5 Werkstofftechnik
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Iron aluminides depict a sustainable and light-weight material class which could be employed in many applications requiring high strength at intermediate to high temperatures. According to first results, the alloy Fe-26Al-4Mo-0.5Ti-1B surpasses conventional materials in wet corrosion resistance and creep resistance up to 650 °C. For these reasons, the AiF research project “WAFEAL – Materials applications for iron aluminides” was initiated to transfer these findings into a standardised materials dataset and to derive best practices for processing. In the first place, a set of different microstructures adjusted by varying casting methods, wall thicknesses and heat treatments was investigated and correlated with hardness on macro and micro scale. Correlations were drawn between solidification rates and resulting grain sizes and hardness. The effect of vacancy hardening was only verified for wall thickness as low as 2.5 mm. Moreover, a common decrease of macrohardness after a heat treatment at 1000 °C for 100 h was observed irrespective of casting process or wall thickness. This effect was linked with an unexpected decrease of the complex boride phase fraction which acts as a hardening phase.
Due to the increasing scarcity of critical raw materials current high-temperature materials are sought to be replaced by alloys based on more abundant metals. One possibility within the class of intermetallics are iron aluminides, which combine sustainability and cost-efficiency with the prospect of mass savings. Iron aluminides show competitive specific strength up to 700 °C and excellent creep and wet corrosion resistance by small additions of Mo, Ti and B. Nevertheless, a Mo content of above 2 at.% which is needed for optimum corrosion resistance results in enhanced brittleness, especially at room temperature. This is why alloys with these Mo fractions were only mechanically tested under compressive loading so far. Still, testing of static and creep properties under tensile loading is required for reliable component design. Besides high standards for crack-free processing, data acquisition for tensile loads is especially complicated by environmental embrittling effects for iron aluminides. To cope with these challenges, the AiF research project “WAFEAL – Materials applications for iron aluminides” was initiated. The main goal is to collect standardised data on ambient and high-temperature tensile properties and creep properties. Samples with a nominal composition of Fe-26Al-4Mo-0.5Ti-1B [at.%] were manufactured via centrifugal casting in ceramic shell moulds followed by machining. Heat treatment for homogenisation and final polishing were carried out where appropriate. A summary of the achieved tensile and creep properties such as yield and tensile strength, maximum elongation, secondary creep rate and stress exponents will be given. Results will be also discussed regarding the influence of temperature, stress level and microstructure on the damage mechanisms. Furthermore, the effect of different alloy concentrations on the mechanical response at different temperatures will be outlined within a small experimental series.
With an increasing demand in more efficient fuel consumption to reduce CO2 emissions, weight reductions in high-temperature materials at affordable costs gain increasing attention. One potential candidate is the intermetallic material class of iron aluminides, combining the advantages in mass savings, high temperature performance and recyclability of resources. The alloy Fe-26Al-4Mo-0.5Ti-1B was selected to study the microstructural features evolving from two casting processes, five wall thicknesses and three final conditions. Conclusions are drawn upon the correlations of processing variables, grain sizes and hardness.
The increasing importance of resource availability and closed-loop material cycles are driving materials research to reduce alloying content in conventional materials or even substitute them with more sustainable alternatives. Intermetallic iron aluminide alloys (FeAl) present a potential alternative. Many alloy concepts for improved high-temperature properties or ductility have already been successfully implemented in casting technologies on a laboratory scale. However, successful testing of FeAl alloys on an industrial scale was still pending at the beginning of the project.
Therefore, the aim of the project was to develop simulation-based casting concepts for industrial casting processes using the base alloy Fe-26Al-4Mo-0.5Ti-1B and to narrow down process limits by means of hot cracking tests. Findings were transferred into practice-oriented guidelines for casting of iron aluminides, which is accessible to future applicants in SMEs. The focus was placed on centrifugal casting combined with investment casting or die casting. In addition to numerous design and casting process parameters, heat treatments and alloying additions (Al, Mo, B) were varied to determine the influence of alloying elements on castability, microstructure and mechanical properties. Data from microstructure analyses (microscopic imaging, determination of grain sizes as well as phase compositions and volume fractions, fractography), mechanical tests (hardness measurements, compression tests, ambient and high-temperature tensile tests, creep tests) as well as measurements of thermophysical properties could be generated on the base alloy. Correlations of materials data with process variables allowed conclusions to be drawn on strengthening mechanisms and ductility of the alloy and how they can be controlled in terms of processing and component design. Successful casting of highly complex components with thin wall thicknesses and optimised alloy compositions points out prospects for new fields of application.
9-12% Cr ferritic-martensitic stainless steels are widely used as high temperature construction materials in fossil fueled power plants due to their excellent creep and oxidation resistance, but changes in electricity markets during the last two decades have considerably changed the typical working conditions of these facilities. The growing share of renewable energy sources in power generation forces most of these plants into flexible operation with frequent load shifts or shutdowns. These cyclic operation profiles constitute a major lifetime issue, raising the question which fundamental processes govern the reaction of ferritic-martensitic steels to cyclic load and temperature variations.
The present contribution reports on current findings obtained in a multidisciplinary project funded by German Ministry of Education and Research (BMBF) which combines cyclic mechanical and cyclic oxidation testing of different 9-12% Cr grades with detailed microstructural analyses and related micromechanical modeling.
In the present first part of our contribution, an overview will be given on the results obtained in the mechanical testing programme of the project. Mechanical analyses were carried out on P91 and (mainly) P92 steel grades, particularly looking at softening phenomena and lifetimes obtained in isothermal cyclic loading (low cycle fatigue, LCF), non-isothermal cyclic loading (thermo-mechanical fatigue, TMF), and service-like combinations of creep and fatigue periods. For this purpose, cylindrical specimens were extracted from thick-walled steam pipes, orthogonal to the pipe axis, and subjected to strain controlled cyclic loading (± 0.2 to ±0.5 % mechanical strain) to different degrees of softening at temperatures up to 620 °C.
The test results will be presented and discussed with a focus on the impact of hold periods (i.e. combined creep-fatigue conditions) on mechanical softening, lifetime and crack formation. Details on the microstructural evolution and their representation in a micromechanical model will be given in a second, complementary contribution to this conference.
This contribution presents the results of an experimental study on the LCF behavior of an austenitic 316L stainless steel produced by laser powder bed fusion featuring a low defect population, which allows for an improved understanding of the role of other typical aspects of a PBF‑LB microstructure. The LCF tests were performed between room temperature and 600 °C. A hot‑rolled 316L variant was tested as a reference. The mechanical response is characterized by strain-life curves, a Coffin‑Manson‑Basquin fitting, and cyclic deformation curves. The damage and deformation mechanisms are studied with X-ray computed tomography, optical and electron microscopy. The PBF‑LB/M/316L exhibits lower fatigue lives at lower strain amplitudes. The crack propagation is mainly transgranular. The solidification cellular structure seems to be the most relevant underlying microstructural feature determining the cyclic deformation behavior.
Die Untersuchung und Charakterisierung der Entwicklung/Änderung der Mikrostruktur, der mechanischen Eigenschaften sowie der Lebensdauer additiv gefertigter metallischer Werkstoffe hat bisher, vor allem im Hinblick auf die komplexe Belastungsfälle bei sicherheitsrelevanten Anwendungen, mit der rasanten Entwicklung der Fertigungstechniken nicht Schritt gehalten. Im Rahmen dieser Arbeit wurde eine Charakterisierung des Ermüdungsverhaltens von additiv gefertigten TiAl6V4 im Low-Cycle-Fatigue Bereich (niederzyklische Ermüdung) nach Norm ISO 12206 mit Dehnungsamplituden von 0.3 bis zu 1.0 % und bei Raumtemperatur, 250°C und 400°C durchgeführt. Die TiAl6V4 Proben wurden aus zylindrischen Halbzeugen gefertigt, welche durch Laser-Pulver-Auftragsschweißen mit einer optimierten Aufbaustrategie hergestellt wurden. Die optimierte Aufbaustrategie beinhaltet variierende Spurüberlappungsgraden, die die Fertigung der dünnen zylindrischen Körper ohne weitere Ausgleichslagen ermöglicht. Das Werkstoffverhalten wird anhand von Wechselverformungskurven sowie einer Darstellung der Lebensdauer in einem Wöhler-Diagramm beschrieben. Ein Fitting der Lebensdauer-Daten erfolgt anhand der Manson-Coffin-Basquin Beziehung. Eine Eingangscharakterisierung der mikrostrukturellen Merkmale inklusive Bindefehler aus dem Herstellungsprozess wird durch Lichtmikroskopie und hochauflösende Computertomographie (CT) durchgeführt. Der Versagensmechanismus während der Belastung wird anhand von Zwischenuntersuchungen mit CT und einem unterbrochenen Versuch mit ausgewählten Versuchsparametern beschrieben. Nach dem Versagen wurden die Proben am REM, mit Lichtmikroskopie und mit CT fraktographisch in Längs- und Querrichtung untersucht. Die erfassten Lebensdauern sind ähnlich zu denen aus herkömmlichen Studien und liegen unter derjenigen von dem konventionell hergestellten (geschmiedeten) Werkstoff. In dieser Arbeit wurden für den untersuchten Werkstoff bei anwendungs- und sicherheitsrelevanten Belastungszuständen (hohe Temperaturen, zyklische Plastizität) neue experimentelle Daten und Kennwerte ermittelt und Verständnis über das mechanische Verhalten und die Entwicklung der Mikrostruktur aufgebaut. Darüber hinaus wurde Verständnis über die Rolle von Bindefehlern und anderen typisch für AM auftretenden Gefügemerkmalen auf das Versagensverhalten von DED-L TiAl6V4 gewonnen.
Despite of the significant advances in AM process optimization there is still a lack of experimental results and understanding regarding the mechanical behavior and microstructural evolution of AMparts, especially in loading conditions typical for safety-relevant applications e.g. in the aerospace or power engineering. Within the scope of the presented investigations, a characterization of the fatigue behavior of additively manufactured Ti-6Al-4V in the low cycle fatigue regime was carried out in the range of 0.3 to 1.0 % strain amplitude at room temperature, 250°C and 400°C. The Ti-6Al-4V specimens are machined out of lean cylindrical rods, which were fabricated using powder laser metal deposition (LMD) with an improved build-up strategy. The improved strategy incorporates variable track overlap ratios to achieve a constant growth in the shell and core area. The low-cycle-fatigue behavior is described based on cyclic deformation curves and strain-based fatigue life curves. The lifetimes are fitted based on the Manson-Coffin-Basquin relationship. A characterization of the microstructure and the Lack-of-Fusion (LoF)-defect-structure in the as-built state is performed using optical light microscopy and high-resolution computed tomography (CT) respectively. The failure mechanism under loading is described in terms of LoF-defects-evolution and crack growth mechanism based on an interrupted LCF test with selected test parameters. After failure, scanning electron microscopy, digital and optical light microscopy and CT are used to describe the failure mechanisms both in the longitudinal direction and in the cross section of the specimens. The fatigue lives obtained are comparable with results from previous related studies and are shorter than those of traditionally manufactured (wrought) Ti-6Al-4V. In this study new experimental data and understanding of the mechanical behavior under application-relevant loading conditions (high temperature, cyclic plasticity) is gained. Furthermore, a better understanding of the role of LoFdefects and AM-typical microstructural features on the failure mechanism of LMD Ti-6Al-4V is achieved.
Die Untersuchung und Charakterisierung der Entwicklung/Änderung der Mikrostruktur, der mechanischen Eigenschaften sowie der Lebensdauer additiv gefertigter metallischer Werkstoffe hat bisher, vor allem im Hinblick auf die komplexe Belastungsfälle bei sicherheitsrelevanten Anwendungen, mit der rasanten Entwicklung der Fertigungstechniken nicht Schritt gehalten. Im Rahmen dieser Arbeit wurde eine Charakterisierung des Ermüdungsverhaltens von additiv gefertigten TiAl6V4 im Low-Cycle-Fatigue Bereich (niederzyklische Ermüdung) nach Norm ISO 12206 mit Dehnungsamplituden von 0.3 bis zu 1.0 % und bei Raumtemperatur, 250°C und 400°C durchgeführt. Die TiAl6V4 Proben wurden aus zylindrischen Halbzeugen gefertigt, welche durch Laser-Pulver-Auftragsschweißen mit einer optimierten Aufbaustrategie hergestellt wurden. Die optimierte Aufbaustrategie beinhaltet variierende Spurüberlappungsgraden, die die Fertigung der dünnen zylindrischen Körper ohne weitere Ausgleichslagen ermöglicht. Das Werkstoffverhalten wird anhand von Wechselverformungskurven sowie einer Darstellung der Lebensdauer in einem Wöhler-Diagramm beschrieben. Ein Fitting der Lebensdauer-Daten erfolgt anhand der Manson-Coffin-Basquin Beziehung. Eine Eingangscharakterisierung der mikrostrukturellen Merkmale inklusive Bindefehler aus dem Herstellungsprozess wird durch Lichtmikroskopie und hochauflösende Computertomographie (CT) durchgeführt. Der Versagensmechanismus während der Belastung wird anhand von Zwischenuntersuchungen mit CT und einem unterbrochenen Versuch mit ausgewählten Versuchsparametern beschrieben. Nach dem Versagen wurden die Proben am REM, mit Lichtmikroskopie und mit CT fraktographisch in Längs- und Querrichtung untersucht. Die erfassten Lebensdauern sind ähnlich zu denen aus herkömmlichen Studien und liegen unter derjenigen von dem konventionell hergestellten (geschmiedeten) Werkstoff. In dieser Arbeit wurden für den untersuchten Werkstoff bei anwendungs- und sicherheitsrelevanten Belastungszuständen (hohe Temperaturen, zyklische Plastizität) neue experimentelle Daten und Kennwerte ermittelt und Verständnis über das mechanische Verhalten und die Entwicklung der Mikrostruktur aufgebaut. Darüber hinaus wurde Verständnis über die Rolle von Bindefehlern und anderen typisch für AM auftretenden Gefügemerkmalen auf das Versagensverhalten von DED-L TiAl6V4 gewonnen.
Towards Interoperability: Digital Representation of a Material Specific Characterization Method
(2022)
Certain metallic materials gain better mechanical properties through controlled heat treatments. For example, in age-hardenable aluminum alloys, the strengthening mechanism is based on the controlled formation of nanometer sized precipitates, which represent obstacles to dislocation movement. Precise tuning of the material structure is critical for optimal mechanical behavior in the application. Therefore, analysis of the microstructure and especially the precipitates is essential to determine the ideal parameters for the interplay of material and heat treatment. Transmission electron microscopy (TEM) is utilized to identify precipitate types and orientations in a first step. Dark-field imaging (DF-TEM) is often used to image the precipitates and to quantify their relevant dimensions.
The present work aims at the digital representation of this material-specific characterization method. Instead of a time-consuming, manual image analysis, an automatable, digital approach is demonstrated. Based on DF-TEM images of different precipitation states of a wrought aluminum alloy, a modularizable digital workflow for quantitative precipitation analysis is presented. The integration of this workflow into a data pipeline concept will also be discussed. Thus, by using ontologies, the raw image data, their respective contextual information, and the resulting output data from the quantitative precipitation analysis can be linked in a triplestore. Publishing the digital workflow and the ontologies will ensure the reproducibility of the data. In addition, the semantic structure enables data sharing and reuse for other applications and purposes, demonstrating interoperability.
The presented work is part of two digitization initiatives, the Platform MaterialDigital (PMD, materialdigital.de) and Materials-open-Laboratory (Mat-o-Lab).