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Erscheinungsjahr
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Die thermische Historie beim additiven Aufbau von komplexen Realkomponenten und geometrisch primitiven Prüfkörpern unterscheidet sich signifikant. Daraus können Eigenschaftsunterschiede resultieren, die zu unterschiedlichem Materialverhalten führen können. In diesem Vortrag wird das Konzept repräsentativer Probekörper eingeführt, das eine Übertragung thermischer Historien von komplexen Geometrien auf einfache Geometrien ermöglicht und hierdurch zu einer besseren Vergleichbarkeit der Werkstoffeigenschaften führen soll.
Compound semiconductors (CS) are promising materials for the development of high-power electrical applications. They have low losses, can withstand high temperatures and can operate at very high voltages and currents. This makes them a key technology for the electrification of many high energy applications, especially electromobility and HVDC power lines.
The challenge with CS technology is that most of the process technology has to be developed anew to the high standards required by electronic applications. Today, compound semiconductors can be produced in thin layers on top of substrates fabricated from classical crystal growth processes that are already well established. A promising method for this is metal organic vapour phase epitaxy (MOVPE). With this method, many different compounds with semiconducting properties can be synthesized. Additionally, this process technology is a direct thin layer deposition method. Therefore, complex multilayer systems can be generated directly by the deposition process and without the need of doping after growing.
There are a number of critical defects that can originate from the deposition process of these thin film devices. Within this project, we intend to develop new correlative imaging and analysis techniques to determine defect types, to quantify defect size and number density, as well as to characterise defects for process optimisation.
We report here on the use of spectroscopic ellipsometry and imaging ellipsometry to investigate defects in several different compound semiconductor materials used in high-power electronic devices. The materials we investigated are β-Ga2O3, SiC, GaN, AlN, and AlGaN materials as well as oxidised SiC surfaces. All of these materials have their typical defects and require optimised measurement and analysis schemes for reliable detection and analysis. Spectroscopic ellipsometry is a highly sensitive method for determining the thicknesses and dielectric function of thin layers, yielding potentially a high number of microscopic properties. The combined method between ellipsometry and optical microscopy is called imaging ellipsometry and is especially powerful for the large amount of data it produces. We have analysed defects in SiC- and AlN-based thin film semiconductors as well as characterised the properties of different types of SiO2 layers created on top of SiC monocrystals. We developed ellipsometric models for the data analysis of the different semiconductor materials.
If the defects have geometric features, it is useful to combine the ellipsometric analysis with topometry method like interference microscopy and scanning probe microscopy. We have successfully characterised function-critical defects in MOVPE SiC layers and correlated the findings with topography from WLIM measurements. We have developed an imaging ellipsometric measurement methodology that allows to estimate the relative defect area on a surface by a statistical raw data analysis.
Compound semiconductors (CS) are promising materials for the development of high-power electrical applications. They have low losses, can withstand high temperatures and can operate at very high voltages and currents. This makes them a key technology for the electrification of many high energy applications, especially electromobility and HVDC power lines.
The challenge is that most of the process technology has to be developed specifically and tailored to the high standards required by electronic applications. Today, many different CS materials can be produced in thin layers on top of substrates fabricated from classical crystal growth processes that are already well established. A promising method for this is metal organic vapour phase epitaxy (MOVPE). This technology is a direct thin layer deposition method capable of producing complex multilayer systems directly from one deposition process without the need of doping after growing.
There are a number of critical defects that can originate from the deposition process when targeting electronic thin film devices. Within this project, we intend to develop new correlative imaging and analysis techniques to determine defect types, to quantify defect size and density, as well as to characterise defects for further process optimisation.
We report here on the use of spectroscopic and multispectral imaging ellipsometry to investigate defects in several different compound semiconductor materials used in high-power electronic devices. The materials we investigated are β-Ga2O3, SiC, GaN, AlN, and AlGaN as well as oxidised SiC. All of these materials have their typical defects and require optimised measurement and analysis schemes for reliable detection and analysis. Spectroscopic ellipsometry is a highly sensitive method for determining the thicknesses and dielectric function of thin layers, yielding potentially a high number of microscopic properties. The combined method between ellipsometry and optical microscopy is known as imaging ellipsometry and is especially powerful for the large amount of data it produces. We have analysed defects in SiC- and AlN-based thin film semiconductors as well as characterised the properties of different types of SiO2 layers created on top of SiC monocrystals. We developed ellipsometric models for the data analysis of the different semiconductor materials.
If the defects have geometric features, it is useful to combine the ellipsometric analysis with topometry methods like interference microscopy and scanning probe microscopy. We have successfully characterised function-critical defects in MOVPE SiC layers and correlated the findings with topography from WLIM measurements. We have developed an imaging ellipsometric measurement methodology that allows to estimate the relative defect area on a surface by a statistical raw data analysis.
Development of representative test specimens by thermal history transfer in laser powder bed fusion
(2024)
The use of components manufactured by laser powder bed fusion (PBF LB/M) and subjected to fatigue loading is still hampered by the uncertainty about the homogeneity of the process results. Numerous influencing factors including the component’s geometry contribute to the risk of process instability and resulting inhomogeneity of properties. This drastically limits the comparability of different built parts and requires expensive full component testing. The thermal history as the spatiotemporal temperature distribution has been identified as a major cause for flaw formation. Therefore, it can be hypothesized that a similar thermal history between components and test specimens enhances their comparability. Following this assumption, a strategy is developed to transfer the intrinsic preheating temperature as a measure of comparability of thermal histories from a region of interest of a complex component to a simple test specimen. This transfer concept has been successfully proved by the use of FEM-based macroscale thermal simulations, validated by calibrated infrared thermography. An adoption of the specimen manufacturing process by the adjustment of the inter layer times was established to manufacture specimens which are representatives of a specific region of a large-scale component in terms of the thermal history similarity criterion. The concept is schematically illustrated in Figure 1 and was demonstrated using a pressure vessel geometry from the chemical industry.
Ellipsometry as optical metrology method for analysis of reference materials for nanoelectronics
(2024)
Electrical properties of materials at the nanoscale can be characterized using scanning microwave microscopes (SMM) and conductive atomic force microscopes (C AFM). However, the measurement results are difficult to compare since different setups and different reference standards are used. The development of new “out-of-lab” reference standards can contribute to the traceability and reliability of these scanning probe microscopy methods (SPM) and facilitate their broader industrial application.
In this study, we discuss the capability of optical methods such as ellipsometry for the characterization of existing and the development of new reference calibration samples for scanning microwave microscopy. Ellipsometry is a fast and non-destructive method, which enables very accurate determination of the layer thickness and the dielectric functions of the materials. Imaging ellipsometry is suitable for spatially resolved measurements when analyzing thin layers in microstructured samples.
We show how the electrical resistivity of indium tin oxide (ITO) layers in newly designed resistive calibration samples can be obtained from spectroscopic ellipsometric measurements. The extension of the measurement range into the mid-infrared region was necessary when analyzing ITO layers with low conductivity. This parameter was obtained by fitting a Drude function describing the absorption of the free carriers. The impact of the coating process conditions on the layer properties is discussed.
Imaging ellipsometry was applied for the characterisation of thin ITO and SiO2 layers in microstructured resistive and capacitance calibration kits. The uncertainties of determined layer thicknesses were specified according to standardized practice guides used in ellipsometry. We show how statistical fingerprint analysis of the measured ellipsometric transfer quantities can be used to validate the quality of potential reference materials for nano-electronics and to monitor the processing of structured samples.
Packages for the transport of spent nuclear fuel are designed to endure severe accidents. To obtain approval, these transport packages must adhere to the specification-based criteria of the international transport regulations SSR-6 of the International Atomic Energy Agency (IAEA). To ensure compliance with these requirements, specific mechanical and thermal tests need to be addressed with respect to the package type. Typically, SSR-6 prescribes a mechanical test followed by a thermal fire test as part of different testing scenarios. To approve the latter test of the sequence, BAM performs calorimeter tests in advance with so-called fire reference packages for characterizing the actual fire and its impact on the package to be tested. Packages are designed with different geometry sizes depending on their purpose. For previous tests, the implemented test setups in the fire test stand were sufficiently dimensioned and could cover all requirements in this respect. However, to cover additional testing needs in the future, BAM is expanding the test setup for the purpose of testing significantly larger packages.
In previous test setups one ring burner for propane surrounding the test specimen was sufficient. The limiting size in this configuration was the design height of the transport package to be tested. According to the thermal test of the IAEA-Regulations [1], a 30-minute fully engulfing 800°C pool fire or an equally severe fire, e.g., propane gas fire, must be applied to the transport package. Possible adjustments such as nozzle cross-section and propane mass flow can be adjusted to a certain extent. Further modifications, to cover significantly higher and larger packages all-around with a fully engulfing fire, must be accomplished with an additional, second burner ring. Both burner rings had the same dimensions and were mounted on top of each other at different heights to create a significantly larger volume of fire that completely engulfs the package including its impact limiter.
To meet the IAEA regulatory boundary conditions, the enhanced fire test stand with the second burner ring is tested with a large fire reference package and will then be used for real-size transport packages after all parameters are successfully met. This fire reference package represents the external geometry of a generic transport cask for radioactive material and is equipped with numerous temperature sensors to record temperature curves at the interior wall surfaces.
As industries move for ever faster development and adoption cycles of emerging new technologies in the field of welding, the meticulous and longer-winded approach of the scientific research process can feel harder to integrate. To help bridge this gap and increase the speed, quality, and adoption rate of publicly funded research, the Bundesanstalt für Materialforschung und -prüfung (BAM) continues to work towards enabling scientists with direct access to necessary software tools and - in the future – highest quality welding research reference data to further foster collaborations.
On the experimental side, the arc welding group at BAM division 9.3 “welding technologies” is continuing to expand and upgrade its capacities of robotic welding systems with integrated state of the art sensor technologies and software solutions. This allows all experiments to be recorded and measured in micro-millimeter accuracy and at sub-millisecond precision, including welding process data, complete spatial geometry and temperature measurements, process video recordings and more. The custom software-based solutions and interfaces allow scaling of the welding systems from large thick plate offshore applications to small additive repair weldments in wind turbine blades to multi-hour continuous weldments in additive manufacturing applications. In addition to the data gathered during the welding process itself, the relevant testing results and materials properties produced at BAM or externally can be integrated seamlessly. This allows detailed traceability of all results back to the actual welding process.
Regardless of the scope and application, complete datasets can be made accessible for research or industry partners in the highest resolution based on the open source WelDX (welding data exchange) file format.
Figure 1. Welding experiment representation including dynamic process data, cross-section imaging and hardness measurements from a single weldx file.
The talk will give an overview of the experimental facilities and workflows as well as current software developments with a focus on research data quality assurance, traceability, and accessibility.
Based on the integration into latest research trends and activities of the “welding technologies” division, the path to publishing reference datasets for arc welding process for various applications and materials is outlined and discussed.
Although intense wildfire research has been done in the US and in Australia, it cannot be transferred directly to the situation in Europe as the local vegetation has a significant influence on the fire spread. The EU-funded project TREEADS and the so-called German pilot within the project are concentrating on wildfire in Europe. Extensive experimental research is done on local vegeta-tion in Germany and the experimental results are used to adjust the Fire Dynam-ics Simulator (FDS) to local vegetation as a fuel in the calculations. The particle model and the boundary fuel model are developed for the simulation of forest fires. Both models require the kinetic input for the dehydration, pyrolysis, and char oxidation process. This three-step simplified model describes the basic fuel combustion kinetic. Most published simulations use the default kinetic input of pine needles from FDS user manual.
To adjust the simulation to local vegetation, the corresponding kinetic parame-ters have been experimental investigated. Samples of pine needles, moss and other falling leaves were collected, air dried and grinded into powder. The TG analysis of all these samples were done under different heating rate of 5, 10 and 20K/min.
The activation energy and the corresponding pre-exponential factor were calcu-lated. The results show that fire spread depends significantly on the vegetation and comparison with small scale experiments show good agreement using the new kinetic parameters. The new model is applied to a larger scenario and will be compared to the results of large-scale experiments for further validation of the model.
Um die Ausbreitungsmechanismen von Vegetationsbränden und besonders bei Bodenbränden besser zu verstehen, wurden die Einflussfaktoren auf die Brandausbreitung näher untersucht. Da die Brandausbreitung auch in starkem Maße von der lokalen Vegetation abhängt, war eine Charakterisierung der lokalen Vegetation und der Bodenverhältnisse wichtig. Die Wetterverhältnisse spielen einerseits im Vorfeld des Brandes durch längere Dürreperioden als auch während des Brandes, z.B. durch den Windeinfluss, zusätzlich eine große Rolle.
Durch die numerische Simulation kann eine größere Variation der Einflussgrößen abgebildet werden als durch die zeitlich und finanziell begrenzten experimentellen Möglichkeiten. Für die Berechnungen wird der Fire Dynamic Simulators (FDS) mit dem Paket WFDS verwendet. Dadurch kann mit einem vereinfachten 3-Phasen-Reaktionskinetikmodell, bestehend aus Dehydrierung, Pyrolyse, Kohleoxidation, die Ausbreitung von Vegetationsbränden verschiedener Waldbodenarten untersucht werden. Es wurden dazu 6 typische Pflanzenarten und Bodenproben aus Kiefern-, Buchen und Eichenbeständen ausgewählt.
Die gesammelten Waldbodenproben wurden alle hinsichtlich des Wassergehalts, des organischen Gehalts, der Packungsdichte, der Dichte und der statistisch ermittelten Pflanzenartenverteilung charakterisiert. Das kinetische Abbrandverhalten wurde durch Thermogravimetrische Analyse (TGA) untersucht. Alle diese Daten wurden als Eingabeparameter für die Simulation verwendet. Die numerischen Simulationen werden mit Experimenten im kleinen, mittleren und Real-Maßstab validiert.
Direct energy deposition additive manufacturing technologies that utilize an electric arc have great potential for generating large volume metal components. However, selecting process parameters that yield the desired near net shape design and requested mechanical component behavior is not a trivial task due to the complex relationship between all process parameters and material characteristics. This presentation exemplifies the application of a newly developed solid welding wire doped with TiB to enhance grain refinement in the deposited metal for additive manufacturing based on DED-Arc of high-strength precipitation hardening AlMgSi-aluminum alloys. It is worth noting that the solid wire is the result of our preliminary metallurgical studies on grain refinement in aluminum weld metal.
Consequently, research focuses on the correlation between process parameters and component quality to understand the underlying mechanisms. This is crucial for evaluating a robust process parameter space that yields component quality in line with corresponding standards which are mainly taken from welding technology.
Specifically, we examine component quality by analyzing pore size and distribution, as well as grain morphology. To enhance the mechanical properties of the deposited metal, a post-weld heat treatment was conducted, comprising of solution treatment, quenching, and artificial aging. The study also evaluates the effects of various heat treatment strategies on the final mechanical properties of the material.
To demonstrate the applicability of 3D metal printing of high-strength aluminium alloys, a more complex demonstrator was created. It has been shown that DED-Arc can produce high-volume aluminium parts with the same quality as the corresponding subtractive processing strategy.
Additionally, the entire additive manufacturing chain has been digitally integrated, enabling traceability of all relevant process steps, which is essential for reliable subsequent quality assessment.
Lecture-like introduction in the topic. Fundamental aspects are discussed: Burning of polymers, fire risks, pyrolysis, combustion in the flame, physical chemistry of ignition, flame spread and steady state burning, flame retardancy mechanisms and groups of flame retardants, fire hazards (smoke, toxic products) and environmental concerns, fire testing.
The manufacture of sintered glasses and glass-ceramics, glass matrix composites, and glass-bounded ceramics or pastes is often affected by un-expected gas bubble formation also named foaming. Against this background, in this presentation the main aspects and possible reasons of foaming are shown for completely different glass powders: a barium silicate glass powders used as SOFC sealants, and bioactive glass powders using different powder milling procedures.
Sintering and foaming were measured by means of heating microscopy backed up by XRD, differential thermal analysis (DTA), vacuum hot extraction (VHE), optical and electron microscopy, and infrared spectroscopy, and time-of-flight secondary ion mass spectrometry (ToF-SIMS).
Different densification was reached followed by significant foaming starting partly immediately, partly at higher temperature. Foaming increased significantly as milling progressed. For moderately milled glass powders, subsequent storage in air could also promote foaming. Although the milling atmosphere significantly affects the foaming of uniaxially pressed powder compacts sintered in air.
VHE studies show that foaming is driven by carbon gases and carbonates were detected by Infrared spectroscopy to provide the major foaming source. Carbonates could be detected even after heating to 750 °C, which hints on a thermally very stable species or mechanical trapping or encapsulating of CO2. Otherwise, dark gray compact colors for milling in isopropanol indicate the presence of residual carbon as well. Its significant contribution to foaming, however, could not be proved and might be limited by the diffusivity of oxygen needed for carbon oxidation to carbon gas.
Introduction: Effective disinfection is crucial to maintain hygiene and to prevent the spread of infections. Phenotypic heterogeneity in disinfection survival (i.e. tolerance) may result in failure of disinfection, which in turn may foster the evolution of resistance to both disinfectants and antibiotics. However, the consequences of phenotypic heterogeneity for disinfection outcome and resistance evolution are not well understood. Goal: This study investigates the impact of phenotypic heterogeneity on the survival and evolution of Escherichia coli during disinfection with six commonly used substances. Furthermore, the consequences of evolved disinfectant tolerance for antibiotic resistance evolution are studied. Materials & Methods: The extent of population heterogeneity during disinfection is derived by determining time-kill kinetics and analysis with mathematical modelling. The link between population heterogeneity and evolvability of disinfectant tolerance was assessed by laboratory evolution experiments under periodic disinfection. The ability of disinfectant tolerant strains to evolve antibiotic resistance is assessed by serial transfer experiments with increasing concentrations of different antibiotics and by whole genome sequencing. Results: Multi-modal time-kill kinetics in three of the six disinfectants suggest the presence of disinfectant-tolerant subpopulations (i.e. persister cells). Importantly, the ability and extent to evolve population-wide tolerance under periodic disinfection is related with the presence of persister cells and the level of phenotypic heterogeneity during disinfection. Interestingly, the probability of high-level resistance evolution to certain antibiotics is attenuated in disinfectant tolerant strains as compared to the sensitive ancestor. Whole-genome sequencing reveals epistatic interactions between disinfectant tolerance and antibiotic resistance mutations, preventing access to canonical evolutionary paths to resistance. Summary: Our findings suggest that phenotypic heterogeneity can facilitate disinfection survival and the evolution of population wide tolerance, which can impact future antibiotic resistance evolution.
Up to now, oriented surface crystallization phenomena are discussed controversially, and related studies are restricted to few glasses. For silicate glasses we found a good correlation between the calculated surface energy of crystal faces and oriented surface nucleation. Surface energies were estimated assuming that crystal surfaces resemble minimum energy crack paths along the given crystal plane. This concept was successfully applied at the Institute of Physics of Rennes in calculating fracture surface energies of glasses. Several oriented nucleation phenomena can be herby explained assuming that high energy crystal surfaces tend to be wetted by the melt. This would minimize the total interfacial energy of the nucleus. Furthermore, we will discuss the evolution of the microstructure and its effect on the preferred crystal orientation.
We investigated the phase transformations during butt-welding of supermartensitic steel plates with help of Neutron-Bragg-Edge Imaging (NBEI). Gas tungsten arc welding (GTAW) was used with a motorized torch allowing for automated weldments. The austenitization in the heat affected zone (HAZ) could be clearly visualized at λ = 0.39 nm, a wavelength smaller than the Bragg edge wavelengths of both austenite and martensite. The re-transformation into the martensitic phase during cooling was clearly detected. However, we observed an unexpected additional change in transmission at λ = 0.44 nm, a wavelength larger than the wavelength of the Bragg edges of both the martensitic and austenitic phases. We attribute this change to the Deybe-Waller-Factor that describes the temperature dependence of coherent scattering at a crystal lattice. The observed two-dimensional attenuation map corresponds well with a temperature distribution modelling by software macros in ANSYS [3]. Here, the absolute temperature values could be achieved by calibrating the modelled attenuation with help of a thermocouple placed at the steel plate. This allows in return for a direct two-dimensional temperature reading based on the Debye-Waller-relation between neutron attenuation and sample temperature.
We developed a two-step semi-synthesis for the preparation of isotopically labeled EAs, starting from native EAs. This universal strategy enabled the successful synthesis of all isotopically labeled priority EAs. The structure of the isotopically labeled EAs was confirmed by HPLC-HR-MS/MS using native, unlabeled EAs as a reference standard. The next step will be the implementation of the isotopically labeled standards in the European standard procedure EN 17425 to improve the quantification of EAs in foodstuffs.
Bislang wird das Phänomen der orientierten Oberflächenkristallisation kontrovers diskutiert und entsprechende Studien beschränken sich auf nur wenige Gläser. Für Silikatgläser haben wir eine gute Korrelation zwischen der berechneten Oberflächenenergie von Kristallflächen und der orientierten Oberflächenkeimbildung gefunden. Die Oberflächenenergien wurden unter der Annahme abgeschätzt, dass die Kristalloberflächen bei der Keimbildung den Kristallebenen mit minimaler Energie entsprechen, denen ein Riss beim Bruch folgt. Dieses Konzept wurde am Institut für Physik in Rennes erfolgreich bei der Berechnung der Bruchflächenenergien von Gläsern angewandt. Mehrere orientierte Keimbildungsphänomene lassen sich dadurch erklären, dass man annimmt, dass Kristalloberflächen mit hoher Energie dazu neigen, von der Schmelze benetzt zu werden. Dies minimiert die gesamte Grenzflächenenergie des Keims. Darüber hinaus werden wir die Entwicklung der Mikrostruktur beim weiteren Kristallwachstum und ihre Auswirkungen auf die bevorzugte Kristallorientierung diskutieren.