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Eingeladener Vortrag
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Die Wasserstofftechnologien der näheren Zukunft erfordern sichere Komponenten. Die Füge- und Schweißtechnik ist hier von zentraler Bedeutung, insbesondere für die Transportinfrastruktur (wie Pipelines). Der vorliegende Vortrag gibt hierzu einen umfassenden Überblick, beginnend bei der Erzeugung, Speicherung über Transport und Nutzung. Zusätzlich wird die zunehmende Bedeutung der additiven Fertigung beleuchtet und ein kurzer Ausblick auf die aktuelle Normungsroadmap der Wasserstofftechnologien gegeben.
Offshore-Windenergieanlagen erfordern Gründungskonzepte aus unterpulver-(UP-)geschweißten Dickblechen (bspw. der Güte S420ML). Während der Schweißfertigung kann eine zeitverzögerte wasserstoffunterstützte Kaltrissbildung auftreten, deren Bewertung aufgrund der Bauteilgröße von Offshore-Strukturen sehr komplex ist. Deswegen wurde eine bauteilähnliche Geometrie (Mock-Up) entwickelt, um reale Steifigkeitsverhältnisse auf den Labormaßstab zu übertragen. Zusätzliche Versteifungen simulieren die Wirkung einer Einspannung bzw. Schrumpfbehinderung der Schweißnaht. Über die Verwendung von Schweißpulvern mit definierter Feuchte wurden zudem ein Extremszenario der Wasserstoffaufnahme simuliert. Entsprechend der vorgegebenen Mindestwartezeit für die ZfP von bis zu 48 h wurde die Schweißnaht zerstörungsfrei mit Phased-Array-Ultraschall-Prüfung (PAUT) geprüft und die Eigenspannungen über Röntgendiffraktometrie (XRD) bestimmt. Zusätzlich wurde die Wasserstoffverteilung in der Schweißverbindung numerisch simuliert. Außer zulässigen Defekten (wie Poren), wurde keine verzögerte Kaltrissbildung in den Mock-Ups festgestellt, was auf hohe Rissbeständigkeit hindeutet.
In the course of tomorrow's hydrogen-based energy transition, the construction of the corresponding infrastructure will play a central role. The majority of materials used to date are typically welded for component fabrication. In that context, steels are widely applied and can be prone to hydrogen embrittlement. This includes the classical delayed cold cracking during welding processing as well as embrittlement phenomena during operation. For the evaluation of any hydrogen effect on, for example, the mechanical properties of a welded metallic material, the hydrogen content must be precisely determined. In the case of welds, for example, according to ISO 3690, this is the isothermal carrier gas hot extraction (CGHE). CGHE is based on accelerated hydrogen degassing due to thermal activation of hydrogen at elevated temperatures. In addition to the pure quantification of hydrogen, thermal desorption analysis (TDA) with varied heating rates can be used to determine and evaluate the bonding state at microstructural defects in the material. For both techniques, experimental and measurement influences have to be considered, which have a great effect on the result. For CGHE, for example, ISO 3690 suggests different sample geometries as well as minimum extraction times. The present study summarizes results and experiences of numerous investigations with different sample temperatures and geometries (ISO 3690 type B and cylindrical TDA samples) regarding: the influence of the sample surface (polished/welded), measurement accuracies depending on the sample volume as well as the insufficient monitoring of the effect of the PI controller on the extraction temperature. In particular, a deviating extraction temperature to the set temperature, can significantly falsify the measurement results. Based on the results, methods are shown to quickly reach the desired extraction temperature without having to physically interfere with the measurement equipment. This serves to substantially improve the reliability of hydrogen measurement through increased signal stability and accelerated hydrogen desorption. In general, an independent temperature measurement with dummy samples for the selected heating procedure is advisable to exclude possible unwanted temperature influences already before the measurement. In addition (and way more important), the methods described can be transferred directly to industrial applications.
Multi-principal element alloys (MPEAs) are innovative materials that have attracted extensive research attention within the last decade. MPEAs are characterized by a solid solution of equiatomic metallic elements. Depending on the number of elements, they are also referred as high entropy alloys (HEAs with n ≥ 4 elements like CoCrFeMnNi) and medium-entropy alloys (MEA with n = 3 elements CoCrNi). Depending on the alloy concept, MPEAs show exceptional properties in terms of mechanical performance or corrosion resistance at extreme environments. In that connection, hydrogen and its challenges for the most metallic materials gets more and more important. MPEAs are candidate materials for the substitution of conventional materials like austenitic stainless steels e.g., at very high-pressure up to 1000 bar. Those pressures are typically reached in valves or compressors for refueling of tanks with operational pressure of 700 bar. So far, the susceptibility of HEA/MEAs to hydrogen assisted cracking (if any) and the especially the underlying hydrogen uptake and diffusion was not within the scientific scope and not investigated in detail yet. For that reason, we focused on the hydrogen absorption the characterization of the hydrogen diffusion and trapping at elevated temperatures in a CoCrFeMnNi-HEA (each element with 20 at.-%) and CoCrNi-MEA, each element with 33.3 at.-%). As reference grade, the commercially available austenitic stainless steel AISI 316L was investigated. High-pressure hydrogen charging was conducted at different pressures in autoclave environment with maximum value of 1,000 bar. Thermal desorption analysis (TDA) via carrier gas hot extraction with coupled mass spectrometry was used with a max. heating rate of 0.5 K/s up to 650 °C. The measured desorption spectra of the different samples were deconvoluted into a defined number of individual peaks. The individually calculated peak temperatures allowed the definition of activation energies for predominant trap sites in the respective materials as well as the percentage share of the totally absorbed hydrogen concentration. The results present for the first time the complex interaction of both MPEAs and high-pressure hydrogen charging. A deconvolution of four peaks was selected and a main desorption peak was identified the dominant hydrogen trap containing the biggest share of the absorbed hydrogen concentration. The chemical composition an austenitic phase of both MPEAs is responsible for delayed hydrogen diffusion and strong, but mostly reversible, trapping. The comparison with the 316L samples showed significantly higher activation energies in the MPEAs, whereas hydrogen was also trapped at very high extraction temperatures. The absorbed maximum hydrogen concentration at 1,000 bar was 130 ppm for the CoCrFeMnNi-HEA, 50 ppm for the CoCrNi-MEA and 80 ppm for the 316L. It is interesting that the CoCrFeMnNi-HEA has obviously a way higher trapping capability compared to the conventional austenitic 316L, which could be a major advantage in terms of resistance to hydrogen assisted cracking.
The study provides an overview of the aspects of joining and its importance in manufacturing of components for the more and more important field of hydrogen as key factor for the energy transition to a decarburized future. To this end, the fundamentals of the technology fields of hydrogen production, storage, transport, and application are presented and the state of the art of manufacturing of components for hydrogen technologies by joining is summarized. Based on representative examples from practice, research and development, the importance of joining technology in hydrogen technologies is clearly highlighted and perspectives for the future are derived. From a macroeconomic perspective, the focal points, or trends of joining technologies here include: the erection of new infrastructure for hydrogen storage and transport, and the safe conversion of existing natural gas infrastructure and its challenges for welded materials. In addition, we show the problems that are anticipated with in-service repair welding of hydrogen pipelines. In hydrogen applications, the efficient mass production of fuel cells and electrolysers is becoming increasingly important. For that reason, the importance of additive manufacturing is highlighted. Finally, the challenges for technical regulations and standardization by using hydrogen are shown.
Der Vortrag gibt einen tiefen Überblick über die Bedeutung der Füge- und Schweißtechnik in Wasserstofftechnologien. Dazu gliedert sich der Vortrag in die Komplexe H2-Erzeugung, Speicherung, Transport, Anwendung auf und gibt jeweils repräsentative Industriebeispiele für den heutigen Anwendungsstand. Insbesondere werden hier Fertigungstechnologien für Brennstoffzellen vorgestellt, sowie Herausforderungen beim Reparaturschweißen von Wasserstoffpipelines. Zeitgleich wird in einem eigenen Kapitel die Bedeutung der additiven Fertigung ebenso erläutert, wie die aktuellen und umfassenden Tätigkeiten auf dem Gebiet der Normung zu H2-Technologien.
Im Zuge der wasserstoffbasierten Energiewirtschaft von morgen, kommt der Errichtung der dementsprechenden Infrastruktur die zentrale Rolle zu. Der überwiegende Teil bisher eingesetzter und meist geschweißter Werkstoffe, wie Stähle, kann unter bestimmten Bedingungen zur Wasserstoffversprödung neigen. Dies umfasst die klassische verzögerte Kaltrissbildung während der Schweißverarbeitung als auch Versprödungsphänomene während des Betriebs. Für die Bewertung eines jeden Wasserstoffeffektes auf bspw. die mechanischen Eigenschaften eines geschweißten metallischen Werkstoffes, muss der Wasserstoffgehalt präzise bestimmt werden, Im Fall von Schweißnähten ist die beispielsweise nach der ISO 3690, die klassische isotherme Trägergas-Heißextraktion (TGHE). Die TGHE basiert dabei auf der beschleunigten Wasserstoffentgasung aufgrund der thermischen Aktivierung des Wasserstoffs bei erhöhten Temperaturen. Neben der reinen Quantifizierung des Wasserstoffs, kann über die thermische Desorptionsanalyse (TDA) mit variierten Heizraten, der Bindungszustand an mikrostrukturellen Defekten im Material festgestellt und bewertet werden. Für beide Techniken sind experimentelle und messtechnische Einflüsse zu beachten, die großen Effekt auf das Ergebnis haben. Für die TGHE schlägt die ISO 3690 schlägt beispielswiese verschiedene Probengeometrien sowie Mindestextraktionszeiten vor. Die vorliegende Studie fasst Ergebnisse und Erfahrungen zahlreicher Untersuchungen an der Bundesanstalt für Materialforschung und -prüfung (BAM) mit unterschiedlichen Probentemperaturen und Geometrien (ISO 3690 Typ B und zylindrische TDA-Proben) zusammen hinsichtlich: Einfluss der Probenoberfläche (poliert/geschweißt), Messgenauigkeiten in Abhängigkeit des Probenvolumens sowie die unzureichende Überwachung des Effektes des PI-Reglers auf die Extraktionstemperatur. Insbesondere eine abweichende Extraktionstemperatur zur eingestellten Temperatur, kann die Messergebnisse wesentlich verfälschen. Basierend auf den Ergebnissen werden Methoden aufgezeigt, um schnell die gewünschte Extraktionstemperatur zu erreichen, ohne physisch in das Messequipment eingreifen zu müssen. Dies dient der wesentlichen Verbesserung der Zuverlässigkeit der Wasserstoffmessung durch erhöhte Signalstabilität und beschleunigte Wasserstoffdesorption. Im Allgemeinen ist eine unabhängige Temperaturmessung mit Dummy-Proben für die gewählte Heizprozedur angeraten, um mögliche unerwünschte Temperatureinflüsse bereits vor der Messung auszuschließen. Die beschriebenen Methoden können ohne großen Aufwand direkt in die industrielle Anwendung überführt werden.
Dissimilar metal TIG weld joints of multiple principal element alloys (MPEA) to austenitic steel 304
(2023)
Multi-element alloys (MPEA - Multiple Principal Element Alloys) represent a new class of materials consisting of at least three alloying elements, each with 5 to 35 atomic %. This material class includes high-entropy alloys (HEA, with n ≥ 4 elements). The underlying alloying concept differs fundamentally from conventional materials such as the Fe-based steel. For this purpose, the alloying elements are specifically selected, and the microstructures are adjusted in a single-phase and, in some cases, multi-phase manner. The aim is to identify highly innovative MPEA with individually adjustable properties for industrial applications. In the last 20 years, however, the focus has been on pure material synthesis. With the increase in available material quantities, the focus is on processing issues such as joining and welding processes. In that connection, the weldability of MPEAs has received very little attention so far. Experience with dissimilar metal welds (DMWs) is completely lacking but is essential for the application of these materials if joint to conventional materials. This study presents selected experimental results on the weldability of MPEA-DMWs and the resulting microstructures. For this purpose, the equiatomic CoCrFeMnNi (HEA) was investigated in cold-rolled (CR) and heat-treated (HT) condition and joined by tungsten inert gas (TIG) welding to an austenitic stainless steel 304. The DMWs showed defect-free conditions (no lack of fusion, cracks and so on), whereas the cold-rolling increases the microhardness. The global mechanical properties were obtained by instrumented tensile tests of cross-weld samples and showed sufficient yield and tensile strength comparable to that of the individual base materials (BM). The local strain conditions were determined by digital image correlation and showed the highest local strains to occur in the intermixed weld metal. Indeed, the preferred fracture location of the cross-weld tensile samples was in the weld metal. Finally, the experiments proofed the weldability of the MPEAs to conventional 304. This enables targeted further considerations for example as structural materials.
The hydrogen economy requires large-scale storage and transportation options like long-distance transmission pipelines. The applied materials (typically steels) must be carefully tested under different conditions (pressure, temperature, impact of impurities, etc.) for their suitability and service with hydrogen. In combination with mechanical load, as occurs in every gas network, hydrogen can induce degradation of the mechanical properties and promote finally resulting in embrittlement, i.e., the formation of cracks. The conventional testing procedures consist of autoclaves in which samples are strained under pressurized hydrogen. The test apparatus requires large amounts of hydrogen and thus a high level of safety and costs. In very specific cases, these tests might be replaced by simplified electrochemical charging. However, these test alternatives raise several questions regarding the equivalency of both testing scenarios. In the early 1980’s the idea of a so-called hollow tensile sample raised and was reinitiated 2021 in ISO TC 164 by T. Ogata (NIMS, Japan) and further developed (e.g. by Fraunhofer IWM, Germany). The idea was: the sample itself represents the autoclave instead of charging a sample from outside. For that reason, a hole is drilled through the sample and the inner surface is pressurized by hydrogen gas during the mechanical testing. Indeed, this represents the main advantage as no expensive pressure-resistant autoclave equipment for large H-volumes is necessary, which significantly reduces the safety-related issues and thus the high costs. In the following, we show recent activities at BAM Berlin on adaption of the hollow-specimen technique for slow strain rate testing (SSRT). The current research activities are focussed on macroscopic influences like the sample geometry, minimum necessary dimensions, and microscopic influences e.g., on the surface by the processing method (drill hole quality and geometric precision) as well as the gas pressure effect (mechanical deformation of surface in different media).
Microalloying elements, such as Nb and Ti, are essential for the targeted mechanical strength of quenched and tempered, high-strength fine-grained structural steels with a nominal yield strength ≥ 690 MPa. Current specifications for chemical composition only provide upper limits for manufacturers. But even small deviations in the alloying route can have a drastic effect on the mechanical properties. Thus, an adequate prediction of the weldability and the integrity of the welded joint becomes difficult or even impossible due to the varying composition and, hence, the microstructures. Undesirable side effects are the possible softening of the heat-affected zone (HAZ) as well as the opposite effect of hardening. Against this background, different microalloying routes with varying Ti and Nb contents are systematically investigated for the first time on specially designed lab-cast alloys. The basis of each alloy route was the common S690QL in terms of both the chemical composition as well as the heat treatment. To investigate the weldability, three-layer welds were performed using metal active gas welding (MAG) and critical microstructural areas with high softening/hardening were identified. The scope was here on the identification of phase transformations during cooling and on the respective metallurgical precipitation behavior. Isothermal and non-isothermal phase calculations were performed using Thermo-Calc® and showed that the prediction of the non-equilibrium precipitation characteristics during welding is not trivial, especially for this relatively complex chemical composition. The mechanical properties of the welded joints were identified by both Charpy tests (toughness) and tensile tests (strain and strength). During the test, the local straining behavior of the welded joints, was identified using a digital image correlation (DIC) system, see Figure 1. Despite the generally good weldability of the materials, the results show a significant influence of the microalloying route as well as the welding heat input on the different precipitation kinetics.