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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.