Ingenieurwissenschaften und zugeordnete Tätigkeiten
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Diese Arbeit zeigt erstmals die Anwendung einer elektromagnetischen Schmelzbadstütze beim einlagigen MSG-Schweißen von dickwandigen Stählen. Die innovativen Entwicklungen im Bereich des Lichtbogenschweißverfahrens ermöglichen eine Erhöhung der Abschmelzleistung, um die Einschweißtiefe zu steigern. Somit kann die Lagenanzahl reduziert und die Produktivität gesteigert werden. Allerdings besteht insbesondere beim einlagigen Schweißen von dickwandigen Bauteilen in PA-Position ein erhöhtes Risiko für das gravitationsbedingte Austropfen der Schmelze an der Wurzel. Zur Verhinderung werden Badstützen eingesetzt, die mechanisch angebracht und nach dem Schweißen entfernt werden müssen, was zeit- und kostenintensiv ist.
Die im Rahmen dieser Studie eingesetzte elektromagnetische Schmelzbadstütze wirkt dem gravitationsbedingten Austropfen der Schmelze entgegen und kompensiert den hydrostatischen Druck. Sie wirkt kontaktlos, was im Gegensatz zu herkömmlichen Badstützen vorteilhaft ist, so dass auf eine zeit- und kostenintensive Nachbearbeitung der Schweißnahtwurzel verzichtet werden kann. Das auf extern angelegten oszillierenden Magnetfeldern beruhende Verfahren wird dabei unterhalb des zu schweißenden Bauteils positioniert. Die Magnetfeldlinien sind quer zur Schweißrichtung ausgerichtet, sodass längs zur Schweißrichtung Wirbelströme im Werkstück und eine stets nach oben gerichtete Lorentzkraft generiert werden. Mit Hilfe der elektromagnetischen Badstütze konnten beim einlagigen MSG-Schweißen von 8 mm bis 12 mm die Tropfenbildung vermieden werden. Die innovative Technologie ermöglicht es dickwandige Bauteile einlagig zu schweißen und reduziert die Nachbearbeitungszeit deutlich.
The study deals with the influence of the heat input and the resulting cooling times on the microstructure and Charpy impact toughness of single-pass laser hybrid welded 20-mm thick high-strength steel S690QL. The main focus is on the change of the mechanical properties over the entire seam thickness. The cooling times were measured in-situ using a pyrometer and an optical fibre in three different depths of the seam where Charpy impact test specimens were also later taken. Thereby, three different heat inputs from 1.3 kJ/mm to 2 kJ/mm were investigated. Despite the observed decreased values of both t8/5-cooling time and the Charpy impact toughness in the root part of the seam, the required impact toughness of 38 J/cm2 could be reached in dependance on applied heat input, especially at the heat input of 1.6 kJ/mm.
Laser powder-based directed energy deposition (DED-L) is a technology that offers the possibility for 3D material deposition over hundreds of layers and has thus the potential for application in additive manufacturing (AM). However, to achieve broad industrial application as AM technology, more data and knowledge about the fabricated materials regarding the achieved properties and their relationship to the manufacturing process and the resulting microstructure is still needed. In this work, we present data regarding the low-cycle fatigue (LCF) behavior of Ti-6Al-4V. The material was fabricated using an optimized DED-L process. It features a low defect population and excellent tensile properties. To assess its LCF behavior two conventionally manufactured variants of the same alloy featuring different microstructures were additionally tested. The strain-controlled LCF tests were carried out in fully reversed mode with 0.3 % to 1.0 % axial strain amplitude from room temperature up to 400°C. The LCF behavior and failure mechanisms are described. For characterization, optical microscopy (OM), scanning electron microscopy (SEM), and micro-computed tomography (µCT) were used. The low defect population allows for a better understanding of the intrinsic material’s properties and enables a fairer comparison against the conventional variants. The fatigue lifetimes of the DED-L material are nearly independent of the test temperature. At elevated test temperatures, they are similar or higher than the lifetimes of the conventional counterparts. At room temperature, they are only surpassed by the lifetimes of one of them. The principal failure mechanism involves multiple crack initiation sites.
Powder bed technologies are amongst the most successful Additive Manufacturing (AM) techniques. Powder bed fusion and binder jetting especially are leading AM technologies for metals and polymers, thanks to their high productivity and scalability. The application of these techniques to most ceramics has been difficult so far, because of the challenges related to the deposition of homogeneous powder layers when using fine powders. In this context, the “layerwise slurry deposition” (LSD) has been developed as a layer deposition method which enables the use of powder bed AM technologies also for advanced ceramic materials. The layerwise slurry deposition consists of the layer-by-layer deposition of a ceramic slurry by means of a doctor blade, in which the slurry is deposited and dried to achieve a highly packed powder layer. This offers high flexibility in the ceramic feedstock used, especially concerning material and particle size. The LSD technology can be combined with binder jetting to develop the so-called “LSDprint” process for the additive manufacturing of ceramics. The LSDprint technology combines the high-speed printing of binder jetting with the possibility of producing a variety of high-quality ceramics with properties comparable to those achieved by traditional processing. In this presentation, the LSD process will be introduced and several examples of application ranging from silicate to high-performance ceramics will be shown. Recent developments towards the scale-up and industrialization of this process will be discussed, alongside future perspectives for the multi-material additive manufacturing.
Powder bed technologies are amongst the most successful Additive Manufacturing (AM) techniques. Powder bed fusion and binder jetting especially are leading AM technologies for metals and polymers, thanks to their high productivity and scalability.
The application of these techniques to most ceramics has been difficult so far, because of the challenges related to the deposition of homogeneous powder layers when using fine powders.
In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method which enables the use of powder bed AM technologies also for advanced ceramic materials. The layerwise slurry deposition consists of the layer-by-layer deposition of a ceramic slurry by means of a doctor blade, in which the slurry is deposited and dried to achieve a highly packed powder layer. This offers high flexibility in the ceramic feedstock used, especially concerning material and particle size.
The LSD technology can be combined with binder jetting to develop the so-called “LSDprint” process for the additive manufacturing of ceramics.
The LSDprint technology combines the high-speed printing of binder jetting with the possibility of producing a variety of high-quality ceramics with properties comparable to those achieved by traditional processing.
In this presentation, the LSD process will be introduced and several examples of application ranging from silicate to high-performance ceramics will be shown.
Recent developments towards the scale-up and industrialization of this process will be discussed, alongside future perspectives for the multi-material additive manufacturing.
This presentation focuses on the basic ideas and current status of the development of an arithmetical method to predict the failure rotational speed of turbine disks. The certification specification requires that a gas turbine aero-engine must hold 5 minutes at overspeed conditions without critical failure. Therefore, instead of experimental proof from spin-tests using test-disks similar to engine components, it is considered to use simple specimen with similar test conditions compared to real overspeed scenarios. These test conditions, or stress fields are determined using arithmetical method, e.g. finite element method, with consideration of fracture mechanics under quasi-static conditions with a given rotational speed.
Failure modes like hoop burst and rim peeling are considered during determination of stress fields. Various crack-tip parameters are used to explore the similarity of stress field between simple specimen and real overspeed scenarios. Additionally, probabilistic aspects and the implementation of a global stability criterion for overspeed analysis are also considered.
Aero-engine turbine disks are safety-relevant components which are operated under high thermal and mechanical stress conditions. The actual part qualification and certification procedures make use of spin-tests conducted on production-similar disks. While these tests provide, on the one hand, a reliable definition of the critical conditions for real components, on the other hand they represent a relevant cost item for engine manufacturers. The aim of this work is to present part of a fracture mechanics-based procedure under development which aims at replacing the tests on production-similar disks with lab tests on fracture mechanics specimens. In particular, the rim-peeling failure mode is considered as case study. A semi-circular surface crack is modelled at the most stressed region at the diaphragm of a turbine disk, with the crack plane perpendicular to the radial direction. The crack is therefore subjected to a biaxial stress state and grows under increasing rotational speed until it triggers the rim-peeling failure. The finite element simulation of the cracked disk considers the real thermal and mechanical loading conditions. In order to design a lab representative specimen, beside the crack driving force, expressed in terms of J-integral, also the constraint to plastic deformation e.g., stress triaxiality, at the crack-tip must be similar for the same crack in the specimen and in the disk. This has been achieved and as expected, both the highest J-integral and constraint factor are calculated at the same location along the crack front for both disk and specimen. The results of the structural integrity assessment in the form of a Failure Assessment Diagram (FAD) show good agreement between designed specimen and disk both in terms of expected failure mode and value of the critical speed. Probabilistic aspects are also considered in the calculations.
Turbinenscheiben sind thermisch und mechanisch hochbeanspruchte, sicherheitsrelevante Komponenten in Gasturbinen. Ihre Integrität wird in Bauteiltests unter Überdrehzahlbedingungen nachgewiesen. Kontext des Aufsatzes ist die Erarbeitung einer zusätzlichen Bewertungsebene auf der Grundlage von Versuchen unter monotoner Beanspruchung, die die Beanspruchung im Bauteil realistisch wiedergeben soll. Dazu werden zwei Typen von bruchmechanischen Proben anwendungsnah ausgelegt und aus einer Turbinenscheibe ausgeschnitten: Der erste Typ ist eine biaxiale Probe, die die Beanspruchung und den Dehnungsbehinderungszustand am Diaphragm der Turbinenscheibe abbildet, die zweite eine bruchmechanische Probe, die die einachsige Beanspruchung und den Dehnungsbehinderungszustand am Bore der Turbinenscheibe wiedergibt.
Im Rahmen eines Schadentoleranzansatzkonzepts ist anschließend jeweils ein halbelliptischer Riss an den genannten Stellen der Turbinenscheibe zu betrachten. Mittels numerischer Berechnungen wird ein kritischer Punkt auf der Rissfront des Risses am Diaphragm bestimmt, dort wo die höchste Rissspitzenbelastung (J-Integral) auftritt. Auf der Basis der Rissspitzenbelastung, des Dehnungsbehinderungszustands und des entsprechenden Spannungsverhältnisses an diesem kritischen Punkt wird eine Kreuzprobe mit einem Durchriss konzipiert, die diese Verhältnisse im Bauteil widerspiegelt. Die Versuche werden unter der Temperatur am Diaphragm der Turbinenscheibe durchgeführt. Die J-R-Kurve und die plastische Kollapsgrenze werden bestimmt. Auch die einachsigen Versuche werden unter der Temperatur am Bore der Turbinenscheibe durchgeführt. Die Zugprobe enthält halbelliptische Oberflächenrisse. Ähnlich wie bei der Auslegung der Kreuzproben werden die Rissspitzenbelastung, der Dehnungsbehinderungszustand und das Spannungsverhältnis vergleichbar mit der Turbinenscheibe eingestellt. Die J-R-Kurve und die plastische Kollapsgrenze werden bestimmt.
Mit den Versuchsergebnissen werden die kritischen Lasten für verschiedene Versagensmechanismen (instabiles Risswachstum, plastischer Kollaps) der bruchmechanischen Proben ermittelt, die der kritischen Überdrehzahl der Turbinenscheibe entsprechen.
Turbinenscheiben sind thermisch und mechanisch hochbeanspruchte, sicherheitsrelevante Komponenten in Gasturbinen. Ihre Integrität wird in Bauteiltests unter Überdrehzahlbedingungen nachgewiesen. Kontext des Aufsatzes ist die Erarbeitung einer zusätzlichen Bewertungsebene auf der Grundlage von Versuchen unter monotoner Beanspruchung, die die Beanspruchung im Bauteil realistisch wiedergeben soll. Betrachtet wird ein halbelliptischer Riss, der bei der weiteren Ausbreitung als Umfangsriss wächst (rim peeling). Die Simulation dieser Stelle im Bauteil schließt die mechanische und thermische Beanspruchung sowie sie Dehnungsbehinderung ein. Letztere wird anhand zweier Parameter, der Spannungsmehrachsigkeit ℎ und des (allerdings modifizierten) Constraint-Parameters nach Newman, der die Spannungen über den plastisch verformten Bereich mittelt, bestimmt. Erwartungsgemäß zeigt sich, dass die höchste Dehnungsbehinderung weder an den Oberflächenpunkten, noch an den tiefsten Punkten, sondern an einer Stelle zwischen beiden auf der Rissfront auftritt. Als Versuchsgeometrie für die monotonen Tests soll eine Kreuzprobe mit wanddurchdringenden Rissen ausgehend von einer Innenbohrung dienen. Durch geeignete Wahl der Risstiefe sowie der in beiden Richtungen angreifenden Kräfte gelingt es, bauteiladäquate Zustände zu erzeugen.
Hexakis(n-alkyloxy)triphenylene) (HATn) consisting of an aromatic triphenylene core and alkyl side chains are model discotic liquid crystal (DLC) systems forming a columnar mesophase. In the mesophase, the molecules of HATn self-assemble in columns, which has one-dimensional high charge carrier mobility along the columns. Here, a homologous series of HATn with different length of the alkyl chain (n=5,6,8,10,12) is investigated using differential scanning calorimetry (DSC), broadband dielectric spectroscopy (BDS) and advanced calorimetric techniques including fast scanning calorimetry (FSC) and specific heat spectroscopy (SHS). The investigation of the phase behavior was done utilizing DSC experiments and the influence of the alkyl chain length on the phase behavior was revealed. By the dielectric investigations a γ-relaxation due to localized fluctuations as well as two glassy dynamics the αcore and αalkyl relaxation were observed in the temperature range of the plastic crystalline phase. Moreover, the observed glassy dynamics were further studied employing advanced calorimetry. All observed relaxation processes are attributed to the possible specific molecular fluctuations and discussed in detail. From the results a transition at around n=8 from a rigid constrained (n=5,6) to a softer system (n=10,12) on a molecular lenght scale was revealed with increasing alkyl chain length. A counterbalance of two competing effects of a polyethylene like behavior of the alkyl chains in the intercolumnar domains and self-organized confinement is discussed in the context of a hindered glass transition. The results were confirmed by in- and quasielastic neutron scattering
The contactless magnetohydrodynamic technology has been considered as a potential and promising method to improve the weld qualities of deep penetration laser beam welding. In this paper, numerical investigations are conducted to study the influence of the auxiliary oscillating magnetic field on the porosity suppression in laser beam welding of 5754 aluminum alloy. To obtain a deeper insight into the suppression mechanism, a three-dimensional transient multi-physical model is developed to calculate the heat transfer, fluid flow, keyhole dynamic, and magnetohydrodynamics. A ray tracing algorithm is employed to calculate the laser energy distribution on the keyhole wall. A time-averaged downward Lorentz force is produced by an oscillating magnetic field. This force acts in the molten pool, leading to a dominant downward flow motion in the longitudinal section, which blocks the bubble migration from the keyhole tip to the rear part of the molten pool. Therefore, the possibility for the bubbles to be captured by the solidification front is reduced. The electromagnetic expulsive force provides an additional upward escaping speed for the bubbles of 1 m/s ~ 5 m/s in the lower and middle region of the molten pool. The simulation results are in a good agreement with experimental measurements. Based on the results obtained in this study, a better understanding of the underlying physics in laser beam welding enhanced by an auxiliary oscillating magnetic field can be provided and thus the welding process can be further optimized reducing the porosity formation.
Numerical analysis of ultrasonic vibration enhanced friction stir welding of dissimilar Al/Mg alloys
(2022)
The ultrasonic vibration enhanced friction stir welding (UVeFSW) process has unique advantages in joining dissimilar Al/Mg alloys. While there are complex coupling mechanisms of multi-fields in the process, it is of great significance to model this process, to reveal the influence mechanism of ultrasonic vibration on the formation of Al/Mg joints.
In this study, the acoustic-plastic constitutive equation was established by considering the influence of both ultrasonic softening and residual hardening on the flow stress at different temperatures and strain rates. And the ultrasonic induced friction reduction (UiFR) effect on friction coefficient in different relative directions at the FSW tool-workpiece interface was quantitatively calculated and analyzed.
The Al/Mg UVeFSW process model was developed through introducing the above acoustic effects into the model of Al/Mg friction stir welding (FSW). The ultrasonic energy is stronger on the aluminum alloy side. In the stirred zone, there is the pattern distribution of ultrasonic sound pressure and energy. The heat generation at the tool-workpiece contact interface and viscous dissipation were reduced after applying ultrasonic vi-bration. Due to the UiFR effect, the projection of friction coefficient and heat flux distributions at the tool-workpiece interface present a "deformed" butterfly shape. The calculated results show that ultrasonic vibration enhanced the material flow and promoted the mixing of dissimilar materials.
The optical properties of these materials strongly depend on the excitation power density, i.e., the number of photons absorbed per time interval. The upconversion quantum efficiencies (ΦUC) of these materials, the excitation power dependent population i.e. the emission characteristics, and the deactivation dynamics are influenced by nanoparticle architecture, doping concentration, and the microenvironment. We will discuss how time resolved measurements can help to understand the fundamental photophysical mechanisms and discuss differences to other nanocrystals like quantum dots.
Downsizing (power-to-weight ratio) and higher speeds lead to a rise in Hertzian contact pressures in combination with an increase in surface or oil temperatures. Under such conditions, commonly used bearing steels, such as 100Cr6, reach their limits, creating a demand for alternative slip-rolling resistant steel alloys. The present work therefore compares the slip-rolling performance of various steel types with Maraging- and PM-type steel alloys in the Hertzian contact pressure range up to P0max of 4 GPa.
The importance of high-temperature materials made of iron aluminides (FeAl) has been increasing in light weight applications, e.g., airplane turbines, due to the high material’s specific strength. However, the highly economic production by means of permanent mold casting involves special microstructures for Fe26Al4Mo0.5Ti1B alloy components leading to difficult machinability for subsequent finishing milling and low surface qualities. Major effects of tool and machining parameter variation incorporating ultrasonic assistance on the milling process and surface integrity are shown. Loads for tool and component surface are significantly adjustable to enable an economic process chain regarding the surface integrity of safety-relevant components.
Die Niobvorkommen übersteigen die von Wolfram um ein Vielfaches. Mit 92 % ist Brasilien heute der weltweit größte Niobproduzent. Daher ist NbC eine nachhaltige und wirtschaftliche Alternative zu konventionellen Schneidstoffen, insbesondere zu Wolframkarbid (WC). Darüber hinaus kann NbC in einer Ni-Legierungsmatrix verwendet werden und bietet somit als Ersatz für WC in einer Co-Matrix als Schneidstoff erhebliche Vorteile in Bezug auf Gesundheitsrisiken sowie Rohstoffpreis- und Versorgungsrisiken. Auf der Grundlage jüngster Studien, in denen eine höhere Leistung von NbC im Vergleich zu WC-Schneidwerkzeugen festgestellt wurde, ist in dieser Studie die Zusammensetzung NbC-12Ni-4Mo-4VC für die Fertigbearbeitung eines hochfesten Stahls S960QL gewählt worden. Die Versuche wurden auf einer ultraschallunterstützten 5-Achsen-Fräsmaschine mit speziell angefertigten NbC-Werkzeugen durchgeführt, um sie mit handelsüblichen beschichteten WC-Schneideinsätzen zu vergleichen. Darüber hinaus wird der Einfluss eines Beschichtungssystems für die NbC-Schneidplatten getestet und hinsichtlich seiner Leistung im Zerspanungsprozess bewertet. Werkzeugverschleiß- und Schnittkraftanalysen werden durchgeführt, um optimale Parameterkonstellationen und Werkzeugeigenschaften für das neue NbC-Werkzeug zu ermitteln. Zusammen mit der Oszillation des ultraschallunterstützten Fräsens können die Belastungen auf die Bauteiloberfläche und das Werkzeug reduziert und das Verschleißverhalten des neuartigen NbC-Werkzeugs verfeinert werden. Diese Fräsversuche werden von standardisierten Verschleißtests mit den oben genannten Materialkombinationen begleitet und die Ergebnisse miteinander korreliert. Schließlich wird auch das Verhalten beim Einsatz schwer zerspanbarer Werkstoffe wie Ni-Legierungen oder innovativer Materialien wie Eisenaluminid getestet. Mit dieser Strategie lassen sich umfassende Erkenntnisse für den zukünftigen effizienten Einsatz von NbC für Fräswerkzeuge erzielen, die bereits seit Jahrzehnten in Form von WC erforscht werden.
Das Wire and Arc Additive Manufacturing (WAAM) ist dank hoher erreichbarer Aufbauraten prädestiniert für die Fertigung großvolumiger Bauteile. Dabei ist auf die Wirkmechanismen zwischen Prozessparametern und den daraus resultierenden mechanisch-technologischen Eigenschaften zu achten. Dies gilt insbesondere für die Fertigung dickwandiger Bauteile aus Al-Mg-Si-Aluminiumlegierungen, die eine hohe Anfälligkeit gegenüber Erstarrungsrissen und wasserstoffinduzierter Porosität aufweisen. Der Einfluss der Prozessparameter und des resultierenden Temperaturregimes auf die Bauteilqualität wurde durch die Analyse der Größe und Verteilung von Poren sowie der resultierenden Festigkeit untersucht. Darüber hinaus wurde der Einfluss einer Wärmenachbehandlungsstrategien auf das Festigkeitsverhalten analysiert.
The climate and energy crisis are extreme challenges. One possible solution could be hydrogen technology. Safety is a big concern. Steel used for pipelines and storage is under permanent stress from low temperatures and high pressures. The content of different alloyed metals determines the performance of the steel. Nitrogen microwave inductively coupled atmosphere pressure plasma mass spectrometry (N2-MICAP-MS) is a promising method for trace metal analysis in steel. Nitrogen is cheap and can be generated on site. It has fewer interferences than argon. Additionally, MICAP-MS is very matrix tolerant, proving the matrix-matched calibration expendable. Safety in technology and chemistry is the mission of BAM. Providing reference methods and materials can create trust in future technologies like hydrogen.
Investigation of degradation of the aluminum current collector in lithium-ion batteries by GD-OES
(2022)
Lithium-ion batteries (LIBs) are one technology to overcome the challenges of climate and energy crisis. They are widely used in electric vehicles, consumer electronics, or as storage for renewable energy sources. However, despite innovations in batteries' components like cathode and anode materials, separators, and electrolytes, the aging mechanism related to metallic aluminum current collector degradation causes a significant drop in their performance and prevents the durable use of LIBs. Glow-discharge optical emission spectroscopy (GD-OES) is a powerful method for depth-profiling of batteries' electrode materials. This work investigates aging-induced aluminum deposition on commercial lithium cobalt oxide (LCO) batteries' cathodes. The results illustrate the depth-resolved elemental distribution from the cathode surface to the current collector. An accumulation of aluminum is found on the cathode surface by GD-OES, consistent with results from energy-dispersive X-ray spectroscopy (EDX) combined with focused ion beam (FIB) cutting. In comparison to FIB-EDX, GD-OES allows a fast and manageable depth-profiling. Results from different positions on an aged cathode indicate an inhomogeneous aluminum film growth on the surface. The conclusions from these experiments can lead to a better understanding of the degradation of the aluminum current collector, thus leading to higher lifetimes of LIBs.
Aging Mechanisms of Lithium Batteries: How can we make batteries more durable and more sustainable in the future?
Lithium batteries are particularly susceptible to ageing processes. During each charging and discharging process in an electric battery, lithium ions are deposited in the electrodes of the cell like in the pores of a sponge. Over time, however, fractures and cracks occur in the filigree structures. The result: more and more lithium ions no longer fit into the hollow spaces of the „sponge“, instead they accumulate in heaps around the electrodes and hinder the movement of other ions. The performance of the battery decreases.
We present our new project, in which we are developing a fast and cost-effective method with which companies that produce lithium batteries can already assess the ageing behaviour of their batteries in the laboratory.
Daten und Informationen zu physikalisch-chemischen Eigenschaften und Gefahren von Stoffen und Gemischen sind im Sicherheitsdatenblatt in Abschnitt 9 anzugeben. Die Anforderungen stammen aus REACH Anhang II und sind Anfang 2021 neugefasst worden. REACH implementiert damit die Neufassung des entsprechenden Abschnitts 9 aus dem UN-GHS – mit einigen europäischen Ergänzungen.
Der Vortrag gibt einen Überblick über die Änderungen und stellt die Ergänzungen, die sich an die Ersteller von Sicherheitsdatenblättern richten, anhand einiger aussagekräftiger Beispiele vor.
Das zyklische plastische Verformungsverhalten von additiv gefertigtem Edelstahl AISI 316L wurde in dehnungsgeregelten Kurzzeitfestigkeitsversuchen (LCF-Versuchen) untersucht. Dabei wurden zwei Wärmebehandlungszustände betrachtet: Beim ersten Zustand war die fertigungsbedingte zelluläre Struktur vorhanden, während sie durch die zweite Wärmebehandlung aufgelöst wurde. Untersuchungen im Transmissions-Elektronen-Mikroskop (TEM) zeigten, dass die zyklische Verformung die Zellstruktur lokal zerstörte und Gleitbänder entstanden, was die Entfestigung in diesem Fall erklärt. Für Material ohne Zellstrukturen resultierten nach zyklischer Verformung ähnliche Versetzungsstrukturen wie in konventionell gefertigtem (warmgewalzten) Material.
MALDI-ToF mass spectrometry for the characterization of biobased polymers suitable for depollution
(2022)
In this work, bio-based polymers were synthesized and designed as polymers phases for adsorption of a variety of pollutants from aqueous solutions. The obtained adsorption results showed that the integration of bio-sourced synthons generate attractive hydrophilicity, and wettability of the resulting adsorbent phase. Such polymers phases enable stronger interactions with the organic and inorganic pollutants in water.
A wide variety of different bio-based polymers structures (e. g. poly(ethersulfones, poly(etherphosphines or poly(etherpyridines) with different functional groups were successfully designed in order to adapt chemical structure to different pollutants type and matrice nature.
In order to characterize and to determine the correlation between polymer structures and nature of interaction with pollutants, different analytical technics (NMR, GPC, ATG, DSC, Mass spectrometry) were successfully used. Amongst them, MALDI TOF mass spectrometry plays a superior role since this technique enables the simultaneous determination of the polymer structure, polymer end groups and molecular weight.
This work focusses on the characterization of synthesized polymers. The chemical structure of the repeating unit, the nature of the end groups, as well as the molecular weight, which are all important for the specific interactions of the polymer with the pollutants were clearly determined and suggestions to improve these interactions by changing the synthetic pathway could be given.
Fatigue strength estimation is a costly manual material characterization process in which state-of-the-art approaches follow a standardized experiment and analysis procedure. In this paper, we examine a modular, Machine Learning-based approach for fatigue strength estimation that is likely to reduce the number of experiments and, thus, the overall experimental costs. Despite its high potential, deployment of a new approach in a real-life lab requires more than the theoretical definition and simulation. Therefore, we study the robustness of the approach against misspecification of the prior and discretization of the specified loads. We identify its applicability and its advantageous behavior over the state-of-the-art methods, potentially reducing the number of costly experiment.
Fluorescent semiconductor nanocrystals, also known as quantum dots (QDs), enabled many advancements in biotechnology, photovoltaics, photocatalysis, quantum computing and display devices. The high versatility of this nanomaterial is based on their unique size-tunable photoluminescence properties, which can be adjusted from the visible to the near-infrared range. In contrast to other nanomaterials, QDs made the transition from a laboratory curiosity to the utilization in commercial products, like the QLED television screen or in smartphone displays. The best investigated QDs are composed of heavy metals like cadmium or lead, which is not the best choice in terms of toxicity and environmental pollution. A more promising material is Indium Phosphide (InP), which is also currently used by Samsung, Sony and co. in the QLED displays.
In this contribution, I would like to give you a sneak peek behind the curtains of nanomaterial synthesis and show how this material is produced, how to stabilize their structural properties, and assess their toxicity in environmentally relevant conditions. Furthermore, I would like to present a synthesis method to accomplish the last open challenge in display technology of a blue luminescent LED based on QDs by introducing a new element to the InP QDs.
Elastomer seals are mounted as barrier seals in lid systems of containers designed for transport and disposal of negligible heat generating radioactive waste and as auxiliary seals in spent fuel storage and transportation casks (dual purpose casks (DPC)). When the behavior of mounted seals under normal and hypothetical accident conditions of disposal and transport is to be simulated, a comprehensive knowledge of their complex mechanical properties at every state of aging is necessary. In previous works, BAM’s efforts in experimental investigations on specimen artificially aged at different temperatures and times and the implementation of the found results in finite element material models were presented. Additionally, our approaches to reproduce the aging process itself and to extrapolate the results of artificially accelerated aging to longer times were presented. Numerical simulations have shown that the behavior of the seal during mounting and one-sided pressurizing and the resulting performance values such as leakage rate strongly depend on the coefficient of friction (COF) between flange and seal. The friction coefficient, in turn, depends on the aging state of the elastomer material as several publications suggest (see below).
Dynamic COF between an exemplary ethylene propylene diene rubber (EPDM) material and a stainless steel ball were determined by using a self-designed linear oscillation tribometer. Unaged and artificially aged EPDM specimen stored for 30 days and 100 days at a temperature of 150 °C were tested. A stainless steel ball (d=10 mm) is brought in contact with the specimen’s surface und loaded by normal forces of 2.5 N, 5 N, 10 N and 20 N. During a reciprocating movement of the EPDM sheet, the horizontal force/friction force is continuously measured, and the COF can be derived.
It is well known that friction is a complex phenomenon especially in soft materials. It cannot be excluded that the measured friction force is influenced by additional force components, resulting from the ball’s grooving through the elastomer’s surface. This force depends on the penetration depth of the ball and on the resistance of the elastomer in its different states of aging. The latter results from microstructural changes i.e., chain scission and additional crosslinking that occur during aging which in turn influence the softening or hardening of the material.
A finite element (FE) ABAQUS® model was developed to reproduce the measurement process. It should help to better understand the physical mechanisms and to quantify the percentage of measured forces resulting from real friction on the one hand and forces resulting from unintended side effects that could falsify the result on the other hand. The behavior of the elastomer in its different states of aging is reproduced by a FE material model already presented in previous works of BAM.
Although the slow crack growth in glass is dominated by stress-corrosion phenomena, it also should reflect the underlaying intrinsic fracture behavior controlled by glass chemistry and structure. To investigate such underlaying phenomena, crack growth velocity in alkali silicate glasses was measured in vacuum across 10 orders of magnitude with double cantilever beam technique. Measured and literature crack growth data were compared with calculated intrinsic fracture toughness data obtained from Young’s moduli and theoretical fracture surface energy. Data analysis reveals slight correlation with the packing density and significant deviations from the intrinsic brittle fracture behavior. These deviations do not follow simple compositional trends. Two opposing processes may explain this finding: a decrease in the apparent fracture surface energy due to stress-induced chemical changes at the crack tip and its increase due to energy dissipation during fracture.
Reference materials are essential to analyze the impact of micro- and nanoplastics. The particle size D50 has been chosen as property of interest. They can be produced top-down by milling. For size separation down to a particle size D50 of 50 µm sieving is suitable while smaller particle sizes can be obtained by filtration. After production it is important to control the stability because microplastic in the size range below 10 µm tend to agglomerate.
Micro- and nanoplastic particles became a topic of public concern all over the world e.g. in water, soil, sludge and air. For a profound risk assessment, it is necessary to identify the origins, hotspots, or transport between different media. Therefore, a representative repeatable analysis is required and reference materials (RM) to proof and compare methods.
The basis of MNP investigations is a harmonized analysis which includes sampling, sample preparation and detection. In recent years, spectroscopic methods like µRaman and µFTIR for the determination of particle numbers or thermoanalytical methods like Pyrolysis gas chromatography/mass spectrometry (py-GC/MS) and Thermo extraction/ desorption gas chromatography / mass spectrometry (TED-GC/MS) for mass determination have proven to be particularly suitable.
The technical committees (TC) of ISO TC 61 “plastics” and TC 147 “water quality" are working on harmonisation processes on international level. For all standardization approaches, it is necessary that the detection methods and analysis processes can be validated. Therefore, BAM develops reference material for microplastic (MP) analysis for several years with focus on the most common polymers PE, PP, PS, PET and PA.
MP particles with a close to reality fragment shape are obtained by cryomilling and sieving. For sample preparation purposes with mass detection methods MP particles are pressed into pills with a water-soluble matrix. Thereby losses due to sample preparation e.g. filtration are included in the verification of an analysis.
To ensure a constant quality throughout all MP RM batches the homogeneity and stability is controlled according to ISO Guide 35. Next to TED-GC/MS measurements particle size distribution, infrared spectroscopy and differential scanning calorimetry spectra are taken as accompanying parameters.
This presentation aims to introduce into the MP RM production process with ensured quality and special focus on pointing out customized setups for particle comminution, separation, and characterization for standardization.
Hochfeste Feinkornbaustähle verfügen über großes Potenzial für gewichtsoptimierte, effiziente Strukturen in vielen modernen Stahlkonstruktion. Weitere Effizienzsteigerungen können durch additives Fertigen sowie bionische Bauweisen erreicht werden. Hochfeste Zusatzwerkstoffe für additives MSG-Schweißen (engl.: Wire Arc Additive Manufacturing, WAAM) sind bereits von den Schweißzusatzherstellern lieferbar. Eine breite industrielle Anwendung insbesondere für KMU ist aufgrund fehlender quantitativer Erkenntnisse und Richtlinien bezüglich schweißbedingter Beanspruchungen und Bauteilsicherheit während der Herstellung und des Betriebs derzeit stark limitiert. In einem gemeinsamen Forschungsprojekt (FOSTA-P1380/IGF21162BG) der BAM und der TU Chemnitz werden daher die mit Eigenspannungsausbildung und der Gefahr einer Kaltrissbildung verbundenen prozess- und werkstoffbedingten sowie konstruktiven Einflüsse beim WAAM hochfester Stähle untersucht. Der vorliegende Beitrag fokussiert die Analyse der Auswirkungen von Schweißwärmeführung und Design der WAAM-Bauteile auf die Abkühlbedingungen, Gefüge, mechanisch-technologischen Eigenschaften und Eigenspannungen. Hierfür werden geometrisch definierte Probenkörper (Hohlquader) vollautomatisiert mit einem speziellen, hochfesten WAAM-Massivdraht (Streckgrenze >790 MPa) geschweißt. Die Wärmeführung und Probenabmessungen werden innerhalb eines statistischen Versuchsplans variiert. Die Schweißwärmeführung wird dabei so eingestellt, dass die t8/5-Abkühlzeiten im empfohlenen Verarbeitungsbereich (ca. 5 s bis 20 s) sichergestellt sind. Hierzu ließen sich über zusätzliche thermo-physikalische Umformsimulationen mittels Dilatometer die komplexen Wärmezyklen abbilden und die resultierende Zugfestigkeit des Schweißgutes bestimmen. Das WAAM-Schweißen komplexer Geometrien mit variierenden Schweißwärmeführungen und geometrischen Verhältnissen bzw. Wanddicken bedingt neben den Auswirkungen auf die Abkühlbedingungen, Abkühlzeiten und Gefüge deutliche Einflüsse auf die konstruktiven Steifigkeitsverhältnisse beim Schweißen. Es zeigen sich anhand der Schweißexperimente signifikante Auswirkungen durch Probenskalierung und Wärmeeinbringung auf die resultierenden lokalen Eigenspannungen. Die Folge können ungünstige Bauteileigenschaften und risskritische Zugeigenspannungen sein.
Im Rahmen der Normungssitzung werden praktikable Verarbeitungsempfehlungen basierend auf den Erkenntnissen des Vh. mit Vertretern aus Industrie und Forschung diskutiert.
Hochfeste Feinkornbaustähle verfügen über großes Potenzial für gewichtsoptimierte, effiziente Strukturen in vielen modernen Stahlkonstruktion. Weitere Effizienzsteigerungen können durch additives Fertigen sowie bionische Bauweisen erreicht werden. Hochfeste Zusatzwerkstoffe für additives MSG-Schweißen (engl.: Wire Arc Additive Manufacturing, WAAM) sind bereits von den Schweißzusatzherstellern lieferbar. Eine breite industrielle Anwendung insbesondere für KMU ist aufgrund fehlender quantitativer Erkenntnisse und Richtlinien bezüglich schweißbedingter Beanspruchungen und Bauteilsicherheit während der Herstellung und des Betriebs derzeit stark limitiert. In einem gemeinsamen Forschungsprojekt (FOSTA-P1380/IGF21162BG) der BAM und der TU Chemnitz werden daher die mit Eigenspannungsausbildung und der Gefahr einer Kaltrissbildung verbundenen prozess- und werkstoffbedingten sowie konstruktiven Einflüsse beim WAAM hochfester Stähle untersucht. Der vorliegende Beitrag fokussiert die Analyse der Auswirkungen von Schweißwärmeführung und Design der WAAM-Bauteile auf die Abkühlbedingungen, Gefüge, mechanisch-technologischen Eigenschaften und Eigenspannungen. Hierfür werden geometrisch definierte Probenkörper (Hohlquader) vollautomatisiert mit einem speziellen, hochfesten WAAM-Massivdraht (Streckgrenze >790 MPa) geschweißt. Die Wärmeführung und Probenabmessungen werden innerhalb eines statistischen Versuchsplans variiert. Die Schweißwärmeführung wird dabei so eingestellt, dass die t8/5-Abkühlzeiten im empfohlenen Verarbeitungsbereich (ca. 5 s bis 20 s) sichergestellt sind. Hierzu ließen sich über zusätzliche thermo-physikalische Umformsimulationen mittels Dilatometer die komplexen Wärmezyklen abbilden und die resultierende Zugfestigkeit des Schweißgutes bestimmen. Das WAAM-Schweißen komplexer Geometrien mit variierenden Schweißwärmeführungen und geometrischen Verhältnissen bzw. Wanddicken bedingt neben den Auswirkungen auf die Abkühlbedingungen, Abkühlzeiten und Gefüge deutliche Einflüsse auf die konstruktiven Steifigkeitsverhältnisse beim Schweißen. Es zeigen sich anhand der Schweißexperimente signifikante Auswirkungen durch Probenskalierung und Wärmeeinbringung auf die resultierenden lokalen Eigenspannungen. Die Folge können ungünstige Bauteileigenschaften und risskritische Zugeigenspannungen sein.
High-strength steels have great potential for weight optimization due to reduced wall thicknesses in many modern steel constructions. Further advances in efficiency can be achieved through the application of additive manufacturing processes, such as Wire Arc Additive Manufacturing (WAAM). These technologies enable the sustainable and resource-efficient manufacturing of high-strength steels into near-net-shape, efficient structures. During the production of steel structures, unacceptable defects may occur in the weld area or in the WAAM component, e.g., due to unstable process conditions. The economical solution for most of the cases is local gouging or machining of the affected areas and repair welding. With respect to the limited ductility of high-strength steels, it is necessary to clarify the effects of machining steps on the multiaxial stress state and the high design-induced shrinkage restraint. In this context, the component-related investigations in two research projects are concerned with the residual stress evolution during welding and slot milling of welds and WAAM structures made of high-strength steels with yield strengths ≥790 MPa. In-situ digital image correlation (DIC) and ex-situ X-ray diffraction (XRD) were used to analyse the stresses and strains induced on specimens during and after milling. The systematic analyses revealed a significant interaction of the stiffness and relaxation of the specimens with the initial residual stresses induced by welding.
Influence of the WAAM process on residual stresses in high-strength steels (IIW-Doc. II-A-408-2022)
(2022)
High-strength fine-grain structeural steels have great potential for weight optimization of many modern engineering structures. Efficient manufacturing can be achieved here above all by Wire Arc Additive Manufacturing (WAAM). First commercial high-strength welding consumables for WAAM are already available. However, due to a lack of knowledge and guidelines for the industry regarding welding residual stresses and component safety in manufacturing and operation, their application is still severely limited. Residual stresses play a crucial role here, as the sensitive microstructure of high-strength steels carries a high risk of cold cracking. For this reason, process- and material-related influences, as well as the design aspects on residual stress formation and the risk of cold cracking, are being investigated in a recent project (FOSTA-P1380/IGF21162BG). This high strength of the WAAM welding consumables is adjusted via a martensitic phase transformation. The volume expansion associated with martensite formation has a significant influence on residual stress evolution. However, this has not yet been investigated in relation to the processing of high-strength steels by WAAM. The aim of this work is to establish a WAAM cold crack test and easy-to-apply processing recommendations that will allow economical, expedient, and crack-resistant fabrication of high-strength steels, especially for SME. This paper focuses on the analysis of the effects of welding heat control and design of WAAM components on cooling conditions, microstructure, mechanical-technological properties and residual stresses. For this purpose, geometrically defined specimens (hollow cuboids) are welded fully automatically with a special, high-strength WAAM solid wire (yield strength >790 MPa). The heat control and specimen dimensions are varied within a statistical experimental design. The weld heat control is adjusted in such a way that the t8/5 cooling times are ensured within the recommended processing range (approx. 5–20 s). For this purpose, additional thermo-physical forming simulations using a dilatometer allowed the complex heat cycles to be reproduced and the resulting ultimate tensile strength of the weld metal to be determined. The WAAM welding of complex geometries with varying welding heat control and geometric factors or wall thicknesses not only has an effect on the cooling conditions, cooling times and microstructure, but also has a significant influence on the structural restraint conditions during welding. Hence, the welding experiments show significant effects of specimen scaling and heat input on the welding residual stresses, which may be detrimental regarding component properties and crack-critical tensile residual stresses. These complex interactions are analyzed within this investigation.
High-strength fine-grain structural steels have great potential for weight optimization of many modern engineering structures. Efficient manufacturing can be achieved here above all by Wire Arc Additive Manufacturing (WAAM). First commercial high-strength welding consumables for WAAM are already available. However, due to a lack of knowledge and guidelines for the industry regarding welding residual stresses and component safety in manufacturing and operation, their application is still severely limited. Residual stresses play a crucial role here, as the sensitive microstructure of high-strength steels carries a high risk of cold cracking. For this reason, process- and material-related influences, as well as the design aspects on residual stress formation and the risk of cold cracking, are being investigated in a recent project (FOSTA-P1380/IGF21162BG). This high strength of the WAAM welding consumables is adjusted via a martensitic phase transformation. The volume expansion associated with martensite formation has a significant influence on residual stress evolution. However, this has not yet been investigated in relation to the processing of high-strength steels by WAAM. The aim of this work is to establish a WAAM cold crack test and easy-to-apply processing recommendations that will allow economical, expedient, and crack-resistant fabrication of high-strength steels, especially for SME. This paper focuses on the analysis of the effects of welding heat control and design of WAAM components on cooling conditions, microstructure, mechanical-technological properties and residual stresses. For this purpose, geometrically defined specimens (hollow cuboids) are welded fully automatically with a special, high-strength WAAM solid wire (yield strength >790 MPa). The heat control and specimen dimensions are varied within a statistical experimental design. The weld heat control is adjusted in such a way that the t8/5 cooling times are ensured within the recommended processing range (approx. 5–20 s). For this purpose, additional thermo-physical forming simulations using a dilatometer allowed the complex heat cycles to be reproduced and the resulting ultimate tensile strength of the weld metal to be determined. The WAAM welding of complex geometries with varying welding heat control and geometric factors or wall thicknesses not only has an effect on the cooling conditions, cooling times and microstructure, but also has a significant influence on the structural restraint conditions during welding. Hence, the welding experiments show significant effects of specimen scaling and heat input on the welding residual stresses, which may be detrimental regarding component properties and crack-critical tensile residual stresses. These complex interactions are analyzed within this investigation
Genormte künstliche Bewitterungstests sind häufig nicht spezifisch für die Anwendungssituation oder das Material. Das macht die Entwicklung spezifischer Tests erforderlich. Für deren Entwicklung müssen Maximalparameter der Anwendungssituation bekannt sein, womit dann der künstliche Test formuliert wird und dessen Bedingungen werden dann solange optimiert, bis die Korrelation der Effekte von natürlichem und künstlichem Test ausreichend ist.
Für Untersuchungen der Freisetzung kann der verbleibende Rest in der Probe und/oder die freigesetzte Menge in Luft, Boden, Wasser bestimmt werden.
Im ersten Beispiel der Witterungswirkung wurde die Freisetzung von Kohlenstoff-Nanoröhrchen (CNT) aus Polymer-Kompositen untersucht (unter Verwendung von empfindlich-nachweisbarer radioaktiver 14C-Markierung für einzelne CNT-Partikel), in einem zweiten die Freisetzung von anorganischen und organischen Bestandteilen aus elastomeren Bestandteilen von Sportböden (Bahnen und Kunstrasen) in Wasser.
In den letzten Jahrzehnten wurde die Degradation der polymeren Matrix von flammgeschützten Polymeren eingehend untersucht. Erst in den letzten Jahren jedoch hat sich die Frage der Lebensdauer der Funktionalität des Flammschutzes selbst als wichtige Fragestellung herauskristallisiert, z.B. bei Kabeln. Deshalb sollte diese Fragestellung durch systematisch-variierte künstliche Klima- und Bewitterungstests an flammgeschützten Polymerwerkstoffen untersucht werden
With 8% of man-made CO2 emissions, cement production is an important driver of the climate crisis. By using alkali-activated binders, part of the energy-intensive clinker production process can be dispensed. However, as numerous raw materials are involved in the manufacturing process here, the complexity of the materials increases by orders of magnitude. Finding a properly balanced binder formulation is like looking for a needle in a haystack. We have shown for the first time that artificial intelligence (AI)-based optimization of alkali-activated binder formulations can significantly accelerate research.
The "Sequential Learning App for Materials Discovery" (SLAMD) aims to accelerate practice transfer. With SLAMD, materials scientists have low-threshold access to AI through interactive and intuitive user interfaces. The value added by AI can be determined directly. For example, the CO2 emissions saved per ton of cement can be determined for each development cycle: the more efficient the AI optimization, the greater the savings.
Our material database already includes more than 120,000 data points of alternative binders and is constantly being expanded with new parameters. We are currently driving the enrichment of the data with a life cycle analysis of the building materials.
Based on a case study we show how intuitive access to AI can drive the adoption of techniques that make a real contribution to the development of resource-efficient and sustainable building materials of the future and make it easy to identify when classical experiments are more efficient.
High greenhouse gas emissions from the production of building materials are a major contributor to the current climate crisis. However, developing alternative building materials is complex. Traditional laboratory methods are reaching their limits. Artificial intelligence, on the other hand, can give research a new dynamic.
Novel materials are usually developed manually in the laboratory rather than on a computer. This makes the processes time-consuming, difficult and expensive. With the app SLAMD (Sequential Learning App for Materials Discovery), materials researchers can explore the potential of artificial intelligence to speed up materials research and easily apply AI in the lab. The app was developed by our team at the Federal Institute for Materials Research and Testing (BAM) led by Prof. Sabine Kruschwitz together with a team in the Department of Building Materials and Construction Chemistry at TU Berlin led by Prof. Dietmar Stephan.
It uses material composition and characterization data to predict ideal material candidates. It can be used to optimize many material properties simultaneously and even incorporates database information such as carbon footprint, material cost or resource availability. Unlike the usual data-intensive AI methods, SLAMD optimally integrates existing knowledge and human feedback, and provides numerous decision support tools to precisely navigate complex scientific knowledge processes towards success.
In this talk, we will present some case studies where we were able to find suitable advanced materials in a few months instead of several years. We will talk about the challenges we overcame and the future potential we see for this approach to developing the green materials of the future.
For the construction of hot water storage tanks, ultra high performance concrete proofed to be a suitable building material to ensure water tightness. Common storage tanks build with concrete are designed to endure temperatures up to 90 °C. To increase the energy efficiency however, modern tanks need to withstand temperatures above 100 °C. With increasing temperature and correlating water vapor pressures, the cement must meet new requirements. Thermodynamic modelling is a promising tool for predicting the phase stabilities of minerals in the cement within these temperature and pressure ranges (T/P). Thus, mixture designs can be investigated and optimized with regard to the expected mineral phases in selected T/P-ranges. Additionally, predictions of the long-term material behavior can be derived from thermodynamic data and subsequently the experimental effort can be reduced notably. On the other hand, validation of predictions is needed. The base for the thermodynamic model is a thermodynamic equilibrium and thus, the experimental data for validation should approach the presumed conditions of the equilibrium. This study investigates variable experimental conditions for the hydration of Portland cement at 100 °C to reach a sufficiently progressed development of the phase composition. In case of Portland cement, the highest degree of hydration achievable within a reasonable time span is the most significant parameter. Therefore, Portland cement pastes with w/c ratios from 0.4 to 0.6 and dwell times up to three weeks were examined with powder X-ray diffraction to identify mineral phase changes. At 100 °C and high humidity, Portland cement paste shows the expected mineral phases like portlandite, katoite, and remaining clinker phases. The cement pastes with high water content and long dwell time seem to have the highest degree of hydration, even though the AFm phases stabilize with increasing w/c ratio. A dwell time of two weeks and a w/c ratio of 0.5 was found to provide the mineral composition with the highest degree of hydration including the major phase transitions.
The adaption of the set-up for gas permeability measurements for ultra-high performance concrete
(2022)
In the framework of this project, a steam pressure vessel was to be developed from ultra-high perfor-mance concrete (UHPC) to withstand process temperatures of 200 °C and the respective steam pressure of 15,5 bar. To guarantee the long-term water vapour tightness of the system, the permeability of two UHPC mixtures were tested after long-term cyclic autoclaving. As UPHC shows a high density and therefore low permeability, measurements after the RILEM-Recommendation (TC 116-PCD) reached their detection limit. Therefore, the measurement set-up was adapted to measure the permeability of highly dense UHPC more reliably and quickly. This adaption includes measurements in a higher pres-sure range, the change of sample size thickness and the usage of Ar as a medium compared with the RILEM Recommendation. Additionally, the system was equipped with two pressure sensors and Ar-flowmeters to guarantee a continuous record of the experimental parameters. The new system was tested and evaluated by comparing measurements with the RILEM recommended system. Preliminary results show that the adapted system is capable to provide efficient and reliable results of concrete with low permeability.
Most of the in-service failures of welded structures are due to fatigue damage occurring in the joints. Damage tolerant approaches based on the principles of Fracture Mechanics have been shown to play a key role in this framework, as the fatigue limit is defined by the non-propagating condition of multiple defects at the weld toe. The fatigue limit assessment can be performed using the cyclic R-curve analysis which consists in comparing the driving force of a crack propagating into a component, which depends on the geometry, material and external loads, with its resistance curve, i.e. the cyclic R-curve. The crack propagation occurs whenever the crack driving force is higher than the resistance to fatigue crack propagation, while the crack is arrested in the opposite case. Consequently, this suggests that the fatigue limit of a component is defined as that stress level at which the crack driving force curve is tangent to the crack resistance curve. In the present work, the cyclic R-curve analysis has been adopted for determining the fatigue limit of stress-relieved transverse non-load-carrying joints made of S355 structural steel and subjected to fatigue axial loadings. Experimental tests have been performed to evaluate the fatigue limit of the joints. The driving force, identified by the applied Stress Intensity Factor (SIF), has been evaluated by means of linear elastic finite element analysis taking advantage of the Peak Stress Method for its rapid estimation. Based on the experimental observations that the crack initiation and early crack growth phases in welded joints occur within the Heat Affected Zone (HAZ) the cyclic R-curve has been experimentally derived for both the base metal and HAZ material.
Ein Umlaufkühler ist im Betrieb explodiert. Splitter des zerborstenen Gehäuses aus Kunststoff wurden mit dem Kühlwasser in die Umgebung geschleudert, am Betriebsort entstand Personenschaden. Bei Funktionsprüfungen am beschädigten Gerät traten unerwartet - aber reproduzierbar - Knalleffekte bei Berührung der Außenoberfläche der Kupfer-Kühlschlange auf. Ein möglicher Mechanismus konnte im Labor durch Synthese von Kupferazid auf Kupferproben und Auslösung vergleichbarer Knalleffekte nachgestellt werden. Damit ist die Plausibilität des beschriebenen Schadensereignisses mit diesem oder einem ähnlich reagierenden Stoff belegt. Ein eindeutiger Nachweis darüber, dass bei dem aufgetretenen Schadensfall dieselbe chemische Reaktion stattgefunden hat, war nicht möglich, da die Belag-Überreste aus dem explodierten Kühlgerät für eine Analyse nicht mehr in ausreichender Menge verfügbar gewesen sind.
Quantification of the Total and Accessible Number of Functional Groups and Ligands on Nanomaterials
(2022)
Surface-functionalized organic and inorganic nanoparticles (NP) are of great interest in the life and material sciences, as they can be used e.g. as drug carriers, fluorescent sensors, and multimodal labels in bioanalytical assays and imaging applications. NP performance in such applications depends not only on particle size, size distribution, and morphology, but also on surface chemistry, i.e. the total number of surface functional groups (FG) and the number of FG accessible for subsequent functionalization with ligands or biomolecules, which in turn determines surface charge, colloidal stability, biocompatibility, and toxicity. Methods for FG quantification should be simple, robust, reliable, fast, and inexpensive, and allow for the characteriza-tion of a broad variety of nanomaterials differing in size, chemical composition, and optical properties.
Aiming at the development of simple, versatile, and multimodal tools for the quantification of many bioanalytically relevant FG such as amine, carboxy, thiol and aldehyde functionalities, we investigated and compared various analytical methods commonly used for functional group quantification. This includes electrochemical titration methods, dye-based optical assays, and other instrumental analytical techniques such as nuclear magnetic resonance, mass spectrometry, and thermal analysis methods.
The diversity of fused filament fabrication (FFF) filaments continues to grow rapidly as the popularity of FFF-3D desktop printers for the use as home fabrication devices has been greatly increased in the past decade. Potential harmful emissions and associated health risks when operating indoors have induced many emission studies. However, the lack of standardization of measurements impeded an objectifiable comparison of research findings. Therefore, we designed a chamber-based standard method, i.e., the strand printing method (SPM), which provides a standardized printing procedure and quantifies systematically the particle emission released from individual FFF-3D filaments under controlled conditions. Forty-four marketable filament products were tested. The total number of emitted particles (TP) varied by approximately four orders of magnitude (1E9 ≤ TP ≤ 1E13), indicating that origin of polymers, manufacturer-specific additives, and undeclared impurities have a strong influence. Our results suggest that TP characterizes an individual filament product and particle emissions cannot be categorized by the polymer type (e.g., PLA or ABS) alone. The user's choice of a filament product is therefore decisive for the exposure to released particles during operation. Thus, choosing a filament product awarded for low emissions seems to be an easily achievable preemptive measure to prevent health hazards.
Concrete has a long history in the construction industry and is currently one of the most widely used building materials. Especially precast concrete elements are frequently utilized in construction projects for standardized applications, increasing the quality of the composite material, as well as reducing the required building time. Despite the accumulated knowledge, continuous research and development in this field is essential due to the complexity of the composite combined with the ever-growing number of applications and requirements. Especially in view of global climate change, design aspects as CO2 emissions and resource efficiency require new mix designs and optimization strategies. A result of the material’s high complexity and heterogeneity on multiple scales is that utilizing the full potential with changing demands is highly challenging, even for the established industry. We propose a framework based on an ontology, which automatically combines experimental data with numerical simulations. This not only simplifies experimental knowledge transfer, but allows the model calibration and the resulting simulation predictions to be reproducible and interpretable. This research shows a way towards a more performance oriented material design. Within this talk we present our workflow for an automated simulation of a precast element, demonstrating the interaction of the ontology and the finite element simulation. We show the automatic calibration of our early-age concrete model [1, 2], to improve the prediction of the optimal time for the removal of the form work.
The aim of the project LeBeDigital is to present opportunities of digitalization for concrete applications and show a way towards a performance oriented material design.
Due to the high complexity of the manufacturing process of concrete and the range of parameters affecting the effective composite properties, a global optimization is challenging.
Currently, most optimization is only carried out on a narrow scope related to the respective players, e.g. a mix optimization for a target strength, or a design optimization for minimum weight, using a given mix. To enable a path toward a full global optimization
requires a reproducible chain of data, accessible for all contributors.
We propose a framework based on an ontology, which automatically combines experimental data with numerical simulations. This not only simplifies experimental knowledge transfer, but allows the model calibration and the resulting simulation predictions to be
reproducible and interpretable. In addition to an optimized set of parameters, this setup allows to study the quality and uncertainty of the data and models, as well as giving information about optimal experiments to improve the data set.
We will present the proposed optimization workflow, using the example of a precast concrete element. The contribution will focus on the workflow and challenges of an interoperable FEM formulation.
2D layered nanoparticles enable a distinct reduction of filler loadings in rubber compounds combined with a boost in performance due to their high surface to volume ratio. They often enable unique property profiles providing a great potential as effective fillers in rubber, especially by enhancing mechanical and barrier properties.
As the best possible incorporation into the elastomer matrix is crucial for the efficiency of the nanofiller, dispersing and exfoliation of the nanoparticles without formation of agglomerates usually constitutes an outstanding challenge - especially when using conventional processing methods. Laboratory-scale approaches for highly dispersed nanocomposites sometimes solve this problem, but these are often too energy and time consuming and provide no scale up possibility for real applications. Therefore, a latex premixing process was established to produce highly filled masterbatches, enabling the processing with conventional techniques.
The presence of nanoparticles greatly impacts the behavior of elastomeric compounds, besides affecting the properties of the final product also the processing is influenced (rheology, crosslinking).
In this study, nanocomposites of natural rubber and multilayer graphene (MLG) were prepared via a latex masterbatch route. Different strategies for masterbatch premixing are compared (stirring vs. ultrasonication, coagulation vs. drying). Dispersion and exfoliation of MLG were determined by transmission electron microscopy. The reinforcing effect of MLG affects the viscosity while the dispersed graphene layers may also act as diffusion barrier/absorbent for the crosslinking agents. In contrast to that, MLG forms physical crosslinks in the final product. Swelling measurements and differential scanning calorimetry allow a differentiation between chemical and physical network links. Different technical properties of the nanocomposites were measured with respect to mechanical and application relevant behavior.
The incorporation of nanoscale particles into elastomers enable a boost in performance and/or a distinct reduction of conventional filler loadings due to their high surface to volume ratio. 2D layered nanoparticles like graphene and graphene-related materials provide a great potential as effective fillers in rubber, especially by enhancing mechanical and barrier properties. The type and properties of the nanoparticles, their interface and the elastomeric matrix materials influence the technical behavior, and therefore the potential application fields of such rubber nanocomposites. Especially crucial for the efficiency of the nanofiller, however, is its best possible incorporation into the elastomer. The dispersing of nanoparticles without agglomerates usually constitutes a challenge when using conventional two-roll milling or internal mixing. Academic approaches for highly dispersed nanocomposites solve this problem but are often energy and time consuming with no feasible scale up possibility. Therefore, an ultrasonic assisted NR latex premixing process was established to produce highly filled masterbatches, enabling the main processing with conventional rubber processing techniques.
Two carbon-based nanoparticles with similar specific surface areas were investigated and incorporated in natural rubber as nanocomposites: A commercially available multilayer graphene (MLG) and a nanoscale carbon black (nCB). The mentioned premixed masterbatches were further processed to nanocomposites by the addition of matrix NR, two-roll milling, and hot pressing (vulcanization). By this procedure an increase in Young’s modulus of 157% (MLG) and 71% (nCB) could be obtained at a concentration level of 3 phr. As anisotropic material behavior was observable for the nanocomposites containing MLG, different measurement methods were investigated to quantify the orientation of the nanoparticles in the nanocomposites: Sorption measurements (swelling in 2 dimensions), hardness and dynamical mechanical analysis (in-plane vs. cross-plane), X-Ray diffraction and transmission and scanning electron microscopy.
Numerical simulations are essential in predicting the behavior of systems in many engineering fields and industrial sectors. The development of accurate virtual representations of actual physical products or processes (also known as digital twins) allows huge savings in cost and resources. In fact, digital twins would allow reducing the number of real, physical prototypes, tests, and experiments, thus also increasing the sustainability of production processes and products’ lifetime. Standard numerical methods fail in providing real time simulations, especially for complex processes such as additive manufacturing applications.
This work aims to use a reduced order model for efficient wire arc additive manufacturing simulations, calibrations and real-time process control. Model reduction, e.g. the proper generalized decomposition [1,2] method, is a popular concept to decrease the computational effort. A new mapping approach [3] was applied to simulate a moving heat source with the proper generalized decomposition. Using this procedure even complex models can be simulated in real-time. The physical model is later on calibrated with the use of a stochastic model updating process and the reduced order model, leading to an optimized real-time simulation.
In this contribution, a proper generalized decomposition model for a bead-on-plate wire arc additive manufacturing is presented. It is also coupled with a stochastic model updating process identifying the heat source characteristics as well as the boundary conditions of the transient thermal problem, whereas the heat source shape is simulated using a Goldak heat source
Laser metal deposition (LMD) as an additive manufacturing technique became increasingly important in recent years and thus the demand for component safety. This is the reason, for the need for reliable in-situ defect detection techniques. For laser beam weld seams an optical measurement technique based on an optical flow algorithm was successfully used to define the critical straining conditions that lead to hot cracking. This algorithm was adapted for bead-on-plate weld seams on LMD deposited layers of IN718 alloy while performing external strain on the specimen in an externally loaded hot cacking test facility. The resulting transversal hot cracks along the weld seam were localized via X-Ray inspection and the type of cracking confirmed by Scanning Electron Microscopy (SEM). The strain distribution was measured in the vicinity of the solidification front and correlated to the detected hot cracks. Based on the results this technique could be adopted for LMD experiments.
In recent years, the demand for new and sustainable products has been constantly rising. Especially cementitious materials are known for their high carbon footprint and novel approaches will be needed to counterbalance that. The BAM departments 7.1 (building materials) and 4.0 (Material and the environment) try to improve the sustainability of concrete panels by establishing a biofilm on the weather protection layer. Using an ultra-high-performance-concrete allows the production of very thin facade tiles with a small carbon footprint. Furthermore, the durability of these tiles is expected to surpass the one of “normal” concrete facades and offer the possibility of modular renewing of defective tiles instead of a wall, or even remodeling a whole building. The controlled application of biofilms on facades aims to improve biodiversity, microclimate, and air quality in cities. Furthermore, the greening of typically gray surfaces could improve the mental health of the residents. The project focuses on testing a multiplicity of concrete samples, varying e.g., in roughness or pH. The bioreceptivity is analyzed via laboratory tests, as well as in perennial outdoor experiments.
In pursuing the automated synthesis of metal nanoparticles (NPs), the capabilities of the “Chemputer” are deployed, for the first time, into the field of inorganic chemistry. Metal NPs have a substantial impact across different fields of science, such as photochemistry, energy conversion, and medicine. Among the commonly used nanoparticles, silver NPs are of special interest due to their antibacterial properties and applications in sensing and catalysis. However, many of the methods used to synthesize Ag NPs often do not result in well-defined products, the main obstacles being high polydispersity or a lack of particle size tunability.
The Chemputer is a modular, automated platform developed by the Cronin group for execution of multi-step, solution based organic synthesis. The machine has been further implemented at BAM, where we used this setup to perform automated organic syntheses, autonomously controlled by feedback derived from online NMR. In the Chemputer liquids can be transferred across a backbone, constructed from HPLC selection valves and syringe pumps. The Chemputer operates in a batch mode, common laboratory devices, such as heaters and glassware like round bottom flasks, are connected to the backbone, forming reaction modules. Solutions can be manipulated in these modules, and as all operations are controlled through a software script, reproducibility among individual syntheses is high. Likewise, any adjustments of the synthesis conditions, if required, are straightforward to implement and are documented in the reaction log file and a code versioning system.
We characterised Chemputer-synthesized nanoparticles using small-angle X-ray scattering, dynamic light scattering and further methods, showing that automated synthesis can yield colloids with reproducible and tuneable properties. The approach is an important first step towards the automation of nanoparticle syntheses in a modular, multipurpose platform. The modularity of the Chemputer opens many possibilities for the synthesis of a variety of different NP morphologies and sizes and potentially more complex structures. These advances and further work can help in the general investigations of silver nanoparticles by supplying a reliable and reproducible method of their synthesis and removing tacit knowledge by significantly reducing the experimental bias.
Calcium sulfate minerals are abundant in natural and engineered environments and they exist in the form of three hydrates: gypsum (CaSO4·2H2O), bassanite (CaSO4·0.5H2O), and anhydrite (CaSO4). Due to their relevance in natural and industrial processes, the formation pathways of these calcium sulfate phases from aqueous solution have been the subject of intensive research1.
The state-of-the-art of the calcium sulfate formation mechanisms builds upon and goes beyond what we have come to appreciate in the astounding intricacy of other mineral formation processes from ions in aqueous solutions. The original, and rather naive, '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 species2. These include solute clusters (e.g. prenucleation clusters, PNCs), liquid(-like) phases, as well as amorphous and nanocrystalline solids etc.. In this context, a number of studies have already revealed that nucleation in the CaSO4-H2O system is non-classical, where the formation of the different crystalline phases involves several steps including a common amorphous precursor1, 3, 4.
In this contribution we show that the formation of the amorphous phase involves the aggregation of small primary particles into larger disordered aggregates exhibiting a "brick-in-the-wall" structure5, 6. The actual crystallization occurs by the restructuring and coalescence of the particles ("bricks") into a given calcium sulfate phase depending on the physicochemical conditions of the solution. Importantly, the rearrangement process does not continue until a (nearly-)perfect homogeneous single crystal is obtained. Instead it comes to a stop, or at least significantly slows down. Such a process thus yields a final imperfect mesocrystal, composed of smaller domains rather than a continuous crystal structure, within which the domains are separated by an amorphous (i.e. less ordered) calcium sulfate phase.
Hence, the non-classical crystallization process of CaSO4 yields a final imperfect mesocrystal with an overall morphology resembling that of a single crystal, yet composed of smaller nano-domains. Importantly, these observations reveal that organic-free calcium sulfate mesocrystals grown by a particle mediated-pathway preserve in the final crystal structure a “memory” or “imprint” of their non-classical nucleation process, something that has been overlooked until now. Furthermore, the nano-scale misalignment of the structural sub-units within these crystals can propagate through the length-scales, and be expressed macroscopically as misaligned zones/domains in large single crystals (Fig. 1). Indeed, by considering large anhydrite crystals from the famous Naica Mine (“Cueva de los cristales”) we observed a suite of correlated self-similar void defects spanning multiple length-scales7 (Fig 2). These flaws, in the macroscopic crystal, stem from “seeds of imperfection” originating from a particle-mediated nucleation pathway. Hence, building a crystal could be viewed as Nature stacking blocks in a game of Tetris, whilst slowly forgetting the games core concept and failing to fill rows completely.
Calcium sulfate minerals are abundant in natural and engineered environments and they exist in the form of three hydrates: gypsum (CaSO4·2H2O), bassanite (CaSO4·0.5H2O), and anhydrite (CaSO4). Due to their relevance in natural and industrial processes, the formation pathways of these calcium sulfate phases from aqueous solution have been the subject of intensive research1.
The state-of-the-art of the calcium sulfate formation mechanisms builds upon and goes beyond what we have come to appreciate in the astounding intricacy of other mineral formation processes from ions in aqueous solutions. The original, and rather naive, '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 species2. These include solute clusters (e.g. prenucleation clusters, PNCs), liquid(-like) phases, as well as amorphous and nanocrystalline solids etc.. In this context, a number of studies have already revealed that nucleation in the CaSO4-H2O system is non-classical, where the formation of the different crystalline phases involves several steps including a common amorphous precursor1, 3, 4.
In this contribution we show that the formation of the amorphous phase involves the aggregation of small primary particles into larger disordered aggregates exhibiting a "brick-in-the-wall" structure5, 6. The actual crystallization occurs by the restructuring and coalescence of the particles ("bricks") into a given calcium sulfate phase depending on the physicochemical conditions of the solution. Importantly, the rearrangement process does not continue until a (nearly-)perfect homogeneous single crystal is obtained. Instead it comes to a stop, or at least significantly slows down. Such a process thus yields a final imperfect mesocrystal, composed of smaller domains rather than a continuous crystal structure, within which the domains are separated by an amorphous (i.e. less ordered) calcium sulfate phase.
Hence, the non-classical crystallization process of CaSO4 yields a final imperfect mesocrystal with an overall morphology resembling that of a single crystal, yet composed of smaller nano-domains. Importantly, these observations reveal that organic-free calcium sulfate mesocrystals grown by a particle mediated-pathway preserve in the final crystal structure a “memory” or “imprint” of their non-classical nucleation process, something that has been overlooked until now. Furthermore, the nano-scale misalignment of the structural sub-units within these crystals can propagate through the length-scales, and be expressed macroscopically as misaligned zones/domains in large single crystals. Indeed, by considering large anhydrite crystals from the famous Naica Mine (“Cueva de los cristales”) we observed a suite of correlated self-similar void defects spanning multiple length-scales7. These flaws, in the macroscopic crystal, stem from “seeds of imperfection” originating from a particle-mediated nucleation pathway. Hence, building a crystal could be viewed as Nature stacking blocks in a game of Tetris, whilst slowly forgetting the games core concept and failing to fill rows completely.
Calcium sulfate minerals are abundant in natural and engineered environments in the form of three phases: gypsum (CaSO4·2H2O), bassanite (CaSO4·0.5H2O), and anhydrite (CaSO4). Due to their relevance in natural and industrial processes, the formation pathways of these phases from aqueous solution have been the subject of intensive research, a number of studies have already revealed that nucleation in the CaSO4-H2O system is non-classical, The formation of the different crystalline phases involves several steps including a common amorphous precursor.
In this contribution we show that the formation of the amorphous phase involves the aggregation of small primary particles into larger disordered aggregates exhibiting a "brick-in-the-wall" structure. The actual crystallization occurs by the restructuring and coalescence of the "bricks" into a given calcium sulfate phase depending on the physicochemical conditions of the solution. Such a process yields a final imperfect mesocrystal, composed of smaller domains rather than a continuous single crystal structure.
These observations reveal that organic-free calcium sulfate mesocrystals grown by a particle mediated-pathway might preserve in the final crystal structure an “imprint” of their growth pathways. Indeed, by considering large anhydrite crystals from the famous Naica Mine we observed a suite of correlated self-similar void defects spanning multiple length-scales. These flaws, in the macroscopic crystal, stem from “seeds of imperfection” originating from an original particle-mediated growth. Hence, building a crystal could be viewed as Nature stacking blocks in a game of Tetris, whilst slowly forgetting the games core concept and failing to fill rows completely.
Thermal spraying provides a rapid method for additive deposition of various ceramics as electrical insulation in applications where polymers are not suitable. New applications in complex shaped additive manufactured metal parts are emerging for example in large scale electrical devices. Microstructural and dielectric evaluation of coatings is crucial to the employment of such free-form processes. The properties and microstructure of the plasma sprayed alumina coatings are compared with dense reference samples of the same powder produced by spark plasma sintering (SPS). To obtain dense bulk samples from the coarse alumina powder for spray coating, SPS is used.
Samples are fabricated by atmospheric plasma spraying (APS) of commercially available alumina powder (d50 = 33 µm) on copper substrates and by SPS of the same powder. Microstructure and porosity were analyzed by optical microscopy and scanning electron microscopy (SEM). Phase compositions were determined by X-ray diffraction (XRD). Dielectric properties such as DC resistance, dielectric strength, dielectric loss, and relative permittivity were determined according to the standards. The microstructure and dielectric properties of the coating and bulk material are compared to assess whether the coating is suitable for use in electrical insulation application.
Design of freedom, performance improvement, cost reduction and lead time reduction are key targets when manufacturing parts in a layer-by-layer fashion using the laser powder bed fusion process (LPBF). Many research groups are focussed on improving the LPBF process to achieve the manufacturing of sound parts from a structural integrity perspective. In particular, the formation and distribution of residual stress (RS) remains a critical aspect of LPBF. The determination of the RS in LPBF benefits from the use of neutron diffraction (ND), as it allows the non-destructive mapping of the triaxial RS with a good spatial resolution. Two case studies are presented based on experiments carried out on the angular-dispersive neutron diffractometers Strain Analyser for Large Scale Engineering Applications (SALSA) (Institut Laue Langevin, Grenoble) and STRESS-Spec (FRM II, Garching). The RS in LPBF parts having a rectangular and more complex geometry (lattice structure) is analysed. The former example discusses the mapping of the RS in a rectangular body manufactured from stainless steel 316L. The manufacturing of these parts was monitored using an in-situ thermography set-up to link the RS to the thermal history. The latter discusses the RS in a lattice structure manufactured from the nickel base superalloy IN625. This geometry is challenging to characterise, and the use of a X-ray computed tomography twin is presented as tool to support the alignment of the ND experiment. The results from these case studies show a clear link between the thermal history and the RS magnitudes, as well as giving insights on the RS formation.
The influence of the inter-layer-time and the scanning velocity on the surface and bulk residual stress in laser powder bed fused 316L specimens was investigated. This study combines X-ray and neutron diffraction results with the thermal history of the specimens acquired through in-situ process monitoring. The process parameter variations were observed to directly influence the thermal history, which gave new insights in the assessment of the residual stress results.
In this study the so-called laser-induced periodic surface structures (LIPSS, ripples) were produced on titanium alloy (Ti6Al4V) surfaces upon scan processing in air by a Ti:sapphire femtosecond (fs) laser. The tribological performance of the resulting surfaces was qualified in linear reciprocating sliding tribological tests (RSTT) against balls made of different materials (100Cr6 steel/Al2O3/Si3N4) using different oil-based lubricants. The admixture of the additive 2-ethylhexylzinc-dithiophosphate (ZDDP) to a base oil containing only anti-oxidants and temperature stabilizers disclosed the synergy of the additive with the laser-oxidized nanostructures. This interplay between the laser-textured sample topography and the local chemistry in the tribological contact area reduces friction and wear.
Ziel von fraktographischen Untersuchungen ist die Auswertung von makroskopischen und mikroskopischen Bruchflächenmerkmalen und daraus resultierend die Bestimmung des Bruchmechanismus eines Bauteils aus einem Schadensfall. Die Grundlage für die Bewertung von Bruchmerkmalen stammt dabei aus zuvor durchgeführten eigenen Vergleichsversuchen und aus der Literatur. Eine fraktographische Analyse kann sehr aufwändig sein und setzt in jedem Fall erhebliches Erfahrungswissen voraus. Im IGF-Vorhaben „iFrakto“ wird Software entwickelt, die auf Basis von digitalisiertem Expertenwissen, Machine Learning und unter Zuhilfenahme von Topographie-Daten anhand von REM-Aufnahmen Bruchmerkmale und Bruchmechanismen quantitativ bestimmt, s. Abbildung. Solche Software soll mittelfristig direkt am REM oder bei der nachfolgenden Auswertung wissensbasierte Vorschläge für die Bewertung von Bruchflächen liefern. Als Grundlage hierfür wurden Ringversuche unter Fraktograph/inn/en durchgeführt, um die Wissensbasis zu schaffen, die praxisrelevanten Anforderungen an solche Software abzufragen und erste Praxistests durchzuführen. Die bisherigen Ergebnisse werden vorgestellt und die Relevanz der Auswertestrategie und unterschiedlicher Sensordaten bewertet.
Tempered martensite-ferritic steels, such as the grade P92 steel studied in this contribution, exhibit pronounced macroscopic cyclic softening under isothermal low-cycle fatigue (LCF) and non-isothermal thermomechanical fatigue (TMF) conditions, which is considered to be the predominant degradation mechanism in high-temperature fatigue in this and other material groups. However, such softening processes are highly complex since microscopic (e.g., recovery) and macroscopic (e.g., crack initiation and growth), as well as global and local effects superimpose, especially under creep-fatigue conditions. In this contribution, we discuss the cyclic deformation and softening behavior of P92 in strain-controlled LCF, in-phase (IP) TMF, and out-of-phase (OP) TMF tests with and without dwell times in the temperature range from 300 °C to 620°C. EBSD-based dislocation analysis on various fatigued material states confirms the continuous redistribution and annihilation of geometrically necessary dislocations in all studied states, which can be quantitatively correlated with macroscopic softening despite different damage mechanisms for different test types. Deviations from this correlation are observed for OP TMF and LCF with dwell times, i.e., for conditions where optical microscopy reveals pronounced crack-oxidation interactions at the specimen surfaces.
In typical material oriented research projects numerous types and sources of data need to get connected to form the final outcome. The data-structures have to be described in a manner semantically concise enough so that all participants share the meaning and at the same time flexible enough to allow connecting findings and facts that have not been connected before.
The present contribution describes the approach that is being taken in a public funded research project with two cooperating research institutes. The aim of the data-management solution is to describe and interlink three main entity types: material entities like a test specimen that is under observation, immaterial entities like a fatigue life model and processes that generate and transform the immaterial and material entities.
The shared understanding of what is described by the data is achieved by referring to existing linked data resources. In addition a common thesaurus that is subject to ongoing discussion is used for concepts and terms that need precision beyond publicly available concept descriptions. The data associated with the entities and processes and entities is rather small and well structured. The entities and processes covered by the vocabularies are typical to laboratories performing fatigue testing and microstructure analysis. Through the interlinking of the entities and processes it becomes possible to intuitively understand the knowledge that is accumulating in the database. For example it is easy to trace the history of a creep test specimen starting from the chemical composition that has been analyzed for the heat, continuing with the heat treatment of the material, going into the creep test itself with the associated creep data and finally finding the transmission electron microscopy images that have been taken from the crept sample.
The presented approach is prototypical way to tackle the sustainable management of structured open research data. Open questions remain for example with the management of attributions, the acceptance of an increased effort in data creation and the access control to specific regions of the data. On the other hand the approach sketches what added value can be created, if the community adopts and contributes to the linked data principles.
The mechanical strength of wrought high-strength aluminum alloys is essentially based on precipitation hardening, possibly in combination with prior forming, e. g. by stretching. Important parameters for achieving an optimum combination of hardness, strength, ductility, toughness, and further properties such as corrosion resistance are age-hardening temperature and time.
During thermal (mechanical) treatment, nucleation and growth of precipitates takes place, leading to the desired degree of hardening. In aluminum alloys, precipitation sequences are usually passed through, i. e. a sequence of metastable precipitates is formed before the stable phase can precipitate. The optimum combination of properties is therefore based on a certain (optimum) microstructure, which can, however, change during the use of a component, since the microstructure is not stable. This happens in particular when the operating temperatures are close to the aging temperature and/or the operating times are sufficiently long. An external mechanical load may accelerate the processes. The presentation gives some examples for this.
Laser welding is an appropriate technique for joining Laser Powder Bed Fusion (L-PBF) parts together and to conventional wrought ones. The potential consists of profiting from synergies between additive and conventional manufacturing methods and overcoming the existing limitations of both. On the one hand, L-PBF is a widely spread metal-based additive manufacturing technique suitable for generating complex parts which can present intrinsic designed cavities, conformal cooling channels, and filigree structures contributing to sustainable manufacturing and efficiency-oriented designs. On the other hand, chamber sizes for producing L-PBF parts are limited, and the process is time-consuming. Thus, its employment is not for every geometry justified. Additionally, they are in most cases individual elements of a larger assembly and need to be joined together to conventionally fabricated parts.
The present research suggests laser welding parameters to adequately bond pairs of wrought and L-PBF processed plates and two L-PBF plates of Inconel 718 in butt position. L-PBF samples are printed in three different build-up orientations. Additionally, the influence of as-built L-PBF roughness qualities and usual pre-weld preparations such as edge milling are examined. The effect of normed pre-weld heat treatments is also contemplated. Identified cracks are analyzed by means of EDS in order to confirm the present phases on the areas of interest. EBSD is also employed to obtain a clear depiction of the crystallographic texture and distribution of the hot cracks.
The quality of the weldment was examined according to existing standards. Substantial differences in seam geometry and microstructure across different edge’s surface qualities and build directions of stress relieved L-PBF parts have not been detected. Nevertheless, even if no other irregularities are present in the seam, variability in liquation cracking susceptibility has been confirmed. This defect is prone to happen when parts made of this nickel-based superalloy are welded together when not enough precautions are taken. It has been determined that grain size and ductility of the material before welding play a crucial role and mitigating or intensifying these imperfections. Moreover, recommendations are presented to avoid this potential welding defect.
With regard to efficient production, it is desirable to combine the respective advantages of additively and conventionally manufactured components. Particularly in the case of large-volume components that also include filigree or complex structures, it makes sense to divide the overall part into individual elements, which afterwards have to be joined by welding.
The following research represents a first step in fundamentally investigating and characterizing the joint welding of Laser Powder Bed Fusion (L-PBF) components made of Inconel 718. For this purpose, bead-on-plate welds were performed on plates manufactured using the L-PBF process and compared with the conventionally manufactured material. Conventional laser beam welding was used as welding process. The weld geometry was investigated as a function of the L-PBF build-up orientation. It was found that the welding depth and weld geometry differ depending on this orientation and in comparison to the conventional material.
Geosynthetic materials are applied in measures for coastal protection. Weathering or any damage of constructions, as shown by a field study in Kaliningrad Oblast (Russia), could lead to the littering of the beach or the sea (marine littering) and the discharge of possibly harmful additives into the marine environment. The ageing behavior of a widely used geotextile made of polypropylene was studied by artificial accelerated ageing in water-filled autoclaves at temperatures of 30 to 80° C
and pressures of 10 to 50 bar. Tensile strength tests were used to evaluate the progress of ageing, concluding that temperature rather than pressure was the main factor influencing the ageing of geotextiles. Using a modified Arrhenius equation, it was possible to calculate the half-life for the loss of 50% of the strain, which corresponds to approximately 330 years.
The complexity of any microstructural characterization significantly increases when there is a need to evaluate the icrostructural evolution as a function of temperature. To date, this characterization is primarily performed by undertaking elaborative ex-situ experiments where the material’s heating procedure is interrupted at different temperatures or times. Moreover, these studies are often limited to a region smaller than the representative elementary volume, which can lead to partial or even biased interpretations of the collected data. This limitation can be greatly overcome by using in-situ synchrotron X-ray refraction (SXRR).
To assess the ability of cracks to grow, a robust determination of the threshold against fatigue crack propagation ∆Kth is of paramount importance. The standards ASTM E647 and ISO 12108 introduce operational definitions of ∆Kth based on the crack propagation rate da/dN. For evaluating ∆Kth, both suggest fitting a linear function to a defined subset of the logarithmic ∆K – da/dN test data, where ∆Kth follows by evaluating the linear function at da/dN = 10-7 mm/cycle and da/dN = 10-8 mm/cycle, respectively.
In general, this kind of fit suffers from a bad representation of the actual curvature of the crack propagation curve. Therefore, we propose a robust method for evaluating ∆Kth using a non-linear function that reduces the artificial conservativeness induced by the evaluation method as well as the susceptibility to scatter in test data and the influence of test data density. The method is calibrated against a large set of S690QL crack growth data obtained from a total of 48 specimens, and validated against a set of S355NL and S960QL data (3 specimens each), obtained as a part the IBESS (integral fracture mechanics determination of the fatigue strength of welds) project.
Hexakis(n-alkyloxy)triphenylene) (HATn) consisting of an aromatic triphenylene core and alkyl side chains are model discotic liquid crystal (DLC) systems forming a columnar mesophase. In the mesophase, the molecules of HATn self-assemble in columns, which has one-dimensional high charge carrier mobility along the columns. Here, a homologous series of HATn with different length of the alkyl chain (n=5,6,8,10,12) is investigated using differential scanning calorimetry (DSC), broadband dielectric spectroscopy (BDS) and advanced calorimetric techniques including fast scanning calorimetry (FSC) and specific heat spectroscopy (SHS). The investigation of the phase behavior was done utilizing DSC experiments and the influence of the alkyl chain length on the phase behavior was revealed. By the dielectric investigations probing the molecular mobility, a γ-relaxation due to localized fluctuations as well as two glassy dynamics the αcore and αalkyl relaxation were observed in the temperature range of the plastic crystalline phase. Moreover, the observed glassy dynamics were further studied employing advanced calorimetry. All observed relaxation processes are attributed to the possible specific molecular fluctuations and discussed in detail. From the results a transition at around n=8 from a rigid constrained (n=5,6) to a softer system (n=10,12) on a molecular lenght scale was revealed with increasing alkyl chain length. A counterbalance of two competing effects of a polyethylene like behavior of the alkyl chains in the intercolumnar domains and self-organized confinement is discussed in the context of a hindered glass transition.
Polymers with intrinsic microporosity are promising candidates for the active separation layer in gas separation membranes. These polymers are characterized by a high permeability and reasonable permselectivity. The latter point is somehow surprising because for microporous systems a more Knudson-like diffusion is expected then a size dependent temperature activated sieving process. It was argued in the framework of a random gate model that molecular fluctuations on a time scale from ps to ns are responsible for the permselectivity.
Her a series of microporous polynorbornenes with bulky Si side groups and a rigid backbone are considered which have different microporosity characterized by BET surface area values.
First inelastic time-of-flight neutron scattering measurements were carried out to investigate the low frequency density of state (VDOS). The measured data show the characteristic low frequency excess contribution to the VDOS above the Debye sound wave level, generally known as the Boson peak in glass-forming materials. It was found the maximum position of the Boson peak correlates with the BET surface area value.
For two selected comparable polynorbornenes elastic scans as well as QENS measurements by a combination of neutron time-of-flight and backscattering are carried out. A low temperature relaxation process was found for both polymers. This process was assigned to the methyl group rotation. It was analysed in terms of a jump diffusion in a three-fold potential. The analysis of the dependence of the elastic incoherent structure factor on the scattering vector yields the number of methyl groups which might be immobilized.
Der Vortrag stellt die neuesten Entwicklungen an der BAM zur Bestimmung der elektrostatischen Empfindlichkeit von Explosivstoffen dar. Ausgehend von der Motivation unsererseits diese Thematik wieder intensiver zu bearbeiten werden ein neues Messgerät und erste Ergebnisse vorgestellt. Lücken im sicherheitstechnischen Regelwerk zur Einstufung von Explosivstoffen hinsichtlich ihrer elektrostatischen Empfindlichkeit und daraus abgeleiteter Schutzmaßnahmen in der Industrie werden dargestellt.
Differential Scanning Calorimetry (DSC) may be used to avoid testing for explosive and self-reactive properties according to the legal regulations of chemicals substances and dangerous goods.
Demonstrated measured exothermic decomposition energy value significantly affected by numerous factors - choice of sample vessel, sample mass, baseline shape, peak shape, heating rate.
High-strength fine-grained structural steels have great potential for modern weight optimized steel construc-tions. Efficient manufacturing and further weight savings are achievable due to Wire Arc Additive Manu-facturing (WAAM). First commercial high-strength welding consumables for WAAM are already available. However, the application is still severely limited due to a lack of knowledge and guidelines for the industry regarding welding residual stresses and component safety in manufacturing and operation. Residual stresses may be critical regarding the special microstructure of high-strength steels in context with the risk of cold cracking and component performance in service. Therefore, process- and material-related influences, as well as the design effects on residual stress formation and cold cracking, are being investi-gated in a research project (IGF 21162 BG) focusing a high-strength WAAM welding consumable with yield strength of over 800 MPa. Objectives are the establish-ment of special WAAM cold cracking tests and pro-cessing recommendations allowing economical, suita-ble, and crack-safe WAAM of high-strength steels. First studies on process-related influences showed transfor-mation residual stresses arising during cooling, which significantly influence stress evolution of the compo-nent during layer-wise build-up. This has not yet been investigated for WAAM of high-strength steels. Focus of this study is on the systematic investigation of interactions of the WAAM welding process and design with cooling time, hardness, and residual stresses.
Defined open hollow cuboids were welded and investi-gated under systematic variation (design of experi-ments, DoE) of the scale/dimensions (cf. Fig. 1a) and heat control (interlayer temperature Ti: 100–300 °C), heat input E: 200–650 kJ/m. The welding parameters were kept constant as possible to avoid any influence by the arc and the material transfer mode. The heat input adjusted primarily via the welding speed. The resulting different weald bead widths were considered by different build-up strategies (weld beads per layer) to ensure defined wall thicknesses. The hardness was determined on cross-sections taken from the manufac-tured hollow cuboids (Fig. 1c) and the analysis of the residual stress state was carried out by means of X-ray diffraction (XRD) at defined positions on the lateral wall (Fig. 1b).
The hardness is higher at the top compared to the lower weld beads, as shown in Fig. 1c exemplarily for central test parameters of the DoE = 425 kJ/mm, Ti = 200 °C). This may be attributed to the specific heat control of the top weld beads, i.e., quenching effects, which are not tempered by weld beads above as is the case for lower weld beads implying a higher hardness. It was observed that the hardness level decreases with increasing energy per unit length, while the in-terpass temperature has a rather low influence on the hardness
Residual stress analysis was performed on the lat-eral wall in the welding direction, cf. Fig. 1b, to deter-mine the influence of heat control and design. In the top area of the wall, maximum longitudinal residual stress-es of up to over 500 MPa exhibit, which corresponds to approx. 65% of the nominal yield strength of the mate-rial. The statistic evaluation of stress levels in welding direction of all test specimens show that adaption of heat input may reduce welding stresses up to 50%. In-terpass temperature has less pronounced effect on cool-ing times, microstructure, and on the residual level within parameter matrix. Overall, the results show a significant influence of heat input and component di-mensions on the residual stresses and minor effect of the interpass temperature. Hence, the properties of the specimens may be effectively adjusted via heat input. The working temperatures should be considered for global shrinkage behavior or restraints. Such investiga-tions of residual stress are necessary to further deter-mine local and global welding stresses regarding the consequences on the component safety during manu-facturing and service.
Additive manufacturing methods such as laser powder bed fusion (LPBF) allow geometrically complex parts to be manufactured within a single step. However, as an aftereffect of the localized heat input, the rapid cooling rates are the origin of the large residual stress (RS) retained in as-manufactured parts. With a view on the microstructure, the rapid directional cooling leads to a cellular solidification mode which is accompanied by columnar grown grains possessing crystallographic texture. The solidification conditions can be controlled by the processing parameters and the scanning strategy. Thus, the process allows one to tailor the microstructure and the texture to the specific needs. Yet, such microstructures are not only the origin of the mechanical anisotropy but also pose metrological challenges for the diffraction-based RS determination. In that context the micromechanical elastic anisotropy plays an important role: it translates the measured microscopic strain to macroscopic stress. Therefore, it is of uttermost importance to understand the influence of the hierarchical microstructures and the texture on the elastic anisotropy of LPBF manufactured materials.
This study reveals the influence of the build orientation and the texture on the micro-mechanical anisotropy of as-built Inconel 718. Through variations of the build orientation and the scanning strategy, we manufactured specimens possessing [001]/[011]-, [001]-, and [011]/[111]-type textures. The resulting microstructures lead to differences in the macroscopic mechanical properties. Even further, tensile in-situ loading experiments during neutron diffraction measurements along the different texture components revealed differences in the microstrain response of multiple crystal lattice planes. In particular, the load partitioning and the residual strain accumulation among the [011]/[111] textured specimen displayed distinct differences measured up to a macroscopic strain of 10 %. However, the behavior of the specimens possessing [001]/[011]-and [001]-type texture was only minorly affected. The consequences on the metrology of RS analysis by diffraction-based methods are discussed.
Laser powder bed fusion (PBF-LB/M) of metallic alloys is a layer wise additive manufacturing process which provides significant scope for more efficient designs of components, benefiting performance and weight, leading to efficiency improvements for various sectors of industry. However, to benefit from these design freedoms, knowledge of the high produced induced residual stress and mechanical property anisotropy associated with the unique microstructures is critical. X-ray and neutron diffraction are considered the benchmark for non-destructive characterization of surface and bulk internal residual stress. The latter, characterized by the high penetration power in most engineering alloys, allows for the use of diffraction angle close to 90° enabling a near cubic sampling volume to be specified. However, the complex microstructures of columnar growth with inherent crystallographic texture typically produced during PBF-LB/M of metallics present significant challenges to the assumptions typically required for time efficient determination of residual stress. These challenges include the selection of an appropriate set of diffraction elastic constants and a representative strain-free reference for the material of interest. In this presentation advancements in the field of diffraction-based residual stress analysis of L-PBF Inconel 718 will be presented. The choice of an appropriate set of diffraction-elastic constants depending on the underlying microstructure will be described.
Immunoanalytical Techniques, i.e., antibody-based analytical methods, have been used for decades in clinical diagnostics. What makes them attractive for other fields of application is their short time-to-result and high sensitivity. Microplate-based assays such as ELISA have been adopted early in environmental and food analysis. Yet, to make immunoassays even faster, more sensitive, robust, and, most desirable, portable, advanced materials, sometimes developed for other purposes, can be profitably used to achieve these goals. Materials can be novel labels, e.g., chemical or particle labels, such as fluorophores or nanoparticles. Carrier particles, such as magnetic or polymer beads, make it possible to adopt the assays to meso- or microfluidic set-ups and encoding them opens the path to multiplex analysis. Specialty electrodes can enable for higher sensitivity in electrochemical detection. All this broadens the scope of application and lowers effort and cost for analysis at the point-of-need.
Analytical methods based on the selectivity of antibodies, often called immunoassays, are a back-bone of clinical laboratory diagnostics. To bring them to the field, i.e., to make immunoanalytical methods portable, hopefully even faster, more sensitive, and robust, advanced materials are re-quired. Materials can be novel labels, e.g., chemical or particle labels, such as fluorophores or na-noparticles. Carrier particles, such as magnetic or polymer beads, make it possible to adopt the as-says to meso- or microfluidic set-ups and encoding them opens the path to multiplex analysis. Spe-cialty electrodes can enable for higher sensitivity in electrochemical detection. Without research into better materials, efforts to bring analysis to the point-of-need will not bear fruit.
The aim of a fractographic investigation is the evaluation of macroscopic and microscopic fracture surface characteristics and, as a result, the determination of the fracture mechanism of a component from a failure case. The basis for such evaluations of fracture characteristics comes from actual comparative mechanical testing and from the literature. A fractographic analysis can be very complex and, in any case, requires considerable experience. In the IGF project "iFrakto", software is being developed that quantitatively determines fracture characteristics and fracture mechanisms utilizing digitized expert knowledge, machine learning, and standard 2D and topographical data from SEM imaging. Topographical data are obtained from 4QBSE detector using shape-from-shading technology. In the medium term, a software tool should provide knowledge-based suggestions for the evaluation of fracture surfaces in real time during SEM work or at subsequent evaluation. As a basis for this, round robins were carried out among fractographers in order to create a knowledge base, to query the practice-relevant requirements for such tools and to carry out first practical tests. Actual results are presented and the relevance of the evaluation strategy is evaluated.
In the present talk the basics of the Raman spectroscopy and particularly of Raman microscopy are explained. Advantages and disadvantages of the method are highlighted through selected case studies. In the second part of the lecture examples of correlative imaging with electron, X-ray, ion and optical microscopies from micro- to the nanoscale are highlighted.
Mit der Digitalisierung von Materialien und Prozessen ist ein Paradigmenwechsel in der Materialentwicklung, -gestaltung und -optimierung verbunden, welcher gleichermaßen vielseitige Möglichkeiten eröffnet und eine große Herausforderung darstellt. Insbesondere sind bei den Digitalisierungsbestrebungen die Qualitätssicherung von Prozessen und Ausgabedaten sowie die Interoperabilität zwischen Anwendungen nach FAIR-Prinzipien (Findability, Accessibility, Interoperability, Reusability) sicherzustellen. Dies umfasst die Speicherung, Verarbeitung und Abfrage von Daten in möglichst standardisierter Form, wobei entsprechend auch Normungs- und Standardisierungsgremien beteiligt werden müssen. Um der Herausforderung gerecht zu werden, Materialdaten für alle Beteiligten konsistent zu kontextualisieren, müssen alle notwendigen Informationen zum Zustand des Materials inklusive produktions- und anwendungsbedingter Veränderungen über eine einheitliche, maschinenlesbare Beschreibung verfügbar gemacht werden. Hierfür sollen Ontologien genutzt werden, da sie maschinenverständliche und -interpretierbare Wissensrepräsentationen durch semantische Konzeptualisierungen ermöglichen, die für das Datenmanagement und die Digitalisierung im Bereich der Materialwissenschaften benötigt werden.
Dieses hochaktuelle Thema der Integration und Wiederverwendung von Wissen und Daten aus Herstellung, Bearbeitung und Charakterisierung von Materialien wird in den Projekten Innovationsplattform MaterialDigital (PMD, materialdigital.de) und Materials-open-Lab (Mat-o-Lab, matolab.org) adressiert. Diese beiden unter der Beteiligung der Bundeanstalt für Materialforschung und -prüfung (BAM) durchgeführten Projekte wurden auf der 39. Vortrags- und Diskussionstagung „Werkstoffprüfung“ (2021) grundlegend vorgestellt. In dieser Präsentation sollen die Weiterentwicklungen hinsichtlich der Speicherung von Zugversuchsdaten gemäß einer normenkonformen ontologischen Repräsentation vorgestellt werden. Das umfasst den Weg von der Entwicklung einer Ontologie nach Norm, der Konvertierung von Daten aus Standardtests in das interoperable RDF-Format bis hin zur Verknüpfung von Ontologie und Daten. Letztendlich können die entsprechenden Daten in einem Triple Store abgelegt und abgefragt werden.
Die übliche Standardisierung von mechanischen Prüfverfahren im Bereich der Materialwissenschaft und Werkstofftechnik dient als solide Grundlage für die Ontologieentwicklung. Daher wurde der Zugversuch von Metallen bei Raumtemperatur nach DIN EN ISO Norm 6892-1:2019-11 als einer der ersten Anwendungsfälle in den genannten Projekten ausgewählt. Die Betrachtung und Beschreibung des Zugversuchs beinhaltet sowohl dessen ontologische Darstellung als auch eine exemplarische Datengenerierung. Die semantische Verbindung von Ontologie und Daten führt zu Interoperabilität und einer verbesserten Abfragefähigkeit.
Following the new paradigm of materials development, design and optimization, the digitalization of materials and processes is the main goal which imposes a huge challenge. In this respect, the quality assurance of processes and output data as well as the interoperability between applications following FAIR (findability, accessibility, interoperability, reusability) principles are to be ensured. This includes storage, processing and querying of data in a preferably standardized form, also addressing the incorporation of standardization bodies. To meet the challenge to contextualize material data in a way that is consistent with all stakeholders, all necessary information on the condition of the material including production and application-related changes have to be made available via a uniform, machine-readable description. For this purpose, ontologies are to be used since they allow for machine-understandable knowledge representations and semantic conceptualizations that are needed for data management and the digitalization in the field of materials science.
With respect to this currently ever-growing topic of integration and reuse of data and knowledge from synthesis, production and characterization of materials, this presentation shows the efforts taken within the project Platform MaterialDigital (PMD, materialdigital.de) to store tensile test data in accordance with a standard-compliant ontological representation. The includes the path from developing an ontology in accordance with the respective standard, converting ordinary and arbitrarily selected data gained from standard tests into the interoperable RDF format, up to connecting the ontology and data, respectively. Finally, such data can be queried from a triple store.
In the field of material science and engineering (MSE), most mechanical test methods are standardized which serves as a valid basis for ontology development. Therefore, the well-known tensile test of metals at room temperature (DIN EN ISO standard 6892-1:2019-11) was selected to be considered as one of the first use cases in PMD. This consideration within the PMD features both, the ontological representation of such a tensile test in accordance with the standard as well as exemplary data generation. The semantic connection of the ontology and data leads to interoperability and an enhanced ability of querying.
In-situ Prozessüberwachung in der additiven Fertigung von Metallen (PBF-LB /M) mittels TT und ET
(2022)
Durch die additive Fertigung ergeben sich durch die nun mögliche wirtschaftliche Fertigung hochgradig individueller und komplexer metallischer Bauteile in kleinen Stückzahlen bis hinunter zum Einzelstück für viele Industriebereiche ganz neue Möglichkeiten.
Gleichzeitig entstehen jedoch neue Herausforderungen im Bereich der Qualitätssicherung, da sich auf statistischen Methoden beruhende Ansätze nicht anwenden lassen, ohne wiederum die Vorteile der Fertigung massiv einzuschränken.
Eine mögliche Lösung für dieses Problem liegt in der Anwendung verschiedener In-situ-Überwachungstechniken während des Bauprozesses. Jedoch sind nur wenige dieser Techniken kommerziell verfügbar und noch nicht so weit erforscht, dass die Einhaltung strenger Qualitäts- und Sicherheitsstandards gewährleistet werden kann. In diesem Beitrag stellen wir die Ergebnisse einer Studie über mittels L-PBF gefertigte Probekörper aus der Nickelbasis-Superlegierung Haynes 282 vor, bei denen die Bildung von Defekten durch lokale Variationen der Prozessparameter wie der Laserleistung provoziert wurde. Die Proben wurden in-situ mittels Thermographie, optischer Tomographie, Schmelzbadüberwachung und Wirbelstromprüfung sowie ex-situ mittels Computertomographie (CT) überwacht, mit dem Ziel, die Machbarkeit und die Aussichten der einzelnen Methoden für die zuverlässige Erkennung der Bildung relevanter Defekte zu bewerten.
The formation of defects such as keyhole pores is a major challenge for the production of metal parts by Laser Powder Bed Fusion (LPBF). The LPBF process is characterized by a large number of influencing factors which can be hard to quantify. Machine Learning (ML) is a prominent tool to predict the outcome of complex processes on the basis of different sensor data. In this study, a ML model for defect prediction is created using thermographic image features as input data. As a reference, the porosity information calculated from an x-ray Micro Computed Tomography (µCT) scan of the produced specimen is used. Physical knowledge about the keyhole pore formation is incorporated into the model to increase the prediction accuracy. From the prediction result, the quality of the input data is evaluated and future demands on in-situ monitoring of LPBF processes are formulated.
Emanating from developing flame retarded biocomposites, we have proposed renewable natural fibers (including keratin) taken from industrial waste as an authentic sustainable approach. More recently, we have investigated non-vegan flame retardant approaches. This paper loves to give you an insight into our ongoing projects on biogenic industrial wastes like leather, bone meal, and insects. Materials were characterized multi-methodically, flame retardant modes of action quantified, decomposition mechanism proposed, and synergisms explained. Considering the large quantities of leather waste (LW) in industrial-scale production, we underline LW as multifunctional bio-adjuvants. LW enhances the flame retardancy of poly(ethylene-vinyl acetate) (EVA) containing phosphorus flame retardants (P-FR). Products/by-products of the invertebrate and vertebrate farming, respectively, are promising bio-based adjuvants in flame retarded bio-epoxy thermosets. While the addition of bone meal yields the formation of an inorganic shield, protein-based powders from insects provide an intumescent behavior. In combination with a P-FR superior charring and self-extinguishing are obtained.
Acknowledgement: In part of this work was supported by the Volkswagen Foundation grant “Experiment!” No. 97437.
Overview of the state of the art and current trends with the main topics:
- renewable sources in flame retardant polymers (flame retarded bio-polymers and biocomposites; bio-flame retardants, renewable adjuvants from industrial waste)
- flame retardancy meets sustainability
- concepts between analogy and out-of-the-box.
A few layer/multilayer graphene (MLG) with a specific surface area of BET=250 m2/g is proposed as an efficient multifunctional nanofiller for rubbers. The preparation method, i.e., ultrasonically-assisted solution mixing of master batches followed by two-roll milling, strongly influences the dispersion in the elastomeric matrix and is fundamental for the final properties. When homogenously dispersed, single stacks of only approximately 10 graphene sheets, with an aspect ratio of 34, work at low loadings, enabling the replacement of large amounts of carbon black (CB), an increase in efficiency, and a reduction in filler load. The appropriate preparation yielded nanocomposites in which just 3 phr are sufficient to significantly improve the rheological, curing, gas barrier properties, electrical and thermal conductivity, as well as mechanical properties of different rubbers, as shown for chlorine-Isobutylene-Isoprene rubber (CIIR), nitrile-butadiene rubber (NBR), natural rubber (NR), and styrene-butadiene rubber (SBR). 3 phr of MLG tripled the Young’s modulus of CIIR, an effect equivalent to 20 phr of CB. The stronger interactions between MLG and NR or SBR also resulted in a reduction in the elongation at break by 20% and 50%, respectively, while the same parameter was hardly changed for CIIR/MLG and NBR/MLG. CIIR/MLG and NBR/MLG were stiffer but just as defomable than CIIR and NBR. The strong reinforcing effect of 3 phr MLG was confirmed by the increase of greater than 10 Shore A in hardness. MLG reduces gas permeability, increases thermal and electrical conductivities, and retards flammability, the latter shown by the reduction in heat release rate in the cone calorimeter. We investigated MLG also as a synergist for reducing the aluminium trihydrate loading in flame retardant hydrogenated acrylonitrile-butadiene (HNBR), polybutadiene chloroprene (BR/CR), and chlorosulfonated polyethylene rubber(CSM). The higher the nanofiller concentration is, the greater the improvement in the properties. For instance, the permeability decreased by 30% at 3 phr of MLG, 50% at 5 phr and 60% at 10 phr, respectively. Moreover, the MLG nanocomposites improve stability of mechanical properties against the effects of weathering. In key experiments an increase in UV-absorption and a pronounced radical scavenging were proved as stabilizing mechanisms. In a nutshell, MLG is an efficient multifunctional nanofiller ready to be used for innovative rubber development.
Hochfeste Feinkornbaustähle verfügen über großes Potenzial für gewichtsoptimierte, effiziente Strukturen in vielen modernen Stahlkonstruktion. Weitere Effizienzsteigerungen können durch additives Fertigen sowie bionische Bauweisen erreicht werden. Hochfeste Zusatzwerkstoffe für additives MSG-Schweißen (engl.: Wire Arc Additive Manufacturing, WAAM) sind bereits von den Schweißzusatzherstellern lieferbar. Eine breite industrielle Anwendung insbesondere für KMU ist aufgrund fehlender quantitativer Erkenntnisse und Richtlinien bezüglich schweißbedingter Beanspruchungen und Bauteilsicherheit während der Herstellung und des Betriebs derzeit stark limitiert. In einem gemeinsamen Forschungsprojekt (FOSTA-P1380/IGF21162BG) der BAM und der TU Chemnitz werden daher die mit Eigenspannungsausbildung und der Gefahr einer Kaltrissbildung verbundenen prozess- und werkstoffbedingten sowie konstruktiven Einflüsse beim WAAM hochfester Stähle untersucht. Der vorliegende Beitrag fokussiert die Analyse der Auswirkungen von Schweißwärmeführung und Design der WAAM-Bauteile auf die Abkühlbedingungen, Gefüge, mechanisch-technologischen Eigenschaften und Eigenspannungen. Hierfür werden geometrisch definierte Probenkörper (Hohlquader) vollautomatisiert mit einem speziellen, hochfesten WAAM-Massivdraht (Streckgrenze >790 MPa) geschweißt. Die Wärmeführung und Probenabmessungen werden innerhalb eines statistischen Versuchsplans variiert. Die Schweißwärmeführung wird dabei so eingestellt, dass die t8/5-Abkühlzeiten im empfohlenen Verarbeitungsbereich (ca. 5 s bis 20 s) sichergestellt sind. Hierzu ließen sich über zusätzliche thermo-physikalische Umformsimulationen mittels Dilatometer die komplexen Wärmezyklen abbilden und die resultierende Zugfestigkeit des Schweißgutes bestimmen. Das WAAM-Schweißen komplexer Geometrien mit variierenden Schweißwärmeführungen und geometrischen Verhältnissen bzw. Wanddicken bedingt neben den Auswirkungen auf die Abkühlbedingungen, Abkühlzeiten und Gefüge deutliche Einflüsse auf die konstruktiven Steifigkeitsverhältnisse beim Schweißen. Es zeigen sich anhand der Schweißexperimente signifikante Auswirkungen durch Probenskalierung und Wärmeeinbringung auf die resultierenden lokalen Eigenspannungen. Die Folge können ungünstige Bauteileigenschaften und risskritische Zugeigenspannungen sein.
Hochfeste Feinkornbaustähle verfügen über großes Potenzial für gewichtsoptimierte, effiziente Strukturen in vielen modernen Stahlkonstruktion. Weitere Effizienzsteigerungen können durch additives Fertigen sowie bionische Bauweisen erreicht werden. Hochfeste Zusatzwerkstoffe für additives MSG-Schweißen (engl.: Wire Arc Additive Manufacturing, WAAM) sind bereits von den Schweißzusatzherstellern lieferbar. Eine breite industrielle Anwendung insbesondere für KMU ist aufgrund fehlender quantitativer Erkenntnisse und Richtlinien bezüglich schweißbedingter Beanspruchungen und Bauteilsicherheit während der Herstellung und des Betriebs derzeit stark limitiert. In einem gemeinsamen Forschungsprojekt (FOSTA-P1380/IGF21162BG) der BAM und der TU Chemnitz werden daher die mit Eigenspannungsausbildung und der Gefahr einer Kaltrissbildung verbundenen prozess- und werkstoffbedingten sowie konstruktiven Einflüsse beim WAAM hochfester Stähle untersucht. Der vorliegende Beitrag fokussiert die Analyse der Auswirkungen von Schweißwärmeführung und Design der WAAM-Bauteile auf die Abkühlbedingungen, Gefüge, mechanisch-technologischen Eigenschaften und Eigenspannungen. Hierfür werden geometrisch definierte Probenkörper (Hohlquader) vollautomatisiert mit einem speziellen, hochfesten WAAM-Massivdraht (Streckgrenze >790 MPa) geschweißt. Die Wärmeführung und Probenabmessungen werden innerhalb eines statistischen Versuchsplans variiert. Die Schweißwärmeführung wird dabei so eingestellt, dass die t8/5-Abkühlzeiten im empfohlenen Verarbeitungsbereich (ca. 5 s bis 20 s) sichergestellt sind. Hierzu ließen sich über zusätzliche thermo-physikalische Umformsimulationen mittels Dilatometer die komplexen Wärmezyklen abbilden und die resultierende Zugfestigkeit des Schweißgutes bestimmen. Das WAAM-Schweißen komplexer Geometrien mit variierenden Schweißwärmeführungen und geometrischen Verhältnissen bzw. Wanddicken bedingt neben den Auswirkungen auf die Abkühlbedingungen, Abkühlzeiten und Gefüge deutliche Einflüsse auf die konstruktiven Steifigkeitsverhältnisse beim Schweißen. Es zeigen sich anhand der Schweißexperimente signifikante Auswirkungen durch Probenskalierung und Wärmeeinbringung auf die resultierenden lokalen Eigenspannungen. Die Folge können ungünstige Bauteileigenschaften und risskritische Zugeigenspannungen sein.
Im vorliegenden Beitrag werden einige Verarbeitungsempfehlung auf Basis der Ergebnisse für den Arbeitskreis des DVS AG V 12 (Additive Fertigung) abgeleitet.
Commercial high-strength filler metals for wire arc additive manufacturing (WAAM) are already available. However, widespread industrial use is currently limited due to a lack of quantitative knowledge and guidelines regarding welding stresses and component safety during manufacture and operation for WAAM structures. In a joint research project (FOSTA-P1380/IGF21162BG), the process- and material-related as well as design influences associated with residual stress formation and the risk of cold cracking are being investigated. For this purpose, reference specimens are welded fully automated with defined dimensions and systematic variation of heat control using a special, high-strength WAAM filler metal (yield strength >790 MPa). Heat control is varied by means of heat input (200–650 kJ/m) and interlayer temperature (100–300 °C). The ∆t8/5 cooling times correspond with the recommendations of steel producers (approx. 5–20 s). Welding parameters and AM geometry are correlated with the resulting microstructure, hardness and residual stress state. High heat input leads to a lower tensile stress in the component and may cause unfavorable microstructure and mechanical properties. However, a sufficiently low interlayer temperature is likely to be suitable for obtaining adequate properties at a reduced tensile stress level when welding with high heat input. The component design affects heat dissipation conditions and the intensity of restraint during welding and has a significant influence on the residual stress. These complex interactions are analyzed within this investigation. The aim is to provide easily applicable processing recommendations and standard specifications for an economical, appropriate and crack-safe WAAM of high-strength steels.
In the face of rising energy demand and the impending climate change the development of a sustainable, fossil-free fuel and chemical production is of global importance. One possible goal is the development of electrochemical conversion processes using catalysts. Porous materials play an important role in such energy applications. 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 the development of improved catalysts is a better understanding of the relations between their performance, stability and physico-chemical properties. However, the complex morphology of such catalysts constitutes a challenge even for modern analytical techniques. Spectroscopic ellipsometry (SE) is a versatile method for studying material properties by using appropriate models (e.g., film thickness, optical and electronic properties). Ellipsometric models need to be validated in order to produce accurate results. In a first step, the model for the ellipsometric fit studies of a calcination series of mesoporous iridium oxide films (300 – 600 °C) was investigated and validated with respect to their material properties.[4] The information on electronic structure of the catalysts shows a direct correlation with electrochemical activities. The development of an environmental electrochemical cell offers the possibility of investigations under operando conditions. Thus, changes in optical and electronic properties can be induced and monitored during the electrocatalytic oxygen evolution reaction.
Die mechanischen Eigenschaften und die Standardparametersätze werden im additiven Fertigungsverfahren Laser Powder Bed Fusion (L-PBF) zumeist an Körpern ermittelt, die unter festen Randbedingungen gefertigt werden. In der Literatur wird allerdings von verschiedenen Autoren auf einen Einfluss von Geometrie und Prozess auf die resultierenden Eigenschaften hingewiesen [1, 2, 3]. Aufgrund des häufig großen Komplexitätsgrads von L-PBF Bauteilen und Prozessen, ist eine Abweichung angenommener Eigenschaften daher nicht auszuschließen. Das kann besonders für tragende und sicherheitsrelevante Komponenten kritisch sein und ist eine Herausforderung für die Qualitätssicherung. Aufwendige Trial-and-Error Versuche sind zumeist die Folge. Ein einheitliches und umfassendes Verständnis der Einflussfaktoren auf die resultierenden Eigenschaften im L-PBF Prozess ist zum aktuellen Stand nicht vorhanden.
In diesem Vortrag werden erste Ergebnisse einer Studie vorgestellt, in der systematisch die Bandbreite möglicher Defekt- und Mikrostrukturvariationen in L-PBF Bauteilen am Beispiel der Nickelbasislegierung Haynes 282 untersucht wird. Aufbauend auf einer modellbasierten Beschreibung des lokalen Wärmehaushalts wurden Versuchspläne entwickelt, die eine Vielzahl möglicher Prozess- und Geometriekonfigurationen realer Anwendungen abbilden können. Zur Untersuchung des Geometrieeinflusses wurden typische Geometrieelemente komplexer Strukturen und deren Ausprägungen identifiziert. Prozessseitig wurden die Position im Bauraum, Schwankungen der Laserleistung, die Zwischenlagenzeit und die Belichtungsstrategie innerhalb der Schicht als typische Faktoren berücksichtigt. Die Zwischenlagenzeit bildet dabei Variationen im Bauraumfüllgrad ab. Die Belichtungsstrategie untersucht Effekte wie die Zwischenvektorzeit (engl. inter vector time, IVT) oder die lokale Vektorlänge. Die verschiedenen Konfigurationen wurden metallografisch bewertet. Die bisherigen Ergebnisse können einen Einfluss der Geometrie und des Prozesses auf die Defektbildung und die Mikrostruktur in L-PBF Bauteilen aufzeigen. Durch prozessbegleitende thermografische in situ Messungen konnte außerdem eine Abhängigkeit von lokalen und globalen Temperaturfeldern identifiziert werden. Die Erkenntnisse zeigen zudem, dass der geometrische Einfluss auf den lokalen Wärmehaushalt von Anordnung, Gestalt und Dimensionen der zweidimensionalen Belichtungsbereiche über die Aufbauhöhe abhängt. Das gewonnene Verständnis soll in die Entwicklung von Konstruktionsrichtlinien und Prüfkörpern einfließen, um Variationen lokaler Bauteileigenschaften in der zukünftigen Bauteil- und Prozessauslegung berücksichtigen zu können.
Laser Powder Bed Fusion (L-PBF) allow the fabrication of lightweight near net shape AlSi10Mg components attractive to the aerospace, automotive, biomedical and military industries. During the build-up process, high cooling rates occur. Thus, L-PBF AlSi10Mg alloys exhibit a Si-nanostructure in the as-built condition, which leads to superior mechanical properties compared to conventional cast materials. At the same time, such high thermal gradients generally involve a deleterious residual stress (RS) state that needs to be assessed during the design process, before placing a component in service. To this purpose post-process heat treatments are commonly performed to relieve detrimental RS. In this contribution two low-temperature stress-relief heat treatments (SRHT) are studied and compared with the as-built state: a SRHT at 265°C for 1 hour and a SRHT at 300°C for 2 hours. At these temperatures microstructural changes occur. In the as-built state, Si atoms are supersaturated in the α-aluminium matrix, which is enveloped by a eutectic Si-network. At 265°C the Si precipitation from the matrix to the pre-existing network is triggered. Thereafter, above 295°C the fragmentation and spheroidization of the Si branches takes place, presumably by Al–Si interdiffusion. After 2 hours the original eutectic network is completely replaced by uniformly distributed blocky particles. The effect of the heat and the microstructure modification on the RS state and the fatigue properties is investigated. Energy dispersive x-ray and neutron diffraction are combined to investigate the near-surface and bulk RS state of a L-PBF AlSi10Mg material. Differences in the endurance limit are evaluated experimentally by high cycle fatigue (HCF) tests and cyclic R-curve determination.
Martensitic 9 %-Cr steels like P91 and P92 can show an increased susceptibility to delayed hydrogen assisted cracking. The focus of this study was the microstructure and heat treatment effect on the mechanical properties of P92 base material and P91 multi-layer weld metal in both as-welded and post weld heat treated (PWHT) condition.
Tensile tests with hydrogen free reference samples and electrochemically hydrogen charged samples were carried out, the mechanical properties were assessed and supported by dedicated fractographic analysis. In addition, hydrogen and microstructure dependent fracture criteria were calculated. All investigated microstructures showed a hydrogen influenced degradation of the mechanical properties compared to the hydrogen free reference samples. In that connection, the as welded martensitic P91 weld metal had the highest degree of degradation in presence of hydrogen. The P91 PWHT weld metal and the P92 base material had comparable properties. From that point of view, a significantly increased risk for hydrogen assisted cold cracking during welding fabrication of P91 weld joints must be considered before any heat treatment is conducted.