5 Werkstofftechnik
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- 5.1 Mikrostruktur Design und Degradation (40) (entfernen)
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Low cost, high-efficiency catalysts towards water splitting are urgently required to fulfil the increasing demand for energy. In this work, low-loading (<20 wt%) Ni-confined in layered metal oxide anode catalysts (birnessite and lepidocrocite titanate) have been synthesized by facile ion exchange methodology and subjected to systematic electrochemical studies. It was found that Ni-intercalated on K-rich birnessite (Ni-KMO) presents an onset overpotential (ηonset) as low as 100 mV and overpotential at 10 mA cm−2 (η10) of 206 mV in pH = 14 electrolyte. By combining electrochemical methods and X-ray absorption and emission spectroscopies (XAS and XES), we demonstrate Ni sites are the active sites for OER catalysis and that the Mn3+ sites facilitate Ni intercalation during the ion-exchange process, but display no observable contribution towards OER activity. The effect of the pH and the nature of the supporting electrolyte on the electrochemical performance was also evaluated.
A set of some unexpected and interesting microstructures has put the so-called complex concentrated alloys (CCAs) in the eye of the scientific community. The AlMo0.5NbTa0.5TiZr refractory (r)CCA, aimed at substituting Ni-base superalloys in gas turbine applications, belongs to this alloy family. After a two-stage heat treatment, this rCCA morphologically resembles the typical a two-phase microstructure of the latter. The objective of this work consists in determining the effect of the two stages of the heat treatment on the microstructure of the AlMo0.5NbTa0.5TiZr alloy to eventually improve it in terms of homogeneity and porosity.
Development and characterization of starch film and the incorporation of silver nanoparticles
(2020)
Starch is one of the biopolymers being used for bioplastic synthesis. For production, starch can be combined with different plasticizers, starches from different plant sources and even with nanomaterials to improve or to add film properties. The challenge of adding these, e.g. in the form of silver nanoparticles (AgNp) is to determine the concentration so as to avoid impairing the properties of the film, agglomeration or altering the visual characteristics of the film. In this study, a starch film synthesis route and the incorporation of silver nanoparticles has been proposed in order not to alter the properties of the film while maintaining the transparency and a clear colour of the starch film. The results showed that the proposed synthesis route is promising, efficient, reproducible, fast and the film has good mechanical properties.
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
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.
This contribution provides current findings regarding materials susceptibility for CCUS applications. Basing on results gathered in 2 German long-term projects (COORAL and CLUSTER) suitable materials are introduced as well as dominating impurities of the CO2 stream and corrosion mechanisms. Investigations cover the whole CCUS process chain and provide the following recommendations for certain parts. Commercially available carbon steels are suitable for compression and pipelines as long as moisture content and impurities are limited (water 50 to 100 ppmv, SO2 and NO2 ca. 100 ppmv).
Corrosion rates increase with increasing water content (0.2 – 20 mm/a).
Condensation of acids and therefore droplet formation is always possible, even at low water contents.
A low SO2 content within the CO2-stream might be more important than a low water content.
Cr13-steels showed a general susceptibility to shallow pitting and pitting. So, they seem to be not suitable for CCUS applications.
Low alloyed steels showed better corrosion behavior (predictable uniform corrosion).
For direct contact with saline aquifer fluids only high alloyed steels shall be used.
Carbon Capture Utilization and Storage (CCUS) is a promising technology to reach the target for reduction of CO2 emissions. Crucial points for a sustainable and future-proof CCUS system are reliability and cost efficiency of the whole process chain, including separation of CO2 from the source, compression of CO2, its subsequent transportation to the injection site and injection into geological formations, e.g. aquifers. Recent studies have shown that even at a very low concentration of impurities, condensation of sulfuric and nitric acids in dense phase CO2 are possible and observable. Thus, impact of impure CO2 stream toward corrosion susceptibility of materials to be used in CCUS system need to be considered. In this talk, basing on results achieved from two German long-term projects (COORAL and CLUSTER), the dominating impurities of the CO2 stream and corrosion mechanisms are addressed. Investigations cover the whole CCUS process chain and provide a material recommendation for certain parts.
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.
Fracture mechanics is a key to fatigue assessment in AM metal components. Short fatigue cracks are initiated at defects and pronounced surface roughness intrinsic to AM. The subsequent crack-propagation is strongly influenced by microstructural interactions and the build-up of crack-closure. The aim of the present study is to give an insight into short-crack propagation in AM-metals. Fatigue crack propagation resistance curves were determined experimentally for AISI 316L manufactured by Laser Powder Bed Fusion (L-PBF) which was heat treated at three different temperatures. Differences in the build-up of the fatigue-crack propagation threshold in between the L-PBF specimens and compared to wrought material are due to the residual stress states, a pronounced roughness of the crack-faces in the L-PBF specimens and phase transformation in the vicinity of the crack-tip, resulting in increased crack-closure. This, together with crack-branching found along the crack path, enhances the resistance to the propagation of fatigue cracks.
The high-entropy alloy (HEA) CrMnFeCoNi and the medium-entropy alloy (MEA) CrCoNi with a face-centered cubic (fcc) structure have excellent mechanical properties and are considered for high-temperature applications. Both materials were exposed under several oxidized atmospheres in a wide temperature range/regime. Mn-oxide (Mn3O4, Mn2O3) was mainly formed on the HEA and Cr2O3 on the MEA. The fast diffusion of manganese prevents the formation of a continuous chromia layer on CrMnFeCoNi in Ar-O2, Ar-H2O and Ar-SO2 at 800°C.
The Cantor alloy and his ternary subsystem CrCoNi were exposed in Ar-O2-H2O-SO2 at 800°C up to 96 h to clarify their oxidation behavior in a mixed atmosphere. The oxidized samples were analyzed by weight measurement, scanning electron microscopy (SEM), and X-ray diffraction analysis (XRD). It was found that mass gain of all samples increased with increasing exposure time. The oxidation rate of the Cantor alloy is significantly higher than that of the ternary alloy system.
Eine kritische Aufgabe im Rahmen der Etablierung von Prozess-Struktur-Eigenschafts-Performance-Beziehungen bei der additiven Fertigung (AM) von Metallen ist die Ermittlung von zuverlässigen und gut dokumentierten Kennwerten zum Materialverhalten sowie das Schaffen von Wissen über die Struktur-Eigenschafts-Korrelation. Schließlich ist dies die Grundlage für die Entwicklung gezielterer Prozessoptimierungen und zuverlässigerer Lebensdauer-Vorhersagen. In diesem Zusammenhang zielt dieser Beitrag darauf ab, Daten und Erkenntnisse über das Kriechverhalten des austenitischen Edelstahls 316L zu liefern, der mittels Laser-Powder-Bed-Fusion (L-PBF) hergestellt wird. Um dieses Ziel zu erreichen, wurden Proben aus konventionellem warmgewalztem sowie AM-Material gemäß den bestehenden Normen für konventionelles Material geprüft und vor und nach dem Versagen mikrostrukturell charakterisiert. Die Probekörper wurden aus einzelnen Blöcken des AM-Materials gefertigt. Die Blöcke wurden mit einer Standard-Scan- und Aufbaustrategie hergestellt und anschließend wärmebehandelt. Das Kriechverhalten wird anhand der Kriechlebensdauer und ausgewählter Kriechkurven und Kennwerte beschrieben und vergleichend bewertet. Der Einfluss von Defekten und Mikrostruktur auf das Materialverhalten wird anhand von zerstörenden und zerstörungsfreien Auswertungen an ausgewählten Proben analysiert. Der AM-Werkstoff zeigt kürzere Kriechlebensdauern, erreicht das sekundäre Kriechstadium deutlich schneller und bei geringerer Dehnung und weist eine geringere Kriechduktilität im Vergleich zu seinem konventionellen Gegenstück auf. Das Kriechschädigungsverhalten des AM-Werkstoffs ist eher mikrostruktur- als defektgesteuert und ist durch die Bildung intergranularer Kriechrisse gekennzeichnet. Als kritische Merkmale werden die Versetzungsdichte sowie die Versprödung der Korngrenzen identifiziert. Die Mikro-Computertomographie (µCT) erweist sich als Alternative zur Metallographie, um die Kriechschädigung zu analysieren.
Creep and fracture behavior of conventionally and additively manufactured stainless steel 316L
(2020)
A critical task within the frame of establishing process-structure-property-performance relationships in additive manufacturing (AM) of metals is producing reliable and well-documented material behavior’s data and knowledge regarding the structure-property correlation, including the role of defects. After all, it represents the basis for developing more targeted process optimizations and more reliable predictions of performance in the future. Within this context, this contribution aims to close the actual gap of limited historical data and knowledge concerning the creep behavior of the widely used austenitic stainless steel 316L, manufactured by Laser-Powder-Bed-Fusion (L-PBF). To address this objective, specimens from conventional hot-rolled and AM material were tested under application-relevant conditions according to existing standards for conventional material, and microstructurally characterized before and after failure. The test specimens were machined from single blocks from the AM material. The blocks were manufactured using a standard scan and build-up strategy and were subsequently heat-treated. The creep behavior is described and comparatively assessed based on the creep lifetime and selected creep curves and characteristic values. The effect of defects and microstructure on the material’s behavior is analyzed based on destructive and non-destructive evaluations on selected specimens. The AM material shows shorter creep lives, reaches the secondary creep stage much faster and at a lower strain, and features lower creep ductility compared to its conventional counterpart. The creep damage behavior of the AM material is more microstructure than defect controlled and is characterized by the formation and accumulation of single intergranular damage along the whole volume. Critical features identified are the grain morphology and the grain-boundary as well as the dislocation’s density. Micro-computed tomography (µCT) proves to be an alternative to metallography to analyze the creep damage.
Early Stage of Corrosion Formation on Pipeline Steel X70 Under Oxyfuel Atmosphere at Low Temperature
(2020)
The early stage of corrosion formation on X70 pipeline steel under oxyfuel atmosphere was investigated by applying a simulated gas mixture (CO2 containing 6700 ppmv O2, 100 ppmv NO2, 70 ppmv SO2 and 50 ppmv H2O) for 15 h at 278 K and ambient pressure. Short-term tests (6 h) revealed that the corrosion starts as local spots related to grinding marks progressing by time and moisture until a closed layer was formed. Acid droplets (pH 1.5), generated in the gas atmosphere, containing a mixture of H2SO4 and HNO3, were identified as corrosion starters. After 15 h of exposure, corrosion products were mainly X-ray amorphous and only partially crystalline. In-situ energy-dispersive X-ray diffraction (EDXRD) results showed that the crystalline fractions consist primarily of water-bearing iron sulfates. Applying Raman spectroscopy, water-bearing iron nitrates were detected as subordinated phases. Supplementary long-term tests exhibited a significant increase in the crystalline fraction and formation of additional water-bearing iron sulfates. All phases of the corrosion layer were intergrown in a nanocrystalline network. In addition, numerous globular structures have been detected above the corrosion layer, which were identified as hydrated iron sulphate and hematite. As a type of corrosion, shallow pit formation was identified, and the corrosion rate was about 0.1 mma−1. In addition to in-situ EDXRD, SEM/EDS, TEM, Raman spectroscopy and interferometry were used to chemically and microstructurally analyze the corrosion products.
This poster presents the focused ion beam preparation methodologies developed within the framework of the EU funded EURAMET project ADVENT (Advanced Energy-Saving Technology).
It summarises the key breakthroughs achieved for various in situ investigation techniques, e.g. in situ experiments at the Synchrotron facility BESSY II (IR-SNOM and XRS), TEM and SMM instrumentation.
The created experimental devices from diverse thin-film semiconductor materials paved the way to dynamic structural studies bearing the potential to determine nanoscale correlations between strain and electric fields and, moreover, for the fundamental development of new in situ capabilities.
For the first time, structure−electrochemical relationships of thin films of a plasma-polymerized acrylic acid/carbon dioxide AA/CO2 (75/25%) copolymer modified by implanted silver nanoparticles are discussed. The pulsed plasma polymerization of AA/CO2 was utilized and adjusted to obtain a maximal amount of COOH Groups forming an almost uncross-linked polymer structure. The prepared polymer layer is rinsed by a silver nitrate solution to impregnate Ag+ ions. This step is followed by its reduction of Ag+ with NaBH4 as a chemical route in comparison to the reduction by sunlight as an ecofriendly photoreduction method. The chemical composition and morphology of the topmost surface layer of the AA/CO2 polymer thin film were investigated by X-ray photoelectron spectroscopy and atomic force microscopy. Moreover, the molecular mobility, conductivity, and thermal stability of the polymer layer were analyzed using broadband dielectric spectroscopy. The dielectric properties of the AA/
CO2 polymer thin film were studied in the presence of Ag+ ions or Ag0. It was found that a cross-linked polymer layer with a smooth surface and high conductivity was obtained in the presence of Ag+/ Ag0.
The 13CrMo4-5 ferritic steel is commonly used in power plants, due to its favorable mechanical properties. According to EN 10028-2, this steel can be used at temperatures up to 570°C because of its creep behavior. The inefficient corrosion resistance limits the application of this steel to lower temperatures depending on the gas temperature and slag formation. Therefore, the application of a highly resistant Ni-based coating is proposed to extend the corrosion resistance of elements made of ferritic steel. The corrosion test was performed in an environment containing a mixture of gases, like O2, COx, and SOx, and deposited ashes with elements, e.g., Na, Cl, Ca, Si, C, Fe, and Al. The exposure time was, respectively, 240 h, 1000 h and 4500 h at a temperature of 600°C. The oxide scale formed on the 13CrMo4-5 steel was significantly thicker than on the IN686 coating. The microstructure and chemical and phase compositions of the oxide scale were investigated using light optical microscopy together with scanning and transmission electron microscopy techniques. Energy dispersive x-ray analyses were performed when appropriate.
Development and characterization of starch film and the incorporation of silver nanoparticles
(2020)
Starch is one of the biopolymers being used for bioplastic synthesis. For production, starch can be combined with different plasticizers, starches from different plant sources and even with nanomaterials to improve or to add film properties. The challenge of adding these, e.g. in the form of silver nanoparticles (AgNp) is to determine the concentration so as to avoid impairing the properties of the film, agglomeration or altering the visual characteristics of the film. In this study, a starch film synthesis route and the incorporation of silver nanoparticles has been proposed in order not to alter the properties of the film while maintaining the transparency and a clear colour of the starch film. The results showed that the proposed synthesis route is promising, efficient, reproducible, fast and the film has good mechanical properties.
Fatigue failure of a component can occur at service loads considerably lower than the yield strength of the material. Under fatigue loading condition, the material in the vicinity of the tip of a propagating crack repeatedly deforms plastically, leaving microscopic marks on the crack surface, commonly known as fatigue striations. Counting and measuring fatigue striations is a method in estimating the number of loading cycles a component went through until fracture. Some studies suggest a one-to-one relation between the number of fatigue striations and the number of load cycles, but this relation is still debatable, given that there are many factors influencing the formation of those striations. The main purpose of this work is to analyze the influence of microstructure and mechanical strength on the formation of fatigue striations in structural steels, in order to understand how these material properties are related to the fatigue crack behavior. For such, standard Charpy-V samples were subjected to hardness, fatigue and impact testing. Metallography was performed to characterize the microstructure, and a fractographic analysis by using optical and scanning electron microscopy was carried out to investigate the fracture surface. This study shows that steels with higher ductility have a closer one-to-one relation than those with a higher tensile strength. Above a certain level of tensile strength, fatigue striations do form rarely or completely disappear.
An extensive set of information about the diffracting volume is carried by EBSD patterns: the crystal lattice, the reciprocal lattice, the crystal structure, the crystal symmetry, the mean periodic number of the diffracting phase, the source point from where it has been projected (projection centre), the crystal orientation, the sample topography (local tilt), the (preparation) quality of defect density of the crystal, and possible pattern overlaps. Some of this information is used regularly in conventional EBSD analyses software while others are still waiting for a more widespread application. Despite the wealth of information available, the accuracy and precision of the data that are presently extracted from conventional EBSD patterns are often well below the actual physical limits. Using a selection of example applications, we will demonstrate the gain in angular resolution possible using relatively low-resolution patterns of approximately 20k pixels in combination with pattern matching (PM) approaches. In this way, fine details in a microstructure can be revealed which would otherwise be hidden in the orientation noise.
On the influence of crystallography on creep of circular notched single crystal superalloy specimens
(2020)
The present work contributes to a better understanding of the effect of stress multiaxiality on the creep behavior of single crystal Ni-base superalloys. For this purpose we studied the creep deformation and rupture behavior of double notched miniature creep tensile specimens loaded in three crystallographic directions [100], [110] and [111] (creep conditions: 950 °C and 400 MPa net section stress). Crystal plasticity finite element method (CPFEM) was used to analyze the creep stress and strain distributions during creep. Double notched specimens have the advantage that when one notch fails, the other is still intact and allows to study a material state which is close to rupture. No notch root cracking was observed, while microstructural damage (pores and micro cracks) were frequently observed in the center of the notch root region. This is in agreement with the FEM results (high axial stress and high hydrostatic stress in the center of the notched specimen). Twinning was observed in the notch regions of [110] and [111] specimens, and <112> {111} twins were detected and analyzed using orientation imaging scanning electron microscopy. The present work shows that high lattice rotations can be detected in SXs after creep fracture, but they are associated with the high strains accumulated in the final rupture event.