, we followed the DE-UZ 219 test guideline. In a second round we repeated the tests with all printers adjusted to exactly the same extruder temperatures, i.e., to TE=230°C for ABS and TE=210°C for PLA. All measurements were conducted in a 1 m³ emission test chamber. Particle emissions in the size range between 4 nm and 20 μm were detected. Printing on three different printer models without temperature adjustment resulted for each of the investigated feedstocks in a variation in TP of around two orders of magnitude. After temperature adjustment, this was substantially reduced to approx. one order of magnitude and hence minimizes the bias of printer hardware on the emissions. Our findings suggest that adjustment of the extruder temperature should be mandatory in emission testing standards. It also poses a more accurate benchmark and provides more reliable emission data for evaluation of indoor air quality or for health risk assessments. In addition, a proper temperature setting is in the interest of the user. Some commercial FFF printers may have a higher actual extruder temperature than displayed and unintended overheating may not only impair the print quality but may cause unnecessarily increased exposure to particle emissions.
Packagings for the transport of dangerous goods need to meet special requirements to get an approval. This includes free fall drop testing onto an essentially unyielding surface as a means to assess a package’s resistance to mechanical damage. A main requirement for drop tests is that the impact target’s mass shall be at least 50 times that of the heaviest package to be tested. Nevertheless, many manufacturers do not possess foundation structures with the required mass ratio. Previous evidence highlights that the mass ratio is not a decisive criterion on its own. Parameters such as the impact target foundation’s connection and the impulse experienced by the impacting object are essential as well. However, these factors are not easily verifiable since experimental measurements are not possible at most facilities. The objective of this work is to provide a detailed analysis on the interaction between impact target foundation and subgrade in dynamic impact testing using validated finite-element (FE) models. This research is highly beneficial for industrial application since it allows manufacturers to make informed predictions about the mechanical response of installed impact target foundations.
Material extrusion of thermoplastic polymers enables the realization of complex specific designs with high performance composites. The present study aims at evaluating the mechanical properties of carbon fiberreinforced semi-crystalline thermoplastic polymer polyether ether ketone (CFR-PEEK) manufactured by material extrusion and correlating them with results obtained by micro-CT. Samples in the shape of small bars were provided by Kumovis (Munich, Germany). The determination of surface roughness and density was followed by three-point bending tests. To reveal the pore distribution as well as the fusion quality of CFR PEEK when applied with external forces, micro-CT scans were performed with an X-ray microscope before and after the mechanical test to localize the sites where the fracture is generated. The density of CFR-PEEK bars indicated that they had superior mechanical properties compared with our previous study on unfilled 3D printed PEEK (bending modulus: (5.4 ± 0.5) GPa vs. (1.05 ± 0.05) GPa to (1.48 ± 0.10) GPa; bending strength: (167 ± 11) MPa vs. (51 ± 15) to (193 ± 7) MPa). Micro-CT analyses revealed the local 3D-distribution of voids. Voids of 30 μm diameter are nearly spherical and make up the main part of the total porosity. The larger the voids, the more they deviate from a spherical shape. Significant lack-of-fusion voids are located between the deposited filaments. By growing and merging, they act as seeds for the forming fracture line in the region of the flexural specimens where the maximum local tensile stresses occurred under bending load. Our work provides a detailed analysis of printed PEEK with fiber additive and relates this with mechanical properties.
Defects are still common in metal components built with Additive Manufacturing (AM). Process monitoring methods for laser powder bed fusion (PBF-LB/M) are used in industry, but relationships between monitoring data and defect formation are not fully understood yet. Additionally, defects and deformations may develop with a time delay to the laser energy input. Thus, currently, the component quality is only determinable after the finished process.
Here, active laser thermography, a non-destructive testing method, is adapted to PBF-LB/M, using the defocused process laser as heat source. The testing can be performed layer by layer throughout the manufacturing process. The results of the defect detection using infrared cameras are presented for a custom research PBF-LB/M machine. Our work enables a shift from post-process testing of components towards in-situ testing during the AM process. The actual component quality is evaluated in the process chamber and defects can be detected between layers.
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.
Many advanced materials consist of fibers. They are used as nonwovens, fabrics, or in composite materials. Characterization of individual fibers allows us to predict resulting material properties. We present a measurement setup and analysis software to characterize individual, micrometer-sized fibers fast and reliably. The setup is based on the lock-in thermography principle. Thermal diffusivity values of seven reference samples agree very well with previously reported values. We use our setup to investigate critical measurement parameters like excitation frequency, excitation power, pixel size, and fiber orientation. Our results show that fibers with subpixel diameters can be measured even if they are not aligned. However, special care has to be taken to choose an adequate excitation power. Measurements at high intensities can underestimate thermal diffusivity even though the raw data looks reasonable. By automatically measuring at different excitation powers, our setup solves this issue.
The stress–strain behavior of ceramics, such as aluminum titanate, has certain features that are unusual for brittle materials—in particular, a substantial nonlinearity under uniaxial tension, and load–unload hysteresis caused by the sharp increase of the incremental stiffness at the beginning of unloading. These features are observed experimentally and are attributed to microcracking. Here we compare different degrees of stress–strain nonlinearity of aluminum titanate materials and quantitatively model them. We use advanced mechanical testing to observe the mechanical response at room and high temperature; electron microscopy, and X-ray refraction radiography to observe the microstructural changes. Experiments show that two types of microcracks can be distinguished: (i) microcracks induced by cooling from the sintering temperature (due to heterogeneity and anisotropy of thermal expansion), with typical sizes of the order of grain size, and (ii) much larger microcracks generated by the mechanical loading. The two microcrack types produce different effects on the stress–strain curves. Such microcracks and the features of the stress–strain behavior depend on the density of the cooling-induced microcracks and on the distribution of grain sizes. They are modeled analytically and numerically.
Safety-critical applications of products manufactured by laser powder bed fusion (PBF-LB/M) are still limited to date. This is mainly due to a lack of knowledge regarding the complex relationship between process, structure, and resulting properties. The assurance of homogeneity of the microstructure and homogeneity of the occurrence and distribution of defects within complexly shaped geometries is still challenging. Unexpected and unpredicted local inhomogeneities may cause catastrophic failures. The identification of material specific and machine specific process parameter windows for production of fully dense simple laboratory specimens is state of the art. However, the incorporation of changing thermal conditions that a complexly shaped component can be faced with during the manufacturing process is often neglected at the stage of a process window determination. This study demonstrates the tremendous effect of changing part temperatures on the defect occurrence for the broadly used stainless steel alloy AISI 316L. Process intrinsic variations of the surface temperature are caused by heat accumulation which was measured by use of a temperature adjusted mid-wavelength infrared (MWIR) camera. Heat accumulation was triggered by simple yet effective temporal and geometrical restrictions of heat dissipation. This was realized by a variation of inter layer times and reduced cross section areas of the specimens. Differences in surface temperature of up to 800 K were measured. A severe development of keyhole porosity resulted from these distinct intrinsic preheating temperatures, revealing a shift of the process window towards unstable melting conditions. The presented results may serve as a warning to not solely rely on process parameter optimization without considering the actual process conditions a real component is faced with during the manufacturing process. Additionally, it motivates the development of representative test specimens.
Safety-critical applications of products manufactured by laser powder bed fusion (PBF-LB/M) are still limited to date. This is mainly due to a lack of knowledge regarding the complex relationship between process, structure, and resulting properties. The assurance of homogeneity of the microstructure and homogeneity of the occurrence and distribution of defects within complexly shaped geometries is still challenging. Unexpected and unpredicted local inhomogeneities may cause catastrophic failures. The identification of material specific and machine specific process parameter windows for production of fully dense simple laboratory specimens is state of the art. However, the incorporation of changing thermal conditions that a complexly shaped component can be faced with during the manufacturing process is often neglected at the stage of a process window determination. This study demonstrates the tremendous effect of changing part temperatures on the defect occurrence for the broadly used stainless steel alloy AISI 316L. Process intrinsic variations of the surface temperature are caused by heat accumulation which was measured by use of a temperature adjusted mid-wavelength infrared (MWIR) camera. Heat accumulation was triggered by simple yet effective temporal and geometrical restrictions of heat dissipation. This was realized by a variation of inter layer times and reduced cross section areas of the specimens. Differences in surface temperature of up to 800 K were measured. A severe development of keyhole porosity resulted from these distinct intrinsic preheating temperatures, revealing a shift of the process window towards unstable melting conditions. The presented results may serve as a warning to not solely rely on process parameter optimization without considering the actual process conditions a real component is faced with during the manufacturing process. Additionally, it motivates the development of representative test specimens.
Guided wave ultrasonic features in composite overwrapped pressure vessels towards digital twin
(2023)
The digitalization of quality control processes and the underlying data infrastructures for safety relevant components, such as hydrogen pressure vessels, plays a significant role in the transition towards Industry 4.0. In the current safety regulations for hydrogen pressure vessels, there is no established concept for structural health monitoring. The development of a reliable structural health monitoring methodology for monitoring the structural integrity of pressure vessels enables a fast-forward transition from personnel- and costintensive recurring inspections, a.k.a. periodic maintenance, to predictive maintenance. In the work presented; we investigated the application of ultrasonic guided wave propagation to monitor and assess the condition of Type IV composite overwrapped pressure vessel (COPV). A sensor network of fifteen piezo-electric wafers is placed on the carbon fibre reinforced composite cylinder. Five different artificial damage configurations are created by gluing two different weight blocks on three different locations. The database containing measured guided wave data sets is enriched by two different boundary conditions. We utilized an open-source software, openBIS labnotebook, to store and analyse experimental datasets. The guided wave ultrasonic signals were investigated and analysed by using commonly used ultrasonic features (e.g., amplitude, frequency, time of flight) as well as non-traditional time-series features (kurtosis, skewness, variance). The features were used to calculate damage index and the detection performance for the results has been evaluated. The results suggest that both traditional and non-traditional features assume significant importance in artificial damage detection. The future works will additionally involve the impacts of operational conditions, such as periodic pressure variations temperature loadings as well as material degradations.
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.
For the wide acceptance of the use of additive manufacturing (AM), it is required to provide reliable testing methods to ensure the safety of the additively manufactured parts. A possible solution could be the deployment of in-situ monitoring during the build process. However, for laser powder bed fusion using metal powders (PBF-LB/M ) only a few in-situ monitoring techniques are commercially available (optical tomography, melt pool monitoring) but not researched to an extent that allows to guarantee the adherence to strict quality and safety standards.
In this contribution, we present results of a study of PBF-LB/M printed parts made of the nickel-based superalloy Haynes 282. The formation of defects was provoked by local variations of the process parameters and monitored by thermography, optical tomography and melt pool monitoring. Afterwards, the defects were characterized by computed tomography (CT) to identify the detection limits of the used in-situ techniques.
We discuss the non-linear stress–strain behavior of microcracked polycrystalline ceramics under uniaxial tension and compression (displacement control).
Micromechanics explanation and modeling of its basic features, such as non-linearity and hysteresis in stress–strain curves, are developed, with stable microcrack propagation and “roughness” of intergranular cracks playing critical roles in tension and crack sliding playing a critical role in compression. Experiments involving complex loading histories are explained, and themodel is shown to reproduce the basic features of the observed stress–strain curves.
Great complexity characterizes Additive Manufacturing (AM) of metallic components via laser powder bed fusion (PBF-LB/M). Due to this, defects in the printed components (like cracks and pores) are still common. Monitoring methods are commercially used, but the relationship between process data and defect formation is not well understood yet. Furthermore, defects and deformations might develop with a temporal delay to the laser energy input. The component’s actual quality is consequently only determinable after the finished process.
To overcome this drawback, thermographic in-situ testing is introduced. The defocused process laser is utilized for nondestructive testing performed layer by layer throughout the build process. The results of the defect detection via infrared cameras are shown for a research PBF-LB/M machine.
This creates the basis for a shift from in-situ monitoring towards in-situ testing during the AM process. Defects are detected immediately inside the process chamber, and the actual component quality is determined.
Capillary active interior insulation materials are an important approach to minimize energy losses of historical buildings. A key factor for their performance is a high liquid conductivity, which enables redistribution of liquid moisture within the material. We set up an experiment to investigate the development of moisture profiles within two different interior insulation materials, calcium-silicate (CaSi) and expanded perlite (EP), under constant boundary conditions. The moisture profiles were determined by two different methods: simple destructive sample slicing with subsequent thermogravimetric drying as well as non-destructive NMR measurements with high spatial resolution. The moisture profiles obtained from both methods show good agreement, when compared at the low spatial resolution of sample slicing, which demonstrates the reliability of this method. Moreover, the measured T2- relaxation-time distributions across the sample depth were measured, which may give further insight into the saturation degree of the different pore sizes. In order to explain differences in the moisture profiles between CaSi and EP, we determined their pore-size distribution with different methods: conversion of the NMR T2 relaxationtime distribution at full saturation, mercury intrusion porosimetry and indirect determination from pressure plate measurements. CaSi shows a unimodal distribution at small pore diameters, while in EP, a bi-modal or wider distribution was found. We assume that the smaller pore diameters of CaSi lead to a higher capillary conductivity, which causes a more distributed moisture profile in comparison with that of EP.
Capillary active interior insulation materials are an important approach to minimize energy losses of historical buildings. A key factor for their performance is a high liquid conductivity, which enables redistribution of liquid moisture within the material. We set up an experiment to investigate the development of moisture profiles within two different interior insulation materials, calcium-silicate (CaSi) and expanded perlite (EP), under constant boundary conditions. The moisture profiles were determined by two different methods: simple destructive sample slicing with subsequent thermogravimetric drying as well as non-destructive NMR measurements with high spatial resolution. The moisture profiles obtained from both methods show good agreement, when compared at the low spatial resolution of sample slicing, which demonstrates the reliability of this method. Moreover, the measured T2-relaxation-time distributions across the sample depth were measured, which may give further insight into the saturation degree of the different pore sizes. In order to explain differences in the moisture profiles between CaSi and EP, we determined their pore-size distribution with different methods: conversion of the NMR T2 relaxationtime distribution at full saturation, mercury intrusion porosimetry and indirect determination from pressure plate measurements. CaSi shows a unimodal distribution at small pore diameters, while in EP, a bi-modal or wider distribution was found. We assume that the smaller pore diameters of CaSi lead to a higher capillary conductivity, which causes a more distributed moisture profile in comparison with that of EP.
In dentistry it is of great interest to achieve good sealing interzones between tooth tissue and restoration materials to avoid, e. g. secondary caries. μXRF and CμXRF are suitable to investigate the elemental composition at these interzones in respect to diffusion of elements. Synchrotron X-ray refraction radiography (SXRR) and μCT measurements deliver highly resolved structural information and make structural changes such as micro cracks within the filling and the tooth tissue visible. The presented measurements are part of the DFG funded project IXdent (Integrative X-ray techniques for chemical and structural characterizations of dental interzones.)
The depth-resolved CμXRF measurements are affected by absorption effects, making a quantitative investigation of the interzone in depth difficult. Full 3D quantification of heterogenous samples requires a complete model including dark matrix and density for each voxel. The combination of different techniques paves the way for a quantitative analysis of dental interzones.
Although layer-based additive manufacturing methods such as laser powder bed fusion (PBF-LB) offer an immense geometrical freedom in design, they are typically subject to a build-up of internal stress (i.e. thermal stress) during manufacturing. As a consequence, significant residual stress (RS) is retained in the final part as a footprint of these internal stresses. Furthermore, localized melting and solidification inherently induce columnar-type grain growth accompanied by crystallographic texture. Although diffraction-based methods are commonly used to determine the RS distribution in PBF-LB parts, such features pose metrological challenges in their application. In theory, preferred grain orientation invalidates the hypothesis of isotropic material behavior underlying the common methods to determine RS. In this work, more refined methods are employed to determine RS in PBF-LB/M/IN718 prisms, based on crystallographic texture data. In fact, the employment of direction-dependent elastic constants (i.e. stress factors) for the calculation of RS results in insignificant differences from conventional approaches based on the hypothesis of isotropic mechanical properties. It can be concluded that this result is directly linked to the fact that the {311} lattice planes typically used for RS analysis in nickel-based alloys have high multiplicity and less strong texture intensities compared with other lattice planes. It is also found that the length of the laser scan vectors determines the surface RS distribution in prisms prior to their removal from the baseplate. On removal from the baseplate the surface RS considerably relaxes and/or redistributes; a combination of the geometry and the scanning strategy dictates the sub-surface RS distribution.
With increasing demand and environmental concerns, researchers are exploring new materials that can perform as well or better than traditional materials while reducing environmental impact. The BAMline, a real-life sample materials research beamline, provides unique insights into materials’ electronic and chemical structure at different time and length scales. The beamline specializes in x-ray absorption spectroscopy, x-ray fluorescence spectroscopy, and tomography experiments. This enables real-time optimization of material properties and performance for various applications, such as energy transfer, energy storage, catalysis, and corrosion resistance. This paper gives an overview of the analytical methods and sample environments of the BAMline, which cover non-destructive testing experiments in materials science, chemistry, biology, medicine, and cultural heritage. We also present our own synthesis methods, processes, and equipment developed specifically for the BAMline, and we give examples of synthesized materials and their potential applications. Finally, this article discusses the future perspectives of the BAMline and its potential for further advances in sustainable materials research.
The microstructure has a great influence on short fatigue crack growth in metallic materials. Laser-based Powder Bed Fusion AlSi10Mg alloys exhibit in the as-built condition a fine fibrous Si structure and a supersaturated solid solution of Si in the α-Al matrix, which is significantly modified by heat treatments starting already at temperatures under 260 °C. This study focuses on the influence of post-process heat treatments on the microstructural evolution and the resulting fatigue crack growth resistance. As compared to the as-built condition, two heat treatments at 265 °C/1 h and at 300 °C/2 h are found to be beneficial to the fatigue crack growth resistance of the investigated material.
One of the main advantages of metal additive manufacturing (MAM) techniques is their ability to produce components with site-specific microstructural features. Nevertheless, microstructural defects and lack of repeatability are still major concerns in MAM. In this study, a laser powder bed fusion (PBF-LB/M) IN718 material, produced using two different scan length vectors, is investigated using Bragg-edge neutron 2D imaging (BENI) combined with electron backscatter diffraction (EBSD) analysis. BENI is able to detect, on a macroscopic scale, process-induced changes in texture in a large field of view covering the entire sample (20×80 mm2). In addition, high-resolution BENI (HR-BENI), with a pixel size of 12.8 µm, provides a micro-scale examination of the local variations of texture and grain morphology, otherwise undistinguishable using the standard resolution. As such, HR-BENI offers a straightforward and detailed way of screening the integrity of MAM parts at cm-length scales.
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.
LTCCs (Low-temperature co-fired ceramics) consist of three-dimensionally distributed, hermetically bonded ceramic and metallic components with structure sizes within [10; 100] µm. A non-destructive imaging technique is needed that provides 3D, sharp, high-contrast resolution of these structures, as well as porosity and defect analysis, which is made difficult by the very different X-ray absorption coefficients of the individual components of the microstructure. A HDR method is being developed that allows a combination of different tomograms, each with X-ray energies adapted to individual materials.
Der Vortrag gibt eine Übersicht über aktuelle zerstörungsfreie Prüfmethoden, die verwendet werden können, um eine Zustandsbewertung von Bauteilen im Bestand vorzunehmen und mögliche Wiederverwendungsstrategien zu entwickeln. Ebenfalls zeigt der Vortrag, welche Möglichkeiten es gibt, künstliche Intelligenzmethoden zu verwenden, um aus recykelten Materialien wieder hochwertige, neue Baustoffe zu entwickeln.
The osseointegration in/around additively manufactured (AM) lattice structures of a new titanium alloy, Ti–19Nb–14Zr, was evaluated. Different lattices with increasingly high sidewalls gradually closing them were manufactured and implanted in sheep. After removal, the bone–interface implant (BII) and bone–implant contact (BIC) were studied from 3D X-ray computed tomography images. Measured BII of less than 10 µm and BIC of 95% are evidence of excellent osseointegration.
Since AMnaturally leads to a high-roughness surface finish, the wettability of the implant is increased.
The new alloy possesses an increased affinity to the bone. The lattice provides crevices in which the biological tissue can jump in and cling. The combination of these factors is pushing ossification beyond its natural limits. Therefore, the quality and speed of the ossification and osseointegration in/around these Ti–19Nb–14Zr laterally closed lattice implants open the possibility of bone spline key of prostheses. This enables the stabilization of the implant into the bone while keeping the possibility of punctual hooks allowing the implant to be removed more easily if required. Thus, this new titanium alloy and such laterally closed lattice structures are appropriate candidates to be implemented in a new generation of implants.
Functionally graded porous scaffolds (FGPS) constructed with pores of different size arranged as spatially continuous structure based on sheet-based gyroid with three different scaling factors of 0.05, 0.1 and 0.2 were produced by electron beam powder bed fusion. The pore dimensions of the obtained scaffolds satisfy the values required for optimal bone tissue ingrowth. Agglomerates of residual powder were found inside all structures, which required post-manufacturing treatment. Using X-ray Computed Tomography powder agglomerations were visualized and average wall thickness, wall-to-wall distances, micro- and macro-porosities were evaluated. The initial cleaning by powder recovery system (PRS) was insufficient for complete powder removal. Additional treatment by dry ultrasonic vibration (USV) was applied and was found successful for gyroids with the scaling factors of 0.05 and 0.1. Mechanical properties of the samples, including quasi-elastic gradients and first maximum compressive strengths of the structures before and after USV were evaluated to prove that additional treatment does not produce structural damage. The estimated quasi-elastic gradients for gyroids with different scaling factors lie in a range between 2.5 and 2.9 GPa, while the first maximum compressive strength vary from 52.5 for to 59.8 MPa, compressive offset stress vary from 46.2 for to 53.2 MPa.
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 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.
Die Brechung von Röntgenstrahlen (Röntgenrefraktion) an Grenzflächen zwischen Materialien unterschiedlicher Dichte ist analog zur Ablenkung von sichtbarem Licht an z.B. Glasoberflächen. Es gibt jedoch zwei wesentliche Unterschiede:
a) konvexe Grenzflächen verursachen Divergenz (d.h. der Brechungsindex n ist kleiner als 1), und
b) die Ablenkungswinkel sind sehr klein, und reichen von einigen Bogensekunden bis zu einigen Bogenminuten (d.h. n ist nahe bei 1);
Wie auch bei sichtbarem Licht ist die Ablenkungsrichtung der Röntgenstrahlen abhängig von der Orientierung der durchstrahlten Grenzfläche. Aufgrund dieser Eigenschaften eignen sich Röntgenrefraktionsmethoden hervorragend für:
a) die Erkennung und Quantifizierung von Defekten wie Poren und Mikrorissen und
b) die Bewertung von Porosität und Partikeleigenschaften wie Orientierung, Größe und räumliche Verteilung.
Wir zeigen die Anwendung der Röntgenrefraktionsradiographie (2,5D Technik) und der -tomographie (3D Technik) für die Untersuchung verschiedener Probleme in der Werkstoffwissenschaft und -technologie:
a) Sintern von SiC-Grünkörpern
b) Porositätsanalyse in Dieselpartikelfiltersilikaten
c) Faser-Matrix-Haftung in Metall- und Polymermatrixverbundwerkstoffen
d) Mikrorissbildung in Glaskeramik.
Wir zeigen, dass der Einsatz von Röntgenrefraktionsmethoden quantitative Ergebnisse liefert, die direkt als Parameter in Werkstoffmodellen verwendet werden können.
Die Brechung von Röntgenstrahlen (Röntgenrefraktion) an Grenzflächen zwischen Materialien unterschiedlicher Dichte ist analog zur Ablenk-ung von sichtbarem Licht an z.B. Glasoberflächen. Es gibt jedoch zwei wesentliche Unterschiede:
a) konvexe Grenzflächen verursachen Divergenz (d.h. der Brechungsindex n ist kleiner als 1), und
b) die Ablenkungswinkel sind sehr klein, und reichen von einigen Bogensekunden bis zu einigen Bogenminuten (d.h. n ist nahe bei 1);
Wie auch bei sichtbarem Licht ist die Ablenkungsrichtung der Röntgenstrahlen abhängig von der Orientierung der durchstrahlten Grenzfläche. Aufgrund dieser Eigenschaften eignen sich Röntgenrefraktionsmethoden hervorragend für:
a) die Erkennung und Quantifizierung von Defekten wie Poren und Mikrorissen und
b) die Bewertung von Porosität und Partikeleigenschaften wie Orientierung, Größe und räumliche Verteilung.
Wir zeigen die Anwendung der Röntgenrefraktionsradiographie (2,5D Technik) und der -tomographie (3D Technik) für die Untersuchung verschiedener Probleme in der Werkstoffwissenschaft und -technologie:
a) Sintern von SiC-Grünkörpern
b) Porositätsanalyse in Dieselpartikelfiltersilikaten
c) Faser-Matrix-Haftung in Metall- und Polymermatrixverbundwerkstoffen
d) Mikrorissbildung in Glaskeramik.
Wir zeigen, dass der Einsatz von Röntgenrefraktionsmethoden quantitative Ergebnisse liefert, die direkt als Parameter in Werkstoffmodellen verwendet werden können.
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 peak broadening in neutron diffraction experiments on tensile specimens of pure Al (99.8%) and an Al-Mg alloy pre-deformed at different creep strains is analysed. These results are combined with the kernel angular misorientation of electron backscatter diffraction data from the creep-deformed microstructures. It is found that differently oriented grains possess different microstrains. These microstrains vary with creep strain in pure Al, but not in the Al-Mg alloy. It is proposed that this behaviour can explain the power-law breakdown in pure Al and the large creep strain observed in Al-Mg. The present findings further corroborate a description of the creep-induced dislocation structure as a fractal, predicated on previous work.
The application and benefits of Semantic Web Technologies (SWT) for managing, sharing, and (re-)using of research data are demonstrated in implementations in the field of Materials Science and Engineering (MSE). However, a compilation and classification are needed to fully recognize the scattered published works with its unique added values. Here, the primary use of SWT at the interface with MSE is identified using specifically created categories. This overview highlights promising opportunities for the application of SWT to MSE, such as enhancing the quality of experimental processes, enriching data with contextual information in knowledge graphs, or using ontologies to perform specific queries on semantically structured data. While interdisciplinary work between the two fields is still in its early stages, a great need is identified to facilitate access for nonexperts and develop and provide user-friendly tools and workflows. The full potential of SWT can best be achieved in the long term by the broad acceptance and active participation of the MSE community. In perspective, these technological solutions will advance the field of MSE by making data FAIR. Data-driven approaches will benefit from these data structures and their connections to catalyze knowledge generation in MSE.
The prediction of porosity is a crucial task for metal based additive manufacturing techniques such as laser powder bed fusion. Short wave infrared thermography as an in-situ monitoring tool enables the measurement of the surface radiosity during the laser exposure. Based on the thermogram data, the thermal history of the component can be reconstructed which is closely related to the resulting mechanical properties and to the formation of porosity in the part. In this study, we present a novel framework for the local prediction of porosity based on extracted features from thermogram data. The framework consists of a data pre-processing workflow and a supervised deep learning classifier architecture. The data pre-processing
workflow generates samples from thermogram feature data by including feature information from multiple subsequent layers.
Thereby, the prediction of the occurrence of complex process phenomena such as keyhole pores is enabled. A custom convolutional neural network model is used for classification. Themodel is trained and tested on a dataset from thermographic in-situ monitoring of the manufacturing of an AISI 316L stainless steel test component. The impact of the pre-processing parameters and the local void distribution on the classification performance is studied in detail. The presented model achieves an accuracy of 0.96 and an f1-Score of 0.86 for predicting keyhole porosity in small sub-volumes with a dimension of (700 × 700 × 50) μm3. Furthermore, we show that pre-processing parameters such as the porosity threshold for sample
labeling and the number of included subsequent layers are influential for the model performance. Moreover, the model prediction is shown to be sensitive to local porosity changes although it is trained on binary labeled data that disregards the actual sample porosity.
The microstructure of an apatite-wollastonite (code name AP40) glass-ceramic is analyzed in this study by combining 2D microscopy, phase analysis, X-ray absorption and synchrotron X-ray refraction computed tomography (XCT and SXRCT, respectively). It is shown that this combination provides a useful toolbox to characterize the global microstructure in a wide scale range, from sub-micrometer to millimeter. The material displays a complex microstructure comprising a glassy matrix with embedded fluorapatite and wollastonite small crystals. In this matrix, large (up to 200 μm) spike-shaped structures are distributed. Such microstructural features are oriented around a central sphere, thereby forming a structure resembling a sea urchin. A unique feature of SXRCT, in contrast to XCT, is that internal interfaces are visualized; this allows one to show the 3D distribution of these urchins with exceptionally good contrast. Furthermore, it is revealed that the spike-shaped structures are not single crystals, but rather composed of sub-micrometric crystals, which are identified as fluorapatite and diopside phases by SEM-EDX analysis.
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.
NMR is becoming increasingly popular for the investigation of building materials as it is a non-invasive technology that does not require any sample preparation nor causes damage to the material. Depending on the specific application it can offer insights into properties like porosity and spatial saturation degree as well as pore structure. Moreover it enables the determination of moisture transport properties and the (re-)distribution of internal moisture into different reservoirs or chemical phases upon damage and curing. However, as yet most investigations were carried out using devices originally either designed for geophysical applications or the analysis of rather homogeneous small scale (< 10 mL) samples. This paper describes the capabilities of an NMR tomograph, which has been specifically optimized for the investigation of larger, heterogeneous building material samples (diameters of up to 72 mm, length of up to 700 mm) with a high flexibility due to interchangeable coils allowing for a high SNR and short echo times (50 - 80 m s).
Fused filament fabrication (FFF) is a material extrusion-based technique often used in desktop 3D printers. Polymeric filaments are melted and are extruded through a heated nozzle to form a 3D object in layers. The extruder temperature is therefore a key parameter for a successful print job but also one of the main emission driving factors as harmful pollutants (e.g., ultrafine particles) are formed by thermal polymer degradation. The awareness of potential health risks has increased the number of emission studies in the past years. However, studies usually refer their calculated emission data to the printer set extruder temperature for comparison purposes. In this study, we used a thermocouple and an infrared camera to measure the actual extruder temperature and found significant temperature deviations to the displayed set temperature among printer models. Our result shows that printing the same filament feedstocks with three different printer models and with identical printer set temperature resulted in a variation in particle emission of around two orders of magnitude. A temperature adjustment has reduced the variation to approx. one order of magnitude. Thus, it is necessary to refer the measured emission data to the actual extruder temperature as it poses a more accurate comparison parameter for evaluation of the indoor air quality in user scenarios or for health risk assessments.
Self-healing agents have the potential to restore mechanical properties and extend service life of composite materials. Thermoplastic healing agents have been extensively investigated for this purpose in epoxy matrix composites due to their strong adhesion to epoxy and their ability to fill in microcracks. One of the most
investigated thermoplastic additives for this purpose is poly(ethylene-co-methacrylic acid) (EMAA). Despite the ability of thermoplastic healing agents to restore mechanical properties, it is important to assess how the addition of thermoplastic healing agents affect properties of the original epoxy material. In this work, EMAA was added to epoxy resin and the effect of the additive on fracture toughness of epoxy was evaluated. Results indicate that although added in low concentrations, EMAA can affect fracture toughness.
The hard X-ray beamline BAMline at BESSY II (Berlin, Germany) has now been in service for 20 years. Several improvements have been implemented in this time, and this review provides an overview of the imaging methods available at the BAMline. Besides classic full-field synchrotron X-ray computed tomography (SXCT), also absorption edge CT, synchrotron X-ray refraction radiography (SXRR), and synchrotron X-ray refraction tomography (SXRCT) are used for imaging. Moreover, virtually any of those techniques are currently coupled in situ or operando with ancillary equipment such as load rigs, furnaces, or potentiostats. Each of the available techniques is explained and both the current and the potential usage are described with corresponding examples. The potential use is manifold, the examples cover organic materials, composite materials, energy-related materials, biological samples, and materials related to additive manufacturing. The article includes published examples as well as some unpublished applications.
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).
Al-Si alloys produced by Laser Powder Bed Fusion (PBFLB) allow the fabrication of lightweight free-shape components. Due to the extremely heterogeneous cooling and heating, PBF-LB induces high magnitude residual stress (RS) and a fine Si microstructure. As the RS can be deleterious to the fatigue resistance of engineering components, great efforts are focused on understanding their evolution in as-built state (AB) and after post-process heat treatments (HT). RS in single edge notch bending (SENB) subjected to different HT are investigated (HT1: 1h at 265°C and HT2: 2h at 300°C).
The electron backscatter diffraction (EBSD) technique is used to investigate the dislocation structures formed after steady-state creep deformation of an Al-3.85%Mg alloy. This material is crept at two different stress levels, corresponding to the so-called power-law and power-law breakdown regimes. The results show that, regardless of the creep stress level, the strain tends to localize, leading to the formation of intragranular bands. The thickness of such bands is larger when the material is tested at loads corresponding to the power-law breakdown. This suggests enhanced diffusion by dislocation pipes.
Metastable austenitic stainless steel (304L) samples with a rectangular cross-section were plastically deformed in torsion during which they experienced multiaxial stresses that led to a complex martensitic phase distribution owing to the transformation induced plasticity effect. A three-dimensional characterization of the phase distributions in these cm-sized samples was carried out by wavelength-selective neutron tomography. It was found that quantitatively correct results are obtained as long as the samples do not exhibit any considerable preferential grain orientation. Optical microscopy, electron backscatter diffraction, and finite element modeling were used to verify and explain the results obtained by neutron tomography. Altogether, neutron tomography was shown to extend the range of microstructure characterization methods towards the meso- and macroscale.
Performance of calcium phosphate cements in the augmentation of sheep vertebrae - An ex vivo study
(2021)
Oil-based calcium phosphate cement (Paste-CPC) shows not only prolonged shelf life and injection times, but also improved cohesion and reproducibility during application, while retaining the advantages of fast setting, mechanical strength, and biocompatibility. In addition, poly(L-lactideco-glycolide) (PLGA) fiber reinforcement may decrease the risk for local extrusion. Bone defects (diameter 5 mm; depth 15 mm) generated ex vivo in lumbar (L) spines of female Merino sheep (2–4 years) were augmented using: (i) water-based CPC with 10% PLGA fiber reinforcement (L3); (ii) Paste-CPC (L4); or (iii) clinically established polymethylmethacrylate (PMMA) bone cement (L5). Untouched (L1) and empty vertebrae (L2) served as controls. Cement performance was analyzed using micro-computed tomography, histology, and biomechanical testing. Extrusion was comparable for Paste-CPC(-PLGA) and PMMA, but significantly lower for CPC + PLGA. Compressive strength and Young’s modulus were similar for Paste-CPC and PMMA, but significantly higher compared to those for empty defects and/or CPC + PLGA. Expectedly, all experimental groups showed significantly or numerically lower compressive strength and Young’s modulus than those of untouched controls. Ready-to-use Paste-CPC demonstrates a performance similar to that of PMMA, but improved biomechanics compared to those of water-based CPC + PLGA, expanding the therapeutic arsenal for bone defects. O, significantly lower extrusion of CPC + PLGA fibers into adjacent lumbar spongiosa may help to reduce the risk of local extrusion in spinal surgery.
This study addressed a 7017 Al-alloy tailored for powder bed fusion – laser beam (PBF-LB) process. The alloy was prepared by mixing 3 wt% Zr and 0.5 wt% TiC powder to standard pre-alloyed 7017 grade aluminium powder. This made printing of the alloys possible avoiding solidification cracking in the bulk and achieving high relative density (99.8 %). Such advanced alloys have significantly higher Young’s modulus (>80 GPa) than conventional Al-alloys (70–75 GPa), thus making them attractive for applications requiring high stiffness. The resulting microstructure in as-printed condition was rich in particles originating from admixed powders and primary precipitates/inclusions originating from the PBF-LB process. After performing a T6-like heat treatment designed for the PBF-LB process, the microstructure changed: Zr-nanoparticles and Fe- or Mg/Zn- containing precipitates formed thus providing 75 % increase in yield strength (from 254 MPa to 444 MPa) at the cost of decreasing ductility (∼20 % to ∼9 %). In-situ tensile testing combined with SXCT, and ex-situ tensile testing combined with fracture analysis confirmed that the fracture initiation in both conditions is highly dependent on defects originated during printing. However, cracks are deflected from decohesion around Zr-containing inclusions/precipitates embedded in the Al-matrix. This deflection is seen to improve the ductility of the material.