Ingenieurwissenschaften und zugeordnete Tätigkeiten
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Eingeladener Vortrag
- nein (343)
Se presenta una guía completa del procedimiento experimental para la determinación del valor umbral ΔKth intrínseco y caracterización de curvas FCGR sobre el acero de alta resistencia S960QL empleando probetas de pequeña escala. El análisis se realiza comparando probetas SENB de diferentes geometrías, distinguiendo entre “convencionales” y “miniatura”. Las primeras con espesor (B) de 6 mm y anchura (W) de 19, y las segundas con B = 3 y dos valores distintos de W, 4 y 6 mm. A fin de identificar el valor umbral ΔKth intrínseco, la relación de cargas (R) aplicada en todos los ensayos fue 0,8. La técnica de caída de potencial (DCPD) se utilizó para la monitorización del tamaño de grieta a lo largo de los ensayos.
La evaluación de los resultados experimentales confirma la equiparación de resultados entre las distintas geometrías y configuraciones de ensayo practicadas, así como la viabilidad de emplear probetas de pequeña escala en la determinación del valor umbral ΔKth intrínseco. Esto abre nuevas perspectivas en lo relativo al empleo de probetas de reducidas dimensiones en la caracterización de materiales a fatiga. A su vez, permite ofrecer una serie de recomendaciones para reproducir con éxito ensayos semejantes utilizando probetas de pequeñas dimensiones de acero y otros materiales metálicos.
Für den Anlagenbau werden hochbelastete Komponenten aus Co-Cr-Legierungen hergestellt. Dabei ist die Zerspanung so herausfordernd, dass additive Fertigungsschritte oft wirtschaftlicher sind. Diese bedingen aber vorwiegende heterogene, anisotrope Gefüge und Eigenschaften und bei nachfolgender Fräsbearbeitung unstetige Zerspankräfte und instabile Spanvorgänge. Hierbei können hybride Zerspanprozesse helfen, hohe Belastungen für Werkzeug und Werkstückoberfläche zu minimieren. Diesbezügliche Charakterisierungen erfordern speziell adaptierte Zerspanungsanalysen.
Anhand eines Anwendungsbeispiels, bei dem eine Modifikation der Ausgangslegierung mit 1 % Hf erfolgte, wird die Wechselwirkung zwischen Gefügemorphologie und Fräsprozess dargestellt, der konventionelle mit einem hybriden ultraschallunterstützten Fräsprozess verglichen und die Charakterisierung des Werkzeugverschleißes anhand zweier verschiedener Fräser betrachtet. Analysen auftretender Prozesskräfte mittels Piezo-Mehrkomponenten-Dynamometer, der Werkzeugoszillation mittels Laser-Vibrometer und zusätzliche In-situ-Temperaturmessungen der Werkzeugschneiden mittels Highspeed-Pyrometer bilden den Kern der neuen Zerspanungsprüftechik.
Die vorgestellten Untersuchungsmethoden bilden die Vorgänge bei der Zerspanung additiv gefertigter Werkstoffe detailliert und reproduzierbar ab. Sowohl Legierungsmodifikation als auch hybride Prozessbedingungen lassen gezielte Einflüsse zur deutlichen Verbesserung der Zerspanungssituation zu.
Time resolved in situ monitoring of mechanochemical transformations by X-ray spectroscopy (XAS)
(2021)
Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis.
Time resolved in situ monitoring of mechanochemical transformations by X-ray spectroscopy (XAS)
(2021)
Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis.
Steelmaking slags are a by-product of steel production, that are currently used primarily in road construction, earthwork, and hydraulic engineering. In this use, the iron bound in the steelmaking slags (< 30 wt.%) is lost.
Recovery of iron from steelmaking slags is possible by thermochemical reductive treatment. The reductive treatment of liquid steelmaking slags causes iron oxides to be reduced to metallic iron, which separates from the mineral phase due to its higher density. The chemical composition of the mineral phase is thus adapted to that of the Portland cement clinker and the mineral alite, the most important component of Portland cement, is formed. This way, crude iron can be recovered, and at the same time a hydraulic binder can be produced.
This process, however, is uneconomical due to the high temperatures required (~1800 °C). In the current project, the process is to be adapted so that the reduction of liquid steelmaking slag can be carried out at ~1600 °C. The chemical composition is to be modified in such a way that the melting temperature of the slags as well as their viscosity are in a technically suitable range and still a product with good cementitious properties is obtained.
Experimentelle Charakterisierung der WIG-Schweißeignung einer Hoch- und Mittelentropie-Legierung
(2021)
Hoch- und Mittelentropie-Legierungen (engl. High/Medium Entropy Alloys–HEA/MEA) sind relativ neue Werkstoffklassen. Im Gegensatz zu herkömmlichen Legierungen bestehen HEA aus fünf bzw. MEA aus drei oder vier Legierungselementen im äquiatomaren Gleichgewicht. Um diese als reale Bauteile in die Anwendung zu überführen, muss die Verarbeitbarkeit ausführlich erforscht werden. In dieser Präsentation werden dafür erste Ergebnisse der schweißtechnischen Verarbeitung mittels WIG-Schweißen dargestellt. Dazu wurden zunächst die Schweißparameter mit einer Referenzlegierung (Ni-Basislegierung: 2.4858) bestimmt und auf eine CoCrFeMnNi-HEA sowie eine CoCrNi-MEA übertragen.
Hochfeste Feinkornbaustähle verfügen über ein großes Potenzial für gewichtsoptimierte, effiziente Strukturen in vielen modernen Stahlkonstruktion. Weitere Effizienzsteigerungen können durch additives Fertigen sowie bionische Bauweisen erreicht werden. Kommerzielle hochfeste Zusatzwerkstoffe für additives MSG-Schweißen (engl.: Wire Arc Additive Manufacturing, WAAM) sind bereits von den Schweißzusatzherstellern lieferbar. Derzeit ist jedoch eine breite industrielle Anwendung insbesondere für KMU aufgrund fehlender quantitativer Erkenntnisse und Richtlinien bezüglich schweißbedingter Beanspruchungen und Bauteilsicherheit während der Herstellung und des Betriebs stark limitiert. In einem gemeinsamen Forschungsprojekt (FOSTA-P1380/IGF21162BG) der BAM und der TU Chemnitz werden die mit Eigenspannungsausbildung und der Gefahr einer Kaltrissbildung verbundenen prozess- und werkstoffbedingten sowie konstruktiven Einflüsse untersucht. Im Fokus dieser Analysen steht die Bestimmung der Wechselwirkungen zwischen WAAM-Prozessparametern bzw. der Wärmeführung auf das Gefüge und die Eigenspannungen. Hierfür werden Referenzproben als offene Hohlquader mit definierten Abmessungen vollautomatisiert mit einem speziellen, hochfesten WAAM-Massivdraht (Streckgrenze >790 MPa) geschweißt. Die gezielte Einstellung der geometrischen Eigenschaften erfolgt durch Schweißparameter und Nahtaufbau bei ca. 4 kg/h mittlerer Abschmelzleistung. Die Wärmeführung wird innerhalb eines statistischen Versuchsplanes mittels Streckenenergie (200 kJ/m bis 650 kJ/m) und Zwischenlagentemperatur (100 °C bis 300 °C) so variiert, dass die t8/5-Abkühlzeiten dem empfohlenen Verarbeitungsbereich entsprechen (ca. 5 s bis 20 s). Ziel ist es bei konstanten geometrisch-konstruktiven Randbedingungen, den Einfluss der Wärmeführung auf Gefüge und resultierende Eigenspannungen zu analysieren. Für die Streckenenergie können neben den Gefügeeinflüssen aufgrund der resultierenden Abkühlzeit deutliche Effekte insbesondere auf die lokalen Eigenspannungen im Bauteil belegt werden. Das Schweißen mit zu hoher Wärmeeinbringung bzw. Abschmelzleistung kann zu ungünstigen Gefüge- und Bauteileigenschaften führen, gleichzeitig jedoch niedrigere Zugeigenspannungsniveaus bewirken. Solche komplexen Wechselwirkungen gilt es letztlich mit diesen Untersuchungen zu klären, um leicht anwendbare Verarbeitungsempfehlungen und Normvorgaben für ein wirtschaftliches, anforderungsgerechtes und risssicheres WAAM von hochfesten Stählen den Anwendern zur Verfügung zu stellen.
Cobalt chromium alloys are often used in turbine and plant construction. This is based on their high thermal and mechanical stress resistance as well as their high wear resistance to corrosive and abrasive loads. However, cobalt is a cost-intensive material that is difficult to machine. Moreover, increasingly complex structures and the optimisation of resource efficiency also require additive manufacturing steps for the production or repair of components in many sectors. Concerning inhomogeneity
and anisotropy of the microstructure and properties as well as manufacturing-related stresses, a lot of knowledge is still necessary for the economic use of additive welding processes in SMEs. As a result of the high stresses on the components and requirements for a high surface quality, a complementary use of additive and machining manufacturing processes is necessary. Thereby, Co–Cr alloys are extremely challenging for machining with geometrically defined cutting edges because of their low thermal conductivity combined with high strength and toughness. An approach to solve this problem is to refine and homogenise the microstructure. This is achieved by modifying the alloy with elements zirconium and hafnium, which are added up to a maximum of 1 wt.-%. A reduction of the process forces and stresses on the tool and work piece surface is also achievable via hybrid milling processes. There are already studies on the combined use of additive and machining manufacturing processes based on laser technology. However, knowledge based on powder and wire-based arc processes is
important, as these processes are more widespread. Furthermore, the effects on the surface zone of additively manufactured components by hybrid finish milling have not yet been a subject of research. The results show that the structural morphology could be significantly influenced with the addition of zirconium and hafnium.
Hochfeste Feinkornbaustähle verfügen über ein großes Potenzial für gewichtsoptimierte, effiziente Strukturen in vielen modernen Stahlkonstruktion. Weitere Effizienzsteigerungen können durch additives Fertigen sowie bionische Bauweisen erreicht werden. Kommerzielle hochfeste Zusatzwerkstoffe für additives MSG-Schweißen (engl.: Wire Arc Additive Manufacturing, WAAM) sind bereits von den Schweißzusatzherstellern lieferbar. Derzeit ist jedoch eine breite industrielle Anwendung insbesondere für KMU aufgrund fehlender quantitativer Erkenntnisse und Richtlinien bezüglich schweißbedingter Beanspruchungen und Bauteilsicherheit während der Herstellung und des Betriebs stark limitiert. In einem gemeinsamen Forschungsprojekt (FOSTA-P1380/IGF21162BG) der BAM und der TU Chemnitz werden die mit Eigenspannungsausbildung und der Gefahr einer Kaltrissbildung verbundenen prozess- und werkstoffbedingten sowie konstruktiven Einflüsse untersucht. Im Fokus dieser Analysen steht die Bestimmung der Wechselwirkungen zwischen WAAM-Prozessparametern bzw. der Wärmeführung auf das Gefüge und die Eigenspannungen. Hierfür werden Referenzproben als offene Hohlquader mit definierten Abmessungen vollautomatisiert mit einem speziellen, hochfesten WAAM-Massivdraht (Streckgrenze >790 MPa) geschweißt. Die gezielte Einstellung der geometrischen Eigenschaften erfolgt durch Schweißparameter und Nahtaufbau bei ca. 4 kg/h mittlerer Abschmelzleistung. Die Wärmeführung wird innerhalb eines statistischen Versuchsplanes mittels Streckenenergie (200 kJ/m bis 650 kJ/m) und Zwischenlagentemperatur (100 °C bis 300 °C) so variiert, dass die t8/5-Abkühlzeiten dem empfohlenen Verarbeitungsbereich entsprechen (ca. 5 s bis 20 s). Ziel ist es bei konstanten geometrisch-konstruktiven Randbedingungen, den Einfluss der Wärmeführung auf Gefüge und resultierende Eigenspannungen zu analysieren. Darüber hinaus erfolgt die Bestimmung des Einflusses der t8/5-Abkühlzeit auf die mechanisch-technologischen Eigenschaften des speziellen, hochfesten WAAM-Massivdrahts mithilfe von Dilatometeranalysen. Für die Streckenenergie können neben den Gefügeeinflüssen aufgrund der resultierenden Abkühlzeit deutliche Effekte insbesondere auf die lokalen Eigenspannungen im Bauteil belegt werden. Das Schweißen mit zu hoher Wärmeeinbringung bzw. Abschmelzleistung kann zu ungünstigen Gefüge- und Bauteileigenschaften führen, gleichzeitig jedoch niedrigere Zugeigenspannungsniveaus bewirken. Die Dilatometeranalysen zeigen für den untersuchten WAAM-Schweißzusatzwerkstoff eine großes t8/5-Zeitfenster mit einer vergleichsweise geringen Abnahme der Zugfestigkeit mit zunehmender t8/5-Abkühlzeit. Solche komplexen Wechselwirkungen gilt es letztlich mit diesen Untersuchungen zu klären, um leicht anwendbare Verarbeitungsempfehlungen und Normvorgaben für ein wirtschaftliches, anforderungsgerechtes und risssicheres WAAM von hochfesten Stählen den Anwendern zur Verfügung zu stellen.
Utilisation of alkali-sensitive aggregates for concrete pavements by internal hydrophobisation
(2021)
In order to avoid the increased ASR damage to concrete pavements in the German motorway network in the future, the ARS 04/2013 introduced mandatory suitability tests to exclude alkali-sensitive aggregates in new construction measures. This resulted in a significant reduction of suitable aggregates. Against this background, borderline alkali-sensitive aggregates are to be made usable by adding an internal water repellent agent during concrete casting. The ASR avoidance strategy is based on the significant reduction of the penetration of water and de-icing salt solution into the concrete pavement. Laboratory tests show that, with a suitable active ingredient, the ASR damage process can be significantly reduced with internal hydrophobisation. The disadvantage is that this is associated with a deterioration of the mechanical properties and the resistance to freeze-thaw with de-icing salt. The aim of the ongoing research is to reduce these disadvantages through targeted modification of the hydrophobising agent and air-entraining agent.
Am Ende des 19. und zu Beginn des 20. Jahrhunderts wurden auch in Berlin vermehrt Fassadenverblendung aus Eifeler Tuffsteinen errichtet. Die Eifeler Tuffsteine zeichnen sich aufgrund ihrer hohen Porosität einerseits durch eine gute Verarbeitbarkeit aus. Andererseits sind sie nur schwach gebunden und besitzen deshalb eine geringe Verwitterungsbeständigkeit.
Infrared thermography is a technique that allows to measure the temperatures of objects by analyzing the intensity of the thermal emission without the need of direct contact with very high spatial and temporal resolution. As the temperature is a fundamental factor for the additive manufacturing processes of metals, infrared thermography can provide experimental data that can be used for the validation of simulations and improving the understanding of the processes as well as for in-situ process monitoring for nondestructive evaluation (NDE) for quality control.
In this talk we will provide an overview over the possibilities of state of the art thermographic in-situ monitoring systems for the DED-LB/M and PBF-LB/M processes and the challenges such as phase transitions and unknown emissivity values in respect to the determination of real temperatures. We define the requirements for different camera systems in various configurations and give examples on the selection of appropriate measurement parameters and data acquisition techniques as well as on techniques for data analysis and interpretation. Finally, we compare in-situ monitoring methods against post NDE methods by analyzing the advantages and disadvantages of both.
This research was funded by BAM within the Focus Area Materials.
Laser Powder Bed Fusion (L-PBF), as one of the most promising production process in the field of metal additive manufacturing, enables traditional constructive solutions to be rethought and the manufacturing of optimized components according to the "form follows function" principle. The most significant obstacle for a broad industrial application of the L-PBF process is the inadequate quality assurance during the manufacturing process so far, leading to high production costs. Although several mainly camera based commercial in-process monitoring systems are already available, a deep understanding of the interpretation of the monitored data and correlation with actual defects is still lacking. One reason for this is the reduction of the complex process signature to just one measurement value.
The focus of this contribution is the presentation of the multispectral optical tomography as alternative to single measurand in-situ monitoring systems. The potential of this approach is hereby shown on L-PBF printed samples with induced process instabilities. Beyond that, an in-house developed L-PBF printer for further testing of multi-sensor in-situ monitoring systems is presented.
Das Pergamonmuseum ist eines der am meisten besuchten Museen Berlins. Es wird seit etwa 20 Jahren im Rahmen des 1999 von der Stiftung Preußischer Kulturbesitz beschlossenen Masterplans Museumsinsel schrittweise grundhaft instandgesetzt und um einen weiteren Flügel ergänzt, der 2025 fertig gestellt sein soll. In diesem Kontext wurde auch kurz nach dem Beschluss des Masterplans eine Bauzustandsanalyse an den in Originalgröße in der Antikensammlung ausgestellten Baudenk¬ mälern durchgeführt. Allerdings stellte man dabei fest, dass herkömmliche Erkundungsverfahren wie die Bauaufnahme, die baugeschichtliche Untersu¬ chung, das Quellenstudium sowie die äußerliche Begutachtung nicht ausreichen, um die innere Struktur der antiken Baudenkmäler hinreichend zu charakterisieren. Deshalb wurde die BAM im Jahr 2003 von der ARGE Pfanner Pergamonmuseum
beauftragt, in enger Zusammenarbeit mit zwei Ingenieurbüros, dem Ingenieurbüro Patitz (IGP) und der Gesellschaft für geophysikalische Unter¬ suchungen mbH (GGU) unter Hinzuziehung einer Restauratorin, die innere Struktur ausgewählter an¬ tiker Baudenkmäler zerstörungsfrei zu untersuchen. Das Ziel der zerstörungsfreien Strukturaufklärung zum inneren Aufbau der Bauteile war es, einerseits sicherheitsrelevante Informationen für die statische Nachweisführung bereitzustellen, sowie andererseits eine Planungsgrundlage für die eventuell erforder¬ liche Ertüchtigung der Baudenkmäler zu schaffen. Im Fokus der Untersuchungen standen dabei das Markttor von Milet und das Säulenjoch der Heiligen Halle am Markt von Priene1 • Im nachstehenden Beitrag werden exemplarisch die am Markttor von Milet durchgeführten Untersuchungen vorgestellt.
The paper addresses the “Functional coatings for mechanical applications: characterization and standardization” and the following points are discussed in more detail:
1. Mechanic alapplications (coatings for tools and components, system features vs. material parameters)
2. Mechanical characterization (instrumented indentation testing (IIT), centrifugal adhesion testing (CAT), state of standardization)
3. Topometric characterization (white light interference microscopy (WLIM, 3D), mechanical stylus (MS, 2D), state of standardization)
4. Optical characterization (spectroscopic ellipsometry (SE), inter-laboratory comparison, state of standardization)
Erstellung von Tiefenprofilen auf Schweißnähten mittels Laserinduzierter plasmaspektroskopie (LIPS)
(2021)
Duplexstähle sind hochlegierte, nichtrostende Stähle. Sie bieten aufgrund des ausgewogenen Phasenverhältnisses von Austenit und Ferrit einige physikalische Vorteile gegenüber anderen nichtrostenden Stählen. Beim Schweißen können sich durch die Kondensation von Schweißrauch und verdampftem Material verschiedene chemische Elemente auf der Oberfläche der erstarrten Schweißnaht anreichern. Dann ist die Bildung einer schützenden Chromoxidschicht nicht mehr gewährleistet und es kann an diesen Stellen zu Lochfraß kommen. Frühere Arbeiten haben gezeigt, dass die Anreicherung von Mangan und Chrom an der Oberfläche der Wärmeeinflusszone des geschweißten Edelstahls 304L mit LIBS gemessen werden kann. Wir stellen die Ergebnisse der Optimierung der LIBS-Parameter für präzise Dickenmessungen solcher dünnen Schichten und für Tiefenprofilmessungen vor. Dazu haben wir galvanisch beschichtete Kupferproben mit bekannten Schichtdicken verwendet. Die Mangankonzentration im Schweißgut ist reduziert. Dies hat einen großen Einfluss auf die metallografische Struktur des Materials.
In 1981 the OECD published the Test Guideline on Particle size and size distribution. This TG is still a valid document for the measurement of particles all over the world.
When nanomaterials gained importance, ISO set up a technical commitee for Nanotechnologies in 2005 and the OECD followed this step in 2006 with the Working Party on Manufactured Nanomaterials.
In the following years ISO and OECD published several documents about nanomaterials and the systematisation developed.
In 2017 it was finally clear that nanomaterials need to be adressed in another way than chemicals and in 2020 ECHA revised the REACH-Annexes accordingly and included nanomaterials.
Unfortunately there is a little problem with this: Only a few applicable test guidelines exit for the measurement of the nanomaterials. Several test guidelines date from 1981 and do not address nanomaterials.
The logical next step for the OECD would be to publish a series of test guidelines which are indeed currently prepared and will be shown in this talk.
Finally there is an additional need for the future of NM standardisation: Digitalisation.
The round robin test proves that the CAT-Technology provides statistically indistinguishable test results compared to TTM. A supplement to DIN EN 15870 taking into account CAT-Technology (with reference to equivalent increases of load and displacement) as second normative test method appears to make sense.
A presentation of a revision proposal at CEN TC 193 has been introduced with the decision to conduct a survey using the unchanged German revision proposal.
High-throughput computations are nowadays an established way to suggest new candidate materials for applications to experimentalists. Due to new packages for automation and access to databases of computed materials properties, these studies became more and more complex over the last years. Besides suggesting new candidate materials for applications, they also offer a way to understanding the materials properties based on chemical bonds. For example, we have recently used orbital-based bonding analysis to understand the results of high-throughput studies for spintronic materials, ferroelectric materials and photovoltaic materials in detail. To do so, we have developed Python tools for high-throughput bonding analysis with the programs VASP and Lobster (see www.cohp.de). They are based on the Python packages pymatgen, atomate, and custodian. This implementation will be discussed within the talk. We also expect that these tools offer possibilities to arrive at new descriptors based on chemical bonds for materials properties.
Aging of elastomer O-rings and PE neutron shielding materials for radioactive waste containers
(2021)
Our institution BAM in Berlin, Germany is concerned with research and testing of materials in the context of safety in chemistry and technology. Our working group is involved in the licensing procedures of casks for radioactive waste. Besides, we’re doing research on aging and lifetime prediction of elastomer O-rings and investigate degradation and thermal expansion of PE neutron shielding materials.
Eisenaluminide eignen sich als Werkstoff für sicherheitsrelevante Komponenten welche hohen thermischen, mechanischen und korrosiven Belastungen ausgesetzt sind. Mit ihrer geringen Dichte und der kostengünstigen Verfügbarkeit der Legierungsbestandteile bieten sie ein hohes Marktpotenzial und eignen sich als Substitutionswerkstoff konventioneller Hochtemperaturwerkstoffe. Durch die Verwendung von Dauerformen im Kokillenguss lassen sich FeAl-Bauteile bereits äußerst wirtschaftlich herstellen. Das dabei entstehende komplexe, mehrphasige, sehr feinkörnige Gefüge mit harten Ausscheidungen und hohen Festigkeiten erschwert jedoch eine nachfolgende spanende Bearbeitung mit hohen Belastungen auf Werkzeug und Bauteiloberfläche. Um eine gesamtheitlich wirtschaftliche Herstellungsroute zu ermöglichen, sollen im Hinblick auf die erschwerte Zerspanbarkeit geeignete Werkzeuge und Fräsprozesse entwickelt werden. Durch die Verwendung des hybriden Bearbeitungsverfahrens des ultraschallunterstützten Fräsens können diese Ziele unter Einhaltung der hohen Anforderung an die Oberflächenintegrität sicherheitsrelevanter Bauteile erreicht werden.
Detailed study of multicomponent systems in solid-state as well as in solution using X-ray diffraction and X-ray spectroscopy is one of the most common topics in modern materials chemistry. 5-6 component high-entropy alloys such as fcc- and bcc-structured AlxCoCrFeNi and fluorescent nanoparticles based on fluorite-structured SrF2 doped by rare-earth metals in organic solutions have high complexity and their local structure cannot be resolved using only diffraction. X-ray absorption spectroscopy should be applied to understand peculiarities in their local structure and make a link between structure on short and long ranges and their macroscopic properties. Here, based on two representativee examples, we discuss how a combination of several X-ray absorption edges might give new insights into complex materials.
Extended X-Ray absorption fine structure (exafs) to study local constitution of high-entropy alloys
(2021)
Modern design of superior multi-functional alloys composed of several principal components requires in-depth studies of their local structure for developing desired macroscopic properties. Herein, peculiarities of atomic arrangements on the local scale and electronic states of constituent elements in the single-phase face-centered cubic (fcc)- and body-centered cubic (bcc)-structured high-entropy Alx-CrFeCoNi alloys (x = 0.3 and 3, respectively) are explored by element-specific X-ray absorption spectroscopy in hard and soft X-ray energy ranges. Simulations based on the reverse Monte Carlo approach allow to perform a simultaneous fit of extended X-ray absorption fine structure spectra recorded at K absorption edges of each 3d constituent and to reconstruct the local environment within the first coordination shells of absorbers with high precision.
BAM line is multipurpose high-energy beamline. To extend studies of multicomponent alloys using EXAFS we perform own research and user experiments requiring multiedge spectroscopy, high-temperature and chemically aggressive sample environments. Our study of multicomponent alloys and high-entropy alloys open new perspectives in understanding their reactivity, corrosion, phase transformations and local ordering.
The unambiguous correlation of possible health and sustainability risks to nanoparticle size must be enabled by reliable measurement of nanoparticle size, to ensure comparability and compatibility between results measured under different methods. The NPSIZE project funded by European Metrology Program (EMPIR) develop methods, reference materials and modelling to improve the traceability chain, comparability and compatibility of nanoparticle size measurements. In this work, we present how spherical silica nanoparticles are synthetized with controlled monomodal or bimodal dispersion to be use as reference materials and international round-robin. Improving the fabrication requires a fine understanding of synthesis (1), coupled with an expertise of in-situ or ex-situ analysis methods. This is a new challenge for the analysis : determining not only average characteristics (size, chemical composition and shape ...) but also the concentration and the distribution over the population studied (2). Small-Angle X-ray Scattering (3) allows very precise measurements of the nanoparticles size and concentration that can be directly link to the metric system (4) (metrological traceability) . We developed a SAXS laboratory instrument dedicated to the in-situ characterization of nanoparticles, which enable fast measurements, and the monitoring of the synthesis parameters. Measurement protocols and software processing chain (5) (i.e. size distribution) are also combined & optimized.
Porosity in single-crystal nickel-base superalloys is removed by hot isostatic pressing (HIP) at temperatures above gamma’-solvus where the material is very soft and ductile. For example, single-crystal nickel-base superalloy CMSX-4 is HIPed at temperature 1288 °C, which is slightly higher than the gamma’-solvus temperature of this alloy equal to about 1280 °C. It is assumed that pore shrinking during HIP is mostly due to dislocation creep. Such a modelling of HIP of CMSX-4 was started in our group on the base of results of creep tests of [001] single-crystals at 1288 °C [1]. However, it was found later [2] that the alloy CMSX-4 shows very strong creep anisotropy at 1288 °C. Therefore, for calibration of the creep law, creep tests of different orientations under different stress levels are required at the HIP temperature. This was the main task of present work. Single-crystals of CMSX-4 of axial orientations [001], [011], [123] and [111] were cast by VIAM Moscow and tested by BAM Berlin under creep conditions at 1288 °C and stress levels between 4 MPa and 16 MPa. At all stress levels, the creep rate increases by an order of magnitude when changing the orientation from [001] to [111] with [011] and [123] orientations in between. Such a character of creep anisotropy corresponds to the orientation dependence of the Schmid factor for octahedral glide.
The crystal viscoplasticity model developed in [1] was improved to better represent the time induced softening observed during creep. The creep tests for different stresses and orientations as well as pore closure were simulated. The results of pore closure simulation are compared with measurements of porosity decrease during Hiping.
Duplex steels are high-alloyed, stainless steels. They offer some physical advantages over other stainless steels due to the balanced phase ratio of austenite and ferrite. During welding processes, when welding fumes and vaporized material condensates, different chemical elements can accumulate on the surface of the solidified weld. Then, the formation of a protective chromium oxide layer is no longer guaranteed and pitting corrosion can occur at these places. Previous work has shown that the accumulation of manganese and chromium on the surface of the heat-affected zone of the welded high-grade steel 304L can be measured by LIBS.
We present the results of the optimization of LIBS parameters for precise thickness measurements of such thin films and for depth profile measurements Therefore, we used galvanically coated copper samples with known film thicknesses. The Concentration of manganese is reduced in the weld metal. This has a high impact on the metallografic structure of the material.
For metal-based additive manufacturing (AM) to achieve leaner designs and enable longer life predictions, it is imperative to gain a detailed knowledge of the residual stress (RS) built-up. Laser powder bed fusion (LPBF) is an AM technique particularly prone to RS because of the highly localized heat source, extremely high cooling rates (in the order of 103-107 K/s), and successive cooling and heating cycles of the solidified material. Furthermore, RS analysis of LPBF materials by diffraction methods is peculiar because of the complexity of the thermal history, the possibility of encountering high levels of surface roughness, spatial textural variations and/or changes in solute concentrations at the component scale.
Diverse aspects of the influence of scanning strategies on the as-built residual stress state of a LPBF IN718 alloy will be presented, with particular focus on the challenges that AM microstructures pose for a reliable RS determination.
This lecture deals with the sliding behaviour of polymer materials in hydrogen environment. After a short introduction of the hydrogen activities at BAM, the tribological performances of polymer materials in gaseous hydrogen are presented and compared with air and vacuum environment. The second part focusses on the influence of the counterface materials in hydrogen. Finally, the last section is dedicated to experiments liquid hydrogen.
This lecture deals with the sliding behaviour of polymer composites in vacuum environment. At first, the effect of the polymer matrix and solid lubricants such as graphite and MoS2 are presented. The second part focusses on the influence of the residual pressure with experimental results obtained in high and ultrahigh vacuum.
In recent years, we have come to appreciate the astounding intricacy of the formation process of minerals from ions in aqueous solutions. The original ‘textbook’ image o these phenomena, stemming from the adaptation of classical nucleation and growth theories, has increased in complexity due to the discovery of a variety of precursor and intermediate species [e.g. 1], including solute clusters (e.g. prenucleation clusters PNCs), liquid(-like) phases, as well as amorphous and nanocrystalline solids etc. In general, these precursor or intermediate species constitute different, often short-lived points along the pathway from dissolved ions to the final solids (typically crystals in this context). In this regard synchrotron-based scattering (SAXS/WAXS/HEXD appears to be the perfect tool to follow in situ and in a time-resolved manner the crystallization pathways because of the temporal and spatial length scales that can be directly accessed with these techniques.
Here, I show how we used scattering to probe the crystallization mechanisms o calcium sulfate. CaSO4 minerals (i.e. gypsum, anhydrite and bassanite) are widespread in natural and industrial environments. During the last several years, a number o studies have revealed indeed that nucleation in the CaSO4-H2O system is non-classical My SAXS data demonstrate that gypsum precipitation, involves formation and aggregation of sub-3 nm primary species. These species constitute building blocks o an amorphous precursor phase [2]. Further, I show how in situ high-energy X-ray diffraction experiments and molecular dynamics (MD) simulations can be combined to derive the atomic structure of the primary CaSO4 clusters seen at small-angles [3]. fitted several plausible structures to the derived pair distribution functions and explored their dynamic properties using unbiased MD simulations based on polarizable force fields. Finally, based on combined SAXS/WAXS, broad-q-range measurements, show that the process of formation of bassanite, a less hydrated form of CaSO4, is very similar to the formation of gypsum: it also involves the aggregation of small primary species into larger disordered aggregates [4].
Based on these recent insights I formulated a tentative general model for calcium sulfate precipitation from solution. This model involves primary species that are formed through the assembly of multiple Ca2+ and SO42- ions into nanoclusters. These nanoclusters assemble into poorly ordered (i.e. amorphous) hydrated aggregates which in turn undergo ordering into coherent crystalline units of either gypsum o bassanite (and possibly anhydrite). Determination of the structure and (meta)stability of the primary species is important from both a fundamental, e.g. establishing a general non-classical nucleation model, and applied perspective; e.g. allow for an improved design of additives for greater control of the nucleation pathway
Compared to the clear, real-space images you can get from electron microscopy, X-ray scattering patterns are rather featureless. These patterns, however, contain structural information from all of the material structure illuminated by the X-ray beam. With this technique, you can measure nanoparticle dispersions, catalysts, composites, MOF powders, battery materials, light metal alloys and gels to reveal information on the structural features found within these materials. We have even measured many such materials for several research groups from the University of Birmingham, revealing structure features in the sub-nm to the micrometer range.
Measuring an X-ray scattering pattern is relatively easy, but measuring a high-quality, useful pattern requires significant effort and good laboratory organization. Such laboratory organization can help address the reproducibility crisis in science, and easily multiply the scientific output of a laboratory, while greatly elevating the quality of the measurements. We have demonstrated this for small- and wide-angle X-ray scattering in the MOUSE project (Methodology Optimization for Ultrafine Structure Exploration) [1]. With the MOUSE, we have combined: a) a comprehensive and highly automated laboratory workflow with b) a heavily modified X-ray scattering instrument. This combination allows us to collect fully traceable scattering data, within a well-documented, FAIR-compliant data flow (akin to what is found at the more automated synchrotron beamlines). With two full-time researchers, our lab collects and interprets thousands of datasets, on hundreds of samples, for dozens of projects per year, supporting many users along the entire process from sample selection and preparation, to the analysis of the resulting data.
Introduction
A good laboratory organization can help address the reproducibility crisis in science, and easily multiply the scientific output of a laboratory, while greatly elevating the quality of the measurements. We have demonstrated this for small- and wide-angle X-ray scattering in the MOUSE project (Methodology Optimization for Ultrafine Structure Exploration). In the MOUSE, we have combined: a) a comprehensive laboratory workflow with b) a heavily modified, highly automated X-ray scattering instrument. This combination allows us to collect fully traceable scattering data, with a well-documented data flow (akin to what is found at the more automated beamlines). With two full-time researchers, the lab collects and interprets thousands of datasets, on hundreds of samples for dozens of projects per year, supporting many users along the entire process from sample selection and preparation, to the analysis of the resulting data.
While these numbers do not light a candle to those achieved by our hardworking compatriots at the synchrotron beamlines, the laboratory approach does allow us to continually modify and fine-tune the integral methodology. So for the last three years, we have incorporated e.g. FAIR principles, traceability, automated processing, data curation strategies, as well as a host of good scattering practices into the MOUSE system. We have concomitantly expanded our purview as specialists to include an increased responsibility for the entire scattering aspect of the resultant publications. This ensures full exploitation of the data quality, whilst avoiding common pitfalls.
Talk scope
This talk will present the MOUSE project as implemented to date, and will introduce foreseeable upgrades and changes. These upgrades include better pre-experiment sample scattering predictions to filter projects on the basis of their suitability, exploitation of the measurement database for detecting long-term changes and automated flagging of datasets, extending the measurement range through an Ultra-SAXS module, and enhancing MC fitting with sample scattering simulations for better matching of odd-shaped scatterers.
Heterogene Fehlstellendichten und Mikrostrukturausbildungen sind große Heraus-forderungen für den Einsatz des pulverbettbasierten Laserstrahlschmelzens (L PBF) besonders für sicherheitskritische Bauteile. Unter der Vielzahl an Einflussfaktoren auf die Qualität und die mechanischen Eigenschaften von L PBF-Bauteilen hat die Zwischenlagenzeit (ILT) bisher wenig Beachtung gefunden. Sie nimmt ebenso wie die Bauteilgeometrie Einfluss auf die thermische Historie während der Fertigung. Ihr Einfluss auf die intrinsische Vorerwärmung ist in Kombination mit der Bauteilhöhe mittels thermografischer Temperaturmessung untersucht worden. Signifikante Unterschiede in der thermischen Historie konnten dabei mit variierenden Schmelzbaddimensionen, Korngrößen und Fehlstellendichten am Beispiel der austenitischen Stahllegierung AISI 316L in Zusammenhang gebracht werden.
Die Entwicklung digitaler Prozesse für die Materialwissenschaft und Werkstofftechnik muss naturgemäß auch die Charakterisierungsmethoden der Werkstoffprüfung abbilden, die oft durch eine hohe Komplexität gekennzeichnet sind. Als vorteilhaft erweist sich dabei der hohe Standardisierungsgrad, der sich z.B. in klaren Anforderungen an die eingesetzten Prüfmittel und festgelegten Vorgehensweisen ausdrückt. Diese können (und müssen) in entsprechenden digitalen Versuchsbeschreibungen abgebildet werden, wobei sich die klaren Datenstrukturen und Terminologien als vorteilhaft erweisen.
The laser powder bed fusion of 316L leads to the formation of large residual stress. In this presentation, different stress relieve treatments were employed to assess their potential to relax the residual stress. The residual stress was determined by X-ray and neutron diffraction. The results give insights on the range of relaxation one can obtain by employing low and high temperature heat treatments and relates the relaxation to changes in the microstructure.
Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals.1 The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms.2-4 We recently introduced different setups enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy and thermography. The presented setup allows the detection of crystalline, amorphous, eutectic, and liquid intermediates. Furthermore, the chemical composition of the reaction mixture was found to be directly correlated with changes in the temperature profile of the reaction. The resulting deeper kinetic and thermodynamic understanding of milling processes is the key for future optimization of mechanochemical syntheses. In this contribution, we will discuss our recent results investigating the formation of (polymorphic) cocrystals and coordination polymers.2,3,5 Our results indicate that in situ investigation of milling reactions offer a new approach to tune and optimize mechanochemical syntheses.
Mechanochemistry has emerged as one of the most interesting synthetic protocols to produce new materials. The development of mechanochemistry as a synthetic method is supported by excellent research by many groups worldwide in a wide range of applications. The potential of mechanochemistry is also reflected in the inclusion in IUPAC’s 10 chemical innovations that will change our world’.[1] Solvent-free methodologies lead to unique chemical processes during synthesis with the consequent formation of martials with new properties.2 In this contribution, we will discuss our recent results investigating the formation of (polymorphic) cocrystals, coordination polymers, metal oxides and metal nanoparticles.[3-8] We introduced different setups enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy and thermography.
Der DIN Ringversuch weist nach, dass die CAT Technologie zur ZPM Prüfung statistisch nicht unterscheidbare Prüfergebnisse liefert, so dass lediglich eine Ergänzung der DIN EN 15870 unter Berücksichtigung der CAT-Technologie (mit Bezug auf äquivalente Kraft und Weg zunahmen) als zweiter normativer Prüfmethode sinnvoll erscheint.
Vorstellung des Revisionsvorschlages im CEN TC 193 am 08.04.2021 mit dem Beschluss, eine Umfrage unter Verwendung des unveränderten deutschen Revisionsvorschlages durchzuführen.
The contact between train wheels and rail tracks is known to induce material degradation in the form of wear, and rolling contact fatigue in the railhead. Rails with a pearlitic microstructure have proven to provide the best wear resistance under severe wheel-rail interaction in heavy haul applications. High speed laser cladding, a state-of-the-art surface engineering technique, is a promising solution to repair damaged railheads. However, without appropriate preheating or processing strategies, the utilized steel grades lead to martensite formation and cracking during deposition welding.
In this study, laser cladding of low-alloy steel at very high speeds was investigated, without preheating the railheads. Process speeds of up to 27 m/min and laser power of 2 kW are used. The clad, heat affected zone and base material are examined for cracks and martensite formation by hardness tests and metallographic inspections. A methodology for process optimization is presented and the specimens are characterized for suitability. Within the resulting narrow HAZ, the hardness could be significantly reduced.
Additive manufacturing of metals gains increasing relevance in the industrial field for part production. However, especially for safety relevant applications, a suitable quality assurance is needed. A time and cost efficient route to achieve this goal is in-situ monitoring of the build process. Here, the BAM project ProMoAM (Process monitoring in additive manufacturing) is briefly introduced and recent advances of BAM in the field of in-situ monitoring of the L-PBF and the LMD process using thermography are presented.
High entropy alloys (HEAs) are considered as a new class of alloys containing at least 5 elements with concentrations between 5 and 35 atomic percent. There has been a growing interest in HEAs in the material research field in recent years. Due to their adjustable composition, which enables the modifications of mechanical properties (such as hardness, strength and ductility etc) and their stability at high temperatures, HEAs have been the focus of various studies.
Especially the corrosion behavior of HEAs has been a wide research interest. Since the grazing exit X-ray fluorescence (GEXRF) offers a non-destructive way to collect notable information regarding the high temperature oxidation, we consider it as a useful method to investigate how HEAs behave in corrosive environments.
The main idea of grazing geometry is to enhance the fluorescence signal of the surface. This enables highly sensitive surface analyses of thin protective film on surface in sub-micrometer scale. Position-sensitive area detectors provide information regarding the signal emitted from the sample as a function of emission angle and thus allow depth-sensitive analysis. Furthermore, the data collected from samples of an incidence energy which lays within a specific energy range provides XANES data to determine oxidation states. Moreover, since GEXRF profiles can also be simulated through physical models (Urbach 1999), they enable us to determine the layer thickness of a given sample in a non-destructive way.
In this contribution, we present the preliminary results of a conceptual study regarding layer properties of CrCoNi medium entropy alloy. The successful implementation of such methodological concept will pave the way for the investigation of more complex alloys with multiple layers, which is planned for the later phases of the project.
The performance of functional coatings relies strongly on the stability of the polymer-metal interface. The increasing utilization of multi-material structures in the automotive and aerospace industry necessitates a fundamental understanding of the processes leading to interface degradation for the development of novel strategies to increase corrosion and delamination resistance.
The aim of this project is to investigate the corrosion processes at the buried interface of thin film coated aluminium alloy AA2024-T3 under corrosive and coupled corrosive-mechanical load. A spin coating procedure was developed to synthesize epoxy-like coatings and their nanofiller loaded composites with controlled thickness by layer-by-layer deposition of poly[(o-cresyl glycidyl ether)-co-formaldehyde] and poly-(ethylenimine) bi-layers. Our results indicate that the incorporation of graphene into the epoxy-based coatings leads to the improvement of mechanical and barrier properties. Furthermore, the functional groups play important roles in the interfacial bonding between polymer matrix and the nanofillers. Atomic force microscopy (AFM) results indicate very homogeneous and dense films with a thickness of ~25 nm per bi-layer and the successful integration of the nanofillers into the composite coatings. Ellipsometry measurements of film thickness verified a proportional film growth with the number of deposited layers.
The degradation and delamination behavior of the coating systems was characterized by means of in situ AFM corrosion experiments. Complementary energy dispersive X-ray spectroscopy (EDX) analysis was used to correlate the corrosion and delamination behavior with the different intermetallic particle chemistries and distributions. The presentation will summarize our results on the effect of coating composition and build-up on the local corrosion processes on thin film covered AA2024-T3 aluminium alloys.
This presentation is a summary of the work from the past 20 years’ development of PMC-testing at the BAM-FB 5.3 with respect to safety-relevant design of advanced light weight structures in aircraft, wind turbine and automotive applications. The talk begins with wood as an example from nature, and emphasizes that load case, fiber architectural design and the production process and quality have to go hand in hand to generate an advanced light weight structure. Since PMC-relevant basic findings of mankind span across hundreds of years, high-performance composite applications today are based more on long term experiences than on breakthrough inventions of modern days.
In the second part of the talk, future plans and projects of FB-5.3 are presented, specifically addressing H2-safety, circular economy, recycling by design and digitalization of PMC-technologies.
Im Rahmen des Vortrags werden die neusten Ergebnisse aus dem Fachbereich 5.3 zur Beschreibung des Ermüdungsverhaltens von FKV mittels Mikromechanischer-Modelle präsentiert. Explizit wird der theoretische Ansatz am Beispiel von GFK unter thermomechanischer Beanspruchung hergeleitet und an Hand von Versuchsergebnissen verifiziert.
Wir präsentieren Labor- und Synchrotron-Röntgenrefraktionstechniken, wie sie an der BAM implementiert sind.
Wir zeigen, dass die Labor-Röntgenrefraktionstopographie (XRRT) und die Synchrotron-Röntgenrefraktionsradiographie (SRRR) außergewöhnliche Werkzeuge zur Untersuchung von Schädigungen und inneren Defekten (Poren, Mikrorisse) in leichten Materialien wie Keramiken und Kompositen sind. Tatsächlich nutzen diese Techniken den an Grenzflächen auftretenden Röntgenbrechungseffekt aus, um den Kontrast zwischen dem (schwach absorbierenden) Objekt und dem Hintergrund zu erhöhen. Dies ermöglicht die Erkennung sehr kleiner Objekte (sogar bis zu 1 nm Rissöffnung) und die Quantifizierung ihrer spezifischen Oberfläche, die mit ihrem Einfluss auf die Materialeigenschaften korreliert. Wir zeigen die folgenden Anwendungen: a) Quantifizierung der Faserentbindung in laminaten Epoxid-Kohlenstoff-Verbundwerkstoffen; b) Mapping der Porengröße in gesinterten Keramiken; c) Eindringstiefe von Aschen in Keramikschutzschichten; d) Quantifizierung der Porenorientierung in Diesel Partikelfiltern; e) 3D-Darstellung von Makrorissen und Faserentbindung in Verbundwerkstoffen auf Ti-Basis für Anwendungen in der Luft- und Raumfahrt (unter Verwendung von Röntgenrefraktionstomographie).
Advanced Manufacturing and Advanced Materials have been identified by the European Commission as one of six Key Enabling Technologies (KETs), the full exploitation of which will create advanced and sustainable economies. Metrology is a key enabler for progress of these KETs. EURAMET, which is the association of metrology institutes in Europe, has addressed the vital importance of Metrology for these KETs through the support for the creation of a European Metrology Network for Advanced Manufacturing. The EMN for Advanced Manufacturing (AdvanceManu) was approved in June 2021 and held the formal kick-of meeting in October 2022. The EMN comprises both National Metrology Institutes (NMIs) from across Europe and other designated Institutes (Dis). The EMN is organized in three sections; Advanced Materials, Smart Manufacturing Systems and Manufactured components and products. The aim of the EMN is to engage with stakeholders in the field of Advanced Manufacturing and Advanced Materials (Large & SMEs, industry organisations, existing networks and academia) with the aim to prepare a Strategic Research Agenda (SRA) for Metrology for Advanced Manufacturing. In the shorter term, an orientation paper is aimed to be produce to in the context of the European Partnership for Metrology. In addition to the SRA, the EMN will establish knowledge and technology transfer and promotion plan. This includes leveraging the existing research results from the completed and running EMPIR JRP projects funded through EURAMET.
This presentation will outline the EMN for Advanced Manufacturing, describing the structures and goals, the route to the production of the SRA and the progress made to date identifying the key metrology challenges across the related Key Industrial Sectors (KICs). In particular, the presentation aims to inform the community on how to be involved in the shaping of the strategic research agenda for the future of Metrology for Advanced Manufacturing and Advanced Materials.
The progress of Advanced Manufacturing, which has been identified by the European Commission as a Key Enabling Technology (KET) for future economic and societal progress is strongly reliant on the development of metrology capabilities. EURAMET, the association of metrology institutes in Europe, has established metrology research programs to address the metrology requirements across a spectrum of different thematic areas. In order to leverage the benefits of these developments on the wider industrial landscape, a high-level coordination of the metrology community supporting the Advanced Manufacturing landscape is required. This coordination is aimed to be achieved by the establishment of European Metrology Networks (EMNs), which are intended by EURAMET to provide a sustainable structure for stakeholder engagement and support. The joint networking project 19NET01 AdvManuNet funded by EMPIR for 4 years, started in June 2020 and aims to accelerate the process of establishing an EMN to strengthen Europe’s position in Advanced Manufacturing. The AdvManuNet project aims to support the establishment of an EMN on Advanced Manufacturing via the following specific aims:
1. Creation of a single hub for stakeholder engagement across the landscape of various industrial sectors including relevant societies and standardization bodies.
2. Development of a Strategic Research Agenda (SRA) and roadmaps for Advanced Manufacturing metrology based on the stakeholder engagement activities, considering current gaps in metrological capabilities existing networks and roadmaps.
3. Establish a knowledge-sharing program for Advanced Manufacturing stakeholders, promoting the dissemination and exploitation of the results of the project, including those from previous EU funded research projects.
4. Development of a sustainable web-based platform and service desk for Advanced Manufacturing stakeholders to allow for easy access to European metrology capabilities and support the wider advanced manufacturing community with metrology-based requirements.
5. Develop a plan for a coordinated and sustainable European metrology infrastructure for Advanced Manufacturing via a European Metrology Network.
The project concept followed by the scope and definition of Advanced Manufacturing will be described. The analysis of the current capability of metrology for Advanced Manufacturing and the preliminary concepts for the strategic research agenda will be presented with a focus on dimensional metrology.
Additive manufacturing (AM) technologies are experiencing an exceedingly rapid growth, driven by their potential through layer wise deposition for transformational improvements of engineering design, leading to efficiency and performance improvements. Laser Powder Bed Fusion (LPBF) is an Additive Manufacturing (AM) method which permits the fabrication of complex structures that cannot otherwise be produced via conventional subtractive manufacturing methods. Nevertheless, the rapid cooling rates associated with this process results in the formation of significant and complex residual stress (RS) fields. A large body of both experimental and simulation research has been dedicated in recent years to the control and mitigation of RS in AM. In order to validate simulations with the end goal of being able to model the residual stress state in AM components and to devise strategies for their reduction during manufacturing, experimental methods need to be able to accurately determine 3D residual stresses fields in complex geometries. Several destructive and non-destructive methods can be used to analyze the RS state, the choice of which depends on the geometry and the information required. Diffraction-based methods using penetrating neutron and synchrotron X-rays at large scale facilities offer the possibility to non-destructively spatially resolve both surface and bulk residual stresses in complex components and track their changes following applied thermal or mechanical loads. This presentation will overview the success stories of using large scale facilities by the BAM for the characterization of residual stresses in additively manufactured metallic alloys. In particular, the study of the influence of process parameters on the residual stress state and the relaxation of these stresses through heat treatment will be presented. However there remains challenges to overcome particularly of the hypotheses underlying the experimental determination of residual stresses, which will be discussed.
Introduction to AGIL
(2021)
If the amount of sulfate within the mix design for concrete is not balanced, ettringite formation which first controls solidification continues while the concrete is hardening. Ettringite forms by reaction of sulfate contained in the cement or in some admixture with calcium aluminate (C3A) as cement component. The “late primary
ettringite formation” promotes an increase in volume within the hardened concrete leading to cracks. To analyze the effect of substituting part of ordinary Portland cement (OPC) by a treated brown coal fly ash mortar bars were tested according to ASTM C452. This test method was originally developed to extrapolate from the internal to external sulfate attack and is based on the idea that by testing a concrete mixture containing sulfate the process of deterioration is accelerated because it does not have to diffuse into the concrete before reaction first. In addition to the samples prescribed in ASTM C452 further samples in the size of the German SVA procedure were tested also designed for accessing the external sulfate resistance. The results show that while the replacement of 25 % of cement by brown coal fly ash leads to length changes around the limit defined by ASTM, the substitution of 50 % cement exceeded the limit by a multiple. The progress of expansion is the very similar for the two geometries tested. In-situ XRD measurements confirmed that while for pastes made of OPC the formation of ettringite is completed after 20 hours, this is not true for the mixtures containing the brown coal fly ash.
In a different study the effect of hydrothermal treatment on the phase composition of ultra-high-performance concrete was analyzed. The results show that the sulfate and aluminate resulting from the decomposition of ettringite are bound into new phases. If this binding is permanent this might allow the larger use of sulfate bearing raw
materials.
The stability of materials is a very important property for materials discovery. In recent years, we have explored several approaches for advancing the prediction of the stability of crystals (e.g., classical chemical heuristics and machine-learned interatomic potentials). For example, we have assessed a famous chemical heuristic – the Pauling rules – regarding their usefulness for structure prediction. They are only of limited predictive power, i.e. the rules 2 to 5 only work for 13 % of all tested oxides. Furthermore, we have shown that machine-learned interatomic potentials can be used to predict phonon properties of a range of silicon allotropes accurately and, therefore, they can also be used to assess the dynamic stability of materials. To do so, we have developed new schemes to build reference databases for machine learned interatomic potentials.
Der Fachbereich 7.6 untersucht seit einiger Zeit an Auslagerungsständen auf dem Testgelände in Horstwalde Korrosion im maritimen Bereich. Im Moment läuft das System mit künstlichem Meerwasser und simuliert die Bewitterung von Metallproben unter angenäherten klimatischen Bedingungen ähnlich zum natürlichem Habitat. Im Laufe der Zeit konnte nicht intendierter mikrobieller bewuchs beobachtet werden. Es stellte sich die Frage, welche Mikroorganismen vorlagen und ob diese einen Einfluss auf die Korrosionsuntersuchungen haben könnte. Aus diesem Grund wurden 16S-rRNA Untersuchungen durchgeführt welche alle drei Domänen des Lebens widerspiegeln Bakterien, Archaea und Eukaryoten. Es konnte gezeigt werden, dass über 95% der vorliegenden Biomasse Grünalgen waren, die durch Licht Eintrag in den Container Photosynthese betrieben und dadurch an Biomasse zunahmen. Des weiteren konnten Bakterien detektiert werden, welche in der Regel halophilen und aeroben Habitaten zu finden sind. Allerdings wurden auch Sulfat reduzierende Bakterien (MIC) detektiert, wenn auch in einem geringen prozentualen Anteil. Es muss allerdings Berücksichtigt werden, dass die mikrobielle Zusammensetzung sich im Laufe der Zeit weiter ändern kann. Als Ursprung der Biomasse wird, das künstliche Sediment vermutet. Außerdem wäre es für zukünftige Experiment denkbar, das System mit echtem Sediment aus dem marinen Habitat anzuimpfen.
Both essential aspects of the surface of solid matter, its morphology and chemistry, are studied traditionally at BAM starting in the 60’s with different cyclical research focus areas, mostly related either to applicative research or method development. In the recent years, the focus has shifted almost exclusively to the nano-analytics of advanced materials such as complex nanoparticles, (ultra)thin films/coatings, nanocomposites, 2D materials, energy materials, etc. This is also the reason why BAM has established recently the new Competence Center nano@BAM (www.bam.de/Navigation/DE/Themen/Material/Nanotechnologie/sichere-nanomaterialien.html) with the five sub-fields nanoCharacterisation, nanoMaterial, nanoSafety, nanoData and nanoTechnology. The link to the BAM central guidelines to the safety in technology and chemistry is given by the development of reference products such as reference measurement procedures, reference (nano)materials, and newly reference data sets. Thus, an internationally well-networked group in surface analysis has been established @BAM, with regular contributions to integral analytical characterization with metrological and standardization background.
Examples of newly developed methodical approaches will be given with an emphasis on correlative nano-analysis of morphology and chemistry of nanomaterials. Correlative imaging by STEM-in-SEM with high-resolution SEM and EDX, and further with AFM or the new technique TKD (Transmission Kikuchi Diffraction) will be explained on various examples of nanostructures, both as starting materials and embedded/functionalized nanoparticles in products. The unique analytical benefits of the Auger electron probe as a veritable nano-tool for surface chemistry will be highlighted. The panoply of advanced surface characterization methods @BAM is completed by discussing examples of hybrid analysis of the bulk of nanomaterials by X-ray Spectroscopy with the highest surface-sensitive methods X-ray Photoelectron Spectroscopy (XPS) and Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS). Particularly for the analysis of the surface chemistry of nanostructures, such as the completeness of the shells of core-shell nanoparticles or in-depth and lateral gradients of chemistry within mesoporous thin layers, the latter methods are inherent.
Other special developments like approaches for the quantitative determination of the roughness of particle surface by electron microscopy or for the quantitative determination of the porosity of thin mesoporous layers by electron probe microanalysis (EPMA) with SEM will be presented in conjunction with the corresponding advanced materials studied.
Current research projects, promising ideas, including ongoing (pre-)standardization activities in the field of the challenging nano/surface analysis will be touched systematically, with the open goal of identifying future bilateral cooperation possibilities between EMPA and BAM.
Corrosion is a very expensive and serious problem in the different industry sectors, eg. Petroleum-, On- and off-shore, infrastructure. It is estimated that 20% of all corrosion damage is caused by microorganisms or microbiologically influenced corrosion (MIC). Several microorganisms are known to cause corrosion, including sulfate-reducing bacteria, nitrate-reducing bacteria, methanogens etc. For several years, methanogens were regarded as a mild corroder (~0.065 mm/yr), largely due to a lack of detailed investigation on the corrosion mechanism under real-environment simulated conditions. Resulting in the common belief that siderite, a non-conductive compound, is the sole corrosion product (CP) of methanogen-induced MIC (Mi-MIC).
To simulate natural environmental conditions, we developed and introduced the multiport flow column system (MFC), a multi-sectional corrosion flow-cell. Using the MFC, we obtained ten times higher corrosion rates than previously reported. With a combination of several analytical techniques, such as ToF-SIMS, SEM-EDS and FIB-SEM, we found strong indication that siderite is not the sole corrosion product of Mi-MIC. The corrosion layers contained phosphorus, oxygen, magnesium, calcium and iron. The differences in the CP between static and dynamic environments demonstrated the impact of testing procedures on the corrosive potential of methanogens. To further verify and deepen our understanding of Mi-MIC, we are currently studying the influence of additional environmental parameters (e.g. pH, salinity, flow rate) on Mi-MIC.
Overall, results of this study will expand the current understanding of MIC from both analytical and mechanistic points of view, thus aiding the development of different mitigation strategies for various industry sectors.
The role of methanogens in microbiologically influenced corrosion (Mi-MIC) is often neglected, due to 1) low reported corrosion rates and 2) the suspected corrosion product siderite, which is electrically non-conductive. Typically, MIC corrosion studies are carried out using batch cultures, which did not represent the dynamic conditions, i.e. pipeline and provide insufficient information on the overall corrosion potential.
We established a unique approach, a multiport flow column (MFC), to simulate pipeline conditions and obtained 10-times higher corrosion rates than previously published. Our result showed that testing procedures have a large impact on the corrosive potential of methanogens. We found strong indications with a combination of ToF-SIMS, SEM-EDS and FIB-SEM analyses that siderite is not the sole corrosion product. The corrosion layers contain phosphorus, oxygen, magnesium, calcium and iron. To verify and deepen our understanding of Mi-MIC, we are currently studying the influence of other environmental parameters (e.g. pH) on Mi-MIC.
Microbiologically influenced corrosion (MIC) is a now well-known challenge and affects industry, society and infrastructure. For a long time, the impact of methanogen-induced MIC (Mi-MIC) was underestimated. This was mainly due to the rather low published corrosion rates and the presumed corrosion product siderite, which is not electrically conductive. In our laboratory, we were able to show that this trivialization or underestimation of Mi-MIC was due to the nature of the testing. The static systems used so far do not provide environmentally relevant information about the corrosion rate and the corrosion product, especially for methanogens
To further illustrate the importance of the environment on the MIC process, we established a multiport flow column (MFC), to simulate the natural environment. With this method, and in contrast to published results using the static conditions, we obtained ten times higher corrosion rates. We analyzed the corrosion products with a combination of techniques, like ToF-SIMS, SEM-EDS and FIB-SEM, and found strong evidence that siderite is not the sole corrosion product of Mi-MIC. The corrosion layers contain phosphorus, oxygen, magnesium, calcium and iron and lacked on carbon-related species. It is hypothesized that methanogens may have influenced the nucleation process of siderite, converting bicarbonate into carbon dioxide for methanogenesis. This results in increased localized corrosion and reduced siderite formation. To verify and deepen our understanding of Mi-MIC, we are currently studying the influence of additional environmental parameters (e.g. pH, salinity, flow rate etc.) on Mi-MIC and the subsequent impacts on corrosion rates and the corrosion products.
Overall, results of this study will expand the current understanding of MIC from both analytical and mechanistic points of view, thus aiding the development of different mitigation strategies for various industry sectors.
Metal Additive manufacturing (AM) technologies such as Laser Powder Bed Fusion (LPBF) enable the fabrication of complex structures, giving rise to potential improvements in component and manufacturing efficiency. However, the processes are typically characterized by the generation of high magnitude residual stress (RS) which can have detrimental consequences for subsequent applications. Therefore, the characterization of these RS fields and the understanding of their formation and mitigation through optimized processing is crucial for the wider uptake of the technology. Due to the potential complex nature and high value of components manufactured by LPBF, it is important to have suitable characterisation methods which can determine the spatial variations of RS in a non-destructive manner. Neutron diffraction is considered to be the best suited for these requirements. However, the microstructures developed in the complex thermal cycles experience in the production can pose challenges to the ND method for RS analysis. The BAM has conducted significant research over the past years to overcome these obstacles, enabling higher confidence in the RS determined in LPBF materials by neutron diffraction. This contribution will overview some of these advancements made recently at European neutron sources including on Stress-Spec at FRM2/MLZ.
Die Vortrag gibt einen Überblick, warum Kaltrissprüfung von geschweißten Stählen ständig weiterentwickelt werden muss. Am Beispiel des Implant- und Tekken-Tests werden die Einsatz- u. Anwendungsgrenzen bewertet. Zu berücksichtigen ist, dass beim Schweißen eine äußere mechan. Beanspruchung durch bauteilspezifische Steifigkeitsverhältnisse wirksam ist. Zusätzlich werden weiterführende Prüfverfahren zur Bestimmung der Wasserstoffkonzentration und -diffusion in Schweißnähten vorgestellt, wie die Trägergasheißextraktion (TGHE) für die Ermittlung der Wasserstoffkonzentration (ISO 3690) oder Hochtemperaturdiffusionskoeffizienten. Diese Werte sind für die schweißtechnische Praxis von großer Bedeutung, um Haltezeiten z.B. für das Wasserstoffarmglühen abzuleiten.
Kristalle sind in der Regel spröde und neigen dazu, bei mechanischer Belastung zu brechen. Dieses Verhalten schränkt ihre Anwendungsmöglichkeiten stark ein. Durch die Entdeckung von mechanischer Flexibilität in Kristallen wurde dieses Problem gelöst. Je nach Art der Verformung können Kristalle in plastisch (irreversibel) oder elastisch (reversibel) biegbar unterteilt werden. Die Verbindung 4-Brom-6-[(6-chlorpyridin-2-ylimino)methyl]phenol (BCMPMP) ist ein vielversprechender Kandidat für die Anwendung als flexibler Waveguide. BCMPMP hat zwei verschiedene Polymorphe mit unterschiedlichen optischen und mechanischen Eigenschaften. Die spröden Kristalle der Form I zeigen eine sehr schwache Emission bei 605 nm (λex = 425 nm; Photolumineszenz-Quantenausbeute Φ = 0,4 %). Im Gegensatz dazu zeigt die plastische Form II eine starke Emission bei 585 nm (λex = 425 nm; Φ = 8,7 %). Aufgrund der mechanischen Flexibilität wurde die Eignung der Form II als Waveguide untersucht.
In order to assess new nanomaterials and nanoparticles for potential risks to health and the environment, they need to be well-characterised. The measurement of constituent nanoparticle size, shape, and size distribution are important factors for the risk evaluation process.
EMPIR project Improved traceability chain of nanoparticle size measurements (17NRM04, nPSize) is working to assess a range of traceable nanoparticle measurement approaches, including Electron Microscopy (SEM, TEM, STEM-in-SEM), Atomic Force Microscopy and Small Angle X-ray Scattering, and deliver improved calibration methods to users. For the techniques under investigation, physical models of their response to a range of nanoparticle types are developed. Validated reference materials are also used for inter-comparisons of measurement systems, with an evaluation of the associated measurement uncertainty. With project contributions to standards development work, manufacturers will be better placed to assess the human and environmental risks posed by nanomaterials across a whole range of products.
Hydrogen production via water electrolysis will be an essential cornerstone in development of sustainable, fossil-free fuel and chemical production on a global scale. The activity and stability of each catalyst is highly dependent on the properties of the coating, i.e., phase composition, crystallinity, accessible surface area, and many other factors. The key to developing improved catalysts is a better understanding of the relationships between their performance, stability, and physicochemical properties. However, these relationships can be complex and are also strongly influenced by the reaction environment. Therefore, operando analysis of the catalyst material during catalysis at realistic potentials and current densities is highly desirable. However, many analytical techniques cannot be applied in liquid environments at realistic potentials and current densities.
We propose environmental ellipsometric analysis in a dedicated electrochemical flow cell as a method to evaluate gas evolution reactions operando under realistic working conditions. Figure 1 illustrates schematically the developed technique. Key factors to success are highly active model-type catalysts, a suitable sample environment, and a deep understanding of the appropriate model development, as well as concise cross validation with numerous other analytical techniques.
The method was developed and validated by analyzing a calcination series (300 – 600 °C) of mesoporous templated IrOx films ex-situ and operando under oxygen evolution reaction (OER) conditions. The employed environmental electrochemical spectroscopic ellipsometric (ECSE) analysis revealed during OER the change of optical and electronic properties, i.e. the dielectric functions, resistivity and band-to-band transitions (p-d band transitions). Film thickness and porosity were validated by means of scanning electron microscopy (SEM), X-ray reflectometry (XRR) or ellipsometric porosimetry (EP), electrical and electronic properties by means of conductivity measurements, X-ray photoelectron spectroscopy (XPS) or UV-Vis-NIR absorption spectroscopy. The electronic structures of the catalysts from valence electron energy loss spectra (VEELS) derived from ε1 and ε2 from SE measurements reveal a direct correlation with electrochemical activities in OER.
In the presentation reversible and irreversible potential-dependent changes of the catalyst properties during operation will be discussed along with the dynamics of gas formation, transport and dissolution at different potentials.
One of the challenges of the high-power hybrid laser welding of thick steels is the sensitivity of the process of the process to manufacturing tolerances. This usually leads to a time-consuming preparation of the welding edges, such as milling. The study deals with the influence of the edge quality of milled and plasma-cut steel made of S355J2 with a wall thickness of 20 mm on the laser hybrid welded seam quality. Furthermore, the gap bridgeability and the tolerances towards edge misalignment was investigated. An AC magnet was used as backing support to prevent sagging and positioned under the workpiece, to generate an upwards directed electromagnetic pressure. The profiles of the edges and the gap on the top and root side were measured using a digital camera. Single-pass laser hybrid welds of plasma-cut edges could be welded using a laser beam power of just 13.7 kW. A gap bridgeability up to 2 mm and misalignment of edges up to 2 mm could be achieved successful. Additionally, the independence of the cutting side and the welding side was shown, so that samples were welded to the opposite side to their cutting. For evaluation of internal defects or irregularities, X-ray images were carried out. Charpy impact strength tests were performed to determine the toughness of the welds.
Vorstellung der Ergebnisse bei der Entwicklung einer neuen OECD Prüfrichtlinie zur Bestimmung der Partikelgröße und Anzahlgrößenverteilung von Nanomaterialien.
Ergebnisse:
Ideal sphärische Partikel sind gut und verlässlich mit vielen Methoden charakterisierbar.
Reale (Nicht ideale) Materialien sind gut charakterisierbar, wenn eine gewisse Homogenität und Stabilität vorliegt.
Stark inhomogene und stark agglomerierende Partikel liefern deutlich unterschiedliche Ergebnisse für verschiedene Methoden.
Partikel mit geringen Größenunterschieden lassen sich mit allen Methoden gut charakterisieren.
Partikel mit sehr deutlichen Größenunterschieden führen häufig zu einer Unterbewertung der kleineren Partikel.
Vollautomatische Partikeldetektion bei elektronenmikroskopischen Aufnahmen ist z.Zt. noch stark fehleranfällig und kann daher nicht empfohlen werden.
Es hat sich gezeigt, dass alle Methoden zur Bestimmung der Partikelgrößenverteilung Vor- und Nachteile haben. Es ist dringend zu empfehlen Größenverteilungen immer mit mindestens zwei unterschiedlichen Methoden zu bestimmen: Bildgebend und mit gute Anzahlstatistik.
Verschiedene Durchmesser wurden in der TG-PSD mit einem Indexsystem versehen, welches zukünftig Verwechslungen zwischen unterschiedlichen Durchmessern vermeiden soll.
Wird ein bestimmter Durchmesser benötigt (z.B. hydrodynamisch, aerodynamisch), muss die Methode passend gewählt werden. Eine Umrechnung von einem Durchmesser in einen anderen ist in der Regel fehlerbehaftet.
Es wurde ein einheitliches Reporting-System in der TG-PSD eingeführt.
Vorstellung der Ergebnisse bei der Entwicklung einer neuen OECD Prüfrichtlinie zur Bestimmung der Partikelgröße und Anzahlgrößenverteilung von Nanomaterialien. (Projektteil Fasern.)
Ergebnisse:
Abweichungen zwischen SEM and TEM insbesondere bei langen Fasern
Die Anwendung von TEM auf kurze Fasern < 5 µm beschränkt
Für SEM wurde keine signifikante Abhängigkeit der Bestimmung der Faserdurchmesser von der Pixelgröße der Aufnahmen festgestellt
Für TEM wurde eine Abhängigkeit der Bestimmung der Faserdurchmesser von der Pixelgröße festgestellt
Der Einfluss der Bildauswertenden auf die Varianz der Ergebnisse ist klein im Vergleich zu der gesamten Varianz.
Nanofasern können mit TEM und SEM bestimmt werden!
OECD Prüfrichtlinie zur Bestimmung der Partikelgröße und Anzahlgrößenverteilung von Nanomaterialien
(2021)
Abschlusspräsentation des Projektes "OECD Prüfrichtlinie zur Bestimmung der Partikelgröße und Anzahlgrößenverteilung von Nanomaterialien" - Projektteil Nanopartikel.
Es hat sich gezeigt, dass alle Methoden zur Bestimmung der Partikelgrößenverteilung Vor- und Nachteile haben. Es wird dringend empfohlen Größenverteilungen immer mit mindestens zwei unterschiedlichen Methoden zu bestimmen: Bildgebend und mit gute Anzahlstatistik.
Verschiedene Durchmesser wurden in der TG-PSD mit einem Indexsystem versehen, welches zukünftig Verwechslungen zwischen unterschiedlichen Durchmessern vermeiden soll.
Wird ein bestimmter Durchmesser benötigt (z.B. hydrodynamisch, aerodynamisch), muss die Methode passend gewählt werden. Eine Umrechnung von einem Durchmesser in einen anderen ist in der Regel fehlerbehaftet.
Es wurde ein einheitliches Reporting-System in der TG-PSD eingeführt.
The effect of the environmental conditions on the threshold against fatigue crack propagation
(2021)
The threshold against fatigue crack propagation (ΔKth) is a crucial parameter for the damage tolerance assessment of engineering components subjected to cyclic loading and it is composed by two distinct components, one intrinsic, dependent on the elastic material properties and the lattice type, and one extrinsic, related to the occurrence of crack closure effects. An important issue is that several factors can influence ΔKth and, in general, the fatigue crack propagation behavior. In this work, the influence of the experimental procedure, air humidity and test parameters on da/dN-ΔK data has been investigated. Results are discussed with their potential causes and consequences on the calculations of the residual lifetime.
The lecture focuses on the mechanisms of non-desired gas bubble formation and foaming during the sintering of glass powder compacts. It is shown that foaming is driven by carbon gases and that carbonates, encapsulated in micropores or mechaniacally dissolved beneath the glass surface, provide the major foaming source.
The Kitagawa-Takahashi (KT) diagram is a proven concept for describing the fatigue limit in presence of a defect or crack. It can be determined empirically with great experimental effort. It can also be estimated by means of the El Haddad relationship if the endurance limit and the long fatigue crack propagation threshold are available in reasonable accuracy. A third option is the determination using the cyclic R-curve, which describes the dependency of the fatigue crack propagation threshold on the crack growth at the short crack propagation stage. This can be experimentally determined using a closure-free initial pre-crack. It can then be applied to the determination of crack arrest for a given applied load and a given defect or crack size. Compared to the other two methods mentioned above, this option has considerable advantages: It can be applied to any component and any stress ratio. It allows the treatment of multiple cracks and provides estimations of the S-N curve in the finite life regime as well as at the endurance limit. Compared to the empirical determination of the KT diagram, the experimental effort is significantly lower and compared to the El Haddad approach it avoids problems such as the use of non-conservative long fatigue crack propagation thresholds (when the conventional load reduction method is applied to materials prone to corrosion) and the mathematical predetermination of the curve shape. The work introduces the method and provides a critical discussion as well as quantitative comparison between the different methods.
The damage tolerance approach is widely used in the design and estimation of inspection intervals of safety-relevant metallic components subject to fatigue loading. The approach relies on the knowledge of the fatigue crack propagation characteristics, wherein a relevant role is played by the fatigue crack propagation threshold. Nevertheless, the use of material data determined by testing on conventional specimens is not straightforward in case of thin-walled components such as turbine-blades or additively manufactured parts, in which the local variation of material properties in highly stressed regions must be considered. In these cases, the possibility of investigating the fatigue crack propagation properties on a limited portion of material is crucial. For this purpose, a new test methodology has been developed for small-scale specimens which allows the determination of the intrinsic fatigue crack propagation threshold and the near-threshold regime. The use of small-scale specimens poses a challenge to the applicability of the method to metallic materials, especially regarding the
limitations on material strength and requirements for the application of the linear elastic fracture mechanics concepts. These aspects are discussed in this work. Furthermore, the application on the high strength steel S960QL is presented, along with a comparison with data determined by conventional testing.
In der aktuellen RL-SIB (DAfStB) wie auch in der TR Instandsetzung (DIBt) ist bei Anwendung des Instandsetzungsprinzips W-CL der Erfolg der Maßnahme durch Einbau und Messung von Korrosionsstromsensoren gefordert. Art und Aufbau der Sensoren sowie Kriterien zur Bewertung der Ergebnisse gibt es nicht.
Ziel ist die Ausarbeitung eines Regelwerks-Entwurfes für die Art und den Aufbau von Korrosionsmonitoring-Systemen sowie für Kriterien zur zuverlässigen Bewertung der Messergebnisse, mit denen der Erfolg bei verschiedenen Instandsetzungskonzepten überprüft werden kann.
Accurate and quantitative photoluminescence measurements are mandatory for the comparison of different emitter classes and the rational design of the next generation of molecular and nanoscale reporters as well as for most applications relying on their luminescence features in the life and material sciences and nanobiophotonics. In the following, procedures for the determination of the spectroscopic key parameter photoluminescence quantum yield, i.e., the number of emitted per absorbed photons, in the UV/vis/NIR/SWIR are presented including pitfalls and achievable uncertainties and material-specific effects related to certain emitter classes are addressed. Special emphasis is dedicated to luminescent nanocrystals.
High and medium entropy alloys gained increasing academic and industrial interest as novel materials for engineering applications. This project is aiming to clarify and compare the general and local corrosion properties of high entropy alloy CrMnFeCoNi and medium entropy alloy CrCoNi in different aqueous environments. The focus lies on the local corrosion processes that result either from microstructural imperfections (inclusions, defects at grain boundaries etc.) in the base material or processing related changes in the microstructure and/or local composition.
The corrosion behavior of the alloys was monitored via potentiodynamic polarization experiments and the local corrosion characteristics were further investigated by means of scanning electrochemical microscopy (SECM). Their passivation behavior was analyzed in two different electrolyte systems (NaCl and H2SO4 c = 0.1M). The characterization of the surface morphology and composition of the passive film was performed by means of atomic force microscopy (AFM), scanning electron microscopy coupled with energy dispersive X-Ray spectroscopy (SEM/EDX) and X-Ray photoelectron spectroscopy (XPS), respectively. To analyze the semiconducting properties of the passive film Mott-Schottky analysis was conducted.
Considering long term corrosion effects, electrochemical work was supported with immersion tests and the analysis of corrosion products by SEM/EDX, ICP-MS and XPS depth-profiling. Our results indicate that the medium entropy alloy CrCoNi has a significantly higher corrosion resistance due to the higher concentration of chromium in comparison to the high entropy alloy CrMnFeCoNi. The presentation will summarize our results on the mechanistical aspects of the observed high corrosion resistance.
High and medium entropy alloys gained increasing academic and industrial interest as novel materials for engineering applications. This project is aiming to clarify and compare the general and local corrosion properties of high entropy alloy CrMnFeCoNi and medium entropy alloy CrCoNi in different aqueous environments. The focus lies on the local corrosion processes that result either from microstructural imperfections (inclusions, defects at grain boundaries etc.) in the base material or processing related changes in the microstructure and/or local composition.
The corrosion behavior of the alloys was monitored via potentiodynamic polarization experiments and the local corrosion characteristics were further investigated by means of scanning electrochemical microscopy (SECM). Their passivation behavior was analyzed in three different electrolyte systems (NaCl, H2SO4 and NaClO4; c = 0.1M). The characterization of the surface morphology and composition of the passive film was performed by means of atomic force microscopy (AFM), scanning electron microscopy coupled with energy dispersive X-Ray spectroscopy (SEM/EDX) and X-Ray photoelectron spectroscopy (XPS), respectively.
Considering long term corrosion effects, electrochemical work was supported with immersion tests and the analysis of corrosion products by SEM/EDX and XPS depth-profiling. Our results indicate that the medium entropy alloy CrCoNi has a significantly higher corrosion resistance due to the higher concentration of Chromium in comparison to the high entropy alloy CrMnFeCoNi. The presentation will summarize our results on the mechanistical aspects of the observed high corrosion resistance.
High and medium entropy alloys gained increasing academic and industrial interest as novel materials for engineering applications. This project is aiming to clarify and compare the general and local corrosion properties of high entropy alloy CrMnFeCoNi and medium entropy alloy CrCoNi in different aqueous environments. The focus lies on the local corrosion processes that result either from microstructural imperfections (inclusions, defects at grain boundaries etc.) in the base material or processing related changes in the microstructure and/or local composition.
The corrosion behavior of the alloys was monitored via potentiodynamic polarization experiments and the local corrosion characteristics were further investigated by means of scanning electrochemical microscopy (SECM). Their passivation behavior was analyzed in three different electrolyte systems (NaCl, H2SO4 and NaClO4; c = 0.1M). The characterization of the surface morphology and composition of the passive film was performed by means of atomic force microscopy (AFM), scanning electron microscopy coupled with energy dispersive X-Ray spectroscopy (SEM/EDX) and X-Ray photoelectron spectroscopy (XPS), respectively.
Considering long term corrosion effects, electrochemical work was supported with immersion tests and the analysis of corrosion products by SEM/EDX and XPS depth-profiling. Our results indicate that the medium entropy alloy CrCoNi has a significantly higher corrosion resistance due to the higher concentration of Chromium in comparison to the high entropy alloy CrMnFeCoNi. The presentation will summarize our results on the mechanistical aspects of the observed high corrosion resistance.
In order to find a resource efficient approach for the fatigue lifetime prediction of laser powder bed fusion (L-PBF) processed AlSi10Mg material, results of tensile and fatigue tests were compared. The specimens were manufactured with three different L-PBF machines and studied in different heat treatment conditions (as-built, annealed, T6 heat treated). The investigations showed that the high attainable tensile strength properties after the manufacturing process are not beneficial in the high cycle fatigue (HCF) regime. In contrast, the applied heat treatments, which lead typically to a decrease of ultimate tensile strength, improved dramatically the fatigue behavior. Additionally, a clear correlation between the elongation at fracture and HCF resistance has been found for individual heat treatment conditions. This empiric relationship provides an estimation of the fatigue resistance in the presence of material defects and can be implemented in part and process approvals.
In this presentation tribological investigations on steels, polymers and coatings in gaseous and liquid hydrogen are shown. For steels the results of show that although martensitic steel may suffer from hydrogen embrittlement, application e.g. in roller bearings is possible. On the other hand, martensitic transformation of austenitic steels may cause problems in the application of these materials. Furthermore, the tribological performance of polymer composites with and without solid lubricant fillers in gaseous and liquid hydrogen was investigated. In particular, PEEK- and PTFE-matrix compounds showed low friction and sufficient low wear under these conditions. Among the solid lubricants, carbon-based materials are appropriate for hydrogen applications. Several variants of DLC and ta-C materials were tested. Beside the results for hydrogen, also a comparison with CH4-environment is shown.
Lanthanide-based upconversion nanoparticles (UCNPs) like hexagonal 𝛽-NaYF4 UCNPs doped with Yb3+ and Er3+, which efficiently convert 976 nm light to ultraviolet, visible, and near infrared photons, offer new strategies for luminescence-based sensing, barcoding, and Imaging. Their upconversion (UC) luminescence (UCL) features like UCL intensity, quantum yield, relative spectral distribution / UCL luminescence color, and luminescence decay kinetics are, however, strongly influenced by particle size, dopant ion concentration, particle architecture, surface chemistry including presence and thickness of surface passivation and shielding shells, microenvironment/presence of quenchers with high energy vibrations, and excitation power density (P).
We present here a comprehensive study of the influence of excitation power density on the UCL features of different types of UCNPs, focusing on Yb3+ and Er3+ co-doped NaYF4 core-only and core-shell nanostructures with different sizes and doping ion concentration, which underlines the importance of P-dependent optimum dopant concentrations for UCNP performance and the potential of P-tuning of UCL.
Phase Transformation and Strain Evolution during Welding of Low Transformation Temperature Alloys
(2021)
In this work, the phase and strain formation in multipass welding of LTT gas metal arc welds were observed under realistic restraints by means of time resolved angular-dispersive synchrotron X-ray diffraction at the High Energy Materials Science beamline HEMS at PETRA III (DESY), Hamburg Germany. It was shown that the strain evolution during cooling correlates with the amount of martensite formed. Both, the strain of martensite and austenite are affected during phase transformation. Even though dilution processes limit the LTT effect in the root compared to the top layer, the strains are significantly reduced compared to the conventional weld metal. The observed effects are found for both Ni and Mn based LTT filler metals regardless of their respective Ms temperature.
Welding processes of duplex stainless steels cause an unbalanced austenite (γ)/ferrite (δ) ratio due to high cooling rates and changes in chemical composition. That causes a degradation of mechanical properties and corrosion resistance. In situ monitoring of the weld pool is to be realized with the help of laser-induced breakdown spectroscopy (LIBS). A major advantage of this technique is the highly accurate time and spatially resolved measurement of the chemical composition during welding. Previous research has established that the LIBS method is suitable to detect chemical elements during welding and to show a distribution of selected elements. Chemical composition in the WM and HAZ can now be quantified using calibration curves generated by certified reference materials (CRM). Furthermore, a cooling rate can be plotted against the measured electron temperature.
Rissfortschrittsdaten sind notwendig für die bruchmechanische Bewertung zyklisch beanspruchter Bauteile. Deren zuverlässige experimentelle Ermittlung wird von verschiedenen Faktoren beeinflusst, was wiederum zur Unsicherheit bei der Restlebensdauerprognose führen kann. Der Vortrag befasst sich mit der Untersuchung der Einflussfaktoren auf die Ermittlung von Rissfortschrittsdaten. Eine Prozedur zur Berechnung der Restlebensdauer wird eingeführt, die auf rissschließfrei Rissfortschrittsdaten basiert.
Iron aluminides depict a sustainable and light-weight material class which could be employed in many applications requiring high strength at intermediate to high temperatures. According to first results, the alloy Fe-26Al-4Mo-0.5Ti-1B surpasses conventional materials in wet corrosion resistance and creep resistance up to 650 °C. For these reasons, the AiF research project “WAFEAL – Materials applications for iron aluminides” was initiated to transfer these findings into a standardised materials dataset and to derive best practices for processing. In the first place, a set of different microstructures adjusted by varying casting methods, wall thicknesses and heat treatments was investigated and correlated with hardness on macro and micro scale. Correlations were drawn between solidification rates and resulting grain sizes and hardness. The effect of vacancy hardening was only verified for wall thickness as low as 2.5 mm. Moreover, a common decrease of macrohardness after a heat treatment at 1000 °C for 100 h was observed irrespective of casting process or wall thickness. This effect was linked with an unexpected decrease of the complex boride phase fraction which acts as a hardening phase.
In recent years, we have come to appreciate the astounding intricacy of the formation process of minerals from ions in aqueous solutions. The original ‘textbook’ image of these phenomena, stemming from the adaptation of classical nucleation and growth theories, has increased in complexity due to the discovery of a variety of precursor and intermediate species [e.g. 1], including solute clusters (e.g. prenucleation clusters, PNCs), liquid(-like) phases, as well as amorphous and nanocrystalline solids etc. In general, these precursor or intermediate species constitute different, often short-lived, points along the pathway from dissolved ions to the final solids (typically crystals in this context). In this regard synchrotron-based scattering (SAXS/WAXS/HEXD) appears to be the perfect tool to follow in situ and in a time-resolved manner the crystallization pathways because of the temporal and spatial length scales that can be directly accessed with these techniques.
Here, we show how we used scattering to probe the crystallization mechanisms of calcium sulfate. CaSO4 minerals (i.e. gypsum, anhydrite and bassanite) are widespread in natural and industrial environments. During the last several years, a number of studies have revealed indeed that nucleation in the CaSO4-H2O system is non-classical. Our SAXS data demonstrate that gypsum precipitation, involves formation and aggregation of sub-3 nm primary species. These species constitute building blocks of an amorphous precursor phase [2]. Further, we show how in situ high-energy X-ray diffraction experiments and molecular dynamics (MD) simulations can be combined to derive the atomic structure of the primary CaSO4 clusters seen at small-angles [3]. We fitted several plausible structures to the derived pair distribution functions and explored their dynamic properties using unbiased MD simulations based on polarizable force fields. Finally, based on combined SAXS/WAXS, broad-q-range measurements, we show that the process of formation of bassanite, a less hydrated form of CaSO4, is very similar to the formation of gypsum: it also involves the aggregation of small primary species into larger disordered aggregates [4].
Based on these recent insights we formulated a tentative general model for calcium sulfate precipitation from solution. This model involves primary species that are formed through the assembly of multiple Ca2+ and SO42- ions into nanoclusters. These nanoclusters assemble into poorly ordered (i.e. amorphous) hydrated aggregates, which in turn undergo ordering into coherent crystalline units of either gypsum or bassanite (and possibly anhydrite). Determination of the structure and (meta)stability of the primary species is important from both a fundamental, e.g. establishing a general non-classical nucleation model, and applied perspective; e.g. allow for an improved design of additives for greater control of the nucleation pathway.
Polyethylen hoher Dichte (PE-HD) ist ein weit verbreitetes Material für Transportbehälter, die oft für eine längere Nutzungsdauer vorgesehen sind. Insbesondere in diesem Fall können mikroskopische Schäden im Material auch weit unterhalb der Streckgrenze auftreten, die durch eine Spannungskonzentration verursacht werden, deren Ursprung in intrinsischen Materialfehlern oder äußeren Kratzern liegt. Mit fortschreitender Schädigung bilden sich Rissstrukturen, die von verstreckten Fibrillen aufgespannt werden, bis es zum Versagen dieser Fibrillen kommt und sich der Riss ausbreitet. Dieser Schadensmechanismus des langsamen Risswachstums kann durch eine Vielzahl von Umgebungsmedien beschleunigt werden und wird dann als "environmental stress cracking" (ESC) bezeichnet. Eine international normierte Methode zur Validierung der Spannungsrissbeständigkeit von PE-HD Materialien ist der „Full Notch Creep Test“ (FNCT).
Anhand von Bruchflächenauswertungen mittels Rasterelektronenmikroskopie und Laser-Scanning-Mikroskopie, werden die typischen Schädigungsstrukturen des ESC sichtbar. Die fibrillierten Strukturen des ESC auf der Bruchfläche von PE-HD ergeben sich besonders bei oberflächenaktiven wässrigen Umgebungsmedien. In Lösungsmittel-Umgebungsmedien, im Zusammenspiel mit PE-HD, kommt es aufgrund der plastifizierenden Wirkung zur Herabsetzung der Streckspannung und Bruchflächen aus dem FNCT veranschaulichen keine signifikanten Anzeichen des Schädigungsmechanismus ESC.
Multi-element systems with defined entropy (HEA - High Entropy Alloy or MEA - Medium Entropy Alloy) are rather new material concepts that are becoming increasingly important in materials research and development. Some HEA systems show significantly improved properties or combinations of properties, e.g., the overcome of the trade-off between high strength and ductility. Thus, the synthesis, the resulting microstructures, and properties of HEA have been primarily investigated so far. In addition, processing is crucial to achieve a transfer of potential HEA/MEA materials to real applications, e.g. highly stressed components. Since fusion welding is the most important joining process for metals, it is of vital importance to investigate the weldability of these materials. However, this has rarely been the subject of research up to date. For that reason, in this work the weldability depending on the surface preparation of a CoCrFeMnNi-HEA and a CoCrNi-MEA for TIG welding is investigated. The fusion welding of longer plates is described here for the first time for the CoCrNi alloy. The welds of both materials showed distinct formation of cracks in the heat affected zone (HAZ). Optical and scanning electron microscopy analysis clearly confirmed an intergranular fracture topography. But based on the results, the crack mechanism cannot be conclusively clarified as either a liquid metal embrittlement (LME) or hot cracking like liquid film separation occurred.
High entropy alloys (HEA) are a new class of materials. In contrast to conventional alloys, HEA are single-phase alloys with at least five alloying elements. HEAs have enormous application potential due to (postulated) excellent structural property combinations from low to high temperatures. For HEA-application as structural materials in real components, a key issue is the suitability for joining processing. Requirements for the reliable and safe joining of these materials are crucial regarding economical component manufacture for future applications. In this context, friction stir welding (FSW) is a promising joining process due to the welding process temperature below the material melting point avoiding major issues, e. g. formation of (hard and brittle) intermetallic phases, which may have detrimental influences on the weld joint properties.
This study presents elementary research about the FSW process influences on a CoCrFeMnNi-HEA with focus on the microstructure and mechanical properties. For that purpose, the FSW joint of the HEA is compared to that of an austenitic stainless steel AISI 304. The microstructures of the welds were investigated and characterized by means of light microscopy, SEM, EBSD and XRD. Hardness and tensile testing were applied to determine influences on the mechanical properties. Generally, a comparable weldability of HEA and AISI 304 in terms of metallurgical characteristics and resulting mechanical properties exhibited. For the weld joints of both materials typical characteristics regarding FSW were observed within the weld metal and thermo-mechanically influenced zone: fine-grained stirred zone with increased hardness and reduced fracture elongation compared with the respective base material.
Nickel-iron-alloy modification to enhance additively welded microstructure for subsequent milling
(2021)
The aerospace industry uses nickel-iron-alloys to create moulding tools for composite materials because of the low coefficient of thermal expansion. These tools have a large-sized and complex structure, making them cost-intensive and difficult to manufacture. Therefore, the focus is set on additive manufacturing, which can additionally enable the repair of components in order to eliminate local defects. However, the process usually results in a heterogeneous microstructure and anisotropic mechanical properties. As there is a high demand for a precise and exact fit of the precision moulds and thus the surface quality, the welded components must be subsequently machined. Nickel-iron alloys are difficult to machine and an inhomogeneous microstructure also leads to unstable cutting forces.
Consequently, a refinement and homogenisation of the microstructure morphology is achieved through specific alloy modifications in order to stabilise and improve the subsequent machining process. Studies on the refinement of FeNi 36 based on vacuum arc melting furnaces are used as a starting point. Therefore, titanium and niobium are chosen as modification elements with a maximum 1 % weight percent and are added to nickel-iron base alloy. The elements are alloyed and build-up welded by using plasma-transferred-arc welding. The resulting microstructure morphology of the welded wall structure and the machining properties are then determined. Furthermore, the influence on the coefficient of thermal expansion is investigated in connection with the modification and the welding process itself. It can be shown that even small amounts of niobium have a significant influence on the structural morphology of the welded layers during plasma-transferred-arc welding.
Das DVS-Vorhaben 01.3211 „Herstellung beanspruchungsgerechter Oberflächen durch Kombination innovativer additiver und abtragender Fertigungsschritte an hochbelasteten Komponenten“ ist ein Kooperationsprojekt der Bundesanstalt für Materialforschung und -prüfung (BAM) und dem Institut für Schweißtechnik und Trennende Fertigungsverfahren (ISAF) der Technischen Universität Clausthal. Das Übergeordnete Projektziel ist das Erlangen von Erkenntnissen für eine sichere und wirtschaftliche, kombinierte additive und abtragende Fertigung aus kostenintensiven Werkstoffen hochbelasteter Komponenten insbesondere für KMU. Dabei stehe die beiden Werkstoffe CoCr26Ni9Mo5W (2.4681) und FeNi36 (1.3912) im Fokus. Mittels Modifikation der Schweißzusätze sind homogen und isotrop ausgeprägte Werkstoffeigenschaften und eine Erhöhung der Prozessstabilität und Fertigungsfreiheitsgrade bei der additiven Fertigung erzielbar. Darüber hinaus wird der Einfluss nachfolgender abtragender Bearbeitungsschritte des ultraschallunterstützen und des konventionellen Fräsprozesses untersucht. Die mit dem Forschungsvorhaben verbundenen Nutzen für KMU sind die Stärkung der Innovationsfähigkeit und der Wirtschaftlichkeit sowie die Erhöhung der Wettbewerbsfähigkeit. In AP-1 wurden Zerspanversuche am FeNi- und CoCr-Ausgangswerkstoff durchgeführt. Ziel der Versuche war in erster Linie die Identifikation geeigneter Fräswerkzeuge und -parameter. In AP-2 wurden die Legierungsmodifikationen des CoCr-Ausgangswerkstoffes durchgeführt und die Mikrostruktur sowie die Härte analysiert. In AP-4 wurden erste Zerspanversuche in Abhängigkeit der Legierungsmodifikation der CoCr-Legierung durchgeführt.