Ingenieurwissenschaften und zugeordnete Tätigkeiten
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Eingeladener Vortrag
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Monodisperse iron oxide nanoparticles as reference material candidate for particle size measurements
(2020)
In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important, especially with respect to the assessment of their environmental or biological impact. Furthermore, the European Commission’s REACH Regulations require the registration of nanomaterials traded in quantities of at least 1 ton. Powders or dispersions where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as nanomaterials. This creates a need for industrial manufacturers and research or analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution and will also target other key parameters like shape, structure, porosity or functional properties. In this respect, materials like iron oxide or titanium dioxide are considered as candidates to complement the already available silica, Au, Ag, and polystyrene reference nanoparticles.
The thermal decomposition of iron oleate precursors in high boiling organic solvents can provide large quantities of iron oxide nanoparticles that can be varied in size and shape.[1, 2] The presence of oleic acid or other hydrophobic ligands as capping agents ensures stable dispersion in nonpolar solvents. Such monodisperse, spherical particles were synthesized at BAM and pre-characterized by electron microscopy (TEM, SEM including the transmission mode STEM-in-SEM) and dynamic light scattering comparing cumulants analysis and frequency power spectrum.
1. REACH regulations and nanosafety concerns create a strong need for nano reference materials with diverse properties.
2. Iron oxide nanoparticles are under development as new candidate reference material at BAM.
3. Narrow particle size distribution confirmed by light scattering and electron microscopy.
Thermography is one on the most promising techniques for in-situ monitoring for metal additive manufacturing processes. The high process dynamics and the strong focus of the laser beam cause a very complex thermal history within the produced specimens, such as multiple heating cycles within single layer expositions. This complicates data interpretation, e.g., in terms of cooling rates. A quantity that is easily calculated is the time a specific area of the specimen is at a temperature above a chosen threshold value (TOT). Here, we discuss variations occurring in time-over-threshold-maps during manufacturing of a defect free cuboid specimen.
In-situ Prozessüberwachung in der additiven Fertigung von Metallen mittels optischer Verfahren
(2020)
Einer der aussichtsreichsten Ansätze, die Qualität und Sicherheit der gefertigten Teile in der metallbasierten additiven Fertigung (AM) zu erhöhen und die Notwendigkeit aufwändiger und zeitintensiver, zerstörender oder zerstörungsfreier Prüfungen (ZfP) nach der Fertigung zu verringern, liegt in dem Einsatz von in-situ Prozessüberwachungstechniken. Bereits jetzt werden erste Messsysteme zur Kontrolle der Energiequelle, des Bauraums, des Schmelzbades und der Bauteilgeometrie kommerziell angeboten. Weitere ZfP Verfahren, wie z.B. die aktive und passive Thermografie, werden in der Literatur als geeignet für die in-situ Anwendung angesehen, allerdings gibt es noch wenig konkrete praktische Umsetzungen, da die Möglichkeiten und individuellen Grenzen dieser Methoden, angewendet auf AM, noch nicht ausreichend erforscht sind. Aus diesem Grund verfolgt die BAM mit dem Projekt „Process Monitoring of AM“ (ProMoAM) im Themenfeld Material das Ziel, Verfahren des Prozessmonitorings zur in-situ Bewertung der Qualität additiv gefertigter Metallbauteile weiterzuentwickeln.
Im Beitrag wird zunächst das Projekt vorgestellt und anschließend der Fokus auf eine Messserie gelegt, in der Probekörper aus dem austenitischen Edelstahl 316L mit lokal variierenden Prozessparametern mittels selektiven Laserschmelzen (L-PBF) aufgebaut wurden. Der Bauprozess wurde hierbei durch das maschineneigene, koaxial arbeitende Photodiodensystem (Melt-Pool-Monitoring), einer Mittelwellen-Infrarotkamera und einer optischen Tomografiekamera im sichtbaren Wellenlängenbereich (Langzeitbelichtung für die Dauer eines Lagenaufbaus mit einer CMOS-Kamera mit hoher Ortsauflösung) simultan überwacht. Als Referenz für diese Methoden wurden die Probekörper mittels Computertomografie untersucht. Für die dabei anfallenden teils großen Datenmengen wurden Algorithmen für ein effizientes Preprocessing entwickelt. Es wurden Merkmale der Messdaten in Korrelation zu Fehlern und Inhomogenitäten extrahiert, welche für die einzelnen Methoden vergleichend vorgestellt und diskutiert werden.
All over the world, microplastic (MP) particles (particle size: 1 - 1.000 µm) are found in water, soil, air, biota and even food products. But plenty of these discussed findings are based on a very low number of real datasets, which are extrapolated to general projections. Furthermore, most data are not comparable because the strategies for sampling, sample preparation and detection methods are not harmonised/ or standardised. This would require extensive proficiancy tests. Because of the ubiquity presence and the unclear risks, which might arise from those particles, various political and environmental organisations (i.e. OECD, UNEP, WHO) identify the reduction of plastic entry in the environment as a key challenge for now and the future. This challenge includes the identification of relevant entry pathways but also the demand of harmonised, meaningful and reliable analytical procedures.
Regarding this task within the last few years, a fast practical solution for MP analysis has been developed, which includes the steps of representative sampling, adequate sample preparation and fast detection. Sampling is done by fractional filtration over sieves with mesh sizes of 500, 100, 50 and 5 µm [1]. The received samples are measured by ThermoExtraction/Desorption-Gas Chromatography-Mass Spectrometry (TED-GC-MS) [1,2]. for the most abundant polymers used in practice, which are polyethylene (PE), polypropylene (PP), polystyrene (PS), polyethylene terephthalate (PET), polyamide (PA) and acrylate as well as styrene-butadiene-rubber (SBR), a main component of tires.
The present presentation will give first-time insight in a comprehensive dataset of microplastic analysis for an exemplary urban sewage system. MP mass contents of different waters at several days, such as greywater, stormwater retention tank, influent and effluent of a wastewater treatment plant (WWTP) within an urban sewage system in Germany are determined. Furthermore, the mass of the polymers found in dry weather and rain weather flow are compared. The use of these large datasets allows first expressive conclusions regarding the contribution of urban sewage system to the MP entry sources in the environments.
We found PP and PS in all different waters. Furthermore, there is SBR in influent and also in effluent of the WWTP. Surprisingly, we could also detect hugh amounts of PE in the effluent of the WWTP.
Zur Validierung und Harmonisierung von verschiedenen Methoden in der Mikroplastik-Analytik werden polymere Referenzmaterialien benötigt. In diesem Vortrag wird dargestellt, was bisher an der BAM zu Referenzmaterialien für die Mikroplastik-Analytik entwickelt wurde, wo es hingehen soll und ein Überblick über bisher gelaufene Vergleichsuntersuchungen gebracht.
Microbiologically influenced corrosion (MIC) is a highly unpredictable process involving a complex group of microorganisms, including sulfate-reducing bacteria and methanogens. Standard laboratory MIC testing using static serum bottle enrichments is an easy but limited method, offering poor resolution on the biomineralization process of corrosion products. An example of this is the presumed corrosion product siderite by corrosive methanogens (Mi-MIC). Previous publications reported siderite was the sole corrosion product of M. maripaludis using metal coupons incubated under stationary conditions.
However, the formation of siderite is closely related to the surrounding environmental conditions, i.e. pH, CO2 concentration, flow and temperature. Thus, siderite as the sole corrosion product of Mi-MIC remain inconclusive and questionable. To study Mi-MIC effectively, a novel versatile multiport flow-column corrosion monitoring system (MFC) was developed. MFC allows sectional corrosion rate determination under flow conditions using different types of material, inoculum and packing material. MFC offers great flexibility, ease of operation and accurate corrosion measurements that can be combined with many other techniques. Using MFC, we studied multiple strains of methanogens and compared it with sulfate-reducing bacteria under neutral and low pH conditions. It was revealed by MFC that corrosive methanogens have equally high corrosion potential as sulfate-reducing bacteria. Additionally, siderite is not the dominant nor sole corrosion product of Mi-MIC. Thus, effective corrosion monitoring and establishing standard laboratory practices, i.e. incorporating MFC as part of regular testing process, will provide deeper understanding of MIC. This will allow further microbial electrophysiology understandings, contributing to effective mitigation strategy development.
Recent studies have confirmed the widening of the weld pool interface, known as a bulge effect, during deep penetration high power laser beam welding. The link between such geometric particularities of the weld pool shape and the hot cracking phenomena is significant. The present work seeks to extend the level of understanding by investigating their relationship. A coupled multiphysics, multiscale numerical framework is developed, comprising a series of subsequent analyses. The study examines the influences of the bulge on the three most dominant effects causing hot cracking, namely the thermal cycles, the mechanical loading, and the local microstructure. The bulge in the weld pool shape forms approximately in the middle of the plate, thus correlating with the location of hot cracking. It increases the hot cracking susceptibility by enhancing the three dominant effects. The numerical results are backed up by experimental data.
Der Vortrag stellt ein neuartiges Korrosionsprüfverfahren für Zinküberzüge auf Basis gelartiger Elektrolyte vor und führt die Vorteile gegenüber konventionellen Prüfverfahren auf. Basierend auf den Ergebnissen wird die Idee für einen IGF-Projektantrag in Kooperation mit dem Fraunhofer IKTS vorgestellt.
Die Untersuchungen und Ausführungen im Vortrag belegen, dass verfügbare Modellvorstellungen zur Beschreibung der Deckschichtbildung und Korrosion von Zink unter aktuellen atmosphärischen Bedingungen in Europa nicht mehr gültig sind und neu bewertet werden müssen. So können beispielsweise bisher verfügbare Prognosemodelle den Korrosionsfortschritt nicht mehr ausreichend beschreiben, da durch die Verringerung des Schwefeldioxidgehaltes der Luft veränderte Mechanismen vorliegen.