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The present work deals with the recently confirmed widening of the weld pool interface, known as a bulging effect, and its relevance in high power laser beam welding. A combined experimental and numerical approach is utilized to study the influence of the bulge on the hot cracking formation and the transport of alloying elements in the molten pool. A technique using a quartz glass, a direct-diode laser illumination, a high-speed camera, and two thermal imaging cameras is applied to visualize the weld pool geometry in the longitudinal section. The study examines the relevance of the bulging effect on both, partial and complete penetration, as well as for different sheet thicknesses ranging from 8 mm to 25 mm. The numerical analysis shows that the formation of a bulge region is highly dependent on the penetration depth and occurs above 10 mm penetration depth. The location of the bulge correlates strongly with the cracking location. The obtained experimental and numerical results reveal that the bulging effect increases the hot cracking susceptibility and limits the transfer of alloying elements from the top of the weld pool to the weld root.
Ultrashort PFAS (≤ 3 carbon atoms) were overlooked for a long time in analytical monitoring. Beside through the use of these substances, they contribute to the PFAS background in the environment through (environmental/ bio-) degradation and incomplete destruction3 of PFAS with longer carbon chains or other fluorinated compounds. As part of the German-Israeli Cooperation in Water Technology Research project „Detection, quantification, and treatment of per- and polyfluoroalkyl substances in groundwater“ (DEFEAT-PFAS), we are developing an as simple as possible direct headspace (HS-)GC-MS method to detect trifluoroacetic acid (TFA) and perfluoropropanioc acid (PFPrA), as well as trifluoroethanol (TFEtOH), pentafluoropropanol(PFPrOH) and hexafluoroiospropanol (HFIP) in water samples. Here we present the results of the PFAS mentioned in spiked ultrapure water solutions.
Per- and polyfluoroalkyl substances (PFAS) have been extensively utilized in various industrial processes, resulting in elevated concentrations in landfills and drinking water reservoirs. Despite recognizing that shortchained
PFAS are harmful, they are often overlooked. Short-chain PFAS are more challenging to remove via adsorption and membrane separation processes, and their detection is complex, thus creating a critical gap in understanding their environmental impact. To improve their environmental monitoring, we aim to improve short-chain PFAS adsorption and electro-sorption on novel carbon-based adsorbers such as pristine and functionalized multi-walled carbon nanotubes (MWCNTs) and assess their adsorption mechanisms. Based on the obtained result, we aim to develop a PFAS passive sampling device.
Detection, Quantification and Treatment of Per and Polyfluoroalkyl substances (PFAS) in Groundwater
(2024)
The research project focuses on tackling the detection, measurement, and elimination of per- and polyfluoroalkyl substances (PFAS) from polluted groundwater, with a particular emphasis on addressing short (C4-C7) and ultrashort (C1-C3) chain PFAS. Given the widespread use of PFAS in various products, they are commonly found in groundwater near industrial and military sites in Germany and Israel. Moreover, recent regulations limiting the use of long chain PFAS have led industries to shift towards shorter chain alternatives. Hence, our efforts are geared towards refining detection, quantification, and removal methods for short and ultrashort chain PFAS. In terms of detection, ww are developing passive sampling devices capable of collecting and tracking the temporal distribution of PFAS species in groundwater. This will enable us to analyze contaminations in German and Israeli groundwater using cutting-edge analytical techniques. Additionally, contaminated groundwater will undergo a two-stage treatment process aimed at concentrating the relatively low PFAS concentrations using innovative membrane technologies such as closed-circuit reverse osmosis and mixed matrix composite nanofiltration membrane adsorbers. Subsequently, the streams containing higher PFAS concentrations will be treated through coagulation, with the remaining PFAS being adsorbed onto carbonaceous nanomaterials. The outcome of this research will include the creation of advanced tools for detecting, measuring, and eliminating PFAS from polluted groundwater, while also enhancing our understanding of the scope of these contaminations.
Hydrogen will be one of the most important energy carriers of tomorrow. For the necessary large-scale and long-distance transportation, a reliable pipeline infrastructure is required. It is meanwhile in the most countries accepted to follow a two-way strategy by (I) repurposing the existing natural gas (NG) grid combined with (II) the installation of new pipelines. For example, in Europe a so-called European Hydrogen Backbone (EHB) is planned for 2040. Currently, 28 countries work together to establish a hydrogen pipeline grid of several thousands of kilometers. In that connection, a wide number of materials are used with different thicknesses, strength levels, chemical composition, surface conditions and so on. Worldwide research projects suggest the general compatibility of the currently applied pipeline steels e.g., in Germany the “SysWestH2” project. Nonetheless, the hydrogen gas grid will require regular inspections, repair, and maintenance. In addition, sometimes pipeline tees are required to connect new grids or pipelines the existing infrastructure. From that point of view, existing concepts from NG-grids must be investigated in terms of the transferability to hydrogen service. An overview on occurring challenges for this hydrogen transition, especially for in-service weld repair procedures is given in this presentation.
In order to protect natural gypsum deposits and to compensate for the decreasing amount of Flue Gas Desulfurization (FGD) gypsum it is necessary to develop and explore new sources of gypsum. For this purpose, the potentials of different gypsum wastes are investigated in the study “GipsRec 2.0”, funded by the Federal Ministry of Education and Research (Germany).
On the one hand, the project worked on a new processing technology for gypsum fiberboards (GFB). While the recycling of gypsum plasterboards has already been carried out on an industrial scale for several years, the recycling of gypsum fiberboards (GFB) has proven to be challenging. Gypsum fiberboards from demolition sites and offcuts from GFB production were used for these investigations. The tests were conducted on a technical scale. Furthermore, various synthetic gypsums are being investigated with regard to their suitability for gypsum production. The analyses are carried out on production residues.
In this project, a promising process for gypsum fiberboard recycling could be developed, as well as other waste gypsums are investigated and evaluated with regard to their potential as secondary raw material. In addition, selected process routes are assessed for their environmental impact using a life cycle assessment (LCA) approach.
Brittle Failure Limits of Spent Fuel Claddings Subjected to Long-Term Dry Interim Storage Conditions
(2024)
The mechanical properties of spent fuel claddings can be adversely affected under the conditions of long-term dry interim storage, so that the failure limits may be reached in case of mechanical loads during handling or transport after storage. Pre-storage drying and the early stage of interim storage can expose the cladding to higher temperatures and higher tensile hoop stresses than those associated with in-reactor operation and pool storage. During slow cooling of a cladding tube under internal pressure, radial hydrides may precipitate in zirconium-based cladding alloys. This can lead to embrittlement of the material and sudden failure of the cladding integrity under mechanical stress. In order to prevent brittle failure, numerical methods are being developed to predict the mechanical behaviour and identify limiting conditions. Experimental investigations, numerical analyses and evaluation methods are discussed.
An established experimental method for characterising cladding materials is the Ring Compression Test (RCT). Some test results on irradiated cladding tubes after operation in pressure water reactors are publicly available. However, it is helpful to carry out studies on unirradiated surrogate claddings with similar material properties to reduce the effort associated with irradiated samples in hot cells and to perform material tests with a wider range of parameters. On the basis of such experimental data, load-displacement curves have been numerically analysed for a selection of cladding materials.
Radial hydrides can cause a sample to break suddenly due to fracture even at low deformation. Noticeable load drops in the RCT are caused by unstable crack propagation through the radial hydride network. The failure mechanism is quasi-cleavage in the hydrides and micro-void nucleation, growth, and coalescence in the zirconium matrix, with ductile tearing patches connecting adjacent hydrides. The cohesive zone approach was used to simulate the failure process taking into account the radial hydride morphology.
The developed method can adequately describe both the deformation and failure behaviour of irradiated as well as unirradiated claddings of zirconium-based alloys with radial hydrides under RCT conditions. Limiting conditions can be expressed in terms of fracture energy and cohesive strength.
We present a distributed polymer optical fiber sensor system for deformation monitoring of geotechnical infrastructure. The sensor system is based on the digital incoherent optical frequency domain reflectometry (I-OFDR) for the detection of local strain events along a perfluorinated polymer optical fiber (PF-POF) used as a sensing fiber. For the best possible load transfer, the PF-POFs were integrated onto geosynthetics which pose a sensor carrier for the sensing fiber. By using elastic PF-POF instead of a standard glass fiber as a sensing fiber the strain range of geosynthetics-integrated fiber optic sensors could be extended up to 10 % in accordance with the end-user requirements.
Diese Präsentation stellt die gegenwärtige Situation zur Einstufung von primer caps (Anzündhütchen) gemäß Richtlinie 2014/28/EU und UN Model Regulations Rev.23 (Volume I) dar. Spezifische Eigenschaften und Gefährdungen werden dargestellt und eine Abgrenzung zur Richtlinie 2013/29/EU aufgezeigt.
Gips gehört zu den nachgefragtesten Baustoffen und entsprechend steigt der Gipsverbrauch weltweit schon seit Jahrzehnten an. In Deutschland wird der Gipsbedarf seit vielen Jahren zu einem guten Teil durch REA-Gips, einem Nebenprodukt aus der Abgasreinigung von Kohlekraftwerken, gedeckt. Die weitere Gipsversorgung erfolgt größtenteils durch die Nutzung natürlicher Gipsvorkommen. Ein geringer, aber steigender Anteil an RC-Gips aus dem Baustoffrecycling und die Nutzung synthetischer Gipse aus Nebenprodukten anderer Industriezweige sind ebenfalls zu verzeichnen. Aufgrund der nationalen Klimaschutzziele und der damit verbundenen Abschaltung von Kohlekraftwerken wird das REA-Gipsangebot in den nächsten Jahren jedoch weiter deutlich zurückgehen, so dass andere Gipsquellen erschlossen werden müssen.
Abhängig von der Lebensdauer der verwendeten Gipsprodukte im Bausektor ist infolge des in den vergangenen Jahren erfolgten Anstiegs des Gipsverbrauchs auch mit einer Zunahme von Gipsresten in Bau- und Abbruchabfällen zu rechnen. Im Hinblick auf eine bevorstehende Verknappung von Gips wird die Rückgewinnung dieser Gipse aus Bau- und Abbruchabfällen immer wichtiger. Das Recycling von Gipskartonplatten ist mittlerweile eine etablierte Technik und wird bereits seit einigen Jahren in industriellem Maßstab durchgeführt. Außerdem werden neue Verfahren zur Wiederverwertung weiterer Gipsprodukte aus Rück- und Umbaumaßnahmen untersucht. Von besonderem Interesse sind verschiedene Arten von Gipsplatten, da sie gut für selektiven Rückbau geeignet sind. Daher können sie vergleichsweise frei von Verunreinigungen oder Störstoffen zurückgewonnen werden, was für das Gipsrecycling besonders wichtig ist.
In dem vom Bundesministerium für Bildung und Forschung geförderten Forschungsprojekt "GipsRec 2.0" werden technische, wirtschaftliche und ökologische Aspekte des Recyclings von Gipsfaserplatten sowie von verschiedenen Synthesegipsen untersucht und bewertet. Die Aufbereitung von Gipsfaserplatten erfolgte im halbtechnischen Maßstab, an verschiedenen potentiellen Ausgangsstoffen für synthetische Gipse wurden Laborversuche durchgeführt. Erfolgversprechende Verfahrenswege werden ökobilanziell bewertet. Ziel dieser Arbeiten ist die Erschließung der Sekundärrohstoffpotenziale von weiteren Quellen für die RC-Gipsproduktion um mit einer Steigerung des Gipsrecyclings die in naher Zukunft durch die Reduktion der REA-Gips-Bereitstellung entstehende Lücke in der Rohstoffversorgung zu verringern.
Distributed fiber optic strain sensing for structural health monitoring of 70 MPa hydrogen vessels
(2024)
We report on the development and testing of 70 MPa hydrogen pressure
vessels with integrated fiber optic sensing fibers for automotive use. The paper deals with the condition monitoring of such composite pressure vessels (CPVs) using the optical backscatter reflectometry (OBR) applied for a distributed fiber optic strain sensing along fully integrated polyimide-coated single-mode glass optical fiber (SM-GOF). The sensing fibers were embedded into the vessel structure by wrapping them over the polymer liner during the manufacturing process of the carbon fiber reinforced polymer (CFRP). Detecting local strain events by the integrated fiber optic sensors can be an opportunity for monitoring the material degradation of CPVs under static and cyclic loading.
Low Transformation Temperature (LTT)-Schweißzusätze sind ein innovativer Ansatz, um Eigenspannungen in Schweißnähten zu reduzieren. Dieser Vortrag behandelt neben den Einfluss der LTT-Schweißzusätze auch deren Naht-Ausführungen. Die unterschiedlichen LTT-Nahtgeometrien haben einen signifikanten Einfluss auf den Eigenspannungsabbau in der Schweißnaht und der Wärmeeinflusszone (WEZ).
Surface-modification platforms that are universally applicable are vital for the development of new materials, surfaces, and nanoparticles. Mussel-inspired materials (MIMs) are widely used in various fields because of their strong adhesive properties and post-functionalization reactivity. However, conventional MIM coating techniques have limited deposition selectivity and lack structural control, which has limited their use in microdevices that require full control over deposition. To overcome these limitations, we developed a micropatterning technique for MIMs using multiphoton lithography, which does not require photomasks, stamps, or multistep procedures. This method enables the creation of MIM patterns with micrometer resolution and full design freedom and paves the way for innovative applications of MIMs in various multifunctional systems and microdevices, such as microsensors, MEMS, and microfluidics.
Low transformation temperature (LTT) welding consumables offer an innovative approach to increase the fatigue strength of welded high-strength steel structures. LTT welding consumables are characterized by a martensitic phase transformation near ambient temperature, which generates compressive residual stresses in the weld and heat affected zone (HAZ). The aim is to achieve a weld geometry, which generate high compressive residual stresses at the fatigue crack critical weld toe.
Longitudinal stiffeners were gas metal arc welded using a conventional welding consumable; the base material was a high strength steel S700M. A chromium-nickel alloyed LTT consumable was deposit subsequently just on front sides of the stiffeners. Different welding parameters led to varying cross sections of the weld. The residual stresses were determined using X-ray diffraction (XRD) in the crack critical HAZ.
When using only the conventional, the HAZ is characterized by high tensile residual stresses. The additional application of the LTT alloy leads to a significant reduction of the tensile residual stresses. Depending on the weld geometry, even compressive residual stresses can be observed at the weld toe
The thermal history during additive manufacturing of complex components differs significantly from the thermal history of geometrically primitive test specimens. This can result in differences in properties that can lead to different material behavior. In this talk, the concept of representative test specimens is introduced, which enables the transfer of thermal histories from complex geometries to simple geometries, which can lead to better comparability of material properties.
Laser Powder Bed Fusion (PBF-LB/M) of AISI 316L stainless steel has gained popularity due to its exceptional capacity to produce complex geometries and hierarchical microstructures, which can increase the yield strength while maintaining good ductility. Nevertheless, owing to high thermal gradients encountered during the process, the as printed 316L stainless steel often exhibit microstructural heterogeneities and residual stresses, which can limit its performance in demanding environments. Hence, employing heat treatments which balance the reduction of residual stresses while retaining improved static strength may be beneficial in various scenarios and applications. This study investigates the impact of post-processing heat treatments on the microstructure of 316L stainless steel manufactured via PBF-LB/M, along with its correlation with micro-hardness properties. To this end, 6 different heat treatments, i.e., 450 °C for 4h, 700 °C for 1h, 700 °C for 3h, 800 °C for 1h, 800 °C for 3h, and 900 °C for 1h, were applied to different specimens and Vickers hardness measurements (HV1) were performed in all states. At 800 °C, although the cellular structure appears to be retained, there is an observable increase in cellular size. However, while treatments exceeding 900 °C indicate no significant grain growth compared to other conditions, the cellular structure is entirely dissolved, which leads to a reduced Vickers hardness. The effect of the heat treatments on other microstructural features such as grain size and morphology, melt pool boundaries (MPB), crystallographic texture, chemical segregation, dispersoids and phase stability are also discussed in the present work
This study provides insights into the properties of 316L stainless steel produced by additive manufacturing using fused filament fabrication (FFF). One key finding is particularly noteworthy: in significant contrast to cold-rolled 316L, FFF316L develops a pronounced martensite phase after fabrication. The comprehensive comparative analysis shows that FFF316L not only retains the ferrite volume content, but that this is also significantly influenced by the build-up direction. Despite the sintering process, which typically involves densification of the material, a pore volume fraction of 8.45 % remains, which influences the mechanical properties. Although FFF316L has lower elastic
modulus and tensile strength values compared to cold-rolled 316L, its ductility is still competitive. The study further reveals that deformation-induced martensite forms at the intersections of the deformation twins and ferrite islands form at the grain boundaries during the compression and sintering phases. These findings highlight the challenges associated with FFF316L in specific application fields and signal the need to continue to carefully evaluate and improve the development of manufacturing technologies.
The general term additive manufacturing (AM) encompasses processes that enable the production of parts in a single manufacturing step. Among these, laser powder bed fusion (PBF-LB) is one of the most commonly used to produce metal components. In essence, a laser locally melts powder particles in a powder bed layer-by-layer to incrementally build a part. As a result, this process offers immense manufacturing flexibility and superior geometric design capabilities compared to conventional processes. However, these advantages come at a cost: the localized processing inevitably induces large thermal gradients, resulting in the formation of large thermal stress during manufacturing. In the best case, residual stress remains in the final parts produced as a footprint of this thermal stress. Since residual stress is well known to exacerbate the structural integrity of components, their assessment is important in two respects. First, to optimize process parameter to minimize residual stress magnitudes. Second, to study their effect on the structural integrity of components (e.g., validation of numerical models). Therefore, a reliable experimental assessment of residual stress is an important factor for the successful application of PBF-LB. In this context, diffraction-based techniques allow the non-destructive characterization of the residual stress. In essence, lattice strain is calculated from interplanar distances by application of Braggs law. From the known lattice strain, macroscopic stress can be determined using Hooke’s law. To allow the accurate assessment of the residual stress distribution by such methods, a couple of challenges in regard of the characteristic PBF-LB microstructures need to be overcome.
This presentation highlights some of the challenges regarding the accurate assessment of residual stress in PBF-LB on the example of the Nickel-based alloy Inconel 718. The most significant influencing factors are the use of the correct diffraction elastic constants, the choice of the stress-free reference, and the consideration of the crystallographic texture. Further, it is shown that laboratory X-ray diffraction methods characterizing residual stress at the surface are biased by the inherent surface roughness. Overall, the impact of the characteristic microstructure is most significant for the selection of the correct diffraction elastic constants. In view of the localized melting and solidification, no significant gradients of the stress-free reference are observed, even though the cell-like solidification sub-structure is known to be heterogeneous on the micro-scale.
Unter Passivität versteht man den Korrosionsschutz durch dünne, festhaftende Schichten aus Korrosionsprodukten. Für den schadensfreien Einsatz nichtrostender Stähle ergeben sich daraus zwei grundsätzliche Anforderungen.
Erstens muss sich die Passivschicht vollständig ausbilden können. Dabei sind die Oberflächenausführung, die mechanische Bearbeitung, die Elementverteilung, Ausscheidungen, die Wärmeeinbringung z.B. bei der schweißtechnischen Verarbeitung, Anlauffarben, sowie die chemische Nachbehandlung bzw. Konditionierung der Oberflächen von großer Bedeutung. Zweitens muss die Repassivierung von Defektstellen unter den Einsatzbedingungen möglich sein. Für das Repassivierungsvermögen sind die Legierungszusammensetzung, mögliche kritische Betriebszustände, prozessbedingte Besonderheiten, wie etwa Stagnationsbedingungen und Reinigungsprozesse von Bedeutung.
The damage mechanisms of metallic components produced by process laser powder bed fusion differ significantly from those typically observed in conventionally manufactured variants of the same alloy. This is due to the unique microstructures of additively manufactured materials. Herein, the focus is on the study of the evolution of creep damage in stainless steel 316L specimens produced by laser powder bed fusion. X-ray computed tomography is used to unravel the influence of the process-specific microstructure from the influence of the initial void distribution on creep damage mechanisms. The void distribution of two specimens tested at 600 °C and 650 °C is analyzed before a creep test, after an interruption, and after fracture. The results indicate that the formation of damage is not connected to the initial void distribution. Instead, damage accumulation at grain boundaries resulting from intergranular cracking is observed.
Laser powder bed fusion (PBF-LB/M) of metallic alloys is a layer-wise additive manufacturing process that provides significant scope for more efficient designs of components, benefiting performance and weight, leading to efficiency improvements for various sectors of industry. However, to benefit from these design freedoms, knowledge of the high produced induced residual stress and mechanical property anisotropy associated with the unique microstructures is critical. X-ray and neutron diffraction are considered the benchmark for non-destructive characterization of surface and bulk internal residual stress. The latter, characterized by the high penetration power in most engineering alloys, allows for the use of a diffraction angle close to 90° enabling a near cubic sampling volume to be specified. However, the complex microstructures of columnar growth with inherent crystallographic texture typically produced during PBF-LB/M of metallics present significant challenges to the assumptions typically required for time efficient determination of residual stress. These challenges include the selection of an appropriate set of diffraction elastic constants and a representative lattice plane suitable for residual stress analysis. In this contribution, the selection of a suitable lattice plane family for residual stress analysis is explored. Furthermore, the determination of an appropriate set of diffraction and single-crystal elastic constants depending on the underlying microstructure is addressed.
In-situ loading experiments have been performed at the Swiss Spallation Neutron Source with the main scope to study the deformation behaviour of laser powder bed fused Inconel 718. Cylindrical tensile bars have been subjected to an increasing mechanical load. At pre-defined steps, neutron diffraction data has been collected. After reaching the yield limit, unloads have been performed to study the accumulation of intergranular strain among various lattice plane families.
The presentation is divided in two parts. In the first part the significance of mechanical impacts as ignition source for hydrogen containing atmospheres is shown and recent results of a research project evaluating ignition probabilities under different conditions is presented. In the second part future challenges in the field of hydrogen safety are discussed. Finally, the German National Hydrogen Safety Alliance is introduced.
Die Einstufung von Hausmüllverbrennungsasche (HMVA) als gefährlich oder nicht gefährlich nach der Gefahreneigenschaft HP14 (ökotoxisch) ist nach wie vor umstritten, da es noch keine allgemein anerkannten Methoden zur Bewertung gibt. Wenn die Berechnungsregeln angewendet werden sollen angewendet werden sollen, sind Kenntnisse über die chemische Zusammensetzung von HMVA erforderlich. Informationen über die chemische Zusammensetzung von HMVA können mit einem Ansatz gewonnen werden, der auf der Gruppierung von Substanzen. Für HMVA können vier Stoffgruppen definiert werden: 1. elementare und legierte Metalle, 2. leicht wasserlösliche Stoffe, 3. schwer lösliche Stoffe und 4. Stoffe mit starken chemischen Bindungen. Elementares und legiertes Cu und Zn sind in der HMVA vorhanden und werden in der Regel als Nichteisenmetallfraktion zurückgewonnen, zumindest die größeren Partikel. Zn-Partikel, die kleiner als 1 mm sind, werden als H410 eingestuft, feine Partikel von Cu nur als H411. Die wasserlösliche Fraktion kann mit Standardauslaugungsmethoden quantifiziert werden Auslaugungsmethoden quantifiziert werden, z. B. bei einem Flüssigkeits-Feststoff-Verhältnis (L/S) von 2 oder 10 l/kg. Sowohl die Sulfate von Zn als auch von Cu gehören zu dieser Gruppe. In einer neueren Veröffentlichung wurde gezeigt, dass bei den oben genannten Metalle die ausgelaugte Menge weit unter dem Grenzwert von 1.000 mg/kg liegt, selbst wenn stöchiometrische Faktoren angewendet werden. Stoffgruppe 3 sind potenzielle H410-Stoffe. Dabei handelt es sich um Carbonate, Hydroxide und Oxide der betreffenden Elemente, die löslich sind in schwachen organischen Säuren wie Essigsäure löslich sind. Die Worst-Case-Stoffe der Gruppe 3, d. h. die Verbindungen mit den höchsten stöchiometrischen Faktoren, sind CuCO3xCu(OH)2 und ZnO. Stoffe mit starken chemischen Bindungen wie Silikate oder Sulfide sind nur löslich in starken Säuren (z.B. Königswasser) löslich und haben keinen Ökotoxizitäts-Gefahrencode. Das Mobilisierungsverhalten der relevanten Schwermetalle und damit der Gruppe der schwer schwerlöslichen Verbindungen kann mit der 4-stufigen sequenziellen Extraktion untersucht werden. Für die HP14 Einstufung könnte auch eine einstufige Extraktion ausreichend sein. Nur die Elemente Zn und Cu sind für die HP14-Einstufung der HMVA von Bedeutung, da die Feststoffgehalte aller anderen Schwermetalle unterhalb des Feststoffgehalte aller anderen Schwermetalle unter der Cut-Off-Grenze von 0,1 % liegen, selbst wenn man sie in chemischen Verbindungen mit stöchiometrischen Faktoren. Im Ergebnis wurde gezeigt, dass HMVA in der Regel als nicht gefährlich einzustufen ist.
Hydrogen pressure vessels are among the most essential components for reliable hydrogen technology. Under current regulations, a mostly conservative strategy is employed, restricting the usage time of hydrogen pressure vessels without providing information on the real remaining lifetime. During the service life, pressure vessels are inspected periodically. However, no established method that can provide continuous monitoring or information on the remaining safe service life of the vessel. In this paper, we propose a sensor network for Structural Health Monitoring (SHM) of hydrogen pressure vessels where data from all sensors are collected and centrally evaluated. Specifically, we integrate three different SHM sensing technologies namely Guided Wave ultrasonics (GW), Acoustic Emission testing (AT), and distributed Fiber Optic Sensing (FOS). This integrated approach offers significantly more information and could therefore enable a transition from costly and time-consuming periodic inspections to more efficient and modern predictive maintenance strategies, including Artificial Intelligence (AI)-based evaluation. This does not only have a positive effect on the operational costs but enhances safety through early identification of critical conditions in the overall system in real-time. We demonstrate an experimental set-up of a lifetime test where a Type IV Composite Overwrapped Pressure Vessel (COPV) is investigated under cyclic loading instrumented with AT, FOS, and GW methods. We acquired data from the sensor network until the pressure vessel failed due to material degradation. The data collected using the three different SHM sensor technologies is planned to be evaluated individually, using data fusion, and AI. In the future, we aim to integrate the measurement setup into a hydrogen refueling station with the data stream implemented into a digital signal processing chain and a digital twin.
Metallbasierte additive Fertigungsverfahren werden zunehmend industriell zur Anfertigung von komplex geformten Komponenten eingesetzt. In diesem Zusammenhang ist das Laser-Pulverbettschweißen von Metall (PBF-LB/M) ist ein weitläufig genutztes Verfahren. Im PBF-LB/M-Prozess werden lagenweise aufgetragene Metallpulverschichten selektiv mittels eines Lasers aufgeschmolzen. Die Entstehung von internen Fehlstellen (bspw. Porosität, Lunker oder Risse) während des Fertigungsvorgangs stellt ein ernstzunehmendes Risiko für die Bauteilsicherheit und somit für die weitere industrielle Etablierung des Verfahrens dar. Die Entstehung von Fehlstellen hängt eng mit lokalen Änderungen der thermischen Historie des Bauteils zusammen. Mit Hilfe von thermografischen Kameras zur Prozessüberwachung kann die thermische Historie bereits während der Fertigung erfasst werden. Damit eröffnet sich die Möglichkeit, die Entstehung von Fehlstellen anhand der thermografischen Daten vorherzusagen und somit potenziell Kosten für eine nachgelagerte Qualitätssicherung einzusparen.
In diesem Beitrag soll die Modellierung der Fehlstellenvorhersage anhand thermografischer Prozessdaten diskutiert werden. Hierbei liegt ein Schwerpunkt auf der Fragestellung, mit welcher Genauigkeit unterschiedliche Formen von Fehlstellen, im speziellen Anbindungsfehler und Keyhole-Porosität, auf lokaler Bauteilebene vorhergesagt werden können. Weiterhin werden verschiedenen Modelltypen aus dem Bereich des Maschinellen Lernens auf ihre Eignung für die Fehlstellenvorhersage verglichen. Ein weiterer zentraler Aspekt in diesem Zusammenhang ist die Untersuchung der Eingangsdaten des Modells auf ihre Relevanz für das Vorhersageergebnis.
Als Datengrundlage für die durchgeführten Untersuchungen dienen die Fertigungsprozesse von zwei identischen Haynes-282-Bauteilen (Nickel-Basislegierung), welche mit Hilfe einer im kurzwelligen Infrarotbereich arbeitenden Thermografiekamera überwacht wurden. Das Bauteildesign umfasste lokale Bereiche, in denen mit Hilfe einer Parametervariation die Entstehung von Fehlstellen forciert wurde. Um die Position und Größe der entstandenen Defekte zu quantifizieren, wurden beide Bauteile nach erfolgter Fertigung mittels Computertomografie (CT) geprüft. Im Rahmen der Datenvorbereitung für die Modellierung erfolgte eine Reduzierung der erhobenen Thermogramme zu physikalisch-interpretierbaren Merkmalen (bspw. Schmelzbadfläche oder Zeit-über-Schwellwert). Weiterhin erfolgte eine Registrierung der thermografischen Daten mit den Fehlstellen-Referenzdaten der CT, um eine exakte örtliche Überlagerung von thermischer Information und lokalem Fehlstellenbild zu erzielen. Zur Ermöglichung einer lokalen Fehlstellenvorhersage wurden die thermografischen Daten schichtweise in kleinteiligen Volumina angeordnet, welche als Eingangsgröße für die genutzten ML-Algorithmen dienten.
Die Ergebnisse der Untersuchungen zeigen, dass sich die Porosität auf Bauteilschichtebene mit einer hohen Genauigkeit vorhersagen lässt. Eine Vorhersage der Porosität auf lokaler Bauteilebene erweist sich noch als herausfordernd. Die erprobten ML-Algorithmen zeigen vergleichbare Ergebnisse, obwohl ihnen unterschiedliche Modellierungsannahmen zugrunde liegen und sie variierende Komplexität aufweisen. Mit Hilfe der erzielten Erkenntnisse eröffnet sich die Möglichkeit, Rückschlüsse auf die gewählte Prozessüberwachungshardware und Datenvorverarbeitung zu ziehen und somit langfristig die Leistungsfähigkeit von Modellen zur Fehlstellenvorhersage zu verbessern.
Structural health monitoring of hydrogen pressure vessels using distributed fiber optic sensing
(2024)
We report on distributed fiber optic sensing-based monitoring of hydrogen composite overwrapped pressure vessels (COPV) to simultaneously increase the operational lifespan and mitigate maintenance costs. Our approach represents, to the best of our knowledge, the first application of distributed fiber optic sensing for COPV Type IV monitoring, where the sensing fibers are attached to the surface, rather than integrated into the composite material. Specifically, we attach an optical fiber of 50 m to the pressure vessel's surface, covering both the cylindrical and dome sections. We note that our fiber optic sensing technique relies on swept wavelength interferometry providing strain information along the entire length of the optical fiber with high spatial resolution even at the millimeter scale. When the vessel is pressurized, the sensing optical fiber shows a linear strain response to pressure at every position along the fiber. After thousands of load cycles, the vessel finally fails with the optical fiber detecting and precisely localizing the damage in the vessel’s blind dome area. Furthermore, we discuss the potential of state-of-the-art signal processing methods and machine learning for advancing predictive maintenance. This could reduce the number of regular inspections, mitigate premature maintenance costs, and simultaneously increase the vessel’s remaining safe service life. We believe that the structural health monitoring of hydrogen pressure vessels with fiber optic sensors can enhance trust in hydrogen technology contributing to the energy transition in the future.
Die thermische Historie beim additiven Aufbau von komplexen Realkomponenten und geometrisch primitiven Prüfkörpern unterscheidet sich signifikant. Daraus können Eigenschaftsunterschiede resultieren, die zu unterschiedlichem Materialverhalten führen können. In diesem Vortrag wird das Konzept repräsentativer Probekörper eingeführt, das eine Übertragung thermischer Historien von komplexen Geometrien auf einfache Geometrien ermöglicht und hierdurch zu einer besseren Vergleichbarkeit der Werkstoffeigenschaften führen soll.
Compound semiconductors (CS) are promising materials for the development of high-power electrical applications. They have low losses, can withstand high temperatures and can operate at very high voltages and currents. This makes them a key technology for the electrification of many high energy applications, especially electromobility and HVDC power lines.
The challenge with CS technology is that most of the process technology has to be developed anew to the high standards required by electronic applications. Today, compound semiconductors can be produced in thin layers on top of substrates fabricated from classical crystal growth processes that are already well established. A promising method for this is metal organic vapour phase epitaxy (MOVPE). With this method, many different compounds with semiconducting properties can be synthesized. Additionally, this process technology is a direct thin layer deposition method. Therefore, complex multilayer systems can be generated directly by the deposition process and without the need of doping after growing.
There are a number of critical defects that can originate from the deposition process of these thin film devices. Within this project, we intend to develop new correlative imaging and analysis techniques to determine defect types, to quantify defect size and number density, as well as to characterise defects for process optimisation.
We report here on the use of spectroscopic ellipsometry and imaging ellipsometry to investigate defects in several different compound semiconductor materials used in high-power electronic devices. The materials we investigated are β-Ga2O3, SiC, GaN, AlN, and AlGaN materials as well as oxidised SiC surfaces. All of these materials have their typical defects and require optimised measurement and analysis schemes for reliable detection and analysis. Spectroscopic ellipsometry is a highly sensitive method for determining the thicknesses and dielectric function of thin layers, yielding potentially a high number of microscopic properties. The combined method between ellipsometry and optical microscopy is called imaging ellipsometry and is especially powerful for the large amount of data it produces. We have analysed defects in SiC- and AlN-based thin film semiconductors as well as characterised the properties of different types of SiO2 layers created on top of SiC monocrystals. We developed ellipsometric models for the data analysis of the different semiconductor materials.
If the defects have geometric features, it is useful to combine the ellipsometric analysis with topometry method like interference microscopy and scanning probe microscopy. We have successfully characterised function-critical defects in MOVPE SiC layers and correlated the findings with topography from WLIM measurements. We have developed an imaging ellipsometric measurement methodology that allows to estimate the relative defect area on a surface by a statistical raw data analysis.
Compound semiconductors (CS) are promising materials for the development of high-power electrical applications. They have low losses, can withstand high temperatures and can operate at very high voltages and currents. This makes them a key technology for the electrification of many high energy applications, especially electromobility and HVDC power lines.
The challenge is that most of the process technology has to be developed specifically and tailored to the high standards required by electronic applications. Today, many different CS materials can be produced in thin layers on top of substrates fabricated from classical crystal growth processes that are already well established. A promising method for this is metal organic vapour phase epitaxy (MOVPE). This technology is a direct thin layer deposition method capable of producing complex multilayer systems directly from one deposition process without the need of doping after growing.
There are a number of critical defects that can originate from the deposition process when targeting electronic thin film devices. Within this project, we intend to develop new correlative imaging and analysis techniques to determine defect types, to quantify defect size and density, as well as to characterise defects for further process optimisation.
We report here on the use of spectroscopic and multispectral imaging ellipsometry to investigate defects in several different compound semiconductor materials used in high-power electronic devices. The materials we investigated are β-Ga2O3, SiC, GaN, AlN, and AlGaN as well as oxidised SiC. All of these materials have their typical defects and require optimised measurement and analysis schemes for reliable detection and analysis. Spectroscopic ellipsometry is a highly sensitive method for determining the thicknesses and dielectric function of thin layers, yielding potentially a high number of microscopic properties. The combined method between ellipsometry and optical microscopy is known as imaging ellipsometry and is especially powerful for the large amount of data it produces. We have analysed defects in SiC- and AlN-based thin film semiconductors as well as characterised the properties of different types of SiO2 layers created on top of SiC monocrystals. We developed ellipsometric models for the data analysis of the different semiconductor materials.
If the defects have geometric features, it is useful to combine the ellipsometric analysis with topometry methods like interference microscopy and scanning probe microscopy. We have successfully characterised function-critical defects in MOVPE SiC layers and correlated the findings with topography from WLIM measurements. We have developed an imaging ellipsometric measurement methodology that allows to estimate the relative defect area on a surface by a statistical raw data analysis.
Development of representative test specimens by thermal history transfer in laser powder bed fusion
(2024)
The use of components manufactured by laser powder bed fusion (PBF LB/M) and subjected to fatigue loading is still hampered by the uncertainty about the homogeneity of the process results. Numerous influencing factors including the component’s geometry contribute to the risk of process instability and resulting inhomogeneity of properties. This drastically limits the comparability of different built parts and requires expensive full component testing. The thermal history as the spatiotemporal temperature distribution has been identified as a major cause for flaw formation. Therefore, it can be hypothesized that a similar thermal history between components and test specimens enhances their comparability. Following this assumption, a strategy is developed to transfer the intrinsic preheating temperature as a measure of comparability of thermal histories from a region of interest of a complex component to a simple test specimen. This transfer concept has been successfully proved by the use of FEM-based macroscale thermal simulations, validated by calibrated infrared thermography. An adoption of the specimen manufacturing process by the adjustment of the inter layer times was established to manufacture specimens which are representatives of a specific region of a large-scale component in terms of the thermal history similarity criterion. The concept is schematically illustrated in Figure 1 and was demonstrated using a pressure vessel geometry from the chemical industry.
Ellipsometry as optical metrology method for analysis of reference materials for nanoelectronics
(2024)
Electrical properties of materials at the nanoscale can be characterized using scanning microwave microscopes (SMM) and conductive atomic force microscopes (C AFM). However, the measurement results are difficult to compare since different setups and different reference standards are used. The development of new “out-of-lab” reference standards can contribute to the traceability and reliability of these scanning probe microscopy methods (SPM) and facilitate their broader industrial application.
In this study, we discuss the capability of optical methods such as ellipsometry for the characterization of existing and the development of new reference calibration samples for scanning microwave microscopy. Ellipsometry is a fast and non-destructive method, which enables very accurate determination of the layer thickness and the dielectric functions of the materials. Imaging ellipsometry is suitable for spatially resolved measurements when analyzing thin layers in microstructured samples.
We show how the electrical resistivity of indium tin oxide (ITO) layers in newly designed resistive calibration samples can be obtained from spectroscopic ellipsometric measurements. The extension of the measurement range into the mid-infrared region was necessary when analyzing ITO layers with low conductivity. This parameter was obtained by fitting a Drude function describing the absorption of the free carriers. The impact of the coating process conditions on the layer properties is discussed.
Imaging ellipsometry was applied for the characterisation of thin ITO and SiO2 layers in microstructured resistive and capacitance calibration kits. The uncertainties of determined layer thicknesses were specified according to standardized practice guides used in ellipsometry. We show how statistical fingerprint analysis of the measured ellipsometric transfer quantities can be used to validate the quality of potential reference materials for nano-electronics and to monitor the processing of structured samples.
Packages for the transport of spent nuclear fuel are designed to endure severe accidents. To obtain approval, these transport packages must adhere to the specification-based criteria of the international transport regulations SSR-6 of the International Atomic Energy Agency (IAEA). To ensure compliance with these requirements, specific mechanical and thermal tests need to be addressed with respect to the package type. Typically, SSR-6 prescribes a mechanical test followed by a thermal fire test as part of different testing scenarios. To approve the latter test of the sequence, BAM performs calorimeter tests in advance with so-called fire reference packages for characterizing the actual fire and its impact on the package to be tested. Packages are designed with different geometry sizes depending on their purpose. For previous tests, the implemented test setups in the fire test stand were sufficiently dimensioned and could cover all requirements in this respect. However, to cover additional testing needs in the future, BAM is expanding the test setup for the purpose of testing significantly larger packages.
In previous test setups one ring burner for propane surrounding the test specimen was sufficient. The limiting size in this configuration was the design height of the transport package to be tested. According to the thermal test of the IAEA-Regulations [1], a 30-minute fully engulfing 800°C pool fire or an equally severe fire, e.g., propane gas fire, must be applied to the transport package. Possible adjustments such as nozzle cross-section and propane mass flow can be adjusted to a certain extent. Further modifications, to cover significantly higher and larger packages all-around with a fully engulfing fire, must be accomplished with an additional, second burner ring. Both burner rings had the same dimensions and were mounted on top of each other at different heights to create a significantly larger volume of fire that completely engulfs the package including its impact limiter.
To meet the IAEA regulatory boundary conditions, the enhanced fire test stand with the second burner ring is tested with a large fire reference package and will then be used for real-size transport packages after all parameters are successfully met. This fire reference package represents the external geometry of a generic transport cask for radioactive material and is equipped with numerous temperature sensors to record temperature curves at the interior wall surfaces.
As industries move for ever faster development and adoption cycles of emerging new technologies in the field of welding, the meticulous and longer-winded approach of the scientific research process can feel harder to integrate. To help bridge this gap and increase the speed, quality, and adoption rate of publicly funded research, the Bundesanstalt für Materialforschung und -prüfung (BAM) continues to work towards enabling scientists with direct access to necessary software tools and - in the future – highest quality welding research reference data to further foster collaborations.
On the experimental side, the arc welding group at BAM division 9.3 “welding technologies” is continuing to expand and upgrade its capacities of robotic welding systems with integrated state of the art sensor technologies and software solutions. This allows all experiments to be recorded and measured in micro-millimeter accuracy and at sub-millisecond precision, including welding process data, complete spatial geometry and temperature measurements, process video recordings and more. The custom software-based solutions and interfaces allow scaling of the welding systems from large thick plate offshore applications to small additive repair weldments in wind turbine blades to multi-hour continuous weldments in additive manufacturing applications. In addition to the data gathered during the welding process itself, the relevant testing results and materials properties produced at BAM or externally can be integrated seamlessly. This allows detailed traceability of all results back to the actual welding process.
Regardless of the scope and application, complete datasets can be made accessible for research or industry partners in the highest resolution based on the open source WelDX (welding data exchange) file format.
Figure 1. Welding experiment representation including dynamic process data, cross-section imaging and hardness measurements from a single weldx file.
The talk will give an overview of the experimental facilities and workflows as well as current software developments with a focus on research data quality assurance, traceability, and accessibility.
Based on the integration into latest research trends and activities of the “welding technologies” division, the path to publishing reference datasets for arc welding process for various applications and materials is outlined and discussed.
Although intense wildfire research has been done in the US and in Australia, it cannot be transferred directly to the situation in Europe as the local vegetation has a significant influence on the fire spread. The EU-funded project TREEADS and the so-called German pilot within the project are concentrating on wildfire in Europe. Extensive experimental research is done on local vegeta-tion in Germany and the experimental results are used to adjust the Fire Dynam-ics Simulator (FDS) to local vegetation as a fuel in the calculations. The particle model and the boundary fuel model are developed for the simulation of forest fires. Both models require the kinetic input for the dehydration, pyrolysis, and char oxidation process. This three-step simplified model describes the basic fuel combustion kinetic. Most published simulations use the default kinetic input of pine needles from FDS user manual.
To adjust the simulation to local vegetation, the corresponding kinetic parame-ters have been experimental investigated. Samples of pine needles, moss and other falling leaves were collected, air dried and grinded into powder. The TG analysis of all these samples were done under different heating rate of 5, 10 and 20K/min.
The activation energy and the corresponding pre-exponential factor were calcu-lated. The results show that fire spread depends significantly on the vegetation and comparison with small scale experiments show good agreement using the new kinetic parameters. The new model is applied to a larger scenario and will be compared to the results of large-scale experiments for further validation of the model.
Um die Ausbreitungsmechanismen von Vegetationsbränden und besonders bei Bodenbränden besser zu verstehen, wurden die Einflussfaktoren auf die Brandausbreitung näher untersucht. Da die Brandausbreitung auch in starkem Maße von der lokalen Vegetation abhängt, war eine Charakterisierung der lokalen Vegetation und der Bodenverhältnisse wichtig. Die Wetterverhältnisse spielen einerseits im Vorfeld des Brandes durch längere Dürreperioden als auch während des Brandes, z.B. durch den Windeinfluss, zusätzlich eine große Rolle.
Durch die numerische Simulation kann eine größere Variation der Einflussgrößen abgebildet werden als durch die zeitlich und finanziell begrenzten experimentellen Möglichkeiten. Für die Berechnungen wird der Fire Dynamic Simulators (FDS) mit dem Paket WFDS verwendet. Dadurch kann mit einem vereinfachten 3-Phasen-Reaktionskinetikmodell, bestehend aus Dehydrierung, Pyrolyse, Kohleoxidation, die Ausbreitung von Vegetationsbränden verschiedener Waldbodenarten untersucht werden. Es wurden dazu 6 typische Pflanzenarten und Bodenproben aus Kiefern-, Buchen und Eichenbeständen ausgewählt.
Die gesammelten Waldbodenproben wurden alle hinsichtlich des Wassergehalts, des organischen Gehalts, der Packungsdichte, der Dichte und der statistisch ermittelten Pflanzenartenverteilung charakterisiert. Das kinetische Abbrandverhalten wurde durch Thermogravimetrische Analyse (TGA) untersucht. Alle diese Daten wurden als Eingabeparameter für die Simulation verwendet. Die numerischen Simulationen werden mit Experimenten im kleinen, mittleren und Real-Maßstab validiert.
Direct energy deposition additive manufacturing technologies that utilize an electric arc have great potential for generating large volume metal components. However, selecting process parameters that yield the desired near net shape design and requested mechanical component behavior is not a trivial task due to the complex relationship between all process parameters and material characteristics. This presentation exemplifies the application of a newly developed solid welding wire doped with TiB to enhance grain refinement in the deposited metal for additive manufacturing based on DED-Arc of high-strength precipitation hardening AlMgSi-aluminum alloys. It is worth noting that the solid wire is the result of our preliminary metallurgical studies on grain refinement in aluminum weld metal.
Consequently, research focuses on the correlation between process parameters and component quality to understand the underlying mechanisms. This is crucial for evaluating a robust process parameter space that yields component quality in line with corresponding standards which are mainly taken from welding technology.
Specifically, we examine component quality by analyzing pore size and distribution, as well as grain morphology. To enhance the mechanical properties of the deposited metal, a post-weld heat treatment was conducted, comprising of solution treatment, quenching, and artificial aging. The study also evaluates the effects of various heat treatment strategies on the final mechanical properties of the material.
To demonstrate the applicability of 3D metal printing of high-strength aluminium alloys, a more complex demonstrator was created. It has been shown that DED-Arc can produce high-volume aluminium parts with the same quality as the corresponding subtractive processing strategy.
Additionally, the entire additive manufacturing chain has been digitally integrated, enabling traceability of all relevant process steps, which is essential for reliable subsequent quality assessment.
Lecture-like introduction in the topic. Fundamental aspects are discussed: Burning of polymers, fire risks, pyrolysis, combustion in the flame, physical chemistry of ignition, flame spread and steady state burning, flame retardancy mechanisms and groups of flame retardants, fire hazards (smoke, toxic products) and environmental concerns, fire testing.
The manufacture of sintered glasses and glass-ceramics, glass matrix composites, and glass-bounded ceramics or pastes is often affected by un-expected gas bubble formation also named foaming. Against this background, in this presentation the main aspects and possible reasons of foaming are shown for completely different glass powders: a barium silicate glass powders used as SOFC sealants, and bioactive glass powders using different powder milling procedures.
Sintering and foaming were measured by means of heating microscopy backed up by XRD, differential thermal analysis (DTA), vacuum hot extraction (VHE), optical and electron microscopy, and infrared spectroscopy, and time-of-flight secondary ion mass spectrometry (ToF-SIMS).
Different densification was reached followed by significant foaming starting partly immediately, partly at higher temperature. Foaming increased significantly as milling progressed. For moderately milled glass powders, subsequent storage in air could also promote foaming. Although the milling atmosphere significantly affects the foaming of uniaxially pressed powder compacts sintered in air.
VHE studies show that foaming is driven by carbon gases and carbonates were detected by Infrared spectroscopy to provide the major foaming source. Carbonates could be detected even after heating to 750 °C, which hints on a thermally very stable species or mechanical trapping or encapsulating of CO2. Otherwise, dark gray compact colors for milling in isopropanol indicate the presence of residual carbon as well. Its significant contribution to foaming, however, could not be proved and might be limited by the diffusivity of oxygen needed for carbon oxidation to carbon gas.
Introduction: Effective disinfection is crucial to maintain hygiene and to prevent the spread of infections. Phenotypic heterogeneity in disinfection survival (i.e. tolerance) may result in failure of disinfection, which in turn may foster the evolution of resistance to both disinfectants and antibiotics. However, the consequences of phenotypic heterogeneity for disinfection outcome and resistance evolution are not well understood. Goal: This study investigates the impact of phenotypic heterogeneity on the survival and evolution of Escherichia coli during disinfection with six commonly used substances. Furthermore, the consequences of evolved disinfectant tolerance for antibiotic resistance evolution are studied. Materials & Methods: The extent of population heterogeneity during disinfection is derived by determining time-kill kinetics and analysis with mathematical modelling. The link between population heterogeneity and evolvability of disinfectant tolerance was assessed by laboratory evolution experiments under periodic disinfection. The ability of disinfectant tolerant strains to evolve antibiotic resistance is assessed by serial transfer experiments with increasing concentrations of different antibiotics and by whole genome sequencing. Results: Multi-modal time-kill kinetics in three of the six disinfectants suggest the presence of disinfectant-tolerant subpopulations (i.e. persister cells). Importantly, the ability and extent to evolve population-wide tolerance under periodic disinfection is related with the presence of persister cells and the level of phenotypic heterogeneity during disinfection. Interestingly, the probability of high-level resistance evolution to certain antibiotics is attenuated in disinfectant tolerant strains as compared to the sensitive ancestor. Whole-genome sequencing reveals epistatic interactions between disinfectant tolerance and antibiotic resistance mutations, preventing access to canonical evolutionary paths to resistance. Summary: Our findings suggest that phenotypic heterogeneity can facilitate disinfection survival and the evolution of population wide tolerance, which can impact future antibiotic resistance evolution.
Up to now, oriented surface crystallization phenomena are discussed controversially, and related studies are restricted to few glasses. For silicate glasses we found a good correlation between the calculated surface energy of crystal faces and oriented surface nucleation. Surface energies were estimated assuming that crystal surfaces resemble minimum energy crack paths along the given crystal plane. This concept was successfully applied at the Institute of Physics of Rennes in calculating fracture surface energies of glasses. Several oriented nucleation phenomena can be herby explained assuming that high energy crystal surfaces tend to be wetted by the melt. This would minimize the total interfacial energy of the nucleus. Furthermore, we will discuss the evolution of the microstructure and its effect on the preferred crystal orientation.
We investigated the phase transformations during butt-welding of supermartensitic steel plates with help of Neutron-Bragg-Edge Imaging (NBEI). Gas tungsten arc welding (GTAW) was used with a motorized torch allowing for automated weldments. The austenitization in the heat affected zone (HAZ) could be clearly visualized at λ = 0.39 nm, a wavelength smaller than the Bragg edge wavelengths of both austenite and martensite. The re-transformation into the martensitic phase during cooling was clearly detected. However, we observed an unexpected additional change in transmission at λ = 0.44 nm, a wavelength larger than the wavelength of the Bragg edges of both the martensitic and austenitic phases. We attribute this change to the Deybe-Waller-Factor that describes the temperature dependence of coherent scattering at a crystal lattice. The observed two-dimensional attenuation map corresponds well with a temperature distribution modelling by software macros in ANSYS [3]. Here, the absolute temperature values could be achieved by calibrating the modelled attenuation with help of a thermocouple placed at the steel plate. This allows in return for a direct two-dimensional temperature reading based on the Debye-Waller-relation between neutron attenuation and sample temperature.
We developed a two-step semi-synthesis for the preparation of isotopically labeled EAs, starting from native EAs. This universal strategy enabled the successful synthesis of all isotopically labeled priority EAs. The structure of the isotopically labeled EAs was confirmed by HPLC-HR-MS/MS using native, unlabeled EAs as a reference standard. The next step will be the implementation of the isotopically labeled standards in the European standard procedure EN 17425 to improve the quantification of EAs in foodstuffs.
Bislang wird das Phänomen der orientierten Oberflächenkristallisation kontrovers diskutiert und entsprechende Studien beschränken sich auf nur wenige Gläser. Für Silikatgläser haben wir eine gute Korrelation zwischen der berechneten Oberflächenenergie von Kristallflächen und der orientierten Oberflächenkeimbildung gefunden. Die Oberflächenenergien wurden unter der Annahme abgeschätzt, dass die Kristalloberflächen bei der Keimbildung den Kristallebenen mit minimaler Energie entsprechen, denen ein Riss beim Bruch folgt. Dieses Konzept wurde am Institut für Physik in Rennes erfolgreich bei der Berechnung der Bruchflächenenergien von Gläsern angewandt. Mehrere orientierte Keimbildungsphänomene lassen sich dadurch erklären, dass man annimmt, dass Kristalloberflächen mit hoher Energie dazu neigen, von der Schmelze benetzt zu werden. Dies minimiert die gesamte Grenzflächenenergie des Keims. Darüber hinaus werden wir die Entwicklung der Mikrostruktur beim weiteren Kristallwachstum und ihre Auswirkungen auf die bevorzugte Kristallorientierung diskutieren.