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Sustainable product policy is one pillar of the European Green Deal and the Circular Economy Action Plan. The European Commission is to begin to address recycling, recycled content and repair under the Ecodesign Directive and very likely in the announced European Sustainable Products Regulation. In addition, initiatives on recyclability and other aspects of sustainable products can be observed in France under the Ecomodulation Approach for some electrical and electronic products. Neither the Commission's ambitions nor the Ecomodulation Approach have so far led to a crucially better ecodesign of products.
Therefore, at the EU level, indices for reparability (already developed for smartphones and tablets), recyclability and recycled content of products are being discussed within the Ecodesign legislative framework in an attempt to achieve better ecodesign through advanced consumer purchasing decisions. The product standards requested by the European Commission to assess the recyclability (EN4555) and recycled content (EN4557) of energy-related products have already been published, but are purely based on a mass-based approach. Material-specific aspects such as the environmental impact or the financial, technical and redesign efforts required by manufacturers to facilitate the recycling and use of recycled materials are not addressed. Materials that are easy to recycle and use and have a high recycled content, such as copper, are treated in the same way as plastics that are difficult to recycle and use in products as post-consumer recycled plastics. Including such aspects would be essential to trigger environmentally relevant and significant improvements in product design.
Der Vortrag fasst die Schnittmenge zwischen Normung und Politik bezüglich einer zirkulären Wirtschaft (Circular Economy) zusammen. Es wird an konkreten Schlüsselgremien und praktischen Beispielen gezeigt, wie Circular Economy bereits heute durch Normung gelingen kann und welche Zuarbeit durch die Politik von den Normungsgremien erbeten wird.
With the continuous release of anthropogenic pollutants into the environment, substantial risks for the human health arise. Concerning are especially persistent substances (e.g., PFAS) as they accumulate in food chains which inevitably result in the transgression of negative impact threshold levels. Environmental Analytical Chemsitry interfaces all disciplines of Risk Assessment. Therefore it is the important tool to identify, monitor, and remediate environmental pollutants. Based on the example of PFAS, a workflow to tackle environmental pollutants in a retro- and pro-spective way is shown. Within the project, the worldwide situation of environmental pollutants will be illustrated for the example of PFAS. As the major discipline to confront the problem, analytical chemistry will be shown as a key tool for contesting PFAS and creating safe-by-design materials in the future.
Ellipsometry is a highly valuable technology for bridging different measurement methods. As a fast, highly sensitive, and non-destructive optical technique with low environmental requirements, it is ideal for transporting measurement accuracy and for up-scaling measurements in the production environment. It can be used for highly precise determination of properties, material identity and correctness confirmation, as well as defect detection.
Comparable, traceable, and accurate electrical measurements, especially at small scales are one of the biggest challenges in the development of the electrical and electronic devices of the future.
In this project, we develop structured thin layer systems of the transparent conductive material indium tin oxide (ITO) to prove the concept of using these systems as standards for conductivity and permittivity. The layers are produced in a reactive magnetron sputtering process from raw ITO targets with additional oxidation achieved by oxygen injection. We present results of a study correlating the coating process conditions with the properties of the final layer material. We found that especially the temperature development during coating is of key importance and determines the layer properties to a large extent. We will discuss questions of homogeneity and reproducibility of the coating processes used. The finished layers undergo lithographic structuring and etching to produce patterns to serve as reference structures for scanning probe electrical measurements. TCOs have a large variety of applications. In this work we also study the usability of ITO for other purposes and investigate the stability of this material under application conditions.
The combination of non-target analysis (NTA) based on HPLC-ESI-MS with elemental fluorine speciation analysis based on HPLC-PARCI-MS for the identification and quantification of (unknown) organofluorines in environmental samples is associated with several advantages e.g., reduced non-target data treatment workflow and quantification.
PFASs compromise persistent, bioaccumulative, and toxic properties and are hence, environmental contaminants of emerging concern. Thus, procedures for identifying potential sources of the entrance of these compounds into the environment, identification of new organofluorine species, and closing mass balances need urgent development. The intrinsic fluorine tag appears in a sizable fraction of these and other xenobiotics, making elemental speciation desirable for quantitative NTA in these areas. Current non-target approaches based on ESI-HRMS suffer from a lack of data mining algorithms for identification of PFASs with low fluorine mass percentages. Furthermore, low ionization efficiencies of the compounds hamper detection limits.
Hence, the proposed combination of simultaneous HPLC-ESI-MS and HPLC-PARCI-MS via split-stream coupling is a promising approach for environmental PFAS monitoring. Furthermore, it could serve as an important analytical procedure to set up limiting values in compliance with the desired PFAS ban of the European Union.
Die Bundesanstalt für Materialforschung und -prüfung (BAM) ist eine forschende Bundesoberbehörde und Einrichtung der Ressortforschung der Bundesrepublik Deutschland. Unter ihrer Leitlinie „Sicherheit in Technik und Chemie“ ist sie zuständig für die öffentliche technische Sicherheit und für metrologische Aufgaben in der Chemie. Das Aufgabenspektrum der BAM, das sich an aktuellen Fragestellungen aus Wissenschaft, Wirtschaft, Politik und Normung orientiert, bietet sehr viele interessante Tätigkeitsfelder für Naturwissenschaftler*Innen und Ingenieur*Innen.
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.
Understanding the fundamentals of bioreceptivity enables the developement of functionalized materials. Concrete as the most used building material worldwide is of special interest as microbially greened panels may represent an alternative to classic façade greening with plants.
As standards are not ye established, material characterization in context as well as bioreceptivity assessment itself has been proven to be difficult. The presentation reviews first results of methods adapted for this application.
Monopile-Gründungen sind die mit Abstand am häufigsten verwendete Gründungskonstruktion für Offshore-Windenergieanlagen. Ein wesentliches Problem bei der Bemessung ist das lokale Beulen des Gründungspfahls, welches typischerweise im Bereich der Bettung auftritt. Aufgrund der Nichtlinearität der Bettungsrandbedingung sind klassische Bemessungsansätze nicht anwendbar, so dass der Bemessungsingenieur auf eine vollständig numerische Berechnung zurückgreifen muss. In diesem Vortrag wird eine experimentelle Versuchskampagne zur Erzeugung von Kalibrierungsdaten für solche numerischen Modelle vorgestellt. Eine ausführlichere Darstellung findet sich im gleichnamigen Artikel.
Die additive Fertigung (AM) durch schweißtechnische Verfahren eröffnet vielfach ökonomische Vorteile für eine ressourceneffiziente Bauteilherstellung. Gerade hinsichtlich der Homogenität und Anisotropie der resultierenden Schweißgefüge und den damit verbundenen Eigenschaften gibt es noch offene Fragestellungen. Die Einstellung der finalen Bauteilgeometrie und Oberflächengüte erfordert den komplementären Einsatz abtragender Fertigungsschritte. Hochleistungslegierungen auf der Basis von Nickel oder Kobalt sind aufgrund ihrer niedrigen Wärmeleitfähigkeit verbunden mit hoher Festigkeit und Zähigkeit schwer spanbar. Eine gezielte Gefügebeeinflussung mittels Modifikation der AM-Schweißzusatzwerkstoffe und der Einsatz des ultraschallunterstützten Fräsens (US) bietet das Potential insgesamt die Zerspanungssituation zu verbessern. Dieser Lösungsansatz unter Gewährleistung des Erhalts der geforderten Werkstoff- bzw. Bauteileigenschaften ist Untersuchungsgegenstand eines Gemeinschaftsvorhabens (IGF-Nr. 20.979 N/DVS-Nr. 1.3211) der BAM und TU Clausthal/ISAF. Der vorliegende Beitrag stellt Ergebnisse für die beiden untersuchten FeNi- und CoCr-Legierungen sowie wesentliche Zusammenhänge zwischen Legierungsmodifikation, entstehender Gefügemorphologie und Zerspanungseigenschaften der mittels MAG additiv gefertigter Proben vor. Das größte Potential für die Modifikation zeigten Zr und Hf. Die Zulegierung in das Schweißgut erfolgte durch Beschichtung von Massivdrähten sowie durch Herstellung von Fülldrähten.
Knowing phonon properties is beneficial for predicting low thermal conductivity thermoelectric materials. Employing DFT consumes lots of computational resources. Using ML-driven interatomic potentials (MLIP, e.g., GAP) opens up a faster route, but most potentials are specifically tailored to a certain compound. We aim to generalize the MLIP generation in a Python code-based workflow, combining automatic DFT runs with automated GAP fits. Automation enables easier tests, benchmarks, and validation.
Argyrodite-type materials have lately sparked a lot of research interest due to their thermoelectric properties. One promising candidate is canfieldite (Ag8SnS6), which has a Pna21 orthorhombic crystal structure at room temperature (RT). Recently, experimentalists have found a new low-temperature (LT) phase transition of canfieldite at 120K. Therefore, we investigate structural, vibrational and thermodynamic properties of Ag8SnS6 at room- and low-temperature employing density-functional theory (DFT) and lattice dynamics computations. Thermal properties calculations were based on the quasi-harmonic approximation (QHA) as implemented in phonopy. We achieve good agreement with experiments. Lattice parameters were overestimated by 2%, and thermal properties such as the constant-pressure heat capacity Cp are very close to experimental measurements. Our simulations also reveal a possible new phase transition at around 312 K. Furthermore, we compared RT and LT Ag8SnS6 Grüneisen parameters with some argyrodites analogues, Ag8TQ6 (T = Si, Ge, Ti and Sn; Q = S, Se), finding a relationship between the anharmonicity and low thermal conductivity.
Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material that exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). Therefore, it can be used to create composites with controllable expansion coefficients and prevent thermal stress, fatigue, cracking, and deformation at interfaces. We implement interdisciplinary research to analyze such material. We study the influence of the synthesis methods and their parameters on the sample's purity, crystallinity, and homogeneity. Moreover, we implement ab initio-based vibrational computations with partially treated anharmonicity in combination with experimental methods to follow temperature-induced structural changes and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder.
Through a hybrid use of Low Transforamtion Temperature welding filler, fatigue strength of welds should be increased. Through the hybrid use of LTT welding filler the Integrity of a weld will be less affected. By creating several variants of LTT weld geometries an idea of the optimum residual stress reduction is given.
Bewertung der Innenhydrophobierung als neuartige AKR-Vermeidungsstrategie bei Betonfahrbahndecken
(2023)
Zur Vermeidung von AKR-Schäden an Betonfahrbahndecken im deutschen Autobahnnetz wurden mit dem ARS 04/2013 verbindliche Eignungsprüfungen zum Ausschluss alkaliempfindlicher Gesteinskörnungen bei Neubau- und Erhaltungsmaßnahmen eingeführt. Das hatte eine signifikante Reduzierung geeigneter Gesteinskörnungen zur Folge. Deshalb wird geprüft, ob durch die Zugabe eines Hydrophobierungsmittels während der Betonherstellung grenzwertig alkaliempfindliche Gesteinskörnungen nutzbar gemacht werden können. In diesem Beitrag wird der Einfluss der Dosierung eines Compounds mit Hydrophobierungsmittel (HM) auf die Frisch- und Festbetoneigenschaften eines Waschbetons mit einer reaktiven Grauwacke dargestellt. Es zeigt sich, dass aufgrund des Antagonismus die zunehmende Dosierung des HM-Compounds eine signifikante Erhöhung der Zugabe des Luftporenbildners auf Wurzelharzbasis erfordert. Der AKR-Schädigungsprozess wird ab einer Dosierung des HM-Compounds von 0,75 M.-%, bezogen auf den Zementgehalt, hinreichend vermindert. Die mechanischen Eigenschaften des hydrophobierten Waschbetons verschlechtern sich im betrachteten Dosierungsbereich des HM-Compounds nur geringfügig. Auch der Frost-Tausalz-Widerstand vermindert sich, ohne den normativen Grenzwert für die Abwitterung zu überschreiten.
Mikrolegierungselemente, wie Nb und Ti, sind für die signifikante Festigkeitssteigerung von vergüteten, hochfesten Feinkornbaustählen mit einer Nominalstreckgrenze ≥ 690 MPa unerlässlich. Normvorgaben zur chemischen Zusammensetzung geben dabei nur obere Grenzwerte für die Hersteller vor. Weiterhin wirken sich bereits kleine Abweichungen in der Legierungsroute teilweise drastisch auf die mechanischen Eigenschaften aus. Somit wird eine adäquate Vorhersage der Schweißeignung und der Integrität der Schweißverbindung aufgrund der variierenden Mikrogefüge erschwert bis unmöglich. Unerwünschte Nebeneffekte sind die mögliche Erweichung der Wärmeeinflusszone (WEZ) als auch der gegenteilige Effekt der Aufhärtung. Vor diesem Hintergrund werden erstmals systematisch die unterschiedlichen Mikrolegierungsrouten mit variierenden Ti- und Nb-Gehalten an Versuchsschmelzen untersucht. Die Stahlgüte S690QL bildet dabei die Grundlage der chemischen Zusammensetzung sowie der entsprechenden Wärmebehandlung. Zur Untersuchung der jeweiligen Schweißeignung wurden Dreilagen-Schweißungen mittels moderner MAG-Hochleistungsschweißprozesse durchgeführt und kritische Gefügebereiche mit hoher Erweichung/Aufhärtung identifiziert. Mechanisch-technologische Untersuchungen zur Kerbschlagzähigkeit mittels Kerbschlagbiegeversuchen durchgeführt wurden, bestätigen dabei die Ergebnisse der thermodynamischen Simulation bezüglich des Ausscheidungsverhaltens während der Temperatur-Zeit Schweißzyklen. Daraus lässt sich der Einfluss der Wärmeeinwirkung beim Schweißen auf die Gefügeausbildung in der WEZ und der korrespondierenden mechanischen Eigenschaften qualitativ beschreiben.
Digital Calibration Certificates: Transforming Efficiency and Safety in Hydrogen Refuelling Station
(2023)
Digital Certificates have emerged as a pivotal element in automation and digitalisation. This presentation highlights the added value of a digitalised metrology, its impact on the workflows on the calibration service providing and receiving side as well as their significance in enhancing the quality infrastructure. An overview of digital calibration certificates (DCC) for temperature sensors, including their structure and role in establishing trust in hydrogen refuelling stations (HRS), will be discussed. Additionally, it explores the impact of DCC on optimising efficiency in the hydrogen refuelling process.
Exploring the paradigm shift brought about by Industry 4.0, where machines possess the ability to autonomously interpret digital certificate data, leads to streamlined safety checks and reduced human intervention. We will discuss how automated verification of machine-readable certificates contributes to maintaining and elevating safety standards over human-readable certificates. Furthermore, we will take a deep dive into the application of DCCs in HRS, showcasing how they enhance operational efficiency, accuracy, and maintenance by enabling real-time monitoring and adjustment of process data.
By exploring the interdependent relationship between digital certificates, machine-readable environments, and HRS optimisation, this presentation will provide valuable insights into harnessing cutting-edge technologies to create a safer, more efficient, and technologically empowered hydrogen refuelling process.
Per- and polyfluoroalkyl substances (PFAS) are chemicals which were developed to improve humanity’s quality of life. Due to their high chemical stability and resistance to degradation by heat or acids, PFAS were used in a variety of consumer products. The continuous use of PFAS in household products and the discharge of PFAS from industrial plants into the sewer system resulted in the contamination of effluents and sewage sludge from wastewater treatment plants (WWTPs) (Roesch et al. 2022). Since sewage sludge is often used as fertilizer, its application on agricultural soils has been observed as a significant entry path for PFAS into the environment, specifically in our food chain. In Germany the sewage sludge/biosolid application on agricultural land was banned with the amendment of the German Sewage Sludge Ordinance and by 2029 sewage sludge application will be totally prohibited. However, phosphorus (P) from sewage sludge should still be recycled in WWTPs of cities with a population larger than 50,000 residents. To produce high-quality P-fertilizers for a circular economy, PFAS and other pollutants (e.g. pesticides and pharmaceuticals) must be separated from sewage sludge. Due to the strong diversity of industrial PFAS usage it is not clear if a safe application of novel recycled P-fertilizers from WWTPs can be guaranteed. Therefore, we analyzed various sewage sludges and wastewater-based fertilizers. Sewage sludge (SL) samples from various WWTPs in Germany and Switzerland, six sewage sludge ashes (SSA) from Germany, six thermally treated SL and SSA samples with different additives (temperatures: 700-1050 °C), two pyrolyzed SL samples (temperature: 400 °C) and two struvite samples from Germany and Canada were analyzed. The goal was to quantify PFAS in sewage sludges and wastewater-based P-fertilizers with the sum parameter extractable organic fluorine (EOF) by combustion ion chromatography (CIC). The results were compared with data from classical LC-MS/MS target analysis as well as selected samples by HR-MS suspect screening. The EOF values of the SLs mainly range between 154 and 538 µg/kg except for one SL which showed an elevated EOF value of 7209 µg/kg due to high organofluorine contamination. For the SSA samples the EOF values were lower and values between LOQ (approx. 60 µg/kg) and 121 µg/kg could be detected. For the pyrolyzed SLs no EOF values above the LOQ were detected. Moreover, the two wastewater-based struvite fertilizers contain 96 and 112 µg/kg EOF, respectively. In contrast to the EOF values, the sum of PFAS target values were relatively low for all SLs. Additional applied PFAS HR-MS suspect screening aimed to tentatively identify PFAS that could contribute to the hitherto unknown part of the EOF value. The majority of the detected fluorinated compounds are legacy PFAS such as short- and long-chain perfluorocarboxylic acids (PFCA), perfluorosulfonic acids (PFSA), polyfluoroalkyl phosphate esters (PAPs) and perfluorophosphonic acids (PFPA). Moreover, fluorinated pesticides, pharmaceutical as well as aromatic compounds were also identified, which are all included in the EOF parameter. Our research revealed that the current PFAS limit of 100 µg/kg for the sum of PFOS + PFOA in the German Fertilizer Ordinance is no longer up to date. Since the number of known PFAS already exceeds 10,000, the ordinance limit should be updated accordingly. Recent regulations and restrictions on using long-chain PFAS (≥C8) have resulted in a significant shift in the industry towards (ultra-)short-chain alternatives, and other, partly unknown, emerging PFAS. Ultimately, also fluorinated pesticides and pharmaceuticals, which end up as ultrashort PFAS in the WWTPs, have to be considered as possible pollutants in fertilizers from wastewater, too.
Newly developed methodical approaches with an emphasis on correlative imaging analysis of morphology and chemistry of nanomaterials will be presented. Correlative imaging by high-resolution SEM with STEM-in-SEM as well as with EDS, and further with AFM, or with the new technique TKD (Transmission Kikuchi Diffraction) will be explained on various examples of nanostructures, both as starting materials and as embedded/functionalized nanoparticles in products. The unique analytical benefits of the Auger electron probe as a veritable nano-tool for the local surface chemistry will be highlighted. Examples of hybrid analysis of the bulk of nanomaterials by X-ray Spectroscopy and the highest surface-sensitive methods XPS and ToF-SIMS as advanced surface characterization methods available in the Competence Centre nano@BAM will be showed. Particularly for the spatially resolved analysis of the chemistry of nanostructures, such in-depth and lateral gradients of chemistry within mesoporous thin layers, or the completeness of the shells of core-shell nanoparticles, the latter methods are inherent.
Other dedicated developments like approaches for the quantitative determination of the porosity of thin mesoporous layers by electron probe microanalysis (EPMA) with SEM or the quantitative determination of the roughness of particle surface by high-resolution imaging with electron microscopy will be also presented.
In the course of tomorrow's hydrogen-based energy transition, the construction of the corresponding infrastructure will play a central role. In that context, large diameter long-distance transmission pipelines for hydrogen will be the backbone in the European Union with service pressures from 70 to 90 bar (e.g., depending on national regulations). It is a major goal to rededicate the existing LNG infrastructure despite the necessity of new pipelines. From that point of view repairing of such transmissions pipelines via welding can be necessary. For the LNG infrastructure, it is state of the art that repair welding is conducted at pipelines under service, i.e., the LNG is still flowing as pressurized gas in the steel pipes. The reason is that a shut-down of large diameter pipelines is not so easy or sometimes impossible. In fact, as long no oxygen enters the pipeline, there would be any combustion or (in the worst case) explosion. At the moment, it is entirely open if current repair welding procedures for LNG pipelines can be transferred to pure hydrogen pipelines. In opposite to LNG, hydrogen can be way easier absorbed to the pipeline steels and diffuses through the material. If it accumulates in susceptible regions, i.e., in the welded joint, hydrogen assisted embrittlement could occur. The planned welding procedure requires a so-called preheating and maintenance of the weld joint of up to 300°C for several hours. This temperature is way higher compared to the typical service temperature of max. 40 to 50°C at operational pressures of 100 bar. In accordance to API 941, these low-alloyed pipeline steels are subjected to short-term service loads, which they are not designed for. For that reason, a collaborative project between BAM and DVGW (German Association for Gas and Water professions) was initiated in 2022 to answer the following questions by experiments and numerical simulation of: (1) How many hydrogen is additionally absorbed during the heating of the material to max. 300°C under remaining operational pressures? (2) Is the hydrogen concentration sufficient to reach a critical condition? (3) Which material and weld microstructure is the most susceptible? (4) Is there a significant difference in the repair welding behavior of LNG pipelines that had been already in use for long-term? (5) Which welding parameters and joint dimensions must be ensured for safe repair welding repair of typical pipelines? For that reason, the present study gives an overview on the current practice in repair welding of in-service pipelines, the industrial importance of this topic for the hydrogen-based energy transition and summarizes first results.
Im Rahmen des BMBF-geförderten Forschungsprojekt ReMin - REALight werden in einem Projektteam aus Industriepartnern und Forschungseinrichtungen unter Koordination der Bauhaus-Universität Weimar leichte Gesteinskörnungen aus Bau- und Abbruchabfällen und industriellen Nebenprodukten auf thermischen Weg hergestellt. Die Aufgabe der Bundesanstalt für Materialforschung und -prüfung (BAM) ist es, diese im Drehrohrofen erzeugten Blähgranulate für gebundene Anwendungen in Beton und Mörtel umfassend zu charakterisieren. Gemeinsam mit der Opus Denkmalpflege GmbH wird die Applikation feiner, gebrochener Blähgranulate in leichten Steinergänzungsmörteln für die Restaurierung von Sandsteinobjekten untersucht. Hierzu wird ein zweischichtiges Mörtelsystem bestehend aus Füll- und einem Deckmörtel entwickelt. Erste Ergebnisse der Rezepturentwicklung verschiedener kalkhaltiger Leichtmörtel mit gebrochenen Blähgranulaten werden vorgestellt. Die neuen Leichtmörtel sind hinsichtlich der entwickelten Druckfestigkeit gleichwertig gegenüber herkömmlichen Restauriermörteln.
When reassessing existing concrete bridges, the challenge is often to obtain missing or incomplete information on the internal structure. In particular, the number and position of the existing reinforcement as well as the geometric dimensions of the components are of interest. Non-destructive testing methods, like radar or ultrasound, which work on the basis of the pulse-echo method, have been established for this purpose, as they only require access to the component from one side. The measurement data recorded on the structure require pre-processing to be able to reproduce the internal structure geometrically accurately. Besides different steps of data processing, the geometrical reconstruction of the measured data based on the Synthetic Aperture Focusing Technique (SAFT) is state of the art today. In this paper, the technical possibilities of the ultrasonic echo method are presented based on measurements in the laboratory and on a real bridge structure. The precision of the reconstruction and its limitations are shown. In addition to the state of the art SAFT technique, open questions and the latest research approaches, such as imaging by reverse time migration (RTM) including initial results are discussed.
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 different kind of materials in FB8.5 Micro-NDT BAM. For instance, the manufacturing defects and high RS are inherent of additively manufacturing 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 high corrosion resistance and good mechanical properties of duplex stainless steel (DSS) are due to its special chemical composition, which is a balanced phase ratio of ferrite (α) and austenite (γ). Many industrial applications require the integration of DSS components. For this, tungsten inert gas welding (TIG) is an excellent choice, as it allows an automated operation with high reproducibility. However, when the weld pool solidifies, critical ratios of α- and γ- phases can occur, which leads to solidification cracking, increased susceptibility to corrosion, and a decrease in ductility and critical strength. Previous studies have shown that these defects can be caused by the accumulation of manganese and chromium in the heat affected zone (HAZ), and this accumulation can be detected using LIBS.
Unlike conventional LIBS analyses, which requires reference samples to generate a calibration curve, calibration-free LIBS (CF-LIBS) can determine the chemical composition solely from the emission spectrum of the plasma. Numerous publications show that CF-LIBS is a fast and efficient analytical method for quantitative analysis of metal samples.
We present the results of in situ CF-LIBS analysis during TIG DSS welding. Using a new approach, it is possible to quantitatively determine the chemical composition of the weld metal directly in the welding process. The results of the CF-LIBS analysis are compared with the results of the calibration-based PLS analysis and reasonable agreement is found. Thus, the CF-LIBS method offers the significant advantage of quickly measuring in situ the concentrations of the main alloying elements that prevent the formation of welding defects, without the tedious calibration procedure.
Der MVT-Test ist die an der BAM entwickelte und genutzte Version des Varestraint-Tests der weltweit für die Charakterisierung der Erstarrungsrissanfälligkeit von Schweißzusätzen und Legierungen eingesetzt wird. Die Auswertung solcher Tests erfolgt klassisch unter dem Lichtmikroskop. Durch Automatisierung des Auswerteprozesses mit KI kann der Informationsgehalt des Tests besser ausgeschöpft und eine höhere Vergleichbarkeit zwischen Testergebnissen gewährleistet werden.
This presentation summarizes outcomes of the CUSP projects POLYRISK and PlasticsFatE according to thermoanalytical methods.It highlights the importants of analytical methods to measure physical and chemical properties of the test materials. These informations are neccessary for interpretation of the toxicological test results.
Im Zuge der wasserstoffbasierten Energiewirtschaft von morgen, kommt der Errichtung der dementsprechenden Infrastruktur die zentrale Rolle zu. Der überwiegende Teil bisher eingesetzter und meist geschweißter Werkstoffe, wie Stähle, kann unter bestimmten Bedingungen zur Wasserstoffversprödung neigen. Dies umfasst die klassische verzögerte Kaltrissbildung während der Schweißverarbeitung als auch Versprödungsphänomene während des Betriebs. Für die Bewertung eines jeden Wasserstoffeffektes auf bspw. die mechanischen Eigenschaften eines geschweißten metallischen Werkstoffes, muss der Wasserstoffgehalt präzise bestimmt werden, Im Fall von Schweißnähten ist die beispielsweise nach der ISO 3690, die klassische isotherme Trägergas-Heißextraktion (TGHE). Die TGHE basiert dabei auf der beschleunigten Wasserstoffentgasung aufgrund der thermischen Aktivierung des Wasserstoffs bei erhöhten Temperaturen. Neben der reinen Quantifizierung des Wasserstoffs, kann über die thermische Desorptionsanalyse (TDA) mit variierten Heizraten, der Bindungszustand an mikrostrukturellen Defekten im Material festgestellt und bewertet werden. Für beide Techniken sind experimentelle und messtechnische Einflüsse zu beachten, die großen Effekt auf das Ergebnis haben. Für die TGHE schlägt die ISO 3690 schlägt beispielswiese verschiedene Probengeometrien sowie Mindestextraktionszeiten vor. Die vorliegende Studie fasst Ergebnisse und Erfahrungen zahlreicher Untersuchungen an der Bundesanstalt für Materialforschung und -prüfung (BAM) mit unterschiedlichen Probentemperaturen und Geometrien (ISO 3690 Typ B und zylindrische TDA-Proben) zusammen hinsichtlich: Einfluss der Probenoberfläche (poliert/geschweißt), Messgenauigkeiten in Abhängigkeit des Probenvolumens sowie die unzureichende Überwachung des Effektes des PI-Reglers auf die Extraktionstemperatur. Insbesondere eine abweichende Extraktionstemperatur zur eingestellten Temperatur, kann die Messergebnisse wesentlich verfälschen. Basierend auf den Ergebnissen werden Methoden aufgezeigt, um schnell die gewünschte Extraktionstemperatur zu erreichen, ohne physisch in das Messequipment eingreifen zu müssen. Dies dient der wesentlichen Verbesserung der Zuverlässigkeit der Wasserstoffmessung durch erhöhte Signalstabilität und beschleunigte Wasserstoffdesorption. Im Allgemeinen ist eine unabhängige Temperaturmessung mit Dummy-Proben für die gewählte Heizprozedur angeraten, um mögliche unerwünschte Temperatureinflüsse bereits vor der Messung auszuschließen. Die beschriebenen Methoden können ohne großen Aufwand direkt in die industrielle Anwendung überführt werden.
Multielement-Legierungen (MPEA - Multiple Principal Element Alloys, gemeinhin auch als Hochentropielegierungen bezeichnet) stellen eine neue Klasse von Werkstoffen dar, die aus mindestens drei Legierungselementen mit jeweils 5 bis 35 Atom-% bestehen. Somit unterscheidet sich diese Legierungskonzept fundamental von konventionellen Werkstoffen wie Stahl oder Nickellegierungen. Hierzu werden die Legierungselemente gezielt ausgewählt und die Mikrostrukturen ein- und zum Teil auch mehrphasig eingestellt. Das Ziel ist dabei, hochinnovative MPEA mit individuell einstellbaren Eigenschaften für die industrielle Anwendung zu identifizieren. Dabei werden insbesondere Zielkonflikte, wie bspw. der Trade-off zwischen Festigkeit und Duktilität bei konventionellen Stählen, überwunden. Insbesondere die hohe mechanische Festigkeit bei höchster Korrosionsbeständigkeit sind bei bestimmten Legierungssystemen von hohem Interesse. Hier kann u.a. die Substitution klassischer hochlegierter Stähle oder von Ni-Basislegierungen perspektivisch erfolgen. In den letzten 20 Jahren lag der Fokus jedoch auf der reinen Materialsynthese. Mit der Zunahme verfügbarer Werkstoffquantitäten, stehen Verarbeitungsfragen, wie werkstoff- und beanspruchungsgerechte Füge- bzw. Schweißverfahren jetzt im Mittelpunkt. Der Schweißeignung von MPEA wurde bis Ende 2022 nur äußert wenig Aufmerksamkeit zuteil. Erfahrungen zu Mischverbindungen (sogenannte DMWs - Dissimilar Metal Welds) fehlen dabei vollständig, sind jedoch essenziell für die Anwendung dieser Werkstoffe in Verbindung mit konventionellen Werkstoffen. Die vorliegende Studie präsentiert erstmals im deutschen Sprachraum, die umfassenden experimentellen Ergebnisse zur Schweißeignung von MPEA-Mischverbindungen und der resultierenden Mikrostruktur. Dazu wurden zwei äquiatomare MPEAs CoCrFeMnNi (Hochentropie-) und CoCrNi (Mittelentropielegierung) mittels WIG- und Rührreibschweißen mit einem konventionellen, hochlegierten und austenitischen Cr-Ni-Stahl (1.4301) gefügt. Die erstmals untersuchten DMWs resultierten dabei in sehr interessanten Mikrostrukturen, mechanisch-technologische Eigenschaften wurden durch instrumentierte Zugversuche gewonnen, die gleichzeitig der Ermittlung der lokalen Verformung im Schweißnahtbereich dienten (durch Verwendung der berührungslosen DIC-Digital Image Correlation-Technik). Dabei zeigt sich für beide Schweißverfahren eine Erweichung in der WEZ der MPEAs sowie eine geringfügig verminderte Zugfestigkeit. Durch die Experimente konnte der prinzipielle Nachweis der Schweißeignung der MPEAs für DMWs mit konventionellen Werkstoffen erbracht werden, die auch eine dementsprechende mechanische Beanspruchbarkeit ermöglichen. Dies ermöglicht zielgerichtete weitere Betrachtungen dieser höchst innovativen Werkstoffe.
In the course of tomorrow's hydrogen-based energy transition, the construction of the corresponding infrastructure will play a central role. The majority of materials used to date are typically welded for component fabrication. In that context, steels are widely applied and can be prone to hydrogen embrittlement. For the evaluation of any hydrogen effect on, for example, the mechanical properties of a welded metallic material, the hydrogen content must be precisely determined. According to ISO 3690, carrier gas hot extraction (CGHE) can be used. In addition to the pure quantification of hydrogen, thermal desorption analysis (TDA) with varied heating rates can be used to determine and evaluate the bonding state at microstructural defects in the material. For both techniques, experimental and measurement influences have to be considered, which have a great effect on the result. For CGHE, for example, ISO 3690 suggests different sample geometries as well as minimum extraction times. The present study summarizes results and experiences of numerous investigations with different sample temperatures and geometries (ISO 3690 type B and cylindrical TDA samples) regarding: the influence of the sample surface (polished/welded), measurement accuracies depending on the sample volume. In particular, a deviating extraction temperature to the set temperature, can significantly falsify the measurement results. Based on the results, methods are shown to quickly reach the desired extraction temperature without having to physically interfere with the measurement equipment. This serves to substantially improve the reliability of hydrogen measurement through increased signal stability and accelerated hydrogen desorption. In general, an independent temperature measurement with dummy samples for the selected heating procedure is advisable to exclude possible unwanted temperature influences already before the measurement. In addition (and way more important), the methods described can be transferred directly to industrial applications.
Überblick über die derzeitig wichtigsten additiven Fertigungsverfahren für metallische Werkstoffe in der Industrie (PBF, DED, BJT) und Berücksichtigung der wesentlichen Prozessmerkmale und Nachbearbeitungsschritte. Vorstellung der wichtigsten Defektphänomene und Nennung von Ursachen und Abhilfemaßnahmen.
The phylogeny of the Blattodea boasts a wide degree of sociality spanning from solitary cockroaches to advanced ecosystem-dominating higher termite societies. The emergence of sociality in the termites was associated with the acquisition of a diverse range of social structures and differential expression of specific gene network. Previous work has found evidence for a caste-specific social defence system in termites leading to an immune system that may favour group over individual defence. While preliminary work suggests a correlation between social transitions and a reduction of immune gene family diversity, the lack of available high-quality termite genomes hampers complete knowledge of the true diversity of immune gene evolution across termite phylogeny. Here, we report on the sequencing and assembly of 50 high-quality long-read-based genomes and 180 caste- and sex-specific brain transcriptomes across major termite and cockroach sister-branch lineage. We investigate the diversity and evolutionary history of immune genes across genomes, and the potential gene networks that have evolved with the emergence of termite sociality and some aspect of immune related behaviours.
Adipokinetic hormone (AKH) is a neuropeptide produced in the insect corpora cardiaca that plays an essential role in mobilizing carbohydrates and lipids from the fat body to the hemolymph. AKH acts by binding to a rhodopsin-like G protein-coupled receptor (GPCR), the adipokinetic hormone receptor (AKHR). In this study, we tackle AKH ligand and receptor gene evolution as well as the evolutionary origins of AKH gene paralogues from the order Blattodea (termites and cockroaches). Phylogenetic analyses of AKH precursor sequences point to an ancient AKH gene duplication event in the common ancestor of Blaberoidea, yielding a new group of putative decapeptides. In total, 16 different AKH peptides from 90 species were obtained. Two octapeptides and seven putatively novel decapeptides are predicted for the first time. AKH receptor (AKHRs) sequences from 18 species, spanning solitary cockroaches and subsocial woodroaches as well as lower and higher termites, were subsequently acquired using classical molecular methods and in silico approaches employing transcriptomic data. Aligned AKHR open reading frames revealed 7 highly conserved transmembrane regions, a typical arrangement for GPCRs. Phylogenetic analyses based on AKHR sequences support accepted relationships among termite and cockroach lineages to a large extent, while putative post-translational modification sites do not greatly differ between solitary and subsocial roaches and social termites. This study provides important information not only for AKH and AKHR functional research but also for further analyses interested in their development as potential candidates for biorational pest control agents against invasive termites and cockroaches.
Insecta is one of the most diverse phyla in the animal kingdom, with species living in all types of habitats encountering an even greater diversity of pathogens and parasites. Defence strategies against such harmful threats led to a variety of molecular mechanisms, ecological shifts, and genetic innovations. Gene families underlying the molecular basis of the immune responses have evolved within the boundaries given by the species ecology. Here, we explore the evolution of some emblematic immune gene families throughout the Insecta phylum shedding light on remarkable genetic events such as gene duplication or gene loss. We followed a workflow based on the Hidden Markov model to search for immune genes in 55 high-quality genomes of insects. We highlight the emergence of group defence in social species as an ecological shift that released selection pressure on immune gene families notably in Blattodea. Further, we draw attention to certain gene families and the link between their diversity and the specificities of the species’ microbiota. Overall, we report data on immune gene diversity in insects.
Harnessing near-chromosome level quality genomes to explore the evolution of termite immunity
(2023)
The phylogeny of the Blattodea boasts a wide degree of sociality spanning from solitary cockroaches to advanced ecosystem-dominating higher termite societies. The emergence of sociality in termites was associated with the acquisition of a diverse range of social structures. Previous work has found evidence for a caste-specific social defence system in termites leading to an immune system that may favour group over individual defence. While preliminary work suggests a correlation between social transitions and a reduction of immune gene family diversity, the lack of available high-quality termite genomes hampers complete knowledge of the true diversity of immune gene evolution across termite phylogeny. Here, we report on the sequencing and near-chromosome level assembly of 48 high-quality long-read-based genomes across major termite and cockroach sister-branch lineages. We investigate the diversity and evolutionary history of immune genes across genomes, focusing particular attention on correlations between immune gene evolution and transitions in sociality over termite phylogeny.
Finite element (FE) models are widely used to capture the mechanical behavior of structures. Uncertainties in the underlying physics and unknown parameters of such models can heavily impact their performance. Thus, to satisfy high precision and reliability requirements, the performance of such models is often validated using experimental data. In such model updating processes, uncertainties in the incoming measurements should be accounted for, as well. In this context, Bayesian methods have been recognized as a powerful tool for addressing different types of uncertainties. Quasi-brittle materials subjected to damage pose a further challenge due to the increased uncertainty and complexity involved in modeling crack propagation effects. In this respect, techniques such as Digital Image Correlation (DIC) can provide full-field displacement measurements that are able to reflect the crack path up to a certain accuracy. In this study, DIC-based full field measurements are incorporated into a finite element model updating approach, to calibrate unknown/uncertain parameters of an ansatz constitutive model. In contrast to the standard FEMU, where measured displacements are compared to the displacements from the FE model response, in the force-version of the standard FEMU, termed FEMU-F [1], displacements are applied as Dirichlet constraints. This enables the evaluation of the internal forces, which are then compared to measured external forces, thus quantifying the fulfillment of the momentum balance equation as a metric for the model discrepancy. In the present work, the FEMU-F approach is further equipped with a Bayesian technique that accounts for uncertainties in the measured displacements, as well. Via this modification, displacements are treated as unknown variables to be subsequently identified, while they are allowed to deviate from the measured values up to a certain measurement accuracy. To be able to identify many unknown variables; including constitutive parameters and the aforementioned displacements, the Variational Bayesian technique proposed in [2] is utilized as an approximative technique. A numerical example of a three-point bending case study is presented first to demonstrate the effectiveness of the proposed approach. The parameters of a gradient-enhanced damage material model [4] are identified using noisy synthetic data, and the effect of measurement noise is studied. The ability of the suggested approach on identifying constitutive parameters is then validated using real experimental data from a three-point bending test from [3]. The full field displacements required as input to the inference setup are extracted through a digital image correlation (DIC) analysis of the provided raw images.
Bayesian updating of constitutive laws for Finite Element simulation using full field measurements
(2023)
Developed finite element (FE) models have been recognized as powerful tools for predicting the mechanical behaviour of engineered systems. As a prerequisite, those models need to be improved with respect to various uncertainties; most notably, concerning underlying physics assumptions and unknown parameters. This is very often accomplished by comparing the performance of a model (e.g. the model response) against available data measured from real experiments. Another challenge emerges in doing that, however, which is accounting for uncertainties of measured data. Bayesian methods have been widely considered and utilized as a suitable approach for coping with and quantifying the aforementioned uncertainties. Phenomena like damage - in particular in quasi-brittle materials - introduce further uncertainties due to the complexity underlying the crack propagation of phenomenon. This implies that, the fitting of a numerical model and an associated constitute law that can adequately describe such effects is non-trivial. The standard approach of finite element model updating (FEMU) is therefore modified to account for tracking of the crack propagation, as recorded during an experiment under increasing loading, via full field displacement measurements. The latter are fed as Dirichlet constraints to an available finite element model, leading to the evaluation of force residuals, which quantifies the accuracy of the model. This approach - which is known as FEMU-F (force-version of the standard FEMU) [1] - is here further equipped with a Bayesian technique, which accounts for the measurement uncertainties in the full field displacement. This is achieved by penalizing the discrepancy between the measured displacements and the modeled Dirichlet constraints, where the latter are considered as further unknowns. We specifically employ the Variational Bayesian technique, proposed in [2], as an approximating tool for the estimation of posterior parameters, including displacement variables that are allowed to deviate from the measurements. A Markov chain Monte Carlo (MCMC) is also used for sampling the posterior distribution of the unknown model parameters. The model updating procedure is first demonstrated through a numerically simulated example of threepoint bending, where the parameters of a gradient-enhanced damage material model [4] are identified in accordance with synthetic noisy data (displacements and reaction forces). For the validation, experimental data from a three-point bending test are used, where full field displacements are collected through a digital image correlation (DIC) analysis (raw data taken from [3]). The data is then used for the parameter identification of a gradient damage constitutive law, which is employed as an ansatz model
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.
A steady increase of wind energy infrastructure [1] brings along a challenge of maintaining and operating wind turbines (WT) with its multiple components. Inspection of wind turbine rotor blades (WTB) is an important part of maintaining the overall health and safety of a WT. It involves visually or mechanically examining the blades for signs of damage or wear that could affect their performance and structural integrity of the entire WT. A WTB is a complex structure due to its ever-increasing scale (going beyond 100 m for a 16 MW WT [2]) as well as multi-material construction. Passive infrared thermography offers an alternative to contact- or proximity-based inspection techniques currently in use such as visual inspection performed by technical personnel (using a lift or a drone) and involves looking for signs of damage on the surface of the blades, and ultrasonic testing to detect internal defects. In contrast to active thermography, passive thermography uses the sun as source of heat, instead of conventional heat lamps, flash, or laser. An inspection technique to (semi-autonomously) inspect the WTBs of an operating WT from the ground has been developed [3]. Given the optimum thermal contrast (weather conditions for field measurements), external as well as internal features of the WTB can be visualised with appropriate post-processing. The work presented here is part of an ongoing multi-partner project titled “EvalTherm”: the evaluation of passive thermography as a non-destructive inspection tool of WTBs in operation. In this work, artificial defects representative of realistic defects in glass fibre reinforced plastic (GFRP) WTBs are introduced in out-of-service WTB pieces. These are scanned using X-ray computed tomography to obtain a three-dimensional reconstruction to be used as input for finite-element based thermal simulation using COMSOL Multiphysics. The simulation data is compared with infrared thermal inspection of the same WTB section, in order to compare the effect of thermal contrast caused in certain weather conditions. In addition, the influence of defect characteristics such as defect size, morphology, and location on detectability is investigated. Validated simulation models are used to predict thermal signatures of defects along with the optimal thermal contrast. Such simulation models in combination with weather forecast data can assist operators of wind turbine infrastructure to plan passive thermography inspection without the need of dangerous inspection procedures and associated shutdown of energy production.
Die in den von der BAM anerkannten Prüfstellen für Gefahrgutverpackungen gängigen Schüttwinkel-Messmethoden werden verglichen, anhand der Messung an fünf pulverförmigen oder körnigen Stoffen mit gefährlichen Eigenschaften. Zusätzlich wird die Untersuchung des Einflusses einer unterschiedlichen klimatischen Vorlagerung vorgenommen.
The European Joint Programme on Radioactive Waste Management (EURAD) is working on Spent Fuel Characterization (SFC) in its work package (WP) 8. Inspired by the EURAD activities, the International Atomic Energy Agency (IAEA) established an international Coordinated Research Project (CRP) on SFC. The EURAD WP SFC
participants are collaborating as a team on the IAEA CRP on SFC. The EURAD WP SFC project consists of four tasks. Task 3 investigates the behaviour of nuclear fuel and cladding after discharge. The aim of these activities is to understand and describe the evolution of the cladding-pellet system and its ageing under conditions of extended interim storage, transportation and emplacement in a final disposal system. At a Consultancy Meeting, BAM as contributor to Task 3 presented current results of the failure analysis of irradiated ZIRLO® claddings under conditions of the Ring Compression Test.
This presentation summarizes recent developments within the scope of the national pre-standardization project “ZfPStatik”, which aims to prepare a guideline about NDT-supported structural analyses. The focus is on the purposeful and explicit utilization of geometrical tendon and reinforcement bar positions measured on-site in reliability analysis — shown by means of a prestressed concrete bridge as case study.
To cope with the increase in the manufacturing and operation of wind turbines, wind farm operators need inspection tools that are able to provide reliable information while keeping the downtime low. Current inspection techniques require to stop the wind turbine. This work presents the current progress in the project EvalTherm, in which passive thermography is evaluated as a possible non-destructive inspection tool for operational wind turbine blades (WTBs). A methodology to obtain thermal images of rotating WTBs has been established in this project. However, the quality of the results is heavily dependent on various aspects such as weather conditions, information on the inspected WTB, damage history, etc. In this work, a section of a used WTB is simulated using finite-element modelling (FEM) as well as experimentally tested for evaluating the accuracy of the model. Such a model will provide insight into the potential thermal response of a certain structure (with specific material properties) in given weather (boundary) conditions. The model is able to provide satisfactory predictions of the thermal response of the structure, as well as indicate what thermal contrast(s) result from artificial defects introduced in the structure.
The materials mechanical testing ontology (MTO) was developed by collecting the mechanical testing vocabulary from ISO 23718 standard, as well as the standardized testing processes described for various mechanical testing of materials like tensile testing, Brinell hardness test, Vickers hardness test, stress relaxation test, and fatigue testing. Confirming the ISO/IEC 21838-2 standard, MTO utilizes the Basic Formal Ontology (BFO), Common Core Ontology (CCO), Industrial Ontologies Foundry (IOF), Quantities, Units, Dimensions, and data Types ontologies (QUDT), and Material Science and Engineering Ontology (MSEO) as the upper-level ontologies. Reusing these upper-level ontologies and materials testing standards not only makes MTO highly interoperable with other ontologies but also ensures its acceptance and applicability in the industry. MTO represents the mechanical testing entities in the 230 classes and four main parts: i) Mechanical testing experiments entities like tensile, hardness, creep, and fatigue tests as the subclasses of mseo:Experiment, ii) Mechanical testing quantity concepts such as toughness, elongation, and fatigue strength in the appropriate hierarchies of bfo:Disposition and bfo:Quality classes, iii) Mechanical testing artifacts like indenter as the subclasses of cco:Artifact, and iv) mechanical testing data like the stress-strain, S-N, or creep curves as the subclasses of cco:InformationContentEntity. MTO is publicly available via the KupferDigital GitLab repository.
Nickel-based alloys have been widely used for gas turbine blades owing to their excellent mechanical properties and corrosion resistance at high temperatures. The operating temperatures of modern gas turbines have been increased in pursuit of increased thermal efficiency. Turbine blades are exposed to these high temperatures combined with mechanical stresses, resulting in material damage through creep, fatigue, and other mechanisms. These turbine blades must be regularly inspected and replaced as needed, to prevent the loss of efficiency, breakdown, and catastrophic failure. Repair of the damaged turbine blades is often a more practical and cost-effective option than replacement, as replacement is associated with high costs and loss of material resources. To this end, state-of-the-art repair technologies including different additive manufacturing and brazing processes are considered to ensure efficient repair and optimum properties of repaired components.
In any repaired part, materials property-mismatches and/or inner defects may facilitate the crack initiation and propagation and thus reduce the number of load cycles to failure. Therefore, a fundamental understanding of the fatigue crack growth and fracture mechanisms in joining zones is required to enable the prediction of the remaining life of repaired components and to further improve and adapt the repair technologies.
Fatigue crack growth experiments have been conducted on SEN (Single Edge Notch) specimens joined via brazing, and pre-sintered Preform (PSP) and multi-materials (casted/printed) specimens layered via additive manufacturing (AM). The experiments were performed at 950 °C and various stress ratios. The crack growth was measured using DCPD (Direct Current Potential Drop) method. The stress intensity factors for joined SEN specimens were calculated using the finite element method and then used to derive the fatigue crack growth curves. Metallographic and fractographic analyses were conducted to get insight into the fracture mechanism.
Results show that the experimental technique for fatigue crack growth was successfully adapted and applied for testing joined specimens. Furthermore, the initial tests indicate that the investigated braze filler material provides a lower resistance to crack growth, and bonding defects cause a crack to deviate to the interface of the base material and joining zone. In AM-sandwich specimens, the crack growth rates are significantly reduced when the crack reaches the interface of printed material and casted material. The obtained crack growth data can be used to calibrate a crack growth model, which will further be utilized to predict the remaining life of repaired components.
Experimentally informed multiscale creep modelling of additive manufactured Ni-based superalloys
(2023)
Excellent creep resistance at elevated temperatures, i.e. T / T_m> 0.5, due to γ-γ’ microstructure is one of the main properties of nickel-based superalloys. Due to its great importance for industrial applications, a remarkable amount of research has been devoted to understanding the underlying deformation mechanism in a wide spectrum of temperature and loading conditions. Additive manufactured (AM) nickel-based superalloys while being governed by similar γ-γ’ microstructure, exhibit AM-process specific microstructural characteristics, such as columnar grains, strong crystallographic texture (typically <001> fiber texture parallel to build direction) and compositional inhomogeneity, which in turn leads to anisotropic creep response in both stationary and tertiary phases.
Despite the deep insights achieved recently on the correlation between process parameters and the resulting microstructure, the anisotropic creep behavior and corresponding deformation mechanism of these materials are insufficiently understood so far. One reason for this is the lack of capable material models that can link the microstructure to the mechanical behavior. To overcome this challenge, a multiscale microstructure-based approach has been applied by coupling crystal plasticity (CP) and polycrystal model which enables the inclusion of different deformation mechanisms and microstructural characteristics such as crystallographic texture and grain morphology. The method has been applied to experimental data for AM-manufactured INCONEL-738LC (IN738). The effect of different slip systems, texture, and morphology on creep anisotropy at 850°C has been investigated. Results suggest a strong correlation between superlattice extrinsic stacking fault (SESF) and microtwinning and observed creep anisotropy.
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.
Concrete has a long history in the construction industry and is currently one of the most widely used building materials. Unfortunately, the concrete industry has a significant impact on the environment by contributing to about 9% of the total anthropogenic greenhouse gas (GHG) emissions. Concrete is a highly complex composite material. However, the main source of concrete's GHG emissions is the cement. This leads to two main strategies when trying to reduce the environmental impact. The first is to reduce the cement within the concrete mix. This can be done by substituting it using additives or increasing the amount of aggregates. Usually this will lead to decreased material properties, like compressive strength or stiffness. The second option is to reduce the amount of required concrete by optimizing the topology of the structure. However, this might require higher compressive strength. In addition, there are other properties like to workability which need to be considered. All in all, this leads to a highly complex optimization problem, which requires the estimation of effective concrete properties, based on the mixture as input to a predictive simulation.
We present an automated workflow framework which combines experimental data with simulations, calibrates the simulation and performs the desired optimization. This workflow includes classical FE models, design guidelines based on model codes, as well as data driven methods. The chosen example is a beam, for which the concrete mixture is optimized to reduce GHG emissions. The first step is an estimation of material parameters, based on experimental data. This includes measures of stochastic distribution, allowing the quantification of the quality of the estimated parameters. The second step is the optimization. It takes into account constraints like the loading capacity after 28 days, the maximum allowed temperature during cement hydration and the maximum time till demoulding. The applied models include a Mori-Tanaka-based homogenization method to estimate effective concrete parameters, an FE simulation including the evolution of the concrete compressive strength and stiffness, the temperature field, displacements, and stress. This research shows a way towards a more performance-oriented material design.
Additive manufacturing (AM) has revolutionized the manufacturing industry, offering a new paradigm to produce complex geometries and parts with customized properties. Among the different AM techniques, the wire arc additive manufacturing (WAAM) process has gained significant attention due to its high deposition rate and low equipment cost. However, the process is characterized by a complex thermal history, dynamic metallurgy, and mechanical behaviour that make it challenging to simulate it in real-time for online process control and optimization.
In this context, a reduced order model (ROM) using the proper generalized decomposition (PGD) method is proposed as a powerful tool to overcome the limitations of conventional numerical methods and enable the real-time simulation of the temperature field of WAAM processes. Though, the simulation of a moving heat source leads to a hardly separable parametric problem, which is handled by applying a novel mapping approach. Using this procedure, it is possible to create a simple separated representation of the model, also allowing to simulate multiple layers.
In this contribution, a PGD model is derived for the WAAM procedure simulating the temperature field. A good agreement with a standard finite element method is shown. The reduced model is further used in a stochastic model parameter estimation using Bayesian inference, speeding up calibrations and ultimately leading to a calibrated real-time simulation.
Multiscale modeling of heterogeneous structures based on a localized model order reduction approach
(2023)
Many of today’s problems in engineering demand reliable and accurate prediction of failure mechanisms of mechanical structures. Thus, it is necessary to take into account the heterogeneous structure on the smaller scale, to capture the underlying physical phenomena. However, this poses a great challenge to the numerical solution since the computational cost is significantly increased by resolving the smaller scale in the model. Moreover, in applications where scale separation as the basis of classical homogenization schemes does not hold, the influence of the smaller scale on the larger scale has to be modelled directly. This work aims to develop an efficient concurrent methodology to model heterogeneous structures combining the variational multiscale method (VMM) [1] and model order reduction techniques (e. g. [2]). First, the influence of the smaller scale on the larger scale can be taken into account following the additive split of the displacement field as in the VMM. Here, also a decomposition of the global domain into subdomains, each containing a fine grid discretization of the smaller scale, is introduced. Second, local reduced approximation spaces for the smaller scale solution are constructed by exploring possible solutions for each subdomain based on the concept of oversampling [3]. The associated transfer operator is approximated by random sampling [4]. Herein, we propose to incorporate the actual physical behaviour of the structure of interest in the training data by drawing random samples from a multivariate normal distribution with the solution of a reduced global problem as mean. The local reduced spaces are designed such that local contributions of each subdomain can be coupled in a conforming way. Thus, the resulting global system is sparse and reduced in size compared to the direct numerical simulation, leading to a faster solution of the problem.
HR-CS-GFMAS a new screening tool for per- and polyfluoroalkyl substances (PFAS) in the environment
(2023)
Per- and polyfluorinated alkyl substances (PFASs) are a large group of anthropogenic contaminates. Concerning are especially their persistent, bioaccumulative and toxic properties. Mostly, target-based approaches (e.g., LC-MS/MS) are utilized for the analysis of PFASs in the environment. But these approaches are limited to the availability of analytical grade standards and therefore drastically underestimate the total PFAS burden. Analytical approaches based on total fluorine for PFAS sum parameter analysis become increasingly important to indicate realistic PFAS pollution levels.
PFAS sum parameters display the proportion of organically bound fluorine that can either be extracted (EOF) or adsorbed to activated carbon (AOF). For the instrumental analysis of such sum parameters, a fluorine selective detector is needed. Besides combustion ion chromatography (CIC), high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) is a sensitive and highly selective tool for fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) in a graphite furnace at a temperature of 1550°C. The molecular absorption of GaF can be detected at its most sensitive wavelength at 211.248 nm providing limits of quantification in the low µg F L-1 range.
Here, we present a comparison of total fluorine analysis methods – AOF vs. EOF and HR-CS-GFMAS vs. CIC. Therefore, surface water samples from the Spree River in Berlin, Germany were analyzed at 10 locations for total fluorine (TF), AOF and EOF. The AOF made up 0.14–0.81% of TF and the EOF 0.04–0.28% of TF while AOF concentrations were systematically higher. For the instrumental comparison, HR-CS-GFMAS was the more sensitive and precise method for fluorine analysis compared to CIC.
Leather is a widely used material for thousands of years and in modern days it is produced on industrial scale. This production produces high amounts of organic waste during the tannery process. These fibers can become a resource and act as a multi-functional bio-filler in flame retardant composites.
This project investigates two leather fibers towards their ability to enhance the flame-retardancy in different composites. These composites use ammonium polyphosphate (APP) or aluminum trihydroxide (ATH) as flame retardants. Different synergists support polymers with ATH.
The new composites form a stable char layer resulting in an increase in residue, lower peak heat release rates (pHRR) and higher limiting oxygen index (LOI). In addition, the ratings in the UL94-classification increased up to V-0.
One crucial metric of interest to wind farm operators is the remaining useful life (RUL) of single components, wind turbines, or even entire wind farms. Occasionally, questions arise regarding how to operate a turbine, even in the presence of manufacturing or design errors, which from a computational design standpoint reduce the remaining lifetime below the intended service life. A typical measure involves adapting the monitoring and inspection plan. Using such a maintenance plan, the author intends to simulate the lifetime of jacket-type structure in a fatigue test. The objective of the experiment is to demostrate that systems like three-dimensional jackets possess redundancies that enable reliable continued operation, despite the reduced fatigue life of individual components due to technical flaws, if an appropriate maintenance concept is in place. This presentation discusses the steps leading to the procedure of the experiment including the design process and the maintenance planning.
Glimpses of the Future ✨: Advancing X-ray Scattering in an Automated Materials Research Laboratory
(2023)
In our (dramatically understaffed) X-ray scattering laboratory, developing a systematic, holistic methodology1 let us provide scattering and diffraction information for more than 2100 samples for 200+ projects led by 120+ collaborators. Combined with automated data correction pipelines, and our analysis and simulation software, this led to more than 40 papers2 in the last 5 years with just over 2 full-time staff members.
This year, our new, modular synthesis platform has made more than 1000 additional samples for us to analyse and catalogue. By virtue of the automation, the synthesis of these samples is automatically documented in excruciating detail, preparing them for upload and exploitation in large-scale materials databases. Having developed these proof-of-concepts, we find that materials research itself is changed dramatically by automating dull tasks in a laboratory.
This talk is intended to spark ideas and invite collaborations by providing an overview of: 1) the current improvements in our wide-range X-ray scattering laboratory methodology, 2) Introduce some of our open-source analysis and simulation software, touching on scattering, diffraction and PDF, and 3) introducing our open, modular robotic platform for systematic sample preparation. Finally, the remaining bottlenecks and points of attention across all three are highlighted.
The second talk for the Swiss Society for Crystallography (SSCr) workshop on SAXS will highlight the data processing challenges, holistic experimental workflow developments, and the pitfalls. In particular, the following items will be addressed:
- The importance of data processing and estimating uncertainty
- A universal correction pipeline – away with the headaches, at least for this step!
- Experiment planning part 2, some tips and advice to improve your corrected data.
- Sample preparation, background selection, some tips and advice to improve your corrected data.
- Automate for your mental well-being; electronic logbooks, measurement catalogs and workflow management software
- Life on the edge: several pitfalls to avoid…
This talk for the Swiss Society for Crystallography (SSCr) workshop on SAXS will introduce scattering from various angles, focusing in particular on:
- Information content of X-ray scattering experiments, three entry points…
- An introduction to Fourier Transforms
- Sample criteria, compatibility, and selection
- Key indicators of a measurement – where is the information?
- Key indicators of measurement quality
- Experiment planning, the basics
In our (dramatically understaffed) X-ray scattering laboratory, developing a systematic, holistic methodology let us provide scattering and diffraction information for more than 2100 samples for 200+ projects led by 120+ collaborators. Combined with automated data correction pipelines, and our analysis and simulation software, this led to more than 40 papers in the last 5 years with just over 2 full-time staff members.
This year, our new, modular synthesis platform has made more than 1000 additional samples for us to analyse and catalogue. By virtue of the automation, the synthesis of these samples is automatically documented in excruciating detail, preparing them for upload and exploitation in large-scale materials databases.
This talk is intended to spark ideas and invite collaborations by providing an overview of: 1) the current improvements in our wide-range X-ray scattering laboratory methodology, and 2) introducing our open, modular robotic platform for systematic sample preparation.
Avoiding antimony – effect of Ca(H2PO2)2 on smoke emission and fire behaviour in brominated ABS
(2023)
The replacement of antimony trioxide (Sb2O3) in brominated flame-retardant ABS (ABS/FR) is of great interest. This study investigates the influence of calcium hypophosphite (CaP) in ABS/FR on flame retardancy and smoke emission. Different amounts of talc are added to ABS/FR/CaP to evaluate the influence of an inorganic barrier on smoke emission and flame retardancy. The cone calorimeter unveiled a reduction by 46% in PHRR for ABS/FR/CaP. Additional 8 wt.-% talc (ABS/FR/CaP/8Talc) reduced the PHRR by 61%. ABS/FR/CaP exhibited a more condensed phase action, which resulted in less smoke emission. The study investigates the influence of CaP in ABS/FR on the smoke toxicity, smoke density and the smoke particles distribution in the smoke density chamber (ISO 5659-2) coupled to a FTIR spectrometer and electrical low pressure cascade impactor (ELPI).
In recent years, the use of simulation-based digital twins for monitoring and assessment of complex mechanical systems has greatly expanded. Their potential to increase the information obtained from limited data makes them an invaluable tool for a broad range of real-world applications. Nonetheless, there usually exists a discrepancy between the predicted response and the measurements of the system once built. One of the main contributors to this difference in addition to miscalibrated model parameters is the model error. Quantifying this socalled model bias (as well as proper values for the model parameters) is critical for the reliable performance of digital twins. Model bias identification is ultimately an inverse problem where information from measurements is used to update the original model. Bayesian formulations can tackle this task. Including the model bias as a parameter to be inferred enables the use of a Bayesian framework to obtain a probability distribution that represents the uncertainty between the measurements and the model. Simultaneously, this procedure can be combined with a classic parameter updating scheme to account for the trainable parameters in the original model. This study evaluates the effectiveness of different model bias identification approaches based on Bayesian inference methods. This includes more classical approaches such as direct parameter estimation using MCMC in a Bayesian setup, as well as more recent proposals such as stat- FEM or orthogonal Gaussian Processes. Their potential use in digital twins, generalization capabilities, and computational cost is extensively analyzed.
Dissimilar metal TIG weld joints of multiple principal element alloys (MPEA) to austenitic steel 304
(2023)
Multi-element alloys (MPEA - Multiple Principal Element Alloys) represent a new class of materials consisting of at least three alloying elements, each with 5 to 35 atomic %. This material class includes high-entropy alloys (HEA, with n ≥ 4 elements). The underlying alloying concept differs fundamentally from conventional materials such as the Fe-based steel. For this purpose, the alloying elements are specifically selected, and the microstructures are adjusted in a single-phase and, in some cases, multi-phase manner. The aim is to identify highly innovative MPEA with individually adjustable properties for industrial applications. In the last 20 years, however, the focus has been on pure material synthesis. With the increase in available material quantities, the focus is on processing issues such as joining and welding processes. In that connection, the weldability of MPEAs has received very little attention so far. Experience with dissimilar metal welds (DMWs) is completely lacking but is essential for the application of these materials if joint to conventional materials. This study presents selected experimental results on the weldability of MPEA-DMWs and the resulting microstructures. For this purpose, the equiatomic CoCrFeMnNi (HEA) was investigated in cold-rolled (CR) and heat-treated (HT) condition and joined by tungsten inert gas (TIG) welding to an austenitic stainless steel 304. The DMWs showed defect-free conditions (no lack of fusion, cracks and so on), whereas the cold-rolling increases the microhardness. The global mechanical properties were obtained by instrumented tensile tests of cross-weld samples and showed sufficient yield and tensile strength comparable to that of the individual base materials (BM). The local strain conditions were determined by digital image correlation and showed the highest local strains to occur in the intermixed weld metal. Indeed, the preferred fracture location of the cross-weld tensile samples was in the weld metal. Finally, the experiments proofed the weldability of the MPEAs to conventional 304. This enables targeted further considerations for example as structural materials.
Recent advances in Deep Learning (DL) have significantly impacted the field of materials modelling. DL tools have been recently considered as promising tools to address the complex relationships among processing, microstructure and property of materials. The thermal stability of polycrystalline materials is a highly interesting and complex problem that could be addressed using DL techniques. The Multi-Phase-Field (MPF) method has emerged as a powerful tool for addressing grain growth phenomena from multiple perspectives. Unlike sharp-interface based methods, the MPF approach bypasses the need for detailed information on individual grains. In this work, we use DL to address issues related to MPF simulations of grain growth including numerical efficiency, computing speed, and resource consumption. This presents specific challenges for high-performance computing (HPC) due to the large datasets and complex computations required by both MPF and DL methods. We study various 3D microstructure settings with the goal of accelerating the simulation process while exploring different physical effects. In particular, the impact of grain boundary and triple junction energies on grain growth are to be investigated. The results will be presented in terms of the evolving size and shape distribution of the grains.
The hydrogen economy requires large-scale storage and transportation options like long-distance transmission pipelines. The applied materials (typically steels) must be carefully tested under different conditions (pressure, temperature, impact of impurities, etc.) for their suitability and service with hydrogen. In combination with mechanical load, as occurs in every gas network, hydrogen can induce degradation of the mechanical properties and promote finally resulting in embrittlement, i.e., the formation of cracks. The conventional testing procedures consist of autoclaves in which samples are strained under pressurized hydrogen. The test apparatus requires large amounts of hydrogen and thus a high level of safety and costs. In very specific cases, these tests might be replaced by simplified electrochemical charging. However, these test alternatives raise several questions regarding the equivalency of both testing scenarios. In the early 1980’s the idea of a so-called hollow tensile sample raised and was reinitiated 2021 in ISO TC 164 by T. Ogata (NIMS, Japan) and further developed (e.g. by Fraunhofer IWM, Germany). The idea was: the sample itself represents the autoclave instead of charging a sample from outside. For that reason, a hole is drilled through the sample and the inner surface is pressurized by hydrogen gas during the mechanical testing. Indeed, this represents the main advantage as no expensive pressure-resistant autoclave equipment for large H-volumes is necessary, which significantly reduces the safety-related issues and thus the high costs. In the following, we show recent activities at BAM Berlin on adaption of the hollow-specimen technique for slow strain rate testing (SSRT). The current research activities are focussed on macroscopic influences like the sample geometry, minimum necessary dimensions, and microscopic influences e.g., on the surface by the processing method (drill hole quality and geometric precision) as well as the gas pressure effect (mechanical deformation of surface in different media).
Many metallic materials gain better mechanical properties through controlled heat treatments. For example, in age-hardenable aluminium alloys, the strengthening mechanism is based on the controlled formation of nanometre-sized precipitates, which represent obstacles to dislocation movement and consequently increase the strength. Precise tuning of the material microstructure is thus crucial for optimal mechanical behaviour under service condition of a component. Therefore, analysis of the microstructure, especially the precipitates, is essential to determine the optimum parameters for the interplay of material and heat treatment. Transmission electron microscopy (TEM) is utilized to identify precipitate types and orientations in the first step. Dark-field imaging (DF-TEM) is often used to image the precipitates and thereafter quantify their relevant dimensions. Often, these evaluations are still performed by manual image analysis, which is very time-consuming and to some extent also poses reproducibility problems.
Our work aims at a semantic representation of an automatable digital approach for this material specific characterization method under adaption of FAIR data practices. Based on DF-TEM images of different precipitation states of a wrought aluminium alloy, the modularizable, digital workflow of quantitative analysis of precipitate dimensions is described. The integration of this workflow into a data pipeline concept will also be discussed. Using ontologies, the raw image data, their respective contextual information, and the resulting output data of the quantitative image analysis can be linked in a triplestore. Publishing the digital workflow and the ontologies will ensure data reproducibility. In addition, the semantic structure enables data sharing and reuse for other applications and purposes, demonstrating interoperability.
For extrusion-based 3D concrete printing, the early age mechanical behavior is influenced by various time dependent phenomena: structural build-up, plasticity as well as viscosity. The structural build-up is governing the stability and early-age strength development of the fresh printable cementitious materials and with that influencing the printability, buildability, and open time of the printing process. Generally, it is influenced by a number of factors, i.e. composition of the printable material, printing regime, and ambient conditions (temperature, humidity, etc.). There are several approaches to model the structural build-up of cementitious materials. All models are based on a time-dependent internal structural parameter describing the flocculation state, which is assumed to be zero after mixing and increases with time. The approaches differ in the definition of the time dependency (linear, exponential, bi-linear). Usually, the parameters are defined for a specific material composition without considering the influence of ambient conditions.
In this contribution, the bi-linear structural build-up model [Kruger et al., Construction and Building Materials 224, 2019] is extended by the temperature influence. Temperature changes will occur in real life printing processes due to changing ambient conditions (summer, winter, day, night) as well as the printing process (pressure changes etc.) and have a significant impact on the structural build-up process: an increase of the temperature leads to a faster dissolution of cement phases, accelerates hydration and boosts the Brownian motion. For that reason, the model parameters are simulated as temperature dependent using an Arrhenius function. Furthermore, the proposed extended model is calibrated based on measurement data using Bayesian inference. A very good agreement of the predicted model data with the measured control data was reached. Additionally, the structural build-up model is integrated into a viscoelastic and elastoplastic mechanical model, simulating the whole mechanical behavior during layer deposition.
Microalloying elements, such as Nb and Ti, are essential for the targeted mechanical strength of quenched and tempered, high-strength fine-grained structural steels with a nominal yield strength ≥ 690 MPa. Current specifications for chemical composition only provide upper limits for manufacturers. But even small deviations in the alloying route can have a drastic effect on the mechanical properties. Thus, an adequate prediction of the weldability and the integrity of the welded joint becomes difficult or even impossible due to the varying composition and, hence, the microstructures. Undesirable side effects are the possible softening of the heat-affected zone (HAZ) as well as the opposite effect of hardening. Against this background, different microalloying routes with varying Ti and Nb contents are systematically investigated for the first time on specially designed lab-cast alloys. The basis of each alloy route was the common S690QL in terms of both the chemical composition as well as the heat treatment. To investigate the weldability, three-layer welds were performed using metal active gas welding (MAG) and critical microstructural areas with high softening/hardening were identified. The scope was here on the identification of phase transformations during cooling and on the respective metallurgical precipitation behavior. Isothermal and non-isothermal phase calculations were performed using Thermo-Calc® and showed that the prediction of the non-equilibrium precipitation characteristics during welding is not trivial, especially for this relatively complex chemical composition. The mechanical properties of the welded joints were identified by both Charpy tests (toughness) and tensile tests (strain and strength). During the test, the local straining behavior of the welded joints, was identified using a digital image correlation (DIC) system, see Figure 1. Despite the generally good weldability of the materials, the results show a significant influence of the microalloying route as well as the welding heat input on the different precipitation kinetics.
We report about a joint project aiming at the digitalization of a lab course in materials testing. The undergraduate students were asked to prepare samples of a precipitation hardened aluminum alloy and characterize them using hardness and tensile tests. In a first step, we developed the frames for the digital labor notebook using eLabFTW. The primary data and the relevant metadata of each run were saved in a central database and made available for analysis and report issues. The whole set of results produced in a course was made available in the database. This database can be improved and serve as an open repository for data on this specific alloy.
The logical frame for the joint project was provided by the PMD Core Ontology (PMDco), a mid-level ontology that enables the representation and description of processes and process chains in an MSE-specific manner, ensuring full traceability of generated data. For the digitalization of this lab course, the tensile test ontology (TTO) was applied which is designed as a module of the PMDco using strongly related semantic concepts.
Basic oxygen furnace slag (BOFS) is a by-product of steelmaking of which about 10.4 Mt are produced annually in the EU. BOFS is mostly used in road construction, earthwork and hydraulic engineering. However, in this use, the iron bound in BOFS is lost and the opportunity to produce higher value products from BOFS is forgone.
In recent decades, many researchers have investigated the production of both Portland cement clinker and crude iron from BOFS via a thermochemical reductive treatment. The reductive treatment of liquid BOFS causes a reduction of iron oxides to metallic iron, which separates from the mineral phase due to its higher density and can be recovered. An advantage of this process is that simultaneously the chemical composition of the reduced BOFS is adapted to that of Portland cement clinker and the hydraulic reactive mineral alite (Ca3SiO5) is formed.
In this study, German BOFS was reduced in a small-scale electric arc furnace and a low-iron mineral product rich in alite was produced. Despite a chemical and mineralogical composition similar to that of Portland cement clinker, the reduced BOFS produced less heat of hydration, and its reaction was delayed compared to Portland cement. However, adding gypsum accelerated the hydration rate of the reduced BOFS.
Further research to improve the hydraulic properties of the reduced BOFS is essential. If successful, the production of a hydraulic material and crude iron from BOFS could have economic and ecological benefits for both the cement and steel industry.
Many microstructural features exhibit non-trivial geometries, which can only be derived to a limited extent from two-dimensional images. E.g., graphite arrangements in lamellar gray cast iron have complex geometries, and the same is true for additively manufactured materials and three-dimensional conductive path structures. Some can be visualized using tomographic methods, but some cannot be due to weak contrast and/or lack of resolution when analyzing macroscopic objects. Classic metallography can help but must be expanded to the third dimension. The method of reconstructing three-dimensional structures from serial metallographic sections surely is not new. However, the effort required to manually assemble many individual sections into image stacks is very high and stands in the way of frequent application. For this reason, an automated, robot-supported 3D metallography system is being developed at BAM, which carries out the steps of repeated preparation and image acquisition on polished specimen.
Preparation includes grinding, polishing and optionally etching of the polished surface. Image acquisition comprises autofocused light microscopic imaging at several magnification levels. The image stacks obtained are then pre-processed, segmented, and converted into 3D models, which in the result appear like microtomographic models, but with high resolution at large volume. Contrasting by classical chemical etching reveals structures that cannot be resolved using tomographic methods. The integration of further imaging and measuring methods into this system is underway. Some examples will be discussed in the presentation.
Knowledge representation in the materials science and engineering (MSE) domain is a vast and multi-faceted challenge: Overlap, ambiguity, and inconsistency in terminology are common. Invariant and variant knowledge are difficult to align cross-domain. Generic top-level semantic terminology often is too abstract, while MSE domain terminology often is too specific.
In this presentation, an approach how to maintain a comprehensive and intuitive MSE-centric terminology composing a mid-level ontology–the PMD core ontology (PMDco)–via MSE community-based curation procedures is shown.
The PMDco is designed in direct support of the FAIR principles to address immediate needs of the global experts community and their requirements. The illustrated findings show how the PMDco bridges semantic gaps between high-level, MSE-specific, and other science domain semantics, how the PMDco lowers development and integration thresholds, and how to fuel it from real-world data sources ranging from manually conducted experiments and simulations as well as continuously automated industrial applications.
The surface corrosion behaviour is a key issue which determines whether the material is applicable at a given atmosphere. Medium-entropy alloy FeCrNi alloy was exposed to synthetic air at 1000°C, 1050°C, and 1100 °C for up to 1000 h using a thermobalance. The oxidation rate was parabolic at 1000 and 1050°C, but breakaway occurred at 1100°C after 5 h of aging time. The whole oxide scales formed under the isothermal oxidation tests spalled off and additional oxidation tests were carried out at 1000 °C and 1050°C for 24 h and up to 100 h at 1000°C in a tubular furnace. The corrosion behaviour of the MEA was analysed by scanning electron microscope, energy-dispersive X-ray spectroscopy, and X-ray diffraction and compared to the behaviour of 316 L. The experimental results showed that under all conditions chromium is the main diffusion element resulting in the formation of a Cr2O3 layer at the MEA surface. Spallation of the layer induces the formation of additional oxidation products under the surface of the (spalled off) chromia layer.
The present work is part of the AIFRI project (Artificial Intelligence For Rail Inspection), where we and our project partners train a neural network for defect detection and classification. Our goal at BAM is to generate artificial ultrasound and eddy current training data for the A.I. This paper has an exploratory nature, where we focus on the simulation of eddy current signals for head check cracks, one of the most important rail surface defects. The goal of this paper is twofold. On the one hand, we present our general simulation setup. This includes geometric models for head check cracks with features like branching and direction change, a model for the HC10 rail testing probe, and the configuration of the Faraday simulation software.
On the other hand, we use the Faraday software to simulate eddy current testing signals with a strong focus on the influence of the damage depth on the signal, while differentiating between different crack geometries. Here, we observe an early saturation effect of the test signal at a damage depth of 2 mm (at a crack angle of 25◦ to the surface). That is about 2 mm earlier than we would expect from measurements at a crack angle of 90◦. This behavior will be investigated further in a future paper. Finally, we interpolate the simulated signals in a two-step curve fitting process. With these interpolations we may generate eddy current test signals for any damage depth within the simulated range.
The development of offshore wind turbines (WTGs) presents many challenges in terms of safe operation over extended periods of time. One of these is the corrosive environment towards metallic materials, which can lead to a loss of material thickness and thus to a deterioration of mechanical performances, especially the strength of infrastructures. This can be counteracted by painting and cathodic protection (CP). Much research has already been done in this area about inhibiting the corrosion process. However, gaps exist regarding free corrosion. This plays a greater role especially for time intervals during the installation of the systems and their maintenance, during which often no CP can be operated. This is especially true for areas where painting surfaces is impossible e.g., sediment areas. This problem is exacerbated by the different corrosion rates caused by the different zones (water and sediment), with their different amounts of dissolved oxygen.
This presentation deals with experiments in artificial seawater and sediment. Classical S355J2 steel samples in the form of coupons were fitted with welding wires that carried out the electrical contact to the outer side of the basin. Inside the basins, the specimens are stored in different zones like water and sediment which should simulate the foundation situation of monopiles. The mass loss was determined gravimetrically, elemental currents between specimens in water and sediment were measured and electrochemical investigations were carried out. The influences of the zones, based on different solved oxygen contents, and the rolling skin towards the corrosion behavior of the mild steel samples were determined in this work. Especially the influence of the sediment showed unexpected behavior, determined by electrochemical investigations. These results allow better conclusions to be drawn about the corrosion behavior of low alloy steels in offshore environments used in sediment and seawater, which cannot always be protected.
The basic principles of generation of electrons and X-rays and the operation of SEM/EDS instruments are presented. Examples, recent successes and challenges in the analysis of nano-structures are given. Multi-method analytical approaches with the focus on imaging the nanoscale are highlighted. Details on the sample preparation and persepective on the automated analysis (sample preparation, measurement, data analyis and storage) are given. Metrological aspects, standardisation, and reference materials are also emphasized by examples.
Der Beitrag beschreibt die Entwicklung eines neuartigen in situ Nachweisverfahrens zur Beurteilung des Feuerwiderstandes von bestehenden Stahlkonstruktionen mit gealtertem reaktivem Brandschutzsystem (RBS). Derzeit ist ein solcher Nachweis ausschließlich anhand eines Bauteilbrandversuchs möglich. Hierzu muss ein Bauteil aus der Bestandskonstruktion entnommen und einer zerstörenden Brandprüfung unterzogen werden. In Zusammenhang mit der Dauerhaftigkeitsbewertung von RBS für Zeiträume von mehr als 10 Jahren besteht in der Praxis vermehrt der Bedarf an einem minimal invasiven Prüfverfahren, mit dessen Hilfe sich direkt am Bestandsbauwerk die tatsächlich vorhandene Leistungsfähigkeit des gealterten RBS überprüfen lässt. Durch einen erfolgreichen Funktionsnachweis wäre eine Weiternutzung der Bestandkonstruktion bei Aufrechterhaltung des bestehenden Sicherheitsniveaus möglich.
Corrosion of reinforcement is one of the major reasons in questioning the sturdiness of building structures. The application of cathodic protection techniques plays a big role in controlling the corrosion process to ensure a longer service life of building structures. This systematic study compares the efficiency and durability of various discrete galvanic zinc anode systems available in the current market using different criteria for measuring efficiencies such as potential measurements, electrolyte resistance measurements and several polarization methods to determine the polarizability of the anodes. Results to validate the performance of long-time exposure of discrete zinc anodes in the concrete medium are already shown in 2021. Now the results of analyzing the phase boundary between mortar and anodes by using 3D computer tomography are shown, as also the field application at large-scale specimens where the potential distribution and the current were investigated.
Design and construction of a rainfall simulator to test metal runoff at atmospheric conditions
(2023)
A rainfall simulator was presented as an environmental assessment tool to quantify wash-off concentrations from metallic materials. It is part of the RUNOFF-project, which studies and re-assesses the durability of roofing and facade materials under current atmospheric conditions in Germany.
Studying building materials is important as they have a significant impact on achieving a variety of goals and targets within the sustainable developments goals (SDGs). The durability of materials is essential to reach sustainability. However, the durability of metallic materials is strongly depended on climate conditions, which have changed as a result of technical measures in industry, climate change and increasing urbanisation. In Germany at least, the data base is not up-to-date leading to prediction models regarding corrosion resistance and durability of metallic materials which can no longer be trusted and therefore need to be re-assessed and updated. Also, not only the demand for sustainable but also environmentally friendly building materials has increased dramatically. A number of construction materials produce chemical hazards, and therefore have negative impacts on water quality, soils health and ecosystems. To limit these impacts, environmental assessment methods and tools are needed to measure and quantify the inputs and outputs of building materials throughout their lifetime.
Additive manufacturing of concrete structures is a novel and emerging technology. Free contouring in civil engineering, which allows for entirely new designs, is a significant advantage. In the future, lower construction costs are expected with increased construction speeds and decreasing required materials and workers. However, architects and civil engineers rely on a certain quality of execution to fulfil construction standards. Although several techniques and approaches demonstrate the advantages, quality control during printing is highly challenging and rarely applied. Due to the continuous mixing process commonly used in 3D concrete printing, it is impossible to exclude variations in the dry mixture or water content, and a test sample cannot be taken as a representative sample for the whole structure. Although mortar properties vary only locally, a defect in one layer during printing could affect the entire integrity of the whole structure . Therefore, real-time process monitoring is required to record and document the printing process. At the Bundesanstalt für Materialforschung und -prüfung (BAM) a new test rig for the additive manufacturing of concrete is built. The primary purpose is measuring and monitoring the properties of a mortar during the printing process. The following study investigates an approach for calculating yield stress and plastic viscosity based on experimentally recorded pressure data. The calculations assume that fresh mortar behaves as a Bingham fluid and that the Buckingham-Reiner-equation is applicable. A test setup consisting of rigid pipes with integrated pressure sensors at different positions is utilized. Monitoring the printing process with different sensors is crucial for the quality control of an ongoing process.
Hydrogen has great potential into the decarbonization process of the energy and transport sectors, thus helping to mitigate the urgent issue of global warming. It can be sustainably produced through water electrolysis with potentially zero emissions, and efficiently used in fuel cell systems. Despite its environmental advantages, hydrogen is an extremely flammable substance and its interaction with most metallic materials could result in their mechanical properties degradation to an extent that could make them inherently unsafe.
Extensive material testing under realistic operating conditions is required to determine the criteria under which hydrogen-induced damage is to be expected. In-situ slow strain rate tensile (SSRT) test is an option that allow the quantification of the behavior of metals in hydrogenated environments. The standardized procedure for testing in-situ the pressurized gaseous hydrogen
effect on metals consists of the utilization of an autoclave as a containment volume. Testing inside an autoclave is difficult, expensive, and time-consuming, and requires specialized equipment and trained personnel. A relatively recent method to circumvent these issues and provide affordable and reliable test results consists in using hollow specimens as the gas containment volume, thus applying the hydrogen pressure inside rather than outside the
specimen. This experimental setup allows us to minimize the volume of hydrogen and perform the tests safely and effectively. This study focuses on the evaluation of tensile properties of X65 pipeline steel, which was in vervice for natural gas transport, tested in a high-pressure hydrogen environment using hollow specimens. A constant nominal strain rate of 1ꞏ10-6 s-1 is applied. Tests are performed with different manufacturing techniques for the drilling process, which results in difeerent surface conditions. The effect of the roughness on the HE was investigated. For the evaluation the effect on the reduced area at fracture (RA) and the elongation loss were determined. Further fractographic analysis were performed. In this way, this study provides insights on the applicability of novel, reliable, and safer testing method which can be used to assess HE, particularly in relation with hydrogen-induced loss of ductility in metallic material.
Der Vortrag stellt die Arbeiten der BAM in der Initiative QI-Digital vor, in deren Rahmen Lösungen für eine moderne und digitale Qualitätsinfrastruktur entwickelt werden. Schwerpunkt liegt auf dem zentralen Werkzeug Quality-X sowie dem Pilotprojekt "Moderne Qualitätssicherung in der Additiven Fertigung".
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.
Understanding and Machine Learning of Materials Properties with Quantum-Chemical Bonding Analysis
(2023)
Bonds and local atomic environments are crucial descriptors for material properties. They have been used to create design rules for materials and are used as features in machine learning of material properties. This talk will show how our recently developed tools, that automatically perform quantum chemical bond analysis and enable the study of chemical bonds and local atomic environments, accelerate and improve the development of such heuristics and machine-learned models for materials properties.
The presentation provides an overview and introduction to the need and drivers for the digital transformation of the quality infrastructure (QI). It illustrates the tools and processes that are the fundation of a digital QI and how the initiatve QI-Digital aims at developing accordant solutions. Special emphasis is given to the pilot projects at BAM.
In this presentation, the team security research of division 2.1 informs about current research efforts in the field of traumatic brain injury. The focus lies on the consequences of low-level blast on the human brain. Also the general research approaches of the team for the investigation of the behaviour of shock waves within human tissues are presented.
Current decontamination strategies of PFAS-burdened soils mainly consist of adsorption methods using adsorbents for fixation of PFAS in the ground. A second option is the utilization of a “pump and treat” process, cycling polluted soils through a washing plant leading to the concentration of the pollutants in the fine fraction. Only a subsequent, high-energy consuming pyrolysis process guarantees the total destruction of all fluorinated organic contaminants. These approaches are cost-intensive and not intended for the direct decomposition of all PFAS contaminants. Hence, there is a great demand for innovative developments and chemical treatment technologies, dealing with new strategies of tackling the PFAS problem. Thus, we investigated mechanochemical treatment of PFAS contaminated soils with various additives in a ball mill and analyzed the PFAS defluorination with gas chromatography mass spectrometry (GC-MS) and liquid chromatography tandem mass spectrometry (LC-MS/MS), respectively, as well as the fluoride mineralization by ion chromatography (IC) and fluorine K-edge X-ray absorption near-edge structure (XANES) spectroscopy.
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.
Bei Geräten und Maschinen zur bestimmungsgemäßen Verwendung in explosionsgefährdeten Bereichen gemäß 2014/34/EU muss in der europäischen Union eine Zündgefahrenbewertung durchgeführt werden. Dabei müssen unter anderem die Gefahren von nichtelektrischen Zündquellen betrachtet werden, zu denen auch die mechanischen Schlagvorgänge gehören.
Bei mechanischen Schlagvorgängen kommt es infolge des Zusammenstoßes zweier Werkstücke bzw. Bauteile zu einer Umwandlung der kinetischen Energie. Dabei erhöht sich die Temperatur der Werkstoffe an der Kontaktstelle und es kommt unter Umständen zu einem Abtrennvorgang kleiner Partikel erhöhter Temperatur. Sowohl die heißen Kontaktstellen (Zündquelle "heiße Oberflächen") als auch die abgetrennten Partikel (Zündquelle "mechanisch erzeugte Funken") können eine wirksame Zündquelle für ein explosionsfähiges Gasgemisch darstellen.
Zur Festlegung von Grenzwerten wurden in der Norm DIN EN ISO 80079-36:2016 die Gasgemische anhand ihrer Explosionsgruppe klassifiziert und zu jeder Gruppe die maximale Energie des Schlagvorgangs festgelegt, unter derer die Entstehung einer wirksamen Zündquelle als unwahrscheinlich angenommen werden kann.
Thin polymeric films are of great importance of high number of high-tech applications for instance in sensors and nanoelectronics. Form the scientific point of view thin films with thickness below 100 nm are ideal model systems to study confinement effects on its properties for instance on the molecular relaxation processes. In this contribution an overview is presented about the behavior of different systems as investigated by nanosized relaxation spectroscopy like broadband dielectric spectroscopy employing nano structured capacitors and AC chip calorimetry complimented by ellipsometry. The systems considered are PVME1, PVME/PS blends2,3 P2VP4, PBAC5 and polysulfone6. Besides the film also the adsorbed layer on the substrate prepared by a leaching approach and investigated by AFM is considered.1,4-7. For these investigationsss it is found that the adsorbed layer itself exhibits a relaxation dynamics which might be assigned either to molecular motions or to adsorptions desorption kinetics.
This research deals with the development of the Vickers hardness knowledge graph, mapping the example dataset in them, and exporting the data-mapped knowledge graph as a machine-readable Resource Description Framework (RDF). Modeling the knowledge graph according to the standardized test procedure and using the appropriate upper-level ontologies were taken into consideration to develop the highly standardized, incorporable, and industrial applicable models. Furthermore, the Ontopanel approach was utilized for mapping the real experimental data in the developed knowledge graphs and the resulting RDF files were successfully evaluated through the SPARQL queries.
BAM acts as authority and for service in safety assessment of packages for transport and storage of radioactive materials. We offer extensive test capabilities and application of analytical methods for design verification and simulation for all types of packages for the transport and storage of radioactive materials according with the international IAEA Regulations for the safe transport and for national storage acceptance criteria. BAM operates several test facilities for drop and stacking testing, leak testing and thermal testing. The large drop test tower allows dropping full-scale specimens up to 200,000 kg in any drop orientation as requested. The comprehensive test facilities combined with long-term experience, newest equipment and measurement devices according to the latest state-of-the-art technology ensures realisation of complex test campaigns for package safety evaluation.
Beyond that, non-destructive and destructive material test devices and experts are available. Equipment and application of all kinds of typical measurement categories can be offered for testing campaigns.
In recent years we performed testing of full-scale type B package models with complex handling and preparation procedures. The results were contributed for different package design approval procedures. Type A packages mainly designed for medical related transport purposes, were continuously tested according to the transport regulations over recent years as well. Moreover, we work on research topics with relevance to package safety. The mechanical behaviour of lid closure systems under transport and storage conditions and the thermal behaviour of impact limiters were recently of special importance for the assessment competencies of BAM and were investigated under use of our test facilities.
The paper describes the test facilities and capabilities for package design safety evaluation at BAM and shows examples from our recent work.
In recent years, additive manufacturing technologies have gained in importance. Laser powder bed fusion can be used for complex functional components or the production of workpieces in small quantities. High safety requirements, e.g. in aerospace, demand comprehensive quality control. Therefore, non-destructive offline inspection methods such as computed tomography are used after production. Recently, online non-destructive testing methods such as optical tomography have been developed to improve profitability and practicality. In this presentation, the applicability of eddy current inspection using GMR sensors for online inspection of PBF-LB/M parts is demonstrated. Eddy current testing is performed for each layer during the production process at frequencies uo to 1.2 MHz. Despite the use of high-resolution arrays with 128 elements, the testing time is kept low by an adapted hardware. Thus, the measurement can be performed during the manufacturing process without significantly slowing down the production process. In addition to the approach, the results of an online eddy current test of a step-shaped test specimen made of Haynes282 are presented.
In recent years, the demand for reliable, versatile, fluorescent pH and oxygen sensors has increased rapidly in many biomedical applications since these analytes are important indicators of cell function or certain diseases. Therefore, sensor particles are needed that are small enough to penetrate cells, non-toxic, and allow for close-up optical monitoring. When developing such sensor systems, one must consider the pH and oxygen range detectable by the sensor dye and the matrix material of the used carrier particles. Here, we present the development of pH- and oxygen-responsive polymeric beads functionalized with fluorescent dyad molecules that consist of an analyte-responsive fluorophore and an analyte-inert dye.
Optical pH sensors utilizing colorimetric or fluorescent indicator dyes are highly promising in many biomedical and life science applications where electrochemical sensors fail. For instance, optical sensors are not prone to electrical interferences, they are noninvasive and enable remote measurements. Moreover, fluorescence detection is very fast, highly sensitive, and provides several readout parameters ideal for multiplexing with nanometer resolution using simple, inexpensive, and miniaturizable instrumentation. Here, we present the design of a dyad sensor molecule, consisting of an analyte-responsive and an analyte inert reference fluorophore.
Degradation and damage analysis of composite pressure vessels via experimental modal analysis
(2023)
For mobile gas storage systems, the application of type IV pressure vessels is state of the art. Type IV tanks consist of an inner polymer liner fully wrapped with fibre-reinforced plastic (FRP). Because of the complex fabric of the FRP as well as a difficulty estimable interaction behaviour between the single components under load, there are still no satisfying non-destructive testing methods to assess the current state of failure nor to estimate the level of degradation accurately and economically. At BAM division 3.5, analysing the ageing process of mobile composite pressure vessels is a major task to ensure safe usage over the whole lifetime. In this context, key aspects of our ongoing research activities are the invention of new test procedures and the development of accurate lifetime prediction models. In order to determine the level of degradation or damage, one meaningful non-destructive approach is to analyse the structural dynamic behaviour via an experimental modal analysis (EMA). Over the last few years, different types and sizes of composite pressure vessels have been tested in several research projects. The presented paper gives an insight into how to extract and interpret modal parameters and how to fit them to the results of residual strength tests.
An Amorphous Lewis-acidic Zirconium Chloro Fluoride as HF Shuttle: C-F Bond Activation and Formation
(2023)
In this work, we successfully synthesized amorphous zirconium chloro fluoride (ZCF), which exhibits medium lewis acidity. In addition to investigating the local coordination sphere around the Zr atoms and the material properties, we were able to establish a catalytic behavior of ZCF in C-F bond activation reactions. We present a heterogeneous catalyst that performs dehydrofluorination of a fluoroalkane and consecutive hydrofluorination of an alkyne at room temperature.