Degradation von Werkstoffen
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Currently, corrosion rates (CR) and/or corrosion products (CP) obtained for methanogen-induced microbiologically influenced corrosion (Mi-MIC) on carbon steel are mainly analyzed from static-incubations. By using a multiport-flow-column, much higher CRs (0.72 mm/yr) were observed, indicating static-incubations are not suitable for determining the corrosive potential of Mi-MIC. With the combination of various analytical methods (ToF-SIMS/SEM-EDS/SEM-FIB) and contrary to previously published data, we observed that CPs contained phosphorus, oxygen, magnesium, calcium and iron but lacked carbon-related species (e.g. siderite). Overall, siderite nucleation is disrupted by methanogens, as they convert aqueous bicarbonate into carbon dioxide for methanogenesis resulting in increased localized corrosion.
The importance of high-entropy alloy (HEAs) in the field of materials research is increasing continuously and numerous studies have been published, recently. These are mainly focused on manufacturing of different alloy systems having excellent structural properties from low to high temperatures. Therefore, HEAs are of high potential for many applications in very demanding conditions. However, this is so far limited by poor knowledge and experience regarding economic and reliable component manufacturing. The processability of HEAs has hardly been investigated so far, indicated by the small number of publications worldwide: welding <30 and machining <5.
Hence, this contribution provides an overview about the current state of the art on processing of HEAs. Fundamental principles are shown for safe weld joints while ensuring high component integrity. For safe welding, the combined consideration of complex interactions of material, construction and process is necessary. Recent studies on different HEAs showed the influence of heat input by means of different welding processes on the microstructure and respective properties. Based on intensive literature survey and on our initial study, the main research objectives of processing HEAs are presented.
Hochentropie Legierungen (engl. High Entropy Alloys, HEAs) sind eine relativ neue Werkstoffklasse. Seit ersten Veröffentlichungen im Jahr 2004, steigt das Forschungsinteresse an diesem Werkstoffkonzept stetig an. Im Gegensatz zu herkömmlichen Legierungen bestehen HEAs aus fünf Legierungselementen in äquiatomaren Gleichgewicht. Der Hochentropie-Effekt ist dabei u.a. auf die erhöhte Konfigurationsentropie zurückzuführen, der die Mischkristallbildung fördert. Viele HEAs weisen aufgrund hervorragender struktureller Eigenschaftskombinationen von sehr tiefen bis zu hohen Temperaturen enormes Anwendungspotential auf. Für ihre Anwendung als reale Bauteile stellt sich aber die zentrale Frage der Anwendbarkeit von trennenden Fertigungstechnologien für HEAs. Dies findet in der bisherigen weltweiten Materialforschung bisher kaum Beachtung. Für die Forderung nach wirtschaftlicher Bauteilfertigung ist für potenzielle Anwendungsbereiche, bspw. in der Energietechnik, eine zuverlässige und sichere Verarbeitung von wesentlicher Bedeutung. Fräsen ist dabei ein Standardprozess für die zerspanende Bearbeitung von Metallen. Der vorliegende Beitrag stellt Ergebnisse durchgeführter Zerspanbarkeitsanalysen vor. Diese konzentriert sich auf die aus dem Fräsprozesse resultierende Oberflächenintegrität an einem sogenannten „Cantor-HEA“ (mit der Zusammensetzung Co20Cr20Fe20Mn20Ni20). Hierfür wurden Untersuchungen mit konventionellem Kugelkopffräsen durchgeführt und mit dem an der BAM Berlin verfügbaren innovativen Hybridverfahren, dem ultraschallunterstützten Fräsen (engl. Ultrasonic Assisted Milling, USAM), verglichen. USAM verspricht dabei eine geringere Degradation der Oberflächeneigenschaften aufgrund geringerer Belastungen auf die Werkstückoberfläche beim Spanen. Dazu wurden grundlegende Fräsparameter (Schnittgeschwindigkeit und Zahnvorschub) systematisch variiert und während der Fräsexperimente die Zerspankräfte gemessen, deren anschließende Analyse ein Verständnis für die mechanischen Beanspruchungen ermöglicht, die auf Werkzeug und Bauteiloberfläche wirken. Diese Beanspruchungen bedingen eine topographische, mechanische und mikrostrukturelle Beeinflussung der Oberfläche und letztlich der Oberflächenintegrität. Zur deren Charakterisierung wurden Licht- und Rasterelektronen-mikroskopie eingesetzt, sowie die Rauheit mittels 3D-Mikroskop und die Eigenspannungen mittels Röntgendiffraktion gemessen. Die Ergebnisse belegen einen signifikanten den positiven Effekt beim USAM, insbesondere durch reduzierte Zerspankräfte im Vergleich zum konventionellen Kugelkopffräsen. Dies führt zu geringerer mechanischer Beanspruchung von Werkzeug und Oberfläche verbunden mit geringeren Zugeigenspannungen an und unter der Oberfläche und bewirkt schließlich eine wesentlich höhere Oberflächenintegrität.
Efficiency and flexibility are currently a major concern in the design of modern power plants and chemical processing facilities. The high requirements for economic profitability and in particular climate change neutrality are driving this development. Consequently, plant equipment and chemical reactor components are designed for higher operating pressure and temperature. Creep-resistant CrMo steels had been used as constructional materials for decades but came to operational limitations, for example the resistance against so-called high-temperature hydrogen attack in petrochemical reactors. For that purpose, 20 years ago V-modified CrMo steels had been developed for use in the petrochemical industry due to their very good creep-strength and hydrogen pressure resistance at elevated temperatures enabling long service life of the respective components. For example, the 13CrMoV9-10 steel is applicable for process temperatures of up to 482 °C and hydrogen pressures of up to 34.5 MPa.
Due to the large dimensions and wall thickness of the reactors (wall thickness up to 475 mm) and the special alloy concept, reliable weld manufacturing of the components is extremely challenging. First, low toughness and high strength of the weld joint in the as-welded condition are critical regarding weld cracking. High welding residual stresses are the result of the highly restrained shrinkage of the component welds. For this purpose, the entire component must be subjected to Post-Weld Heat Treatment (PWHT) after completion of the welding operation. The aim is to increase the toughness of the weld joints as well as to reduce the welding induced residual stresses. Before and during PWHT, extreme caution is required to prevent cracking. Unfortunately, V-modified CrMo steels possess an increased susceptibility to cracking during stress relaxation the so-called stress relief cracking (SRC).
Available literature studies have largely focused on thermal and metallurgical factors. However, little attention has been paid on the influence of the welding procedure on crack formation during PWHT considering actual manufacturing conditions. For that reason, we investigated in our previous studies (part I and II), the influence of heat control on the mechanical properties by simulating actual manufacturing conditions prevailing during the construction of petrochemical reactors using a special 3D- acting testing facility. The focus of part I was put on the influence of the welding heat control on mechanical stresses and the effect on cracking during PWHT. Part II was mainly dedicated to the metallurgical causes of SRC during PWHT and the interaction with the occurring mechanical stresses. It could be shown that not only high welding-induced stresses due to increased weld heat input cause higher susceptibility for SRC formation. It was further intensified by an altered precipitation behaviour in presence of mechanical stresses that are caused by the component related restraint. The present part III shows how residual stresses, which are present in such welded components and significantly influence the crack formation, can be transferred to the laboratory scale. As a result, the effect on the residual stresses on the SRC behaviour can be evaluated on simplified small-scale specimens instead of expensive mock-ups. For this purpose, experiments with test set-ups at different scales and under different rigidity conditions were designed and carried out.
High-strength structural steels are used in machine, steel, and crane construction with yield strength up to 960 MPa. However, welding of these steels requires profound knowledge of three factors in terms of avoidance of hydrogen-assisted cracking (HAC): the interaction of microstructure, local stress/strain, and local hydrogen concentration. In addition to the three main factors, the used arc process is also important for the performance of the welded joint. In the past, the conventional transitional arc process (Conv. A) was mainly used for welding of high-strength steel grades. In the past decade, the so-called modified spray arc process (Mod. SA) has been increasingly used for welding production. This modified process enables reduced seam opening angles with increased deposition rates compared with the Conv. A. Economic benefits of using this arc type are a reduction of necessary weld beads and required filler material. In the present study, the susceptibility to HAC in the heat-affected zone (HAZ) of the high-strength structural steel S960QL was investigated with the externally loaded implant test. For that purpose, both Conv. A and Mod. SA were used with same heat input at different deposition rates. Both conducted test series showed same embrittlement index “EI” of 0.21 at diffusible hydrogen concentrations of 1.3 to 1.6 ml/100 g of arc weld metal. The fracture occurred in the HAZ or in the weld metal (WM). However, the test series withMod. SA showed a significant extension of the time to failure of several hours compared with tests carried out with Conv. A.
Recherche verschiedener jeweils nationaler/internationaler Regelwerke
und Prozeduren für die Systematische Schadensanalyse
• Literaturrecherche zu Methoden der systematischen interdisziplinären Schadensanalyse
• Vergleich der Regelwerke VDI 3822, ASTM, ASM sowie der Methoden
• Anwendung der Regelwerke/Prozeduren und Methoden am Beispiel
High Entropy Alloys (HEAs) are a recent class of materials. In contrast to conventional alloys, HEAs consist of five alloying elements in equiatomic equilibrium. The high entropy effect is due, among other things, to the increased configuration entropy, which promotes solid solution formation. Many HEAs have enormous application potential due to excellent structural property combinations from very low to high temperatures. For the introduction of HEAs in real components, however, the question of the applicability of machining production technologies for component manufacture is of central importance. This has so far received Little attention in global materials research. Reliable and safe processing is essential for the demand of economical component production for potential areas of application, e.g. in power plant technology.
For metals, milling is the standard machining process. This article presents the results of machining analyses. It focuses on the surface integrity resulting from the milling process on a Co20Cr20Fe20Mn20Ni20-HEA. For this purpose, investigations were carried out using ball nose end milling tools for conventional milling process in comparison to an innovative hybrid process available at BAM Berlin, Ultrasonic-Assisted Milling (USAM). USAM promises a lower Degradation of the surface properties due to lower loads on the workpiece surface during machining.
For this purpose, basic milling parameters (cutting speed and tooth feed) were systematically varied and cutting forces were measured during the milling experiments. The subsequent Analysis of these forces allows an understanding of the mechanical loads acting on the tool and component surface. These loads cause topographical, mechanical and microstructural influences on the surface and consequently on the surface integrity. For their characterization, light and scanning electron microscopy were used, and the roughness and residual stresses via X-ray diffraction were measured. The results indicate significant advantages using USAM, especially due to reduced cutting forces compared to the conventional milling process. This causes lower mechanical loads on the tool and surface, combined with lower tensile residual stresses on and below the surface, and ultimately results in a significantly enhanced surface integrity.
Hochentropie-Legierungen (HEAs) zeichnen sich durch einen Mischkristall-System aus mindestens fünf und Mittelentropie-Legierungen (MEAs) durch mindestens drei Hauptlegierungselemente aus, in äquiatomarer Zusammensetzung. Sie zeigen außergewöhnliche Anwendungseigenschaften, wie z.B. hohe Festigkeit, Duktilität oder Korrosionsbeständigkeit. Zukünftige HEA/MEA-Komponenten aufgrund ihrer Eigenschaften für wasserstoffhaltige Umgebungen (wie Behälter für kryogene oder Hochdruckspeicherung) von Interesse. Daher ist die Bewertung der Wasserstoffabsorption und die Diffusion in diesen Materialien von großer Bedeutung. Dazu wurden in unserer Studie eine CoCrFeMnNi-HEA und eine CoCrNi-MEA untersucht. Die Proben wurden elektrochemisch mit Wasserstoff beladen. Für die Ermittlung des Wasserstoffdiffusionsverhaltens wurde die thermische Desorptionsanalyse (TDA) mit unterschiedlichen Heizraten bis zu 0,250 K/s angewandt. Die nachfolgende Peakentfaltung der Signale führte zu Hochtemperatur-Desorptionsspitzen und Wasserstofftrapping auch über 280°C. Eine resultierende Gesamtwasserstoffkonzentration > 40 ppm wurde für den MEA ermittelt und > 100 ppm für den HEA. Dies deutet auf zwei wichtige Effekte hin:
(1) verzögerte Wasserstoffdiffusion und (2) eine beträchtliche Menge an getrapptem Wasserstoff auch bei hoher Temperatur. Beide Effekte können hinsichtlich einer wasserstoffunterstützten Rissbildung kritisch werden, dies erfordert jedoch weitere Untersuchungen. Zusätzlich erfolgte die Bestimmung des lokalen Volta-Potentials mittels hochauflösender Kelvin-Sonden-Kraft-Mikroskopie (SKPFM). Die ermittelten Scans zeigen einen bestimmten Einfluss der Wasserstoffbeladung auf die Potentiale.
HEAs represent a relatively new class of materials. The the alloy concept is fundamentally different from the most conventional materials and alloys that are used today. Recently, the focus of HEA designs is more application-based. For that purpose, the elements of interest are carefully selected and multiple phases as well as micro-structures are deliberately adjusted. Currently, only limited attention has been paid to weldability of HEA. This encompasses possible effects on metallurgy and its influence on the desired properties. It remains open if welding causes e.g. considerable number of intermetallic phases or segregations and their effect on weld joint properties. For that reason, the scope of this study is to summarize already available studies on welding of HEAs with respect to the HEA-type, the applied welding process and its influence on the weld joint properties.
Hydrocarbons fuel our economy. Furthermore, intermediate goods and consumer products are often hydrocarbon-based. Beside all the progress they made possible, hydrogen-containing substances can have severe detrimental effects on materials exposed to them. Hydrogen-assisted failure of iron alloys has been recognised more than a century ago. The present study aims to providing further insight into the degradation of the austenitic stainless steel AISI 304L (EN 1.4307) exposed to hydrogen. To this end, samples were electrochemically charged with the hydrogen isotope deuterium (2H, D) and analysed by scanning electron microscopy (SEM), electron back-scatter diffraction (EBSD) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). It was found that deuterium caused a phase transformation from the original γ austenite into ε- and α’-martensite. Despite their low solubility for hydrogen, viz. deuterium, the newly formed phases showed high deuterium concentration which was attributed to the increased density of traps. Information about the behaviour of deuterium in the material subjected to external mechanical load was gathered. A four-point-bending device was developed for this purpose. This allowed to analyse in-situ pre-charged samples in the ToF-SIMS during the application of external mechanical load. The results indicate a movement of deuterium towards the regions of highest stress.
Welded components of P91 9% Cr steel demand for careful welding fabrication with necessary post weld heat treatment (PWHT). Before the PWHT, a hydrogen removal heat treatment is necessary for avoidance of hydrogen assisted cracking (HAC). In this context, the microstructure and temperature-dependent hydrogen diffusion is important, and reliable diffusion coefficients of P91 weld metal are rare. For that reason, the diffusion behavior of P91 multi-layer weld metal was investigated for as-welded (AW) and PWHT condition by electrochemical permeation experiments at room temperature and carrier gas hot extraction (CGHE) from 100 to 400 °C. Hydrogen diffusion coefficients were calculated, and the corresponding hydrogen
concentration was measured. It was ascertained that both heat treatment conditions show significant differences. At room
temperature the AW condition showed significant hydrogen trapping expressed by to seven times lower diffusion coefficients. A preferred diffusion direction was found in perpendicular direction expressed by high permeability. The CGHE experiments
revealed lower diffusion coefficients for the AW condition up to 400 °C. In this context, a hydrogen concentration of approximately 21 ml/100 g was still trapped at 100 °C. For that reason, a certain HAC susceptibility of as-welded P91 weld metal cannot
be excluded, and hydrogen removal should be done before PWHT.