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The combination of microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on porous material properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of porosity in ceramics.
Moreover, I will show how not-so-novel 2D characterization techniques, based X-ray refraction, can allow a great deal of insights in the damage evolution in microcracked (and porous) ceramics. I will show how X-ray refraction can detect objects (e.g. microcracks) below its own spatial resolution.
Finally, I will discuss the link between the microstructural findings and the mechanical properties of porous microcracked ceramics.
Additive Manufacturing (AM) in terms of laser powder-bed fusion (L-PBF) offers new prospects regarding the design of parts and enables therefore the production of complex structures. The quality of the feedstock material receives increasing attention, as it depicts the first part of the L-PBF process chain. The powder quality control in terms of flowability and powder bed packing density is therefore mandatory.
In this work, a workflow for quantitative 3D powder analysis in terms of particle size, particle shape, particle porosity, inter-particle distance and packing density was established. Synchrotron computed tomography (CT) was used to correlate the packing density with the particle size and particle shape for three different powder batches. The polydisperse particle size distribution (PSD) was transformed into a statistically equivalent bidisperse PSD. The ratio of the small and large particles helped to understand the powder particle packing density. While the particle shape had a neglectable influence, the particle size distribution was identified as major contributor for the packing density.
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).
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 focus of the presentation focus will be on 3D imaging by means of X-ray Computed Tomography (XCT) at the lab and at synchrotron, and the non-destructive residual stress (RS) characterization by diffraction of additively manufactured (AM) materials in BAM (Berlin, Germany). The manufacturing defects and high RS are inherent of AM techniques and affect structural integrity of the components. Using XCT the defects size and shape distribution as well as geometrical deviations can be characterized, allowing the further optimization of the manufacturing process. Diffraction-based RS analysis methods using neutron and synchrotron X-rays at large scale facilities offer the possibility to non-destructively spatially resolve both surface and bulk RS in complex components and track their changes following applied thermal or mechanical loads.
The overview of the activity of group 8.5 Micro-NDT (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The research of our group is focused on the 3D imaging of AM materials by means of X-ray Computed Tomography at the lab and at synchrotron, and the residual stress characterization by diffraction (nondestructive technique).
Absorption edge tomography, also known as differential tomography at absorption edges, is a method which exploits the sudden change of the attenuation coefficient, when the photon energy crosses the absorption edge of an element. Synchrotron radiation is the best source for absorption edge tomography, because of its small bandwidth, high intensity and easily adjustable photon energy. The synchrotron beamline BAMline at the synchrotron radiation facility BESSY II in Berlin, which is operated by the Bundesanstalt für Materialforschung und -prüfung (BAM), provides a monochromatized beam in a photon energy range from 5 keV up to 80 keV with a bandwidth of 2%, when the double multilayer monochromator is used. Together with the microtomography setup, this enables differential tomography with submicron resolution at the K edge of the elements from chromium up to the lanthanides, and up to uranium, when the L edges are used as well.
In this work, metal organic frameworks (MOFs) embedded in polymer are characterized using differential tomography. MOFs are microporous structures of metal ions, coordinated by organic linker molecules, that can be used in a broad field of applications, especially in gas storage and catalysis. In this work, polymer embedded MOFs were extruded into filaments, which could be used for 3d-printing to profit from the specific properties of the MOFs in polymeric materials combined with the arbitrary shapes provided by 3d-printing. For the extrusion, different polymer classes like ABS, polyester- and polyetherurethanes, as well as different MOFs (ZIF-8, ZIF-67, HKUST-1) were used to create MOF containing filaments with a nominal diameter of 3.0 mm. Differential tomography at the edges of the Zn, Co, and Cu was then used to find the distribution of the corresponding MOF in the filament and to analyze the shape of the inclusions.
A paradigm shift in the description of creep in metals can only occur through multi-scale imaging
(2022)
The description of creep in metals has reached a high level of complexity; fine details are revealed by all sorts of characterization techniques and different theoretical models. However, to date virtually no fully microstructure-driven quantitative description of the phenomenon is available. This has brought to interesting inconsistencies; the classic description of (secondary) creep rests on the so-called power law, which however: a- has a pre-factor spanning over 10 orders of magnitude; b- has different reported exponents for the same material; c- has no explanation for the values of such exponents.
Recently, a novel description (the so-called Solid State Transformation Creep (SSTC) Model) has been proposed to tackle the problem under a different light. The model has two remarkable features: 1- it describes creep as the accumulation of elementary strains due to dislocation motion; 2- it predicates that creep is proceeding by the evolution of a fractal arrangement of dislocations. Such description, however, needs a great deal of corroborating evidence, and indeed, is still incomplete.
To date, we have been able to observe and somehow quantify the fractal arrangement of microstructures through Transmission Electron Microscopy (TEM), observe the accumulation of dislocations at grain boundaries by EBSD-KAM (Electron Back-Scattered Diffraction-Kernel Angular Misorientation) analysis, quantify the kinetic character (solid state transformation) of experimental creep curves, and estimate the sub-grain size of the fractal microstructure through X-ray refraction techniques. All pieces of the mosaic seem to yield a consistent picture: we seem being on the right path to reconstruct the whole elephant by probing single parts of it. What is still missing is the bond between the various scales of investigation.
To date, there are only very few technologies available for the conversion of low temperature waste heat to electricity. In this talk, we first describe the principle of thermomagnetic generators. Then we focus on the impact of topology of the magnetic circuit within thermomagnetic generators. We demonstrate that the key operational parameters strongly depend on the genus, i.e. the number of holes within the magnetic circuit.
To date, there are only very few technologies available for the conversion of low temperature waste heat to electricity. In this talk, we first describe the principle of thermomagnetic generators. Then we focus on the impact of topology of the magnetic circuit within thermomagnetic generators. We demonstrate that the key operational parameters strongly depend on the genus, i.e. the number of holes within the magnetic circuit.
With 8% of man-made CO2 emissions, cement production is an important driver of the climate crisis. By using alkali-activated binders, part of the energy-intensive clinker production process can be dispensed. However, as numerous raw materials are involved in the manufacturing process here, the complexity of the materials increases by orders of magnitude. Finding a properly balanced binder formulation is like looking for a needle in a haystack. We have shown for the first time that artificial intelligence (AI)-based optimization of alkali-activated binder formulations can significantly accelerate research.
The "Sequential Learning App for Materials Discovery" (SLAMD) aims to accelerate practice transfer. With SLAMD, materials scientists have low-threshold access to AI through interactive and intuitive user interfaces. The value added by AI can be determined directly. For example, the CO2 emissions saved per ton of cement can be determined for each development cycle: the more efficient the AI optimization, the greater the savings.
Our material database already includes more than 120,000 data points of alternative binders and is constantly being expanded with new parameters. We are currently driving the enrichment of the data with a life cycle analysis of the building materials.
Based on a case study we show how intuitive access to AI can drive the adoption of techniques that make a real contribution to the development of resource-efficient and sustainable building materials of the future and make it easy to identify when classical experiments are more efficient.
Acoustic Emission
(2018)
Das Phänomen Schallemission (eng. Acoustic Emission, AE) ist eine Begleiterscheinung bei aktiven Mechanismen und Prozessen wie sie in Werkstoffen auftreten, die einer Belastung durch Krafteinwirkung oder durch Änderung der Umgebungsbedingungen ausgesetzt sind. Plastische Verformung, Risswachstum, Korrosion oder der Übergang zu einer anderen Phase generieren u.a. transiente elastische Wellen, die sich im Werkstoff und an der Materialoberfläche ausbreiten. Auftretende Auslenkungen von wenigen hundert Pikometern sind mit piezo-elektrischen AE Sensoren detektierbar. Aufzeichnungsraten von bis zu 40 MHz ermöglichen dabei zeitliche Auflösungen von einigen Nano- bis Mikrosekunden. Die Dechiffrierung der detektierten Informationen ist für die Material- und Versagenscharakterisierung sowie für Anwendungen in der Struktur- oder Prozessüberwachung ein zentraler Forschungsschwerpunkt.
Nach einem kurzen Überblick zu den Grundlagen werden ausgewählte Ansätze der AE Methode vorgestellt und diskutiert:
1) AE Monitoring von Pipelines als Referenzmessung für die Entwicklung eines akustischen faseroptischen Monitorings (AGIFAMOR)
2) Schwellwertfreie AE Messung im 4-Punkt-Rohrbiegeprüfstand BAM_9.1 (AGIFAMOR)
3) Kombination von AE mit Röntgen-Mikrotomografie und die Anwendung der frequenzbasierten Mustererkennung ermöglichen eine Zuordnung von AE und Mechanismen (Ergebnisse aus dem SNSF Projekt Nr. 127'134, Baensch 2014, Diss. ETH No. 22372)
Typically, the near-eutectic Al-Si alloys consist of highly interconnected three-dimensional network of the eutectic Silicon (Si) and intermetallics embedded into Aluminium (Al) matrix. For further improvement of the mechanical properties of such alloys, often, one single ceramic reinforcement phase, e.g. silicon carbide (SiC) or aluminium oxide (Al2O3) in the form of fibres or particles is added. However, hybrid reinforcements (fibres and particles) can further improve wear resistance and fracture toughness, and additionally, reduce anisotropy of the material. The engineering of metal matrix composites (MMC) for specific application requirements benefits from a comprehensive knowledge of the failure behaviour. Therefore, damage evolution under compression was investigated on:
- pure near-eutectic AlSi12CuMgNi matrix alloy
- type I: matrix reinforced with random-planar oriented Al2O3 short fibres (15 vol.%)
- type II: matrix reinforced with random-planar oriented Al2O3 short fibres (7 vol.%) and additional SiC particles (15 vol.%)
The analysis of damage mechanism was carried out in two rather independent but complementary studies. First, selected sister samples of every material were exposed to quasi-static compression (traverse control). The compression tests were interrupted at different strain levels. Miniature cylinders with a diameter of 1mm were extracted from the pre-strained samples and investigated by synchrotron computed tomography (SX-µCT) with a spatial resolution of about 0.7 µm. For the pure matrix alloy, microcracks are confined to the intermetallic particles and to the eutectic Si, hence no damage was observed in the Aluminium. The composite type II revealed a more effective strain accumulation (less damage) than type I at low plastic strain (up to 5 %), but a more catastrophic damage development due to cracking of the SiC clusters at higher strain levels.
The second approach to study the damage initiation and accumulation in the materials subjected to compressive load was Acoustic Emission (AE) analysis. In this case the in-situ monitoring of the acoustic emission signal was performed during compression tests on specimens with dimension of several mm. For all three material types, AE activity set at 2% strain. Differences in AE behaviour of the three materials was proven based on AE hitrate, signal peak amplitudes as well as weighted peak frequencies (WPF). Future work focuses on combination of AE and SX-µCT aiming for more detailed knowledge on damage mechanism of metal matrix composites.
Acoustic emission testing
(2018)
Es wird ein Verfahren zur Charakterisierung der Beständigkeit und Langzeitstabilität von additiv gefertigten Kunststoff-Bauteilen vorgestellt. Dabei sollen die Prüfkörper über 2000 Stunden künstlich bewittert und währenddessen die Änderungen der Eigenschaften der Bauteile zerstörungsfrei untersucht werden. Die Erkenntnisse dienen für die Entwicklung einer Strategie für eine Qualitätskontrolle von additiv gefertigten Kunststoffteilen.
Es wird ein Verfahren zur Charakterisierung der Beständigkeit und
Langzeitstabilität von additiv gefertigten Kunststoff-Bauteilen vorgestellt. Dabei sollen die Prüfkörper über 2000 Stunden künstlich bewittert und währenddessen die Änderungen der Eigenschaften der Bauteile zerstörungsfrei untersucht werden.
Direct energy deposition additive manufacturing technologies that utilize an electric arc have great potential for generating large volume metal components. However, selecting process parameters that yield the desired near net shape design and requested mechanical component behavior is not a trivial task due to the complex relationship between all process parameters and material characteristics. This presentation exemplifies the application of a newly developed solid welding wire doped with TiB to enhance grain refinement in the deposited metal for additive manufacturing based on DED-Arc of high-strength precipitation hardening AlMgSi-aluminum alloys. It is worth noting that the solid wire is the result of our preliminary metallurgical studies on grain refinement in aluminum weld metal.
Consequently, research focuses on the correlation between process parameters and component quality to understand the underlying mechanisms. This is crucial for evaluating a robust process parameter space that yields component quality in line with corresponding standards which are mainly taken from welding technology.
Specifically, we examine component quality by analyzing pore size and distribution, as well as grain morphology. To enhance the mechanical properties of the deposited metal, a post-weld heat treatment was conducted, comprising of solution treatment, quenching, and artificial aging. The study also evaluates the effects of various heat treatment strategies on the final mechanical properties of the material.
To demonstrate the applicability of 3D metal printing of high-strength aluminium alloys, a more complex demonstrator was created. It has been shown that DED-Arc can produce high-volume aluminium parts with the same quality as the corresponding subtractive processing strategy.
Additionally, the entire additive manufacturing chain has been digitally integrated, enabling traceability of all relevant process steps, which is essential for reliable subsequent quality assessment.
Austenitic stainless steel welds as well as dissimilar metal welds with nickel alloy filler material, used in safety relevant parts of nuclear power plants, still challenge the ultrasonic inspection. The weld material forms large oriented grains which lead on the one hand to high sound scattering and on the other hand – to inhomogeneity and to the acoustic anisotropy of the weld structure. The ultrasonic wave fronts propagate not linearly, as in ferritic weld joints, but along the curves, which depend on the specific grain structure of the weld. Due the influence of these phenomena, it is difficult to analyze the inspection results and to classify the ultrasonic indications, which could be both from the weld geometry and from the material defects. A correct flaw sizing is not possible.
In an ongoing research project, different techniques to improve the reliability of ultrasonic testing at these kinds of welds are investigated. In a first step (in the previous research project) two ultrasonic inspection techniques were developed and validated on plane test specimens with artificial and realistic flaws. In the ongoing project, these techniques are applied to circumferential pipe welds with longitudinal and transverse flaws.
The technique developed at the Federal Institute for Materials Research and Testing (BAM) in Germany uses a combination of ray tracing and synthetic aperture focusing technique (SAFT). To investigate the unknown grain structure, the velocity distribution of weld-transmitting ultrasound waves is measured and used to model the weld by ray tracing.
The second technique, developed at the Fraunhofer Institute for Nondestructive Testing (IZFP) in Germany, uses Sampling Phased Array (Full Matrix Capture) combined with the reverse phase matching (RPM) and the gradient elastic constant descent algorithm (GECDM). This inspection method is able to estimate the elastic constants of the columnar grains in the weld and offers an improvement of the reliability of ultrasonic testing through the correction of the sound field distortion. The unknown inhomogeneity and anisotropy are investigated using a reference indication and the special optimization algorithm.
Both reconstruction techniques give quantitative inspection results and allow the defect sizing. They have been compared to conventional ultrasonic testing with techniques, which are state of the art for components in nuclear power plants. The improvement will be quantified by the comparison of the probability of detection (POD) of each technique.
Laser powder bed fusion (LPBF) is an additive manufacturing process for materials which inherently tends to yield various degrees of metastable hierarchical microstructures, defects and high residual stresses in the as-built condition depending on the process parameters. The understanding of the evolution of these typical features during heat treatment and subsequent thermal and mechanical ageing is crucial for the wider acceptance for safety critical structures. A multi-disciplinary research project at BAM studying the development of the microstructure, defects, residual stresses typical of LPBF 316L and their evolution during thermal and mechanical ageing has led to insights into the stability of these inherent features. This presentation aims to give a broad overview of the project with a few specific cases of investigation. Firstly, the formation of residual stresses, the nature of the initial microstructure, the tensile properties and a modelling approach to understand the anisotropy will be presented. This will be followed by examples of studies of their evolution during heat treatment, long term thermal exposure, and room temperature and high temperature mechanical testing compared to a baseline of conventional wrought variant of the same alloy.
An overview of the BAM funed Focus Area Materials Project "AGIL" will be presented. AGIL focussed on the stdiy of the ageing characteristics of additively manufactured austenitic stainless steel with a "powder to mechanical failure" Approach. Recent Highlights are presented and a perspective for future studies.