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For the hydrogen-based energy economy of tomorrow, the construction of the necessary infrastructure will play a central role. Most materials used to date, such as welded steels, can be prone to hydrogen embrittlement under certain conditions. This includes the classic delayed cold cracking during welding as well as degradation phenomena during service of components in hydrogen-containing environment. For the evaluation of any hydrogen effect, for example, on the mechanical properties of a welded metallic material, the hydrogen content must be precisely determined. In the case of weld seams, the carrier gas hot extraction (CGHE) according to ISO 3690 is meanwhile state-of-the-art. CGHE is based on accelerated hydrogen degassing due to the thermal activation of hydrogen at elevated temperatures. In addition to the quantification of hydrogen, thermal desorption analysis (TDA) with varying heating rates can be used to determine and evaluate the hydrogen trapping at microstructural defects in the material. For both techniques, experimental and metrological influences must be considered, which have a major effect on the result. For example, ISO 3690 suggests different sample geometries and minimum extraction times for CGHE. This study summarizes the results and experiences of numerous investigations at the Federal Institute for Materials Research and Testing (BAM) with different sample temperatures and geometries (ISO 3690 type B and cylindrical TDA samples) regarding the influence of the sample surface (polished/welded), measurement accuracy depending on the sample volume and the insufficient monitoring of the effect of PI control on the extraction temperature. A deviating extraction temperature from the target temperature can significantly falsify the measurement results. Based on the results, methods are shown which allow the desired extraction temperature to be reached quickly without physically interfering with the measuring equipment. This serves to significantly improve the reliability of the hydrogen measurement through increased signal stability and accelerated hydrogen desorption. In general, an independent temperature measurement with dummy samples is recommended for the heating procedure of choice to exclude possible undesired temperature influences before the measurement. The methods described can be transferred directly to industrial applications
The presentation gives an overview of BAM's activities on processing influences and application properties of MPEAs in the form of joined and machined high and medium entropy alloys (CoCrFeMnNi and CoCrNi). In the case of welding, the focus is on defect-free welded joints with sufficient mechanical properties. In the case of machining, the focus is on the possible influence on the surface quality of the materials through adequate milling parameters. In addition, the hydrogen absorption and diffusion properties as well as the electrochemical corrosion behavior are fundamentally examined.
This presentation describes the usability of the hollow tensile specimen technique for in-situ material testing in a hydrogen atmosphere.
In addition, the presentation provides an outlook on the methodology for investigating the suitability of pipeline steels and their weld seams for hydrogen operation.
As energy carrier of the future, green hydrogen can make a decisive contribution to a sustainable energy supply. Particularly important is the decarbonization of heavy industry. Therefore, a reliable supply of hydrogen must be guaranteed. A hydrogen pipeline grid can achieve this purpose. In Europe concrete plans for a hydrogen pipeline grid already exist, as the so called “European Hydrogen backbone”. As building a completely new pipeline grid is economically not justifiable, a dual-way strategy of repurposing natural gas (NG) pipelines and newly built pipelines is intended. Long distance pipeline grids require regular maintenance and repairs. For natural gas (NG) pipelines in-service welding is state of the art. Concepts such as hot-tapping (drilling into pressurized pipelines) and “stoppling” (sealing off pipeline sections after installing bypasses or pressure relieves) allow the repair of damaged pipeline sections or the installation of new branches without shutting the pipeline down, which in most cases isn’t possible from an economic standpoint. The EIGA 121/14 guideline already pointed out in 2014 that “a hydrogen hot-tap shall not be considered a routine procedure”. This shows that the determination of the transferability of these repair concepts to hydrogen pipelines is of utmost importance. Due to the degrading effects of hydrogen on mechanical proper-ties, commonly referred to as “hydrogen embrittlement” it is necessary to understand and investigate the occurring effects. In the special case of repair welding on in-service hydrogen pipelines an increased hydro-gen uptake due to a large heat input and microstructural changes in the material needs to be considered. Therefore, material degradation must be investigated to determine whether modifications of repair procedures are necessary to ensure a reliable and safe hydrogen transportation via pipelines. For this reason, this paper gives an overview on existing weld repair concepts and its risks and limitations in terms of hydrogen absorption and possible embrittlement effects when transferred to hydrogen pipelines. The complexity lies in a large variety of materials (low alloyed steels), pipeline diameters and corresponding welded joints. The material compatibility of materials in used (repurposed NG-pipelines) and new condition must be investigated. Particularly for repurposed/used pipelines the effect of a pre-matured/corroded inner surface and sometimes insufficient documentation of the material “history” needs to be considered. An overview on ongoing and completed R&D-projects with respect to repair concepts for hydrogen pipelines and hydrogen effects on pipeline materials is given. The focus hereby lies on possible methods of material testing and modeling. Its current difficulties, limits and possible solution will be discussed.
Contemporary steels creep-resistant steels like the 13CrMoV9-10 are used as thick plates e.g., for applications in hydrocrackers. The large plate thickness requires high efficiency welding processes like submerged arc welding (SAW) and a mandatory post weld heat treatment (PWHT). The PWHT-parameters stem from a combination of empirical knowledge and traditional experiments on free shrinking (FS) welds. In that connection, the formation of so-called stress-relief cracking (SRC) must be anticipated. The SRC susceptibility of a welded component is a complex combination and interaction of com-ponent specific, thermal, and metallurgical factors. Many of which have to date not been conclusively researched. For example, it is well known that SRCs develop during PWHT due to formation and growth of carbides on prior austenite grain boundaries, resulting in a significant hardness increase (secondary hardening) and toughness decrease. This leads to a high SRC susceptibility of the coarse grain heat-affected zone (CGHAZ) of the last weld bead during PWHT. This is intensified in case of high residual stresses from the component-specific, structurally induced stiffness. In combination with multi-layer welding this leads to a multiaxial stress distribution. Nonetheless, the combined effect of PWHT and high-residual stresses on the SRC formation is merely unknown. For that reason, this study presents the effect of different heating rates in conjunction with a certain component stiffness. For that reason, SAW joints of 13CrMoV9-10 steel were investigated under FS and defined external restraint condition.
Hydrogen has great potential on the path towards decarbonization of the energy and transport sectors and can mitigate the urgent issue of global warming. It can be sustainably produced through water electrolysis with potentially zero emissions, and efficiently used (e.g., in fuel cell systems). Despite its environmental advantages, hydrogen-metal interactions could result in the degradation of the mechanical properties of several structural materials. In order to determine the magnitude of the material degradation in relation to hydrogen exposure, extensive material testing is required. The standardized procedure for in-situ testing for the quantification of the impact of compressed gaseous hydrogen (CGH2) relies on the utilization of an autoclave around the tested specimen. Such test set-up is complex, expensive, time-consuming and requires special equipment, trained personnel, and strict safety procedures. A relatively recent method to circumvent these issues and provide affordable results consists of using hollow specimens, thus applying the hydrogen pressure inside rather than outside the specimen. It allows to reduce the volume of hydrogen by several orders of magnitude and to perform the tests more efficiently and in a safer manner. This study focuses on evaluating the tensile properties of X65 vintage pipeline steel tested in a high-pressure hydrogen environment using hollow specimens. Tests are performed in 6 MPa H2 and Ar at the nominal strain rate of 10−6 s−1 to evaluate the reduced area at fracture and the elongation loss. The effect of surface finishing on crack initiation and propagation is investigated by comparing two different manufacturing techniques. In this way, this study provides insights into the applicability of a novel, reliable, and safe testing method which can be used to assess the hydrogen-assisted ductility loss in metallic materials.
Multiple principal element alloys encompass the well-known high entropy alloys (HEA). The alloy system represents a new class of materials consisting of at least three alloying elements, each containing 5 to 35 at.%. Thus, this alloying concept differs fundamentally from conventional materials such as steel or nickel alloys. For this purpose, the alloying elements are specifically selected, the microstructures are adjusted in a single-phase and, in some cases, multi-phase manner. In particular, conflicting goals, such as the trade-off between strength and ductility in conventional steels, are overcome. However, in the last 20 years, the focus has been on material synthesis. With the increase in available material quantities, the focus is now on processing issues such as joining and welding processes. The weldability of HEAs has received very little attention so far. The experience with dissimilar metal welds is completely lacking but is essential for the application of these materials in combination with conventional materials. The present study presents comprehensive experimental results on the weldability of an equimolar CoCrFeMnNi-HEA in cold-rolled and heat-treated condition, which was joined by tungsten inert gas welding to an austenitic steel AISI 304. The mechanical properties of the dissimilar metal welds were characterized by cross-weld tensile samples, whereas the local deformation in the weld of the different welding zones was measured by digital image correlation. In accordance with the respective initial HEA condition (cold-rolled vs. heat-treated), the local strain behavior was divergent and influenced the global mechanical properties of both DMW types. Nonetheless, the experiments provided proof in principle of the weldability for dissimilar joints of the CoCrFeMnNi-HEA welded to conventional materials like austenitic stainless steels ensuring a corresponding capability for mechanical loading. This allows further considerations on the application of these innovative materials.
The high potential of hydrogen as a key factor on the pathway towards a climate neutral economy, leads to rising demand in technical applications, where gaseous hydrogen is used. For several metals, hydrogen-metal interactions could cause a degradation of the material properties. This is especially valid for low carbon and highstrength structural steels, as they are commonly used in natural gas pipelines and analyzed in this work.
This work provides an insight to the impact of hydrogen on the mechanical properties of an API 5L X65 pipeline steel tested in 60 bar gaseous hydrogen atmosphere. The analyses were performed using the hollow specimen technique with slow strain rate testing (SSRT). The nature of the crack was visualized thereafter utilizing μCT imaging of the sample pressurized with gaseous hydrogen in comparison to one tested in an inert atmosphere.
The combination of the results from non-conventional mechanical testing procedures and nondestructive imaging techniques has shown unambiguously how the exposure to hydrogen under realistic service pressure influences the mechanical properties of the material and the appearance of failure.
Zur Umsetzung der wasserstoffbasierten Energiewende ist eine zuverlässige Transportinfrastruktur unverzichtbar. Hierfür ist die Nutzung großer Teile des vorhandenen Erdgasnetzes vorgesehen. Im Rahmen von Reparatur- und Wartungsarbeiten ist das Schweißen im Betrieb an Erdgaspipelines Stand der Technik. In Verbindung mit Wasserstoff wirft diese Technik jedoch Fragen der Materialverträglichkeit auf. Das im Vortrag vorgestellte Projekt H2SuD leistet Beiträge zur Aufklärung des Einflusses von Reparaturschweißprozessen auf die Wasserstoffaufnahme und Degradation im Betrieb befindlicher H2 Gasleitungen. Ein Schwerpunkt des Vortrages liegt auf der im Projekt erarbeiteten Prüfmethode für Modellversuche, mit denen der Einfluss von Schweißen im Betrieb an Pipelines auf die Wasserstoffaufnahme getestet wird. Die Durchführung erster Versuche und dabei erzielte Ergebnisse werden präsentiert.
Mikrolegierungselemente wie Nb und Ti sind entscheidend für die erwünschte mechanische Festigkeit von vergüteten Feinkornbaustählen mit einer Nennstreckgrenze von ≥ 690 MPa. Aktuelle Spezifikationen geben lediglich Obergrenzen für die chemische Zusammensetzung vor, allerdings können geringfügige Abweichungen erhebliche Auswirkungen auf die mechanischen Eigenschaften haben. Die Vorhersage der Schweißbarkeit und Integrität von Schweißverbindungen stellt aufgrund der variierenden Zusammensetzung und Mikrostrukturen Herausforderungen dar. Unerwünschte Effekte wie Erweichung der Wärmeeinflusszone (WEZ) oder Verfestigung können auftreten. Um dies zu untersuchen, wurden verschiedene Mikrolegierungsrouten mit variierenden Ti- und Nb-Gehalten an Laborschmelzen erforscht. Die Basis jeder Route entsprach der üblichen S690QL in Zusammensetzung und Wärmebehandlung. Dreilagenschweißungen wurden mittels Metallaktivgasschweißens (MAG) durchgeführt, um kritische Gefügebereiche zu identifizieren. Die Analyse konzentrierte sich auf Phasenumwandlungen während der Abkühlung und metallurgisches Ausscheidungsverhalten. Die mechanischen Eigenschaften der Schweißnähte wurden durch Zugversuche ermittelt. Die Ergebnisse zeigen einen bedeutenden Einfluss der Mikrolegierungsroute und Schweißwärmezufuhr auf die Ausscheidungskinetik, trotz insgesamt guter Schweißbarkeit der Werkstoffe.
Mikrolegierungselemente, wie Nb und Ti, sind für die signifikante Festigkeitssteigerung von vergüteten, hochfesten Feinkornbaustählen mit einer Nominalstreckgrenze ≥ 690 MPa unerlässlich. Normvorgaben zur chemischen Zusammensetzung geben dabei nur obere Grenzwerte für die Hersteller vor. Weiterhin wirken sich bereits kleine Abweichungen in der Legierungsroute teilweise drastisch auf die mechanischen Eigenschaften aus. Somit wird eine adäquate Vorhersage der Schweißeignung und der Integrität der Schweißverbindung aufgrund der variierenden Mikrogefüge erschwert bis unmöglich. Unerwünschte Nebeneffekte sind die mögliche Erweichung der Wärmeeinflusszone (WEZ) als auch der gegenteilige Effekt der Aufhärtung. Vor diesem Hintergrund werden erstmals systematisch die unterschiedlichen Mikrolegierungsrouten mit variierenden Ti und Nb-Gehalten an Versuchsschmelzen untersucht. Die Stahlgüte S690QL bildet dabei die Grundlage der chemischen Zusammensetzung sowie der entsprechenden Wärmebehandlung. Zur Untersuchung der jeweiligen Schweißeignung wurden Dreilagen-Schweißungen mittels moderner MAG-Hochleistungsschweißprozesse durchgeführt und kritische Gefügebereiche mit hoher Erweichung/Aufhärtung identifiziert. Der Fokus der analytischen Betrachtungen lag hier auf der Identifikation der Phasenumwandlungen beim Abkühlen und auf dem metallurgischen Ausscheidungsverhalten. Zusätzlich wurden isotherme und nicht-isotherme Phasenberechnungen mit der Software Thermo-Calc durchgeführt. Mechanisch-technologische Untersuchungen zur Kerbschlagzähigkeit mittels Kerbschlagbiegeversuchen durchgeführt wurden, bestätigen dabei die Ergebnisse der thermodynamischen Simulation bezüglich des Ausscheidungsverhaltens während der Temperatur-Zeit Schweißzyklen. Daraus lässt sich der Einfluss der Wärmeeinwirkung beim Schweißen auf die Gefügeausbildung in der WEZ und der korrespondierenden mechanischen Eigenschaften qualitativ beschreiben.
Offshore wind turbines continuously increase in size and weight and demand adequate offshore foundations concepts like monopiles, tripods, or jackets. These components are typically constructed using submerged arc welding (SAW) with high-strength thick steel plates like the S420ML. During welding, the occurrence of delayed hydrogen-assisted cracking (HAC) must be anticipated. HAC is a critical combination of the local hydrogen concentration within a susceptible microstructure under certain mechanical load, i.e., the occurring (welding) residual stresses. The welding sequence of the thick-walled plates complicates the residual stress distribution due to the necessary repeated thermal cycling, i.e., welding seam/layer deposition to fill the joint. For that purpose, SAW with two-wire-technique was used to weld a specially designed and prototype-like mock-up of a real component with a thickness of 50 mm, filled with over 20 passes and a seam length of 1000 mm. Additional welded stiffeners simulated the effect of a high restraint, to achieve critical HAC conditions. The necessity of a minimum waiting time (MWT) before the NDT can be conducted (to exclude HAC) was critically verified by the application of ultrasonic testing of the welded joint at different time-steps of the NDT of up to 48 h after the completion welding. The residual stresses were determined by a robot XRD goniometer. Tensile residual stresses up to the yield limit are found both in the weld metal and in the heat-affected zone. Numerical modeling allowed the qualitative estimation of the hydrogen diffusion in the weld. No noticeable HAC occurrence was identified and confirms the high cracking resistance of the investigated material. Finally, the applicability of the MWT concept should be critically discussed.
Steelmaking slag is a by-product of steel production, of which 4.5 Mt were produced in 2020 in Germany alone. It is mainly used in road construction, earthwork and hydraulic engineering. A smaller part is returned to the metallurgical cycle, used as fertiliser or landfilled.
With this use, iron oxides still contained in steelmaking slag are lost. In addition, the possibility of producing higher-grade products from steelmaking slag is foregone. In recent decades, many researchers have investigated the production of Portland cement clinker and crude iron from basic oxygen furnace slags (BOFS) via a reductive treatment. Carbothermal treatment of liquid BOFS causes a reduction of iron oxides to metallic iron, which separates from the mineral phase due to its higher density. Simultaneously, the chemical composition of the reduced slag is adapted to that of Portland cement clinker.
In this study, German BOFS was reduced in a small-scale electric arc furnace using petrol coke as a reducing agent. The resulting low-iron mineral product has a similar chemical composition to Portland cement clinker and was rich in the tricalcium silicate solid solution alite (Ca3SiO5). Based on its chemical and mineralogical composition, similar to that of Portland cement clinker, the reduced BOFS has the potential to react comparably. In our study, the reduced BOFS produced less hydration heat than OPC, and its hydraulic reaction was delayed. However, adding gypsum has shown to accelerate the hydration rate of the reduced BOFS compared to that known from the calcium silicates of Portland cement clinker.
Further research to improve the hydraulic properties of the reduced slag is essential. If successful, producing a hydraulic binder and crude iron from BOFS has economic and ecological benefits for both the cement and steel industries.
Mikrolegierungselemente, wie Nb und Ti, sind für die signifikante Festigkeitssteigerung von vergüteten, hochfesten Feinkornbaustählen mit einer Nominalstreckgrenze ≥ 690 MPa unerlässlich. Normvorgaben zur chemischen Zu-sammensetzung geben dabei nur obere Grenzwerte für die Hersteller vor. Weiterhin wirken sich bereits kleine Abweichungen in der Legierungsroute teilweise drastisch auf die mechanischen Eigenschaften aus. Somit wird eine adäquate Vorhersage der Schweißeignung und der Integrität der Schweißverbindung aufgrund der variierenden Mikrogefüge erschwert bis unmöglich.
Die Nb-mikrolegierte Güte weist im Vergleich zur Ti-mikrolegierten Güte eine bessere Anlassbeständigkeit auf. Eine divergente Phasenverteilung in den äußeren Zonen der WEZ der Fülllagen erklärt die unterschiedliche Härteverteilung in der WEZ der drei untersuchten Legierungen und die markanten Unterschiede der Kerbschlagzähigkeit. Die quasistatischen Querzugversuche mittels DIC zeigten ein divergentes lokales Dehnungsverhalten auf. Die Ti-mikrolegierte Stahlsorte zeigt ein signifikanten lokales Dehnungsverhalten in der WEZ, wobei hier sich aufgrund der hohen metallurgischen Kerbwirkung Makrostützeffekte während des plastischen Fließens in der WEZ auftreten.
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.
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.
Hydrogen and its derivatives (e.g. ammonia) are considered as a suitable energy carrier in the future supply of renewable energy. Hydrogen transportation systems require pipes, valves and fittings, among other components. In this sense, austenitic stainless steels are commonly used structural materials for pure hydrogen applications. Stable austenitic alloys, like AISI 316L, are often assumed to be practically unsusceptible to hydrogen embrittlement. At the same time, a number of studies show the influence of hydrogen even in 316L under some circumstances. Some other studies state that this embrittlement could be avoided by using steel grades with a higher nickel equivalent which contributes to a more stable austenitic phase. Nonetheless, 316L is widely used in hydrogen atmospheres since many years because of lower costs and positive practical experience. For these reasons, not only 316L but also 304 could be further utilized by identifying the exact constraints.
With increasing demand for components regarding hydrogen applications, additive manufacturing technologies are getting increasingly important complementary to conventional manufacturing. In the context of additive manufacturing, 316L is a common material as well. The manufacturing process offers great advantages due to higher freedoms in design and the possibility for customized components in small batches. For example, valves with improved flow characteristics and reduced component weight can be produced. Nevertheless, there is still lack of experience and experimental results concerning additively manufactured parts under hydrogen service. Therefore, the influence on the material properties for additively manufactured parts in hydrogen environments needs to be further investigated.
In the present work, slow strain rate testing (SSRT) has been applied using hollow specimens. This testing procedure allows to perform practicable and faster in-situ tests in comparison to tests in autoclaves and investigate the influence of hydrogen on the mechanical properties.
Conventional AISI 304 and 316L specimens as well as additively manufactured 316L specimens were tested at room temperature and a pressure of 200 bar. Elongation at fracture and relative reduction of area (RRA) have been used to evaluate the influence of hydrogen. It is shown that the influence of hydrogen is more pronounced in 304 than in 316L. Furthermore, potentially influencing factors such as surface roughness, microstructure and porosity are discussed.