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- 6 Materialchemie (73)
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- 1 Analytische Chemie; Referenzmaterialien (46)
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Eingeladener Vortrag
- nein (399)
Die additive Verarbeitung hochfester Feinkornbaustähle mittels Wire Arc Additive Manufacturing (WAAM) ist ein komplexes, aber zugleich auch effizientes Verfahren, bei dem Werkstoff, Bauteilgeometrie und Schweißprozess gezielt aufeinander abgestimmt sein müssen. Ziel dieser Studie war es, einen Zusammenhang zwischen den Prozessparametern und der generierten Schichtgeometrie zu ermitteln. Dazu wurden definierte Referenzkörper mit einem robotergestützten Schweißsystem additiv gefertigt und hinsichtlich Schichthöhe, Wandstärke und Mikrostruktur analysiert. Fokus der Untersuchung waren sowohl konventionelle als auch für die WAAM-Fertigung speziell entwickelte hochfeste Schweißzusatzwerkstoffe. Die geometrischen Eigenschaften additiv gefertigter Bauteile lassen sich insbesondere durch die Faktoren Drahtvorschubgeschwindigkeit und Schweißgeschwindigkeit gezielt einstellen. Jedoch können diese Parameter nicht beliebig variiert werden, auch aufgrund der rheologischen Eigenschaften der Zusatzwerkstoffe. Zu hohe Streckenenergien führen zu lokalen Überhitzungen und Fehlstellen in der generierten Schicht. Undefinierte Fließ- und Erstarrungsvorgänge im überhitzten Bereich erschweren die maßhaltige Fertigung. Deshalb wird bei speziellen WAAM-Schweißdrähten das Fließverhalten gezielt modifiziert, sodass es über einen größeren Temperaturbereich hinweg konstant ist. Erst die Kenntnis über die komplexen Zusammenhänge zwischen den Prozessparametern und der Bauteilgeometrie ermöglicht die Erzeugung exakter Schichtmodelle für die additive Fertigung. Dies bildet die Grundlage für die Bearbeitung weiterer Fragestellungen auf dem Gebiet der additiven Fertigung mit hochfesten Zusatzwerkstoffen und insbesondere deren Anwendung in modernen hochfesten Bauteilen.
CHG is very different compared to other graphite degenerations or defects;
Filigree, multi-branched string-like, 3d interconnected structure;
Morphology and volumetric amount of CHG cannot be accessed by stereological interpretation of 2d section data;
Field-tested, technically established method to quantify CHG in components not available;
Fatigue: CHG causes substantial reduction in fatigue limit and significant increase in crack growth rate;
Therefore: Avoid or exclude CHG!
High-entropy alloys containing up to 6 platinum group metals can be prepared by thermal decomposition of single-source precursors non requiring high temperature. We prepare the first example of a single-phase hexagonal high-entropy alloy. Heat treat- ment up to 1500 K and compression up to 45 GPa do not result in phase changes, a record temperature and pres- sure stability for a single-phase high-entropy alloy. The alloys show pronounced electrocatalytic activity in methanol oxidation, which opens a route for the use of high-entropy alloys as materials for sustainable energy conversion.
High and medium entropy alloys gained increasing academic and industrial interest as novel materials for engineering applications. This project is aiming to clarify and compare the general and local corrosion properties of high entropy alloy CrMnFeCoNi and medium entropy alloy CrCoNi in different aqueous environments. The focus lies on the local corrosion processes that result either from microstructural imperfections (inclusions, defects at grain boundaries etc.) in the base material or processing related changes in the microstructure and/or local composition.
The corrosion behavior of the alloys was monitored via potentiodynamic polarization experiments and the local corrosion characteristics were further investigated by means of scanning electrochemical microscopy (SECM). Their passivation behavior was analyzed in three different electrolyte systems (NaCl, H2SO4 and NaClO4; c = 0.1M). The characterization of the surface morphology and composition of the passive film was performed by means of atomic force microscopy (AFM), scanning electron microscopy coupled with energy dispersive X-Ray spectroscopy (SEM/EDX) and X-Ray photoelectron spectroscopy (XPS), respectively.
Considering long term corrosion effects, electrochemical work was supported with immersion tests and the analysis of corrosion products by SEM/EDX and XPS depth-profiling. Our results indicate that the medium entropy alloy CrCoNi has a significantly higher corrosion resistance in comparison to the high entropy alloy CrMnFeCoNi. The presentation will summarize some of our results on the mechanistical aspects of the observed high corrosion resistance.
The evaluation of measurement uncertainty is essential for testing and calibration laboratories. This paper provides a general process description for the determination of the measurement uncertainty of quantitative data and its application to the conformity assessment with examples, and how to deal with the uncertainty of qualitative (Boolean) results, e. g. when "Alarm" or "No alarm" occours in an instrument display.
For hazard Assessment purposes we need models to predict what would happen in case of an accident.
The challenge in hazard assessment consists not only in choosing the right model, but beforehand to define the correct scenario .If models can be found for the physical effect to be simulated, the validation of these models is the next challenge.
Even if experimental data can be found it should always be checked, if these data are correct, even if in general experimental data are considered as “failsafe” or “the absolute truth”.
The presentation reflects the questions that have been raised by member states and NGOs.
As background information details on the question how to choose a suitable salvage pressure receptacle (SPR) are provided. This leads to the need for deleting the volume limitation for SPRs and to the discussions in 2014 and 2016 on this issue.
As an adequate substitution for deleting the volume limit for SPRs it is proposed to limit the pressure receptacles to be stored in by a maximum pressure-volume-value of 1.5 Mio bar-litres.
After some explanations to standardisation projects currently also tackling this pV-limit, some risk-based safety criteria for a limitation are mentioned with the focus of the consequence level and the general avoidance of catastrophic worst case scenarios.
First the acceptance rates resulting from the analysis of different minimum burst ratios and standards are displayed and explained. Especially the problems resulting from a further reduction if the minimum burst ratio are shown.
For a better understanding of these results the process of analysing the acceptance rate is explained in detail. This contains the alleged contradiction between safety of samples due to its scatter while the rejected sample provides a higher mean strength.
Then the importance of batch testing is explained and leads to the recommendation to have a strong interaction between provided mean strength and requested maximum of production scatter.
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.
Network modifier ions can decisively influence properties and structure of low melting alkali-zinc-borate glasses and thus cause complex effects on the liquid phase sintering of silver-glass metallization pastes. This effect was studied for X2O-ZnO-B2O3 (X = Li, Na, Rb) glasses for silver-glass metallization pastes. Viscosity and the glass transition temperature, Tg, were measured with rotational viscometry and dilatometry. Dried model pastes with 30 vol% LZB, NZB or RZB glass were prepared for sintering studies by means of heating microscopy measuring the silhouette area shrinkage of uniaxially pressed powder compacts during heating at 5 K/min. For comparison, the silhouette area shrinkage of pure glass and silver powder compacts were determined. Glass-silver wetting was investigated during heating of bulk glass cylinders placed on silver substrates. Glass RZB turned out to have the lowest viscosity among the glasses under study. Its glass transformation temperature, Tg, was found at 444 °C and it caused the lowest sintering onset for its glass and paste powder compacts. Slightly increased values of Tg were found for NZB and LZB (468 °C and 466 °C, respectively) and a slightly retarded sintering was found for both paste powder compacts. These results indicate that liquid phase sintering of silver-glass pastes under air atmosphere is mainly influenced by glass viscosity.
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 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). The fact that the material properties cannot be taken directly from the measured spectra, the developed models have to be validated. 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. Moreover, the electronic structures of the catalysts reveal a direct correlation with electrochemical activities. The development of an environmental cell offers the possibility of investigations under real conditions. This will allow changes in the optical and electronic properties during the electrocatalytic oxygen evolution reaction.
Detektion korrosionsaktiver Bereiche an Brückenbauwerken aus Stahlbeton mittels Potentialfeldmessung
(2020)
Durch das alkalische Porenwassermilieu wird Stahl im Beton durch Ausbildung einer Deckschicht vor Korrosion geschützt. Unter ungünstigen Umgebungsbedingungen (Karbonatisierung, Chlorideintrag) kann die passive Deckschicht auf der Stahloberfläche zerstört werden. Im weiteren Verlauf können sich durch Volumenexpansion der Korrosionsprodukte korrosionsbedingte Folgeschäden, wie Risse und Abplatzungen am Bauwerk ergeben. Um notwendige Sanierungsmaß-nahmen sind frühzeitige und weitgehend zerstörungsfrei ermittelte Informationen über das aktuelle Korrosionsverhalten der Stahlbewehrung von großer Bedeutung. Die Potentialfeldmessung ist ein etabliertes und weit verbreitetes Verfahren zur Beurteilung des Korrosionszustandes der Bewehrung in Stahlbetonbauwerken. Mit Hilfe dieses Verfahrens können Bereiche aktiv korrodierender Bewehrung zerstörungsfrei lokalisiert werden. In der Regel kommt diese Messmethode bei der Detektion chloridinduzierter Korrosion zum Einsatz.
High power laser beam welding has been already introduced in ship building industry since last two decades and is characterized by higher performance as conventional arc welding technologies through its higher welding speed, penetration depth and therefore higher productivity. Moreover, high quality weld joints are achievable thanks to a stronger automatization degree and better repeatability of the process. A further advantage of the laser beam welding is a manufacturing of parts with very low distortion according to much lower heat input, so that rework amount can be reduced significantly. Nevertheless, there are still some unresolved problems limiting the range of application of the technology in part manufacturing within ship building industry, restricted by development and application of new materials or new design of ship vessels.
The present contribution deals with some novel aspects of laser beam welding technology allowing to widen this range significantly. One of the possibilities is to increase the weld seam thickness for single pass laser or laser-hybrid welding is to apply contactless EM-support system based on generation of the Lorentz force counteracting the liquid metal drop out. Also, application of laser-hybrid welding technology for welding novel materials like cold resistant steel X8Ni9 used for construction of LNG tanks brings technological and design advantages comparing to conventional welding technologies by using of a similar alloyed filler wire instead of expensive Ni-based filler material. Finally, it is shown how the application of computational techniques can be used to helps to improve the quality of laser welded joints and avoid the critical weld failure by optimization of the welding process parameters.
Modern air-liners and rotor blades of wind turbines are basically made of fiber reinforced plastics (FRP). Their failure heavily impairs the serviceability and the operational safety. Consequently, knowledge of the failure behavior under static and cyclic loads is of great interest to estimate the operational strength and to compare the performance of different materials. Ideally, the damage evolution under operational load is determined with in-situ non-destructive testing techniques. Here, we report on in-situ synchrotron X-ray imaging of tensile stress induced cracks in carbon fiber reinforced plastics (CFRP) due to inter fiber failure. An in-house designed compact-tensile testing machine with a load range up to 15 kN was integrated into the beam path. Since conventional radiographs do not reveal sufficient contrast to distinct cracks due to inter fiber failure and micro cracking from fiber bundles, the Diffraction Enhanced Imaging technique (DEI) is applied in order to separate primary and scattered (refracted) radiation by means of an analyzer crystal. In the laboratory, scanning X-ray refraction topography of CFRP has been applied long before but it comes along with several disadvantages: the long total measuring time hampers real time (in-situ) measurements and the required small beam size hinders end-to-end imaging. The introduced technique overcomes both drawbacks. Imaging and tensile test rig are run unsynchronized at the greatest possible frame rate (0.7 s-1 at 28.8 µm pixel size) and smallest possible strain rate (5.5∙10-4 s-1). For 0°/90° non-crimped fabrics (ncf) the first inter fiber cracks occurred at 380 MPa (strain 0.7 %). Prior to failure at about 760 MPa (strain 2.0 %) we observe the evolution of a nearly equidistant 1 mm grid of cracks running across the entire sample in the fully damaged state before total failure.
Monitoringsysteme erfassen kontinuierlich Bauwerksdaten wie z.B. Bauwerksbeschleunigungen, auf deren Grundlage Bauwerksschäden mit Hilfe von SHM-Methoden quantifiziert werden können. Mit den gewonnenen Informationen über den aktuellen Bauwerkszustand können Vorhersagen des Bauwerkszustandes und der Bauwerkszuverlässigkeit aktualisiert und erforderliche Inspektionen und Instandhaltungsmaßnahmen vorausschauend geplant werden. Im BMBF-Forschungsvorhaben AISTEC entwickeln der Fachbereich 7.2 „Ingenieurbau“ innovative Monitoringverfahren zur Systemidentifikation und automatischen Detektion, Lokalisierung und Quantifizierung von Schäden an Infrastrukturbauwerken anhand von gemessenen dynamischen und statischen Bauwerksdaten. Im Rahmen dieses Projektes werden die Verfahren an der Maintalbrücke bei Gemünden angewendet, welche Teil der ICE-Strecke Hannover-Würzburg ist. In diesem Vortrag wird das für die Maintalbrücke Gemünden geplante und umgesetzte Monitoingsystem vorgestellt.
Im DGMK-Projekt 780 wurde eine forcierte Prüfmethode entwickelt zur Bestimmung der Beständigkeit von metallenen Werkstoffen gegenüber Brennstoffen aus Mitteldestillaten und Gemischen aus Mitteldestillat und paraffinischen Kohlenwasserstoffen, die jeweils Fettsäuremethylester (FAME) als biogene Komponente enthalten. Bei der Prüfmethode werden Proben des Werkstoffes in einem speziellen Prüfmedien ausgelagert. Die Zusammensetzung von zwei Prüfmedien wurde im Vorhaben erarbeitet. Die Prüfmedien decken für den FAME-Anteil einen Bereich von bis zu 20 % (V/V) ab. Die Auslagerung kann bei geringem Aufwand unter Atmosphärendruck durchgeführt werden.
Die Eignung einer Auswahl von metallenen Werkstoffen und Polymerwerkstoffen, die für Versorgungsanlagen für Mitteldestillat relevant sind, wurde durch Auslagerung in folgenden nicht gealterten Brennstoffen bestimmt: Heizöl EL schwefelarm (B0), Heizöl EL schwefelarm mit 20 % (V/V) FAME (B20), FAME (B100) und hydriertes Pflanzenöl (HVO). Die Temperatur bei der Auslagerung betrug 50 °C für die metallenen Werkstoffe und 40 °C und 70 °C für die Polymerwerkstoffe. Die Ergebnisse der Beständigkeitsbewertung wurden in Beständigkeitslisten zusammengefasst. Die mit dem B20 erhaltenen Werkstoffbeständigkeiten gelten generell für Gemische aus Heizöl EL schwefelarm und FAME mit einem FAME-Gehalt bis zu 20 % (V/V). Sie sind auch auf Gemische aus Dieselkraftstoff und FAME mit einem FAME-Gehalt bis 20 %(V/V) übertragbar.
Die forcierte Prüfmethode kann insbesondere KMUs bei der Weiterentwicklung von bestehenden Produkten und der Entwicklung von neuen Produkten als ein kostengünstiger Schnelltest zur Überprüfung der Werkstoff- und Bauteilbeständigkeit gegenüber Mitteldestillaten mit hohem FAME-Anteil dienen. Sie kann für die Hersteller die Sicherheit erhöhen, dass Bauteile die Freigabeprüfungen der Bauaufsicht bestehen, wobei die Freigabe aber nur für Deutschland gültig ist.
Die Erkenntnisse des Forschungsvorhabens können in eine harmonisierte Europäischen Norm für alternative Brenn- und Kraftstoffe einfließen. Diese ist für die Bauteilhersteller die Voraussetzung für die Erschließung des europäischen Marktes.
Im Beitrag werden die sicherheitstechnischen Eigenschaften von Wasserstoff diskutiert. Sowohl die Herstellung durch Wasserelektrolyse als auch die Einspeisung von Wasserstoff ins Erdgasnetz werden im Hinblick auf mögliche Gefahren durch die Veränderung von sicherheitstechnischen Kenngrößen unter Prozessbedingungen betrachtet.
A summery of previous research regarding surface crystallization is given as well as results regarding thecurrent DFG project are presented.
Wir berichten hier über die Entwicklung plattenbasierter Magnetpartikel-Immunoassays für die Bestimmung des Breitbandantibiotikums Amoxicillin und des nicht-steroidalen Antirheumatikums Diclofenac im Trinkwasser. Für die beiden Analyten wurden unterschiedliche Ansätze entwickelt, mit partikelgebundenen Antikörpern für AMX und Analyt-gekoppelten Partikeln für DCF, die die simultane Detektion beider Kontaminanten im nanomolaren Konzentrationsbereich erlauben.
Bei Geräten und Maschinen zur bestimmungsgemäßen Verwendung in explosionsgefährdeten Bereichen muss in der europäischen Union eine Zündgefahrenbewertung durchgeführt werden. Dabei müssen unter anderem die Gefahren von nichtelektrischen Zündquellen betrachtet werden, zu denen auch die mechanischen Schlagvorgänge gehören. Bei Schlagvorgängen kommt es infolge des Zusammenstoßes zweier Werkstücke zu einer Umwandlung der kinetischen Energie. Dabei erhöht sich die Temperatur der Werkstoffe an der Kontaktstelle und es kommt unter Umständen zu einem Abtrennvorgang kleiner Partikel erhöhter Temperatur. Sowohl die heißen Kontaktstellen als auch die abgetrennten Partikel können eine wirksame Zündquelle für ein explosionsfähiges Gasgemisch darstellen. Zur Festlegung von Grenzwerten wurden in der Norm EN 13463-1:2009 die Gasgemische anhand ihrer Explosionsgruppe klassifiziert und zu jeder Gruppe die maximale Energie des Schlagvorgangs festgelegt, unter derer die Entstehung einer wirksamen Zündquelle als unwahrscheinlich angenommen werden kann.
Bei Geräten und Maschinen zur bestimmungsgemäßen Verwendung in explosionsgefährdeten Bereichen muss in der europäischen Union eine Zündgefahrenbewertung durchgeführt werden. Dabei müssen unter anderem die Gefahren von nichtelektrischen Zündquellen betrachtet werden, zu denen auch die mechanischen Schlagvorgänge gehören. Bei Schlagvorgängen kommt es infolge des Zusammenstoßes zweier Werkstücke zu einer Umwandlung der kinetischen Energie. Dabei erhöht sich die Temperatur der Werkstoffe an der Kontaktstelle und es kommt unter Umständen zu einem Abtrennvorgang kleiner Partikel erhöhter Temperatur. Sowohl die heißen Kontaktstellen als auch die abgetrennten Partikel können eine wirksame Zündquelle für ein explosionsfähiges Gasgemisch darstellen. Zur Festlegung von Grenzwerten wurden in der Norm EN 13463-1:2009 die Gasgemische anhand ihrer Explosionsgruppe klassifiziert und zu jeder Gruppe die maximale Energie des Schlagvorgangs festgelegt, unter derer die Entstehung einer wirksamen Zündquelle als unwahrscheinlich angenommen werden kann.
For the generation of renewable energy offshore wind farms play an important role. The majority of these wind generators are connected to steel foundation structures. Steady increasing power output of these wind turbines leads to new challenges as well for engineers of the related support structures. Caused by the high-cyclic loading of these structures by wind and waves fatigue plays a very important role. Besides the consideration of fatigue within the design process it is additionally an important topic and challenge to monitor the existing steel structures relating to potential fatigue cracks occurring during their lifetime. This plays a role for a fundamental understanding of mechanisms as investigated in testing but also for inspection in real structures.
Since the structures of the offshore wind generators are very large and in addition partially under water effective and reliable methods for fatigue crack detection are required. This contribution will present results of recent investigations on different crack detection methods applied on high-cycle fatigue tests on small welded steel samples as well as on welded steel components. The comparison of these measurements will show what are the advantages and disadvantages of the different methods and which method is potentially more suitable for the application on real offshore wind structures. It is outlined where challenges for detection methods exist.
Furthermore, in this context the resulting challenges for the execution of material testing especially caused by the increasing dimensions of wind energy converters will by exemplarily presented.
The progress in activities on Microbeam Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 is presented and discussed with respect to the possibility of identifying and launching related VAMAS projects. Need of more promotion for the engagement of more participants from industry and academia at national, European and international level is highlighted. Also, the competition with the other technical working areas (on 'nano' or materials-related) is critically discussed.
Anwendungsfelder von verteilter faseroptischer akustischer Sensorik (DAS) werden anhand von früheren, gegenwärtigen und zukünftigen Projekten an der BAM vorgestellt und die Leistungsfähigkeit von DAS demonstriert. Die dargestellten Anwendungen sind Monitoring von Rohrleitungen, von Unterseekabeln, von Zügen und Gleisen, von Brücken, von Strassen und Verkehr, von Erdbebenauswirkungen in urbanen Gebieten, von Bohrlöchern im Kontext Erdgasspeicher und für Exploration und Monitoring von Untergründen für Geothermie-Anwendungen.
Understanding the failure mechanisms that lead to leakage of rubber seals at low temperatures is important. Rubber properties are highly temperature dependent. Changes in behaviour at low temperatures can result from the rubber-glass transition and for some rubbers by partial crystallisation. Experimental results on the low temperature behaviour of different rubber seals were discussed to help understand seal failure processes.
Risiko der Wasserstoffentwicklung an martensitischen Schraubankern unter baupraktischen Bedingungen
(2020)
Die vorliegende Untersuchung beschäftigt sich mit der Fragestellung ob unter praxisrelevanten Bedingungen die Entstehung von Wasserstoff an vollmartensitischen Schraubankern möglich ist. Im Gegensatz zu austenitischen Werkstoffen besteht bei martensitischen Werkstoffen bei Gegenwart von Wasserstoff stets die Möglichkeit einer wasser-stoffinduzierten Versprödung des Materials. Hierfür wurde ein in der Praxis häufig anzutreffendes Szenario gewählt, das ein galvanisches Element, bestehend aus nichtrostenden Schraubankern (in diesem Fall martensitischen) und einer verzinkten Ankerplatte an einem Betonkörper, umfasst. Zum Nachweis einer Wasserstoffentwicklung wird der Elementstrom zwischen den Bauteilen sowie das Korrosionspotential erfasst. Die Ergebnisse der Versuche zeigen, dass über eine zeitlich begrenzte Dauer eine starke kathodische Polarisation der martensitischen Schraubanker durch die korrosive Auflösung des Zinks erfolgt. Als Folge kommt es zur Wasserzersetzung im Phasengrenzbereich der Schraubanker und zur Entstehung von atomarem Wasserstoff. Das berechnete Gasvolumen des entstandenen Wasserstoffs an den Stahlankern wurde bestimmt und lag im Mittel bei 11,14 ± 1,94 ml. Eine Diffusion des an der Stahloberfläche adsorbierten Wasserstoffs in den martensitischen Werkstoff ist somit theoretisch möglich und impliziert eine mögliche Gefährdung durch wasserstoffinduzierte Rissbildung und spontanem Versagen unter Belastung.
Um die Versagensabläufe über die verschiedenen Skalen im Holzwerkstoff verfolgen zu können, werden Zugversuche an Lagenhölzern mittels Schallemissionsmessung überwacht. Synchron erfolgen In-situ-Messungen mit Digitaler Bildkorrelation bzw. Synchrotron-Mikro-Computertomographie. Die Kombination aller Ergebnisse wie auch die Anwendung der frequenzbasierten Mustererkennung und die Simulation ausgewählter Versuche zielen auf die Identifizierung zugrunde liegender Mechanismen hin. Abschließend werden Ansätze für ein Monitoring von Holzstrukturen diskutiert.
Toxic secondary metabolites produced by fungi (aka mycotoxins) are often identified as contaminants in cereals or other food and pose a severe health risk, since they can be carcinogenic, neurotoxic, mutagenic or harmful in other respect. The highly nephrotoxic ochratoxin A (OTA) is one of the most important and widespread mycotoxins found in grains such as rye, wheat or oats. Thus, the fast and cost-effective detection of OTA is of great importance, to ensure that the toxin concentration is below the legal limits. Currently, the mycotoxin detection in mill operations is typically performed by means of the antibody-based ELISA method, which requires extensive laboratory equipment and specialized personnel. It was the aim of this study to develop an ELISA-inspired sensor method enabling the on-site quantification of OTA. Based on a classical competitive ELISA, an electrochemical detection system was developed. Anti-OTA-antibodies were captured on magnetic beads on which the competitive affinity reaction between OTA and an OTA- horseradish peroxidase (HRP) tracer was performed. Here the OTA concentration is inversely proportional to the amount of the bound OTA-HRP tracer, which was electrochemically quantified. For this purpose, oxidized tetramethylbenzidine (TMB), which is enzymatically produced by the reduction of H2O2 by the OTA-HRP tracer, is quantified by amperometry with screen-printed electrodes in a flow system. With this method a detection limit of 250 ng L-1 could be achieved which meets the current requirements for the detection of OTA in food and feed.
Biocides are in contact with soils through direct application and passive leaching from protected materials. Consequently, soil microorganisms are exposed to biocides even though they are not their primary targets. Soil is a large reservoir of microbial diversity and has been hypothesized to be a crucial factor for the evolution and spread of antimicrobial resistance.
Currently, there is little knowledge on how biocides used to protect materials affect the evolution and spread of resistance. Thus, our aim is to investigate the risk for the evolution of biocide resistance and cross-resistance to antibiotics. In addition, we aim to elucidate the affect of biocides on the spread of resistance via horizontal gene transfer (HGT).
In adaptive laboratory evolution experiments we cultured selected model soil microorganism with representative biocides under selection regimes with increasing and stable biocide concentrations followed by antibiotic and biocide cross-resistance determination. Moreover, we investigate if the selected biocides affect the rates of de novo mutations and HGT of plasmids that carry resistance genes among soil microorganism.
Our results show only small increases of biocide resistance during serial transfers under increasing biocide concentrations. One reason for this might be the narrow selective window for biocide resistance due to steep dose-response relationships. Furthermore, our results indicate that a stable low-level biocide regime did not select for high level cross-resistance to antibiotics and other biocides.
Moreover, material preservatives affected the rates of HGT via conjugation and the mutation rates at sub-inhibitory concentrations. The results will enable future risk assessment regarding resistance evolution for biocides used as material preservatives.
Wasserstoff unterscheidet sich hinsichtlich der sicherheitstechnischen Eigenschaften von anderen brennbaren Gassen, v.a. durch die sehr niedrige Mindestzündenergie und die sehr hohe Flammengeschwindigkeit. Durch Beimischung von Wasserstoff zum Erdgas ändern sich die sicherheitstechnischen Eigenschaften zum Teil in kritischer Richtung. Bis zu einem Wasserstoffanteil von 10 Mol-% im Erdgas ist aber keine wesentliche Anpassung der Maßnahmen für den Explosionsschutz erforderlich. Synthesgas ist ein weiteres Wasserstoffgemisch das in Zukunft vermutlich zunehmend relevant sein wird. Die beiden Komponenten Wasserstoff und Kohlenmonoxid haben zwar in mancher Hinsicht ähnliche sicherheitstechnische Eigenschaften unterscheiden sich aber auch sehr stark bzgl. der Mindestzündenergie und der Flammengeschwindigkeit.
The development of high energy laser sources enables single-pass welds of thick plates up to 30 mm, but often additional materials are needed to influence the properties of the weld seams. However, the homogenous distribution of filler materials in form of e.g. electrodes is only possible up to 7 mm while the elements are only traceable up to a depth of 14 mm. To overcome this problem a two-step process is used where first the edges of the weld partners are coated with the filler material by laser metal deposition (LMD) and afterwards are welded by laser beam. Single-pass welds with electromagnetic weld pool support of 30 mm thick S355 J2+N-plates with austenitic AISI 316L-coatings were investigated as well as the influence of the coatings to the penetration depth of the laser beam without electromagnetic weld pool support in double-sided joints. The weld seams were tested by X-ray inspection and cross sections.
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.
In the wake of digitalization, organizations are increasingly exposed to risks associated with security breaches and must take measures to preserve the confidentiality, integrity, and availability of information, and to ensure business continuity. The international standard ISO/IEC 27001 assists organizations in setting up, maintaining and continuously improving their information security management systems. However, despite high growth rates, its international diffusion rates are quite heterogeneous. This paper explores why the diffusion of the international management system standard ISO/IEC 27001 differs across countries. We classify the adoption of ISO/IEC 27001 as a ‘preventive organizational innovation’ and draw from diffusion studies of other management system standards and information security research to develop a set of hypotheses. These relate to the impact of cultural dimensions and national ICT development. We use a negative binomial regression model with panel data covering 57 countries over a 12-year period from 2006 to 2017 to test our hypotheses. We find that the cultural dimensions future orientation, power distance, and institutional collectivism as well as high ICT development are driving factors for the diffusion of ISO/IEC 27001. We derive policy recommendations and avenues for future research.
In many scientific fields, isotopic analysis can offer valuable information. Up to date, typically bulk analysis is aimed at measuring the isotopic composition of the entire elemental content of the sample. However, the analyte element is usually present under the form of different species. Thus, separating species of interest from one another and from matrix components prior to isotope ratio measurements can provide species-specific isotopic information, which could be used for tracing the origin of environmental pollutants and elucidation of (environmental) speciation. Using on-line hyphenations of separation techniques with multicollector-ICP-MS (MC-ICP-MS) can save time and effort and enables the analysis of different species during a single measurement. Whereas some works hyphenating GC and IC with MC-ICP-MS have already been reported, LC and CE hyphenations are still inadequately represented based on the capabilities of these separation techniques.
In this work, we developed an on-line hyphenation of CE with multicollector-ICP-MS (CE/MC-ICP-MS) for isotopic analysis of sulfur species using a multiple-injection approach for instrumental mass bias correction by standard-sample bracketing. With this method, the isotopic composition of sulfur in sulfate originating from river water could be analyzed without sample preparation. The results were compared to data from off-line analysis of the same samples to ensure accuracy. The precision of the results of the on-line measurements was promising regarding the differentiation of the river systems by the isotopic signature of river water sulfate. The great potential of this method is based on the versatility of the applied separation technique, not only in the environmental field but also for, e.g., biomolecules, as sulfur is the only covalently bound constituent of proteins that can be analyzed by MC-ICP-MS.
Tire wear particles (TW) are generated by the abrasions of tires on the road surface through traffic. These particles can be transported by air and surface runoff and might also infiltrate the soil and consequently affect terrestrial ecosystems. The estimated tire wear (TW) emissions are immense, with 1.33 106 t a-1 in Europe. Despite this, only little is known about the environmental contents or the fate of TW.
One reason for this knowledge gap is the challenging analysis of TW in environmental samples. Detection of TW with spectroscopic methods is problematic due to high fluorescence interferences caused by contained black carbon. One analytical approach is to use zinc (Zn), a typical additive in tires, as a specific marker for the quantification of tire wear. However, any Zn originating from the sample matrix must be separated beforehand and requires elaborate sample preparation.
Car tires consist partly of synthetic rubbers, such as styrene-butadiene-rubber (SBR). This SBR could be identified and quantified via Thermal-Extraction-Desorption-Gas Chromatography-Mass Spectrometry (TED-GC-MS). This newly developed and fast screening method allows the simultaneous detection of microplastics and TW mass contents and requires minimal to no sample preparation. Firstly the sample is thermally extracted in a thermobalance under a nitrogen atmosphere. The resulting specific decomposition products are sorbed on a solid phase adsorber, which is then transferred to a GC-MS via an autosampler, where the products are desorbed, separated and identified. Cyclohexenylbenzene is used as a specific marker for SBR.
Here we investigated top layer soil samples, collected at the roadside of highly frequented German highways. Samples were analyzed without sample preparation, and SBR was detected in all investigated samples in mass contents ranging from 67.2 to 2230 mg kg-1. A correlation between SBR and Zn content in the soil was confirmed, while the correlation between SBR and Corg was hardly pronounced. We successfully demonstrated the application of TED-GC-MS as a screening method for tire wear in soil samples.
The present study will discuss these analytical results in detail as well as sampling parameters like sampling depth and distance to the roadside, and the effect of the particle size on the particle transport by water runoff and air.
Dem Fachbeirat Bodenuntersuchungen des BMBF/UBA wurden die abschließenden Ergebnisse zum UFOPLAN-Forschungsvorhaben „Monitoring zur Verwertung von Bodenmaterial“ vorgestellt. Die potentielle Auswirkung der neuen Regularien in der geplanten Novelle der BBodSchV (4. Referentenentwurf der Mantelverordnung) auf die Erweiterung der Verwertungsmöglichkeiten von Bodenmaterialien wurden aufgezeigt.
Additive Manufacturing (AM) opens new possibilities in the design of metallic components, including very complex geometries (e.g. structures optimized for certain loads), optimization of materials (e.g. gradient materials) and cost-effective manufacturing of spare parts. In the recent years, it has been used for the first safety-relevant parts, but the consideration of cyclic mechanical behavior in AM is still at the very beginning. The reason for this is the complexity of mechanical material properties, i.e. inhomogeneity, anisotropy and a large number of defects frequently textured and characterized by large scattering in size. Additionally, high surface roughness and residual stresses with complex distributions are typical of AM. Due to these reasons, the transferability of experimentally determined properties from specimens to components is a challenge. This presentation provides an overview of the questions concerning the application of AM to safety-relevant components. Possible strategies for the fatigue design of such components are presented. Besides the Kitagawa-Takahashi-diagram method and the cyclic R-curve analysis as approaches for damage-tolerant design, the identification of critical locations, the problem of representative material properties and the handling of residual stresses are addressed.
Entwicklung eines luftgekoppelten Ultraschall-Echo-Prüfverfahrens mittels fluidischer Anregung
(2020)
In vielen technischen Bereichen werden Ultraschallverfahren zur zerstörungsfreien Werkstoffprüfung (ZfP) eingesetzt um auf Basis der Signalstärke und der Laufzeit Einbauteile und Beschädigungen zu orten. Luftgekoppelter Ultraschall spielt bisher in kommerziellen Anwendungen vor Allem im Bauwesen eine untergeordnete Rolle, da die Differenz der akustischen Impedanzen von Luft und Festkörpern immense Verluste beim Übergang des Schallsignals hervorruft.
Im Rahmen des Promotionsvorhabens soll die Eignung eines neuartigen Anregungsprinzip untersucht werden, mit dem ein Großteil dieser Verluste vermieden werden soll. Anstelle eines Festkörpers soll mit Hilfe einer fluidischen Düse Druckluft zur Signalerzeugung eingesetzt werden. Die Impedanzverluste zwischen Aktuatormembran und Umgebungsluft entfallen daher.
Die gezielte Schallerzeugung durch einen pulsierenden Freistrahl ist weitgehend unerforscht. Es ist daher notwendig, den so erzeugten Schallpuls in der Interaktion mit dem transienten Strömungsfeld zu untersuchen. Das kompressible Medium Luft und die geringen räumlichen Dimensionen einer hochfrequenten Pulsdüse werfen darüber hinaus einige Herausforderungen hinsichtlich der eingesetzten Messtechnik auf. Hier sollen geeignete Verfahren weiterentwickelt und validiert werden, um die Eignung des fluidisch erzeugten Pulses zu überprüfen.
In diesem Vortrag werden erste Messungen an einem fluidischen Schalter mit denen an einem kommerziellen Luftultraschallprüfkopf verglichen.
This presentation deals with the phenomenology and design of pile foundations for offshore wind turbines, and is divided into two lectures.
The first lecture presents a brief introduction to the context and peculiarities of such foundations, and then focuses on the particular case of axially loaded piles. This part is most relevant for the relatively slender piles of the multi-pile substructures (i.e. jackets and tripods). A clear distinction between physical phenomenology and practical design is drawn here.
Deep foundations for offshore wind turbines. Lecture 2: lateral behaviour and advanced topics
(2020)
This presentation deals with the phenomenology and design of pile foundations for offshore wind turbines, and is divided into two lectures. The second lecture continues with the case of lateraly loaded offshore piles, which bears most relevance for the case of the monopile foundations. Here again, a clear separation between physical reality and design methods is intended.
Finally, the last part of the second lecture introduces several advanced topics which lie outside the classical design approaches, namely the hydromechanical coupling effects (i.e. the excess pore-pressure generation around the monopiles), the cyclic pile fatigue and the so-called pile setup (i.e. the time effects on the axial pile capacity). The relevance of the latter two topics is illustrated with experimental results from a field testing campaign on real large-scale piles.
The Dangerous Goods Regulations currently do not include limit leakage rates or sensitivity requirements for industrial leak testing procedures that are equivalent to the bubble test, which is the prescribed test method for design type testing of dangerous goods packagings. During series production of such packagings, various methods are used which often do not reach the sensitivity of the bubble test. Based on a suitable pragmatic approach, its sensitivity under industrial conditions can be considered 10-4 Pa m³/s (SLR).
For the selection of a suitable industrial leak testing method, however, factors other than the sensitivity are also important, for example flow direction, pressure level and automatability. The following methods are in principal suitable and equally effective as the bubble test: pressure rise test (vacuum chamber), ultrasonic bubble leak detection and gas detection methods (pressure technique by accumulation and vacuum chamber technique).
To ensure a uniform test level during design type testing and production line leak testing and therefore a comparable safety level as required by the Dangerous Goods Regulations, it is necessary to include a more precise specification in these regulations. On the one hand, this requires an information about the sensitivity of the bubble test, on the other hand, the inclusion of a list of suitable, equally effective industrial test methods with their specific boundary conditions
Practical breakdown voltage calculations using dielectric breakdown strength reference values
(2020)
Dielectric breakdown is a catastrophic failure of ceramic substrates and insulators. The use of dielectric breakdown strength (DBS) reference values for the dimensioning of such components is not straightforward, as the DBS depends on sample thickness and electrode area. This fact also hampers a valid comparison of data taken from different literature sources. Based on the empirically confirmed proportionality of DBS to the reciprocal square root of sample thickness and an approach to account for the influence of electrode area on the failure probability, a practical equation is derived to calculate the breakdown voltage for arbitrary sample thickness and electrode area from one set of DBS reference data. To validate the equation, the AC DBS of commercial alumina substrates with thicknesses ranging from 0.3 mm to 1.0 mm was performed using different printed electrodes with varying areas. The breakdown voltages comprise a range from 18 kV for thick samples to 8.5 kV for thin samples, resulting in DBS values from 17 kV/mm for 1.0 mm thick samples to 29 kV/mm for 0.3 mm thin samples, all made from the same material. The influence of electrode area is comparatively smaller. The results calculated with the proposed equation are in reasonable accordance with the measured data. Thus, the equation can be applied for a proper comparison of literature DBS data measured in different setups and for a reasonable estimation of breakdown voltages in DBS tests and applications based on reference data.
Aufgrund der stark korrosiven Atmosphäre in Tunnelbauwerken kommt es aufgrund von Reinigungs- und Sanierungsmaßnahmen an Ein- und Anbauteilen aus nichtrostendem Stahl häufig zu wartungsbedingten Verkehrsbeeinflussungen und Tunnelsperrungen. Bislang ist nur eine kleine Gruppe rostfreier Edelstähle für die Verwendung in Tunnelbauwerken zugelassen. Im Sinne einer mittel- bis langfristigen Reduktion von Wartungsarbeiten besteht jedoch großes Interesse, die Einsatzmöglichkeiten alternativer nichtrostender Stähle zu erhöhen. Ziel ist die Qualifizierung ferritischer-austenitischer Stähle.
Erste Untersuchungen nach 2 Jahren Auslagerung zeigten bisher vielversprechende Ergebnisse.
Reaction sintering and sintering additives for cost-effective production of thermoelectric oxides
(2020)
Thermoelectric oxides attract much interest recently. Although their thermoelectric properties are inferior to non-oxides, they exhibit distinct advantages. Thermoelectric oxides are stable in air at higher temperatures, their raw materials are less toxic, and more abundant. To enhance attractivity of these materials for industrial applications, production costs need to be reduced.
Conventionally, the legs of thermoelectric generators are sintered from green bodies of previously synthesized powder. Reaction-sintering is a fabrication method without a powder synthesis step, as the final phase is formed during the sintering from a raw material mixture. Moreover, the reduction of chemical potential during reaction-sintering is effective as an additional driving force for sintering. We show that reaction-sintering increases the densification of CaMnO3 (n-type, Sm doped). Consequently, the electrical conductivities improved by about 100 % leading to superior power factors (PF = 230 µW/mK² for CaMnO3).
Another approach to reduce the production costs is to lower the sintering temperature by adding sinter additives. The addition of 4 wt% CuO to CaMnO3 lowers the sinter temperature from 1250 °C to 1050 °C. The achieved power factor PF = 264 µW/mK is more than two times higher as reported in literature for the same dopant.
Thermoelectric materials can convert waste heat directly into electrical power by utilizing the Seebeck effect. Calcium cobaltite (Ca3Co4O9, p-type) and calcium manganate (CaMnO3, n-type) are two of the most promising oxide thermoelectric materials. The performance of these materials is evaluated by the power factor PF = S²∙σ and the figure of merit ZT = (PF ∙ T) / κ, demanding high Seebeck coefficient S, high electrical conductivity σ and low thermal conductivity κ. The latter two are increasing with increasing relative sinter density. According to theory, the relative density of ceramics can be improved by increasing the driving force for sintering. This study investigates different approaches to increase the driving force for sintering of Ca3Co4O9 and CaMnO3 to improve densities and thermoelectric properties.
The following approaches were applied: minimizing the energy input during powder synthesis by calcination, fine milling of the powder, using reaction-sintering without a powder synthesis step, and adding a transient liquid phase by sinter additives.
All different approaches led to an increased densification and thus higher electrical conductivity and higher PF. Thermal conductivity increased as well but not to the same extent. E.g. reaction-sintering increased the densification of Ca3Co4O9 (p-type) and CaMnO3 (n-type). Consequently, the electrical conductivities improved by about 100 % for both oxides leading to superior power factors (PF = 230 µW/mK² for CaMnO3). Although the thermal conductivity increased as well by 8 %, the figures of merit (ZT) were significantly higher compared to conventionally sintered bars. The addition of 4 wt% CuO as a sinter additive to CaMnO3 lowers the sinter temperature from above 1250 °C to below 1100 °C and increases the relative density. Due to the increased density, both electrical conductivity and PF increased by more than 200 % even though the sintering temperature was 150 K lower.
Sufficient adhesion/tensile strength are basic requirements for any coating/composite material. For coatings, adhesive strength in N/mm2 is of Major interest for various applications such as decorative and water-repellent coatings on wood (paints and varnishes), optical coatings on glass and polymers (reflectors and filters), electrical coatings on semiconductors, glass and polymers (conducting and bondable layers), mechanical coatings on metals and polymers (wear-reduction, scratch-resistance) and adhesion-promoting layers. For composite materials, tensile strength in N/mm2 is also a key quantity for carbon fiber reinforced composites (CFC), laminates and adhesive-bonded joints. Centrifugal adhesion testing (CAT) transfers the single-sample tensile test from a tensile or universal testing machine into an analytical centrifuge as multiple-sample test of up to eight test pieces. The one-sided sample support instead of a two-sided sample clamping and the absence of mounting- and testing-correlated shear forces provides fast and reliable results both for adhesive strength and bonding strength by means of bonded test stamps. For bonding strength, the evaluation of failure pattern from microscopic inspection is required in order to determine the failure pattern according to ISO 10365 such as adhesive failure (AF), delamination failure (DF) and cohesive failure (CF). Hence, one test run by CAT-technology provides either statistics or ranking of up to eight samples at once. For adhesive strength of coatings, a variety of examples is discussed such as ALD-Al203 layers as adhesion promoters, evaporated Ag-layers on N-BK7 glass, sputtered Cr- and Al-layers on Borofloat 33 glass, evaporated Au-films on N-BK7 glass and sputtered SiO2 -layers on CR39 Polymer. Provided adhesive or bonding strength are high enough, the substrate or the joining part may also fail.
The passage of the train is dominated by the impulses of the static axle loads. The response of the regular homogeneous and irregular soils has been calculated by the finite-element method in frequency domain. The superposition of the impulse responses yields the quasi-static component of the ground vibration which is restricted to very low frequencies and to the close near-field of the track. In case of an irregular soil or ballast of which the stiffness varies randomly in space, a mid-frequency ground vibration component is generated by the scattering of the axle impulses. Measurements will be shown which prove the existence of the mid-frequency ground vibration component and the unique explanation by the scattered axle impulses: many international measurements with a raised mid-frequency component, axle-box measurements with a too low mid-frequency dynamic load, amplitude-speed dependencies which are incompatible with irregularity-induced dynamic loads, and ground vibration reductions due to stiff track elements.
Hochentropie-Legierungen (HEAs) zeichnen sich durch einen Mischkristall-System aus mindestens fünf und Mittelentropie-Legierungen (MEAs) durch mindestens drei Hauptlegierungselemente aus, in äquiatomarer Zusammensetzung. Sie zeigen außergewöhnliche Anwendungseigenschaften, wie z.B. hohe Festigkeit, Duktilität oder Korrosionsbeständigkeit. Zukünftige HEA/MEA-Komponenten aufgrund ihrer Eigenschaften für wasserstoffhaltige Umgebungen (wie Behälter für kryogene oder Hochdruckspeicherung) von Interesse. Daher ist die Bewertung der Wasserstoffabsorption und die Diffusion in diesen Materialien von großer Bedeutung. Dazu wurden in unserer Studie eine CoCrFeMnNi-HEA und eine CoCrNi-MEA untersucht. Die Proben wurden elektrochemisch mit Wasserstoff beladen. Für die Ermittlung des Wasserstoffdiffusionsverhaltens wurde die thermische Desorptionsanalyse (TDA) mit unterschiedlichen Heizraten bis zu 0,250 K/s angewandt. Die nachfolgende Peakentfaltung der Signale führte zu Hochtemperatur-Desorptionsspitzen und Wasserstofftrapping auch über 280°C. Eine resultierende Gesamtwasserstoffkonzentration > 40 ppm wurde für den MEA ermittelt und > 100 ppm für den HEA. Dies deutet auf zwei wichtige Effekte hin:
(1) verzögerte Wasserstoffdiffusion und (2) eine beträchtliche Menge an getrapptem Wasserstoff auch bei hoher Temperatur. Beide Effekte können hinsichtlich einer wasserstoffunterstützten Rissbildung kritisch werden, dies erfordert jedoch weitere Untersuchungen. Zusätzlich erfolgte die Bestimmung des lokalen Volta-Potentials mittels hochauflösender Kelvin-Sonden-Kraft-Mikroskopie (SKPFM). Die ermittelten Scans zeigen einen bestimmten Einfluss der Wasserstoffbeladung auf die Potentiale.
Die dehnungsinduzierte Martensitbildung wurde mittels Röntgen-Diffraktion und -Radiographie mit dem EDDI-Instrument am BESSY II in supermartensitischem Stahl mit Anlassaustenit untersucht. Die Bildung wird durch Wasserstoff im Gefüge unterdrückt. Die Duktilität von wasserstofffreiem SMSS korreliert mit dem Anteil an dehnungs-induziertem Martensit
Packages for the transport of high-level radioactive material are designed to withstand severe accidents. Hypothetical severe accident conditions are defined in the IAEA Regulations for the Safe Transport of Radioactive Materials.
One of these accident conditions is the thermal test, mainly consisting of a 30 minute fully engulfing 800°C pool fire or an equally severe fire test. The heat fluxes into the package depend substantially on the fire characteristics and the Surface temperature of the package.
Fire tests can be performed at BAM on a propane gas fire test facility. In order to investigate the heat fluxes over a wide range of surface temperatures in this test facility a fire reference package was designed for multiple use. The package represented the outer geometry of a specific transport cask for radioactive waste. The fire reference package is a closed steel sheet cylinder with a wall thickness of 10 mm, a length of 1500 mm and a diameter of 1050 mm. The package was instrumented with thermocouples and filled with heat resistant insulation material.
Three open-air fire tests were performed in the BAM propane gas fire test facility. The flames exposure time period varied slightly for the fire tests. The wind direction as well as the wind Speed were measured and changed between and during the tests. Test stand parameters such as wind shield location and propane gas volume flow were chosen constant for the three tests. The locally measured fire reference package steel sheet temperatures were used for the calculation of heat fluxes as function of time and surface temperature. The measured temperatures allowed further calculations. In a first approach effective fire characteristics of the propane gas fire, including the flame temperature, the fire convection coefficient and a Radiation exchange coefficient mathematically describing the determined average heat flux over the surface temperature were calculated.
Alkali-activated materials have been repeatedly reported to exhibit high acid resistance, but no generally accepted hypothesis regarding the underlying mechanisms has emerged yet. To contribute to this issue, K-waterglass-activated metakaolin specimens, with and without the addition of CuSO4·5H2O in the starting mix, were exposed to either a chemically aggressive sewer environment (mortars) or sulfuric acid (pastes). The mode of copper incorporation in the materials and the formation of copper phases in the corroded layers were studied by XANES at the Cu K-edge, and 29Si, 27Al and 1H MAS NMR was employed to understand the processes during acid attack. Copper was found as a spertiniite-like phase in the as-cured materials, while in the deterioration layers of the pastes it was present as copper sulfate. In the corroded regions of the mortars, unequivocal identification of Cu phases was not possible, but the results were reconcilable with the presence of copper carbonate hydroxide. The solid-state NMR results revealed virtually complete dissolution of the K-A-S-H gel and the formation of silica gel, interpreted to be a central mechanism determining the acid resistance. No significant differences between the microstructural alterations of the pastes with and without Cu addition on (chemical) sulfuric acid attack were observed.
Structural health monitoring (SHM) is a term that groups together techniques adopted to evaluate in a continued fashion the structural integrity and degradation of technical appliances. SHM is particularly attractive for components that are difficult to access or expensive to take off-line. Among many other techniques, SHM can be performed using ultrasonic guided waves (UGW) which have an advantage of traveling over Long distances. Various guided wave modes exist along with many methods for their generation and sensing, e.g by means of interdigital transducers (IDT). This contribution is dedicated to the design and characterization of a flexible piezopolymerbased IDT which allows for the selective excitation of UGW, resulting in more straightforward data analysis. The designed IDT was characterized using a 3D Laser Doppler Vibrometer (3D LDV) in the air to identify and analyze the IDT’s Vibration modes. Then the transducer was mounted on an aluminum plate, and the generated wavefield was measured with the 3D LDV.
According to this investigation, we demonstrate that it is possible to selectively excite desired guided wave mode, namely the A0 mode, suppressing the excitation of the S0 mode. Moreover, the measured wavefield allows for analysis of the directivity of the designed IDT. All in all the results show good correlation between theoretical predictions and measured values, thus allowing to use the current design in terms of selective excitation as it is.
Wind turbine rotor blades, made of fiber reinforced polymers (FRP), often fail before their projected 20-year lifespan, largely due to defects that originate during manufacturing and are propagated by operational fatigue and environmental conditions. The cost-intensive replacement outcomes lead to a high loss of earnings, and are one of the inhibitors of wind turbine production [1]. A potential repair alternative is to locally patch these areas of the blades with adhesively bonded structural repairs. However, the effects of such repair methods of the outer shell region on the structural integrity of the rotor blades are still largely unknown, and are thus investigated in this project.
The shell components of rotor blades are made of FRP composite material sandwiching a lightweight core, often a rigid foam or Balsa wood. The repair methods involve replacing the lost load path with a new material that is joined to the parent structure [2]. Repairs in this project focus on the scarf method, which allow for a smoother load distribution across the joint, aiming to study the damage mechanism of glass FRP scarf repairs for wind turbine blade shell applications. Namely, the source and path of the damage initiation and propagation, role of the interface between parent and patch material, and the role of the fiber orientation mismatch at this interface are examined. Biaxial ±45° and 0/90° FRP specimens are produced with the vacuum-assisted resin infusion (VARI) process using E-glass non-crimp fabric. The patch layers are then joined using VARI with a scarf ratio of 1:50, using glass FRP fabric with half the areal weight of the parent side to allow for better drapability. The methods and practices in specimen production are based on common industry practice in rotor blade shell manufacturing and repairs.
The specimens are tested under uniaxial tensile load, during which they are periodically monitored for damage onset. A comparison of the ±45° and 0/90° specimens allows for an understanding of the role of a highly mismatching fiber orientation in the transition zone between parent and patch material on the failure mechanism of the scarf joint. Although failure in both orientations begins as delamination at the joint edge, the difference in the mechanisms at play in the two different specimen types leads ultimately to different fracture paths. Namely, in the inter fiber failure mechanism of the ±45° specimens, the higher interlaminar strength compared to the intralaminar strength of the laminate leads to intralaminar failure of the ±45° scarf joint specimens. Alternatively, the competition in the 0/90° specimens lies between the interlaminar strength and fiber failure strength, and here we experience failure primarily across the scarf joint length. The scarf joint in the 0/90° specimens disrupts the continuity of the load-carrying 0° layers, directing the failure path to remain primarily along the scarf joint. Experimental results are compared to finite element analyses of scarf patch repairs on glass FRP sandwich specimens with the same respective layup orientations, where the damage initiation regions are identified and correlated to fiber orientation, serving as a bridge to future work which will experimentally examine the scarf repair patches on sandwich shell specimens.
The quantitative determination of adhesion and cohesion properties is a key requirement for adhesive-bonded joints and coated components in both R&D and Quality assurance. Because of the huge variety of layer/substrate Systems in terms of materials and large thickness range, adhesion tests display the same diversity as layer/substrate systems. There are only two tensile testing procedures available, that determine adhesive strength in terms of force per area (N/mm²), the single-sample pull-off test in a tensile testing machine and the multiple-sample-test using the Centrifugal Adhesion Testing (CAT) Technology.
The CAT Technology is a testing method which uses centrifugal force as tensile testing force in a multiple-sample arrangement within a drum rotor of a Desktop centrifuge. Hence, the adhesive/bonding strength A/B can be determined on a statistical basis under identical testing conditions for up to eight samples.
A variety of examples for bonding strength of adhesives, adhesive strength of coatings and compound strength of composite materials is discussed such as metalto-metal and glass-to-metal bonding, sputtered SiO2-layers on CR39 Polymer and carbon fiber reinforced polymer.
Vergleichende Fallversuche zur Bewertung von Fallfundamenten - Ausblick auf Untersuchungen der BAM
(2020)
Oft verfügen Produktionsstätten über bereits verbaute Fallfundamente, die nicht das geforderte Massenverhältnis von 1:50 aufweisen. Gemäß ADR ist jedoch auf dem Niveau der Musterprüfung zu prüfen. Es ist daher fraglich, ob die Prüfungen im Rahmen der Eigenüberwachung und die Baumusterprüfungen vergleichbare Ergebnisse liefern, wenn die Fallfundamente unterschiedlich beschaffen sind. Ziel der Untersuchungen ist daher die Entwicklung eines Untersuchungs- und Prüfkonzepts für bereits verbaute Fallfundamente für Gefahrgutverpackungen im Rahmen einer ingenieurwissenschaftlichen Promotionsarbeit.
In 2019 the German federal institute Bundesanstalt für Materialforschung und –prüfung (BAM) conducted a benchmarking to compare the operations of European accreditation bodies and to identify best practices, with the aim of improving key processes in accreditation. Ten European accreditation bodies attended the comparison, four of which had already taken part in the pilot phase of the benchmarking project, which was conducted in 2017 by the German accreditation body Deutsche Akkreditierungsstelle GmbH (DAkkS) and the BAM.
The study, designed to examine and compare the operation of accreditation bodies in Europe, used a management tool called Process Maturity Benchmarking Tool, which was especially elaborated and validated for this purpose in the pilot phase, in order to determine the values of indicators, thus enabling a comparison of the accreditation bodies despite different operational processes and organizational forms. The management tool is based on the analysis of selected processes with high relevance for the operation of accreditation bodies. The processes are derived from a process map designed for accreditation bodies in a universally applicable way. The indicators used to characterize the processes come from two sources: The first source relates to data already available from internal databases, reports, financial audits, and others. The second source is derived from the self-evaluation of process maturity performed by the accreditation bodies. The criteria for evaluating process maturities were designed by applying the criteria of the EFQM excellence model 2013 of the European Foundation for Quality Management (EFQM) to the processes identified in the process map.
The results of the analysis were presented to and discussed with representatives of the ten accreditation bodies at a Results-Workshop that took place at BAM on 21/22 January 2020.
In this presentation a wrap-up of the results was given to the HHC of EA
Material qualification for laser powder bed fusion (L-PBF) processes are often based on results derived from additively manufactured (AM) bulk material or small density cubes, although it is well known that the part geometry has a tremendous influence on the heat flux and, therefore, on the thermal history of an AM component. This study shows experimentally the effect of simple geometrical obstructions to the heat flux on cooling behavior and solidification conditions of 316L stainless steel processed by L-PBF. Additionally, it respects two distinct inter layer times (ILT) as well as the build height of the parts. The cooling behavior of the parts is in-situ traced by infrared (IR) thermography during the built-up. The IR signals reveal significant differences in cooling conditions, which are correlated to differences in melt pool geometries. The acquired data and results can be used for validation of computational models and improvements of quality assurance.
Einfluss von Konstruktion und Wasserstoff auf die Kaltrissbildung hochfester Feinkornbaustähle
(2020)
Der konstruktive Leichtbau erfordert den zunehmenden Einsatz hochfester Feinkornbaustähle mit Streckgrenzen ≥ 690 MPa. Neben den durch die Wandstärkenreduzierung erreichbaren Einsparungen an Ressourcen und Fertigungszeit lässt sich eine weitere Minimierung der Schweißzeit und -kosten mittels abgesenkter Schweißnahtvolumina erreichen. Hierzu wurden moderne Lichtbogenprozesse, wie bspw. der modifizierte Sprühlichtbogen (Mod.SLB), mit erhöhter Abschmelzleistung entwickelt, mit denen auch enge Nahtspalte bzw. Nahtöffnungswinkel geschweißt werden können. Hochfeste Verbindungen unterliegen zunehmend erhöhten Anforderungen in Bezug auf die schweißtechnische Verarbeitung und der resultierenden Bauteilperformance und sicherheit. Dies gilt insbesondere beim Bauteil-schweißen mittels solcher Hochleistungsverfahren in Verbindung mit engen Nahtspalten. In der vorliegenden Arbeit soll dieser Herausforderung durch Klärung der Einflüsse auf die Kaltrissbildung bei einem hochfesten Feinkornbaustahl S960QL Rechnung getragen werden. Für die Kaltrissprüfung werden entsprechende adaptierte Proben analog dem selbstbeanspruchenden TEKKEN-Test verwendet und hinsichtlich Rissbildung, Gefüge, Gehalt an diffusiblem Wasserstoff und Eigenspannungen analysiert. Die Variation der Nahtöffnungswinkel der Prüfnähte erfolgt zwischen 30° und 60°. Zur Vermeidung wasserstoffunterstützter Kaltrissbildung wird die Wirksamkeit einer Nachwärmprozedur aus der Schweißwärme heraus untersucht. Als Ergebnis zeigen die Schweißgüter, die an reduziertem Nahtöffnungs-winkel erzeugt wurden, im Mittel etwas höhere Wasserstoffkonzentrationen. Zudem ist an diesen Schweißgütern eine vermehrte Mikro- als auch Makrorissbildung festzustellen. An allen Proben, die nicht nachgewärmt wurden, treten Kerbrisse aufgrund von Kaltrissbildung auf, deren Vermeidung sich durch ein Nachwärmen unmittelbar nach dem Schweißen als besonders effektiv darstellte.
The fatigue design of metallic components is usually based on two different approaches, namely total life and damage tolerance. The former takes into account both the initiation and propagation stages. The latter is based on fracture mechanics and needs an initial defect, which propagates until the critical size under cyclic loading, provided it is large enough. In this case, a residual life rather than a total life is obtained. The overall lifetime of a cyclically loaded structure involves four consecutive stages: a) crack initiation; b) propagation of microstructurally short cracks; c) propagation of physically/mechanically short cracks; d) propagation of long cracks. Considering the propagation from the short crack regime, the damage tolerance approach can be extended to adequately calculate the total life of a component.
The fatigue strength of metallic materials containing defects depends on the non-propagation condition of small cracks emanating from these defects. In this work, the presence of mechanically short cracks from the beginning of the component's life is considered. Consequently, the methodology of analysis must be able to treat adequately local ligament yielding effects typical for short cracks and must include the thorough description of the crack closure effect up to the long-crack regime. In the analysis based on long cracks, the linear-elastic condition is mostly satisfied which allows the use of the linear elastic parameter ΔK for describing the crack driving force. On the contrary, this assumption is not adequate for mechanically short cracks because the crack depth is in the order of the plastic zone. Instead, an elastic-plastic driving force should be considered. Furthermore, the gradual build-up of the plasticity-induced crack closure effect must be considered, which implies a transition from the intrinsic (effective) threshold value, ΔKth,eff, to the long-crack threshold, ΔKth,LC.
The effective component is a material parameter which is dependent on the elastic properties and crystal lattice. The gradual build-up of crack-closure is described by ΔKth,op which is a function of the plastic properties, grain-size, environment conditions, load ratio and crack-depth. The crack closure can be characterized experimentally by the so-called cyclic R-curve. Some other crack closure effects, such as roughness or oxide-debris induced, might be incorporated as well.
The knowledge of the cyclic R-curve can be useful to determine the largest non-propagating crack size at the material fatigue limit. This is realised by means of the so-called cyclic R-curve analysis: The tangent criterion between the driving force and the cyclic R-curve define the transition between crack arrest and propagation. In this regard, a0 is defined as that crack depth which will only grow into a non-propagating crack due to the development of crack closure.
The procedure outlined briefly here has been successfully applied to the determination of the fatigue limits of steel weldments. Considering the stochastic distribution of the weld geometric parameters (namely, weld toe radius, the flank angle, and the excess weld metal) it is possible to perform a full probabilistic cyclic R-curve analysis and determine this way the statistical distribution of the initial crack size at the weld toe at the fatigue limit.
Biodiesel is viewed as a major source of energy. In areas such as the European Un-ion, where 80 % of the oil-based fuel is imported, there is also the desire to reduce dependence on external oil supplies.
Materials compatibility is a major concern whenever the fuel composition is changed. The question arises of whether polymeric materials are resistant to heating oil with 20 % biodiesel (B20) in comparison to pure heating oil.
The polarity of biodiesel increases its solvency and facilitates permeation and extrac-tion. Solvation, swelling and/or extraction lead to changes in the physical properties. Extraction alters the fuel chemistry. These chemical changes could also accelerate the degradation (hydrolysis and oxidation) of the polymeric material with the loss of additives and stabilizers.
Exposure tests to determine the resistance of polymers frequently used for compo-nents in middle distillate facilities, such as ACM, FKM, HNBR, PA, PE, POM, PUR and PVC in heating oil and a blend of heating oil and 20 % biodiesel (B20) were al-ready performed.
The objective of this research was to determine the resistance of these polymers in 8-year aged heating oil blend B10 and 1-year aged blend B20 at 40 °C.
Mass, tensile strength, breaking elongation and Shore hardness A (D) of the test specimens were determined before and after exposure for 84 (42) days in the test fuels under static conditions.
There is not determined a threshold for the reduction in tensile properties and Shore hardness in the international standards. Therefore, a threshold of 15 % was deter-mined for the evaluation of the compatibility.
A significant reduction in Shore hardness was determined after exposure of ACM and PUR test specimens in 1-year aged B20.
The tensile strength of PUR test specimens in 1-year aged B20 was reduced by more than 50 %, and the breaking elongation by more than 30 %.
A decrease in breaking elongation was measured for POM test specimens after ex-posure to 1-year aged B20 by 25 % (limited resistance).
8-year aged B10 had a stronger effect than 1-year aged B20 on the polymers. ACM test specimens were softened by B10 resulting in a drop of Shore hardness by over 20 %. B10 reduced tensile strength and breaking elongation of PUR test specimens by over 50 %. In contrast, the breaking elongation of POM was increased by over 270 %.
It can be concluded that the polymers HNBR, FKM, PA6, PE and PVC are resistant in 1-year aged B20 whereas ACM and POM are limited resistant. PUR is not re-sistant.
HNBR, FKM, PA6, PE and PVC are resistant in 8-year aged B10, whereas PUR and POM are not resistant, and ACM just limited resistant.
High conductive silver-glass-metallization-pastes are key components in photovoltaics and advanced microelectronics. However, the underlying mechanisms of liquid phase sintering as silver dissolution, diffusion and reprecipitation are poorly understood so far.
In the current work, the influence of different network modifier in alkali-zinc-borate paste-glasses on liquid phase sintering of silver-glass-composites was studied. Therefore, silver-glass-composites containing 30 vol% glass were prepared, using low melting X2O-ZnO-B2O3 glasses with X = Na, Li, and Rb (NZB, LZB, and RZB). Glass transition temperature, viscosity, glass-silver wetting, crystallization and sintering behavior was studied by means of thermal analysis, dilatometry, heating microscopy and microscopy.
Similar glass transition temperatures of 450 °C (RZB), 460 °C (LZB) and 465 °C (NZB) were found by means of thermal analysis for glasses under study. Also, all glasses have a similar crystallization onset at about 550 °C, even though exhibiting with a different degree of crystallization.
Despite these similarities, however, the sintering behavior, measured in terms of area shrinkage, significantly differs for the composites. This finding indicates a different degree of silver dissolution. Assuming that dissolved silver reduces the viscosity, this effect could explain why glass crystallization starts at lower temperature in the composites. For example, the crystallization peak of LZB at 629 °C measured for pure glass powder compacts was decreased to 586 °C for the composite. Confirmatively, microstructure analyses indicate different degrees of silver dissolution, as e.g. revealed by different amount of silver precipitates within the residual glass phase, and reprecipitation. Best silver dissolution appeared for the RZB glass. Nevertheless, the final densification of RZB was retarded probably due to swelling and crystallization.
Es ist bislang noch keine einheitliche Vorgehensweise und kein bestimmtes Prüfverfahren für die Schüttwinkelmessung festgelegt. Bei den Prüffüllgütern handelt es sich nicht nur um gefährliche Ersatzfüllgüter, sondern zum Teil auch um gefährliche Originalfüllgüter. Es liegen noch keine systematische Untersuchungen darüber vor, welche der in den Prüfstellen gängigen Methoden sich prinzipiell für die Anwendung bei bestimmten Extremfällen von Füllgütern eignen. Ziel der Untersuchungen ist daher ein systematischer Vergleich bei der Anwendung verschiedener in den Prüfstellen gängiger Schüttwinkelmessmethoden.
Die Eigenschaften von optischen Fasern und faseroptischen Sensoren werden beschrieben und die Funktionsweise von verteilter faseroptischer akustischer Sensorik (DAS) erklärt. Die Verwendung von DAS für Zustandsmonitoring vor allem von Infrastruktur und Anlagen wird motiviert. Im Folgenden wird die Einsetzbarkeit von DAS für verschiedenste Anwendungen anhand einiger Beispiele (vergangene und gegenwärtige Projekte der BAM zum Thema DAS für Infrastrukturmonitoring) gezeigt. Diese betreffen das Monitoring von Rohrleitungen/Pipelines, von Energiekabeln, von Gleisanlagen und Zügen, von Brücken und von Strassen und Strassenverkehr.
A large amount of data and information is collected in the field of non-destructive testing (NDT) in civil engineering. The weakly structured data are usually evaluated with regard to specific testing tasks (e.g. geometry determination, damage localization, quality assurance). While the data offers great economic potential, i.e. to support construction planning, monitoring and maintenance processes, the evaluation is manual and case-by-case and therefore too inefficient for broader applications. We present recent visions and approaches how these large amounts of data need to be handled in the future and how we aim to make the acquired knowledge accessible to our stakeholders. Building on initiatives in materials research, we stress the importance of further research in the field of semantic data integration particularly motivate why an ontology is needed for the area of NDT in civil engineering.
In recent years, we have come to appreciate the astounding intricacy of the processes leading to the formation of minerals 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 species. These include solute clusters (e.g. prenucleation clusters, PNCs), liquid(-like) phases, as well as amorphous and nanocrystalline solids etc.. Does it, however, mean that all the minerals grow through intermediate phases, following a non-classical pathway?
In general, the precursor or intermediate species constitute different, often short-lived, points along the pathway from dissolved ions to the final solids (typically crystals in this context). In this regard synchrotron-based scattering (SAXS/WAXS/total scattering) appears to be the perfect tool to follow in situ and in a time-resolved manner the crystallization pathway because of the temporal and spatial length scales that can be directly accessed with these techniques. In this presentation we show how we used scattering to probe the crystallisation mechanisms of calcium sulfate, This system contains minerals that are widespread in diverse natural environments, but they are also important in various industrial settings. Our data demonstrate that calcium sulfate precipitation involves formation and aggregation of sub-3 nm anisotropic primary species. The actual crystallisation and formation of imperfect single crystals of calcium sulfate phases, takes place from the inside of the in itial aggregates. Hence, calcium sulfate follows a non-classical pathway.
Modified TEKKEN test for studying hydrogen-assisted cracking in high-strength structural steels
(2020)
In the present work, the complex interactions of the influences of material, welding process and seam configuration and the restraint of shrinkage on the residual stresses and the influence of diffusible hydrogen on hydrogen-assisted cracking (HAC) in the high-strength steel S960QL were investigated. For this purpose, self-restraint specimens were selected using the TEKKEN test with correspondingly adapted seam opening angles and a restraint intensity of approx. RFy = 17 kN/(mm·mm). The variation of the seam opening angle of the test seams was between 30° and 60°. Due to the comparatively high restraint of shrinkage in the transverse direction of the weld, high tensile residual stresses in the weld metal were expected for both weld seam configurations. In addition, a dehydrogenation heat treatment (DHT) for HAC prevention under restraint of shrinkage was verified. In order to keep distortion and heat input as low as possible, the seam geometries were manufactured from the solid material by means of electric discharge machining (EDM). Both, solid wire and metal cored wire were used. In addition, hydrogen was added to the shielding gas in solid wire welding to increase diffusible hydrogen concentration. Moreover, welding residual stresses at the weld seam surface, which were measured by using mobile X-ray diffraction, were taken into account to evaluate the HAC behavior. DHT was carried out at 250 °C for 4 h in an external furnace.
Methods for the rapid and sensitive detection of target analytes are gaining importance in medical diagnostics and environmental monitoring, in the security, occupational health and safety as well as food sectors. Among all the methods employed for rapid tests, lateral flow assays (LFAs) are the most commonly used. However, some drawbacks are that most of these tests either indicate the analyte only indirectly, and in other cases the sensitivity is not high enough.
Keeping in mind these limitations, the use of stimuli-responsive materials for small-molecule sensing relying on chemical signal amplification and utilizing specific interactions between biomolecules such as antibodies and the corresponding analytes are particularly attractive. Such materials can also be incorporated on paper strips for lateral-flow assays in a straightforward manner. These sensing materials comprise mesoporous silica nanoparticles loaded with indicator molecules and containing certain hapten derivative molecules covalently grafted at the surface, which bind to the respective antibody and inhibit the release of a dye as reporter (Scheme 1). In presence of the designated analyte, a displacement of the antibody from the material is observed, allowing the release of dye. Because a large number of indicator molecules can be released when a single analyte molecule binds to an antibody cap, a strong signal amplification is observed.
Considering the modularity, high sensitivity and selectivity of these antibody-gated indicator delivery systems, the presentation discusses general aspects of system design as well as analytical performance and highlights the integration into a lateral-flow assay, showing as an example the determination of the explosives TATP, TNT and PETN with a fluorescence readout, in single-substance and multiplexing modes.
The investigation of the long-term performance of sealing systems employed in containers for radioactive waste and spent nuclear fuel is one research focus area for division 3.4 “Safety of Storage Containers” at the Bundesanstalt für Materialforschung und -prüfung. The behaviour of metallic seals, which are employed in interim storage casks for used fuel and high active waste, over time is of high importance for ensuring safe enclosure. Therefore, investigations on these systems were started at BAM to get a general understanding of the relevant processes. Our investigations comprise investigations on different parameters which influence the seal performance and the main part is focussed on the time and temperature dependent behaviour.
In this contribution an overview of the performed tests and their respective results will be given. A focus will lie on a comparison between seals with large torus diameter in comparison to small diameters.
Our aim is to understand the long-term behaviour of the sealing systems for evaluation of their performance during possible extended interim storage and subsequent transportation.
In addition to molar mass distribution (MMD) synthetic polymers often exhibit an additional chemical heterogeneity distribution, expressed by different end groups and other structural variations (e.g. tacticity, copolymer composition etc.). Ionization in MALDI MS is always strongly affected by such chemical properties. For example, the abundance of cyclics in MALDI TOF mass spectra is frequently reported to greatly exceed that of linears. Thus, the MALDI ionization behavior of various neat end-capped linear poly(L-lactide)s and one cyclic poly(L-lactide) was investigated and compared with that of blends of both structures. Moreover, the influence of the cationizing salt was investigated too.
Neat compounds and various blends of cyclic and linear species were prepared and studied using two MALDI TOF mass spectrometers under identical conditions with regard to sample preparation and instrumental conditions, except for the laser power and the salt used for cationization. Polymer samples were additionally characterized by NMR and SEC.
The steady increase of the laser intensity caused an exponential increase of the peak intensities of both linear and cyclic polylactides.The response of linear polylactides (in the investigated molecular mass range), whether as neat polymer or in blends with other linear polylactides was almost similar. This clearly supports our assumption that ionization in MALDI is probably unaffected by the end group structure.The variation of the laser power shows only little effect on the intensity ratio of linear-to linear and cyclic-to-linear polylactides in blends. Whereas neat linear polylactides at all laser intensities have a significantly higher abundance than neat cyclics, in mixtures of both an overestimation of cyclic species in MALDI TOF mass spectra of polylactides was found. However, this is far less distinct than frequently reported for other polymers.Concluding, peak suppression of linear polymers in mixtures of both architectures can be excluded, which also means, that polylactides showing only peaks of cyclic compounds in their MALDI - TOF mass spectra do not contain a significant fraction of linear analogues.
Our study is the first systematic comparison of the MALDI ionization of neat and blended cyclic and linear polylactides.
Scientific welding data covers a wide range of physical domains and timescales and are measured using various different sensors. Complex and highly specialized experimental setups at different welding institutes complicate the exchange of welding research data further. The project aims to simplify the exchange and quality assurance of scientific welding data by establishing a common open source file format.
Ziel des WelDX Forschungsvorhabens ist es, den Austausch wissenschaftlicher Forschungsdaten aus dem Bereich der Schweißtechnik auf Basis eines einheitlichen Open Source Dateiformates zu ermöglichen und damit die Einhaltung und Dokumentation geeigneter Qualitätsstandards zu fördern. Im Zuge der Projektarbeit wird die Zusammenarbeit und der Wissenstransfer schweißtechnischer Institute zunächst auf nationaler Ebene gefördert und die Bildung eines von der Fachcommunity getragenen Kuratoriums zur Betreuung und Weiterentwicklung des Dateiformates und der Ausarbeitung zugehöriger Qualitätsstandards angestrebt.
Der Vortrag gibt eine Übersicht zur Motivation, der technischen Umsetzung des Dateiformates sowie möglicher Anwendungsfälle.
WelDX – Entwicklung und Anwendung eines einheitlichen Dateiformates für das Lichtbogenschweißen
(2020)
Ziel des WelDX Forschungsvorhabens ist es, den Austausch wissenschaftlicher Forschungsdaten aus dem Bereich der Schweißtechnik auf Basis eines einheitlichen Open Source Dateiformates zu ermöglichen und damit die Einhaltung und Dokumentation geeigneter Qualitätsstandards zu fördern. Im Zuge der Projektarbeit wird die Zusammenarbeit und der Wissenstransfer schweißtechnischer Institute zunächst auf nationaler Ebene gefördert und die Bildung eines von der Fachcommunity getragenen Kuratoriums zur Betreuung und Weiterentwicklung des Dateiformates und der Ausarbeitung zugehöriger Qualitätsstandards angestrebt.
After a colleague sent me a more useful measurement from a laboratory instrument than what I could get from the beamline, I knew it was time to reassess my life's choices. Over the course of several subsequent post-doc and permanent positions around lab instruments, I managed to refine a flexible, comprehensive methodology for data collection, correction and analysis which can be applied to many X-ray scattering investigations at the lab and at the synchrotron. With the help of friends at round places, this methodology was implemented and put into production, and has been delivering high-quality data since then. Now, we have almost all possible data corrections (for X-ray scattering) implemented, and are improving the hardware to deliver higher-quality metadata to enable the corrections to be performed to a higher accuracy.
Simultaneously, we have set up a mini-large facility at BAM with the MAUS, the Multi-scale Analyzer for Ultrafine Structures. The MAUS combines the freedom of a laboratory instrument, with the spectrum of users of a beamline: besides measuring our own samples, and performing our own machine and methodology developments, we have opened this instrument for collaboration with fellow scientists from within BAM and from external institutes and universities. Here, we provide a comprehensive support for these collaborations, guiding the user from concept to sample selection, to interpretation and analysis. In 2019, we have supported over 30 different projects this way, leading to seven co-authored publications involving the MAUS in that year alone. As the MAUS uses the latest iteration of our comprehensive measurement methodology, the data quality is unmatched by any other lab instrument, and fully traceable to boot.
The freedom of the laboratory allows for more proof-of-principle experimentation than what is possible at the synchrotron. Therefore, the MAUS provides a good first (and sometimes final) step towards many experimental materials science investigations, nicely complementing the capabilities of the synchrotron. If and when more flux is needed, the step to the synchrotron is now smaller than ever, in particular with the same method
X-ray generation
(2020)
The nuclear phase out in Germany will lead to a challenge finding skilled staff for all areas in nuclear business. Transport of spent fuel and high-level nuclear waste is an ongoing task over the next decades during the decommissioning of nuclear power plants and after the interim storage. The international regulations were adapted and address the issue of transports after storage now. The topic of aging and assessment of the development of the state-of-art technology are in focus. German research funds are supporting the investigations of future challenges of transport and storage of the nuclear heritage. BAM is involved and works on several topics related to the aging issue of packages. The behaviour of spent fuel claddings, long-term behaviour of metal and elastomeric gaskets and sensor/monitoring techniques of waste disposal are examples of research fields.
A possibility of deposition from laser-induced plasma (LIP) is investigated in search for an economic and simple method to obtain isotopic compounds from enriched gaseous precursors. A breakdown in mixtures of BCl3 and BCl3 with hydrogen, argon, and methane are studied both theoretically and experimentally. Calculations of expanding plasma of different composition are performed with the use of the fluid dynamic code coupled to the equilibrium chemistry solver. Condensed phases of boron, boron carbide, and graphite are predicted showing maximum concentrations in peripheral zones of the plasma.
In experiment LIP is induced in mixtures BCl3, Н2+BCl3, H2+Ar+BCl3, H2+BCl3+CH4, BF3, Н2+BF3, H2+Ar+BF3, and H2+Ar+BF3. The gases are analyzed before, during, and after laser irradiation by optical and mass spectroscopic methods. The composition of reaction products is found to be close to that predicted theoretically. The conversion of precursor gases BCl3 and BF3 into gaseous and condensed products is 100% for BCl3 and 80% for BF3. Solid deposits of up to 30 mg are obtained from all the reaction mixtures. FTIR analysis of BCl3+H2+CH4 deposits points to a presence of condensed boron and boron carbide that are also predicted by the model. Both calculations and preliminary experimental results suggest the chemical vapor deposition by LIP is promising for conversion of gaseous enriched precursors into elemental isotopes and their isotopic compounds.
The dark side of science
(2020)
Recorded at the Better with Scattering workshop 2020, this talk highlights the complete set of data correction steps that we do for the MAUS, and how they can be used elsewhere too. This links well with the talk in this series by Dr. Tim Snow, and also highlights the details of the background subtraction that needs to be done.
The SPONGE
(2020)
Introduction to SAXS
(2020)
DNA basierte Dosimetrie
(2020)
We propose the development of a standardized DNA based dosimeter. This dosimeter will improve the comparability between the results of different laboratories in radiation research. Compared to conventional methods in dosimetry, this Approach provides direct access to the relation between radiation interaction and biological damage. Moreover, it enables the systematic investigation of the relation between the microscopic characteristics of radiation and DNA damage over a wide dose range.
Da Feuchte insbesondere in Form von Flüssigwasser ein hohes Schadenspotential für Baustoffe und Konstruktionen darstellt, finden zerstörungsfreie Verfahren wie die Kernspinresonanz (NMR) zunehmend Einsatz im Bauwesen. Auch wenn zur qualitativen Lokalisierung möglicher Schad- und Risikostellen bereits zahlreiche zerstörungsfreie Verfahren in der Praxis Anwendung finden, so besteht beispielweise bei der Porenraumcharakterisierung und dem Verständnis von Feuchtetransportmechanismen weiterhin Forschungsbedarf. Eine besondere Herausforderung stellt in diesem Zusammenhang die (ortsaufgelöste) Erfassung und Quantifizierung von Feuchteverteilungen bei Teilsättigung dar.
Mittels 1H-NMR lassen sich der Wassergehalt sowie die Relaxationszeiten der Wasserstoffprotonen in Abhängigkeit von ihrer Bindungsart und der Porenumgebung messen. In vollgesättigten porösen Baustoffen kann somit das NMR-Signal als Porengrößenverteilung interpretiert werden. Da aber in der Praxis nur selten bis nie vollgesättigte Zustände vorliegen, befasst sich eine laufende Forschungsarbeit mit dem Verständnis der NMR-Signale teilgesättigter Porensysteme, die teilweise multimodale Porengrößenverteilungen aufweisen.
Im Rahmen dieser Arbeit werden insgesamt 19 Sandsteine aus Deutschland, Tschechien und Italien sowohl im voll- als auch im teilgesättigten Zustand mit NMR untersucht. Definierte teilgesättigte Zustände werden durch Aufsättigen der Proben in Exsikkatoren mit verschiedenen relativen Luftfeuchten (z. B. 33 %, 75 %, 96%) erzeugt. Die Regulierung der Luftfeuchten erfolgt mit Hilfe von gesättigten Salzlösungen. Als Ergebnis wird die Veränderung der Signalamplitude und der T2-Relaxationszeitenverteilungen in Abhängigkeit von dem Feuchtezustand näher betrachtet. Des Weiteren erfolgt die Berechnung des Flüssigwasseranteils bzw. der adsorbierten Wasserfilmdicke einzelner Poren aus der mit Quecksilberporosimetrie bestimmten Porengrößenverteilung und der Annahme einer Porengeometrie (z.B. Schlitz-, Zylinderpore, etc.). Am Ende dieser Arbeit soll der Zusammenhang des NMR-Signals (Amplitude und Relaxationszeiten) mit dem Porensättigungsgrad in einem Porensystem mit multimodaler Porengrößenverteilung bei Teilsättigung aufgezeigt werden.
Multivariate Auswertung von Radarsignalen zur Bestimmung typischer Feuchteschäden in Fußböden
(2020)
Leitungswasserschäden nahmen im Jahr 2018 mit rund 2,9 Milliarden Euro den größten Posten bei Gebäudeversicherungen ein und verursachten damit mehr Kosten, als Elementar-, Feuer, Sturm- und Hagelschäden zusammen. Neutronensonden helfen hier bereits bei der horizontalen Eingrenzung eines Feuchteschadens, wobei die vertikale Unterscheidung betroffener Schichten nur durch die zerstörende Entnahme von Bohrkernen vorgenommen werden kann. Der parallele Einsatz des Radarverfahrens soll hier mit seiner hohen Sensitivität für Wasser künftig zu einem erhöhten Informationsgehalt beitragen und eine kostengünstigere Schadensdiagnose und Planung der Reparaturmaßnahmen ermöglichen.
In einem laufenden Forschungsvorhaben werden in systematischen Laborstudien gängige Schadensfälle an häufig anzutreffenden Fußbodenaufbauten simuliert und deren Einfluss auf das Radarverfahren untersucht. Die Bewertung der Schadensträchtigkeit zugeführter Wassermengen erfolgt mithilfe von Luftfeuchtesensoren, welche in der Dämmebene platziert sind. Beim Aufbau der Fußbodenstrukturen kommen Zement- und Anhydritestriche, sowie die Dämmmaterialen Styropor, Styrodur, Glaswolle und Perlite-Schüttung mit variierenden Schichtdicken zum Einsatz. Die Robustheit der zu entwickelnden Messmethode gegenüber derartig verschiedenen und in der Praxis häufig unbekannten Schichtstrukturen stellt eine besondere Herausforderung dar und soll durch den Einsatz multivariater Datenauswertung erhöht werden. Diesbezüglich empfehlen bisherige Ergebnisse die Betrachtung der örtlichen Verteilungen qualitativer Signalmerkmale wie Amplituden, Laufzeiten und Frequenzen im Radargramm (B-Scan). Deren Eignung für reale Schadensfälle außerhalb der Laborumgebung wird hierbei stets kritisch hinterfragt und soll weiterführend an Praxiseinsätzen validiert werden.
In contrast to the crisp, clear images you can get from electron microscopy, small-angle X-ray scattering (SAXS) patterns are rather featureless. These patterns, however, contain averaged structural information of all of the finest material structures that were illuminated by the X-ray beam. With careful and precise investigation, and supplementary information from complementary techniques, this bulk material structure can be quantified to reveal structural information spanning four or even five decades in size. Additionally, while the data correction and analysis is complex, sample preparation is very straightforward, also allowing for in-situ and operando measurements to be performed without breaking a sweat. In the right hands, then, this technique can be the most powerful tool in your analytical arsenal.