5 Werkstofftechnik
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Organisationseinheit der BAM
- 5.1 Mikrostruktur Design und Degradation (114) (entfernen)
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.
The Topic of the presentationis a discussion on defects which can cause failure in cyclically loaded metallic components. Although also touching Features such as material defects such as pores or micro-shrinkages, etc. and geometric defects such as surface roughness and secondary notches (which are not considered in the design process) which origin in manufacturing, and others the presentation concentrates on non-metallic inclusions. It is prefaced by an introduction to the life cycle of a fatigue crack from initiation up to fracture. Special emphasis is put on the fact that only cracks which are not arrested during one of their distinct Propagation stages can grow to a critical size.
Investigation of degradation of the aluminum current collector in lithium-ion batteries by GD-OES
(2022)
Lithium-ion batteries (LIBs) are one technology to overcome the challenges of climate and energy crisis. They are widely used in electric vehicles, consumer electronics, or as storage for renewable energy sources. However, despite innovations in batteries' components like cathode and anode materials, separators, and electrolytes, the aging mechanism related to metallic aluminum current collector degradation causes a significant drop in their performance and prevents the durable use of LIBs. Glow-discharge optical emission spectroscopy (GD-OES) is a powerful method for depth-profiling of batteries' electrode materials. This work investigates aging-induced aluminum deposition on commercial lithium cobalt oxide (LCO) batteries' cathodes. The results illustrate the depth-resolved elemental distribution from the cathode surface to the current collector. An accumulation of aluminum is found on the cathode surface by GD-OES, consistent with results from energy-dispersive X-ray spectroscopy (EDX) combined with focused ion beam (FIB) cutting. In comparison to FIB-EDX, GD-OES allows a fast and manageable depth-profiling. Results from different positions on an aged cathode indicate an inhomogeneous aluminum film growth on the surface. The conclusions from these experiments can lead to a better understanding of the degradation of the aluminum current collector, thus leading to higher lifetimes of LIBs.
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.
Diese Untersuchung beschäftigt sich mit der Charakterisierung von Kurzrisswachstum in mittels Laser-Pulverbett-Verschmelzen (LPBF - Laser Powder Bed Fusion) hergestelltem rostfreien austenitischen Stahl. Spezifischer wird die Ermittlung zyklischer R-Kurven untersucht. Diese beschreiben den Aufbau des Widerstands gegen Ermüdungsrisswachstum - d.h. des Schwellenwertes - aufgrund von Rissschließeffekten bei physikalisch kurzen Rissen. Mit Hilfe der zyklischen R-Kurven kann die Fähigkeit eines Bauteils, physikalisch kurze Risse zu arretieren, charakterisiert werden. Wir verfügen damit über eine Schnittstelle zwischen klassischer Ermüdung und Bruchmechanik. Das ist gerade auch für additiv gefertigte (AM – Additive Manufacturing) Materialien von Interesse. Diese weisen prozessintrinsische Defekte auf, die als Initiierungsstellen kurzer Ermüdungsrisse agieren. Im Rahmen der experimentellen Untersuchungen wurden zyklische R-Kurven für konventionellen und LPBF AISI-316L-Stahl ermittelt. Insbesondere wurde der Einfluss verschiedener Wärmebehandlungen (WB1: 450°C, WB2: 800°C und WB3: 900°C) auf das Wachstumsverhalten physikalisch kurzer Risse im LPBF-Material untersucht. Aufgrund hoher Eigenspannungen war die Ermittlung des Kurzrisswachstumsverhaltens bei WB1 nicht möglich. Für WB2 und WB3 ergaben sich sehr unterschiedliche zyklische R-Kurven. Untersuchungen der Eigenspannungen, der Bruchfläche (insbesondere der Rauheit) und der Mikrostruktur sollen die Ursachen für das unterschiedliche Verhalten erklären. Die Ergebnisse werden mit den Verhältnissen in konventionellem Material verglichen.
Das zyklische plastische Verformungsverhalten von additiv gefertigtem Edelstahl AISI 316L wurde in dehnungsgeregelten Kurzzeitfestigkeitsversuchen (LCF-Versuchen) untersucht. Dabei wurden zwei Wärmebehandlungszustände betrachtet: Beim ersten Zustand war die fertigungsbedingte zelluläre Struktur vorhanden, während sie durch die zweite Wärmebehandlung aufgelöst wurde. Untersuchungen im Transmissions-Elektronen-Mikroskop (TEM) zeigten, dass die zyklische Verformung die Zellstruktur lokal zerstörte und Gleitbänder entstanden, was die Entfestigung in diesem Fall erklärt. Für Material ohne Zellstrukturen resultierten nach zyklischer Verformung ähnliche Versetzungsstrukturen wie in konventionell gefertigtem (warmgewalzten) Material.
Several studies have been shown that the electron beam can be used to create nanomaterials from microparticle targets in situ in a transmission electron microscope (TEM). Here, we show how this method has to be modified in order to synthesize plasmonic gold nanoparticles (NPs) on insulating silicon oxide substrate by employing a scanning electron microscope with a comparatively low acceleration voltage of 30 kV. The synthesized NPs exhibit a random distribution around the initial microparticle target: Their average size reduces from 150 nm to 3 nm with growing distance to the initial Au microparticle target. Similarly, their average distance increases. The synthesized NP assemblies therefore show distinctly different plasmonic behaviour with growing distance to the target, which allows to study consequences of random hybridization of surface plasmon in disordered system, such as Anderson localization. To reveal the surface plasmons and their localization behaviour we apply electron energy loss spectroscopy in the TEM.
Several studies have shown that the electron beam (e-beam) can be used to create nanomaterials from microparticles in situ in a TEM. However, attempts to produce gold nanoparticles (NPs) on silicon oxide substrate remained to be accomplished. Here, we show that the production of gold NPs is possible by using the e-beam in a SEM, under a set of parameters. The NPs produced present a size gradient along the radial direction. A parameter study shows that the microparticles may: 1) flicker away without producing NPs, 2) fragment to form NPs and/or 3) react with the silicon oxide substrate, depending on the applied current. A hypothesis regarding the driving physical phenomena that lead the microparticles to fragment into NPs is discussed. Fabrication of gold NPs in the SEM provides a more cost-effective option as compared to the established method in the TEM.
Several studies have shown that the electron beam (e-beam) can be used to create nanomaterials from microparticles in situ in a TEM. However, attempts to produce gold nanoparticles (NPs) on silicon oxide substrate remained to be accomplished. Here, we show that the production of gold NPs is possible by using the e-beam in a SEM, under a set of parameters. To understand the physical mechanisms leading to the gold NPs, the mechanisms of e-beam induced charging as well as e-beam induced heating of the MPs were discussed. Several hints point to heating as the driving mechanism.
Gypsum (CaSO4∙2H2O), bassanite (CaSO4∙0.5H2O), and anhydrite (CaSO4) are essential evaporite minerals for the evolution of hyper-arid surface environments on Earth and Mars (Voigt et al. 2019; Vaniman et al. 2018). The formation mechanism of especially anhydrite has been a matter of scientific debate for more than a century (van’t Hoff et al. 1903). To date, there exists no model that can reliably predict anhydrite formation at earth’s surface conditions. While thermodynamics favor its formation, it is hardly achieved on laboratory time scales at conditions fitting either the Atacama Desert on Earth, or the surface of Mars (Wehmann et al. 2023). In light of most recent developments (e.g. Stawski et al. 2016), that advocate for a complex, non-classical nucleation mechanism for all calcium sulphates, we present an analysis of natural samples from the Atacama Desert to identify key features that promote the nucleation and growth of anhydrite under planetary surface conditions. Our analyses reveal at least three distinct anhydrite facies, with differing mineralogy and micro- to nano-structures. The facies are (1) aeolian deposits with sub-μm grain sizes, (2) (sub-)surface nodules that formed from aeolian deposits and (3) selenites with secondary anhydrite rims. Possible mechanisms of their formation will be discussed.
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.
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.
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.
The development of refractory chemically complex alloys (rCCAs) has been explored for potential use in high temperature applications. An example of this is the AlMo0.5NbTa0.5TiZr alloy. It was named as “high entropy superalloy” as it resembles the well-known γ/γ’ microstructure in Ni-Base superalloys with cuboidal particles embedded in a continuous matrix. However, the continuous phase in Ni Base alloys is an fcc solution and the cuboidal γ’ precipitates present the L12 intermetallic structure. On the opposite, this CCA has a reversed microstructure where the continuous matrix is formed by an ordered B2 phase which contains cuboidal precipitates of a disordered BCC phase. Some of the most importat results of microstructural analysis, creep test and oxidation are presented in the following work. The as-cast sample shows a bcc/B2 structure with hexagonal phase precipitates in amorphous state whereas the annealed sample also shows a combination of these phases but with larger bcc precipitates and a fully crystallized hexagonal intermetallic. It was found that porosity was higher in the annealed samples (Kinkerdall effect) and the hardness was higher in samples with faster cooling rate due smaller nanostructure. Norton plots show both diffusion and dislocation controlled deformation, and it was found different kinetics between dry and humid air oxidation with the presence of spallation.
The refractory chemically complex alloy (rCCA) AlMo0.5NbTa0.5TiZr, with a density of 7.4 g/cm3, shows a compressive ultimate strength of 772 MPa at 1000 °C, comparatively surpassing Ni-base and other rCCAs. Its dual-phase microstructure, with a high volume fraction (≈ 62%) of cuboidal and plate-like particles coherently embedded in a continuous matrix, resembles the well-known pattern of the γ/γ" in Ni-base superalloys. Its developers have thus implied that it could stand as structural alloy for high temperature (HT) applications. Here, we report the HT creep properties and the underlying microstructural changes of the rCCA AlMo0.5NbTa0.5TiZr to propose deformation and degradation micromecanisms for this regime. The material was produced by arc-melting and subsequently heat treated in argon: at 1400 °C for 24 h plus a hot isostatic pressure treatment at 1370 °C and 170 MPa for 4 h, with a cooling rate of 10 K/min. Miniaturized tensile specimens (≈ 28 x 7 x 2 mm) were cut and polished to a quality of 1 μm. Creep tests were conducted in vacuum in the respective temperature and stress range 800-1200 °C and 30-120 MPa. For observation, thin slices were extracted from the gauge length, away from the fracture surface, grinded to a thickness of 100 μm, and electropolished to electron transparency. The microstructure was observed on the electropolished specimens using scanning (S) as well as transmission (T) electron microscopy (EM). The Norton plot gives Norton exponents of about 3.1 and 3.2 for temperatures of 1000 and 1100 °C, respectively. Curiously, creep rate minima are very close for a stress level of 30. The starting microstructure reflects a macroscopically lean coarse grain structure and a microscopically fine-meshed basketweave structure with coherency dislocations only around coarsened particles usually close to subgrain boundaries. Results are discussed on the base of variations of this starting microstructure after interrupted and ruptured creep tests.
The chemically complex alloys (CCAs) that contain mostly refractory elements (rCCAs), may be highly resistant to heat and load, which makes them attractive candidates for use at extremely high temperatures associated with many technological applications, e.g. aeroengine turbines. However, the field of CCAs, especially their resistance in harsh (oxidative) and hot environment is still young and not much experimental evidence for the understanding mechanisms in this regime is available, which the proposed study addresses. For safe use in structural applications, in addition to their mechanical performance, the environmental resistance of this alloy is also critical. Surface degradation can significantly decrease the mechanical resistance during high temperature exposure, leading to premature failure. The AlMo0.5NbTa0.5TiZr rCCA only contains Al as a protection candidate and it is composed of a coherent B2/bcc nanoscopic cube-on-cube interweave and an hexagonal phase. The evaluation of the oxidation process in the AlMo0.5NbTa0.5TiZr rCCA in the heat-treated state has not been assessed yet. The proposed study focusses on a deeper understanding of the formation mechanism and growth kinetics of oxides at high temperature in the AlMo0.5NbTa0.5TiZr rCCA using synchrotron radiation. Due to the envisaged high temperature structural applications, the alloy is evaluated in an oxidation environment specifically between 800°C and 1000°C.
The development of refractory CCAs has been explored for potential use in high temperature applications. An example of this is the AlMo0.5NbTa0.5TiZr alloy, which resembles the well-known γ/γ’ microstructure in Ni-Base superalloys with cuboidal particles embedded in a continuous matrix. The aim of this work is to evaluate the alloy’s mechanical behavior under tension in the temperature range 800-1000°C, by applying creep tests under vacuum (excluding oxidation effects). Some little temperature influence on minimum creep rate @ 1000 and 1100 °C was found and at a first glance, and Norton plots shows that deformation is probably both diffusion and dislocation controlled. However, further work is needed to stablish deformation and degradation micro mechanisms in the studied creep regime.
Microstructural characterization of the AlMo 0.5 NbTa 0.5 ZrTi refractory complex concentrated alloy
(2020)
A set of some unexpected and interesting microstructures has put the so-called complex concentrated alloys (CCAs) in the eye of the scientific community and the AlMo0.5NbTa0.5TiZr refractory (r)CCA, aimed at substituting Ni-base superalloys in gas turbine applications, belongs to this alloy family. The AlMo0.5NbTa0.5TiZr rCCA was studied by SEM, EDX, EBSD and TEM, showing the presence of a nanoscopic basket-wave structure inside the grains, with two BCC phases. Additionally, thermodynamic calculations on the AlMo0.5NbTa0.5TiZr alloy were done with two different proprietary databases that anticipate two BCC-disordered phases with distinct constitutions as well as an HCP phase.
Ferritic high temperature alloys are widely used as boiler tube and heat exchanger materials in coal, biomass and co-fired power plants. All technologies have in common that the applied materials are exposed to different temperatures, process pressures and reactive atmospheres that lead to a change of the material properties and a further degradation of the material. Material changes caused by aging in highly corrosive and toxic gases such as SO2 are mainly studied ex situ after the reaction is finished. The solid material is deposited in the atmosphere for a certain period of time, and material changes are then examined by various microscopic techniques such as optical microscopy (OM), electron microprobe analysis (EMPA), scanning electron microscopy (SEM and TEM) and X-ray diffraction (XRD). Nevertheless, extensive efforts were made to study material changes of high temperature alloys under oxidizing and reducing atmospheres by environmental scanning electron microscopy or in situ TEM techniques However, the possibilities of microscopic in situ techniques are very limited for the use of highly corrosive and toxic gases such as SO2. Since Sulfur induced corrosion at temperatures relevant for coal and biomass fired power plants, which is causing breakaway oxidation and sulfide precipitation at grain boundaries, is still of scientific interest, the current work focuses on the effect of SO2 in an initial stage of corrosion of ferritic alloys. For the analysis of early stages of combined oxidation and sulphidation processes of Fe-Cr model alloys the usage of a light furnace to conduct a rapid reactive annealing experiment is feasible. Previous studies presented distinct results of the influence of chromium on early high temperature corrosion by SO2 by this technique and subsequent classical metallographic analyses. However, it is still not possible to trace the corrosion mechanism in real time by conducting single aging experiments. The current work introduces two different approaches to study the initial stages of high temperature oxidation processes by applying above state of the art X-ray diffraction and spectroscopy methods. One part focuses on the real time observation of the formation of corrosion products such as oxides and sulfides by energy dispersive X-ray diffraction (EDXRD). The potential of this technique to study crystallization and growth processes of thin films in a reactive environment in real time was previously shown for different compound semiconductors. This approach was now applied to follow oxidation and sulphidation processes of ferritic model alloys in SO2 and SO2/H2O environments. The diffraction signals of the X-rays were detected during the corrosion process and the peak area and positions were analyzed as a function of time. This procedure enables monitoring external oxide growth and material loss in real time in an early stage of corrosion.
The other part of the current work presents the possibilities of X-ray absorption near edge structure spectroscopy (XANES) to characterize oxide scales and their growth mechanisms. Precise phase identification and quantification of corrosion products in a multi-phase oxide/sulfide scale is a pre-requisite to understand diffusion paths of metal ions and gas components. It is a challenging task to distinguish structurally similar reaction products such as Fe3O4 and FeCr2O4 especially in thin films with texture effects by diffraction. To illustrate for example Cr-out diffusion of an alloy throughout an inner and external oxide scale the differentiation of Fe3O4 and FeCr2O4 is indispensable. XANES uses the photoionization effect at the metal absorption edge in an aging product and accesses by this structural and chemical information. The current work uses XANES at the Fe-K and Cr-K absorption edge to identify various aging products grown as thin layers on alloys after short time aging experiments. A reaction chamber for combining high temperature oxidation experiments with surface sensitive X-ray absorption near edge structure spectroscopy will be introduced and first results of XANES on scales at high temperatures will be presented.