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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.
Monodisperse iron oxide nanoparticles as reference material candidate for particle size measurements
(2020)
In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important, especially with respect to the assessment of their environmental or biological impact. Furthermore, the European Commission’s REACH Regulations require the registration of nanomaterials traded in quantities of at least 1 ton. Powders or dispersions where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as nanomaterials. This creates a need for industrial manufacturers and research or analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution and will also target other key parameters like shape, structure, porosity or functional properties. In this respect, materials like iron oxide or titanium dioxide are considered as candidates to complement the already available silica, Au, Ag, and polystyrene reference nanoparticles.
The thermal decomposition of iron oleate precursors in high boiling organic solvents can provide large quantities of iron oxide nanoparticles that can be varied in size and shape.[1, 2] The presence of oleic acid or other hydrophobic ligands as capping agents ensures stable dispersion in nonpolar solvents. Such monodisperse, spherical particles were synthesized at BAM and pre-characterized by electron microscopy (TEM, SEM including the transmission mode STEM-in-SEM) and dynamic light scattering comparing cumulants analysis and frequency power spectrum.
1. REACH regulations and nanosafety concerns create a strong need for nano reference materials with diverse properties.
2. Iron oxide nanoparticles are under development as new candidate reference material at BAM.
3. Narrow particle size distribution confirmed by light scattering and electron microscopy.
The field of materials science is defined as “the study of the properties of solid materials and how those properties are determined by a material’s composition and structure.”. Many –if not most– of the materials that are produced nowadays owe their properties to structures engineered down to the nanoscopic level. This need has been partly realized thanks to the understanding of materials’ building blocks via characterization techniques that reach this level of resolution. Transmission electron microscopy, since its first implementation in the early 1930s (in Berlin), has been implemented to achieve imaging –and spectral– analysis at lateral resolutions down to the atomic level.
In this contribution, a series of practical examples will be presented, where applied materials are characterized by a range of transmission electron microscopy techniques to understand structural and functional properties of a wide range of materials. Among these materials examples will be presented on structural conventionally and additively manufactured metallic alloys, high entropy alloys, dissimilar aluminum-to-steel welds, magnetic nanoparticles, ceramic coatings, high temperature oxidation products. Addressed will be either the effect of processing route or that of the exposure to experimental conditions similar to those found in the respective intended applications.
Additive manufacturing (AM) of metallic alloys has gained momentum in the past decade for industrial applications. The microstructures of AM metallic alloys are complex and hierarchical from the macroscopic to the nanometer scale. When using laser-based powder bed fusion (L-PBF) process, two main microstructural features emerge at the nanoscale: the melt pool boundaries (MPB) and the solidification cellular substructure.
Here, details of the MPB are revealed to clearly show the three-dimensional nature of MPBs with changes of cell growth of direction and their relation to their surrounding cellular substructure, as investigated by transmission electron microscopy (TEM) for L-PBF 316L austenitic stainless steel (cf. Figure 1). A hitherto unknown modulated substructure with a period of 21 nm is further discovered within cells as the result of a partial Ga+-focused ion beam-induced ferritic transformation of the austenite. Cell cores and cell boundaries differ notably regarding the modulated substructure.
Dislocations are the carriers of plastic deformation. As such, their characterization offers important information on the properties they affect. In this contribution, a new tool is presented, which is incorporated in Amira ZIB Edition and allows for three-dimensional (3D) imaging and quantification of dislocations substructures from thick regions an electron-transparent specimen. In the tool, the dislocation segments are traced on diffraction contrast images that are obtained in the transmission electron microscope (TEM). The uncertainties related to the experimental setup and to the proposed method are discussed on the base of a tilt series.
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.
Unlike conventional alloys, which typically consist of one main element, high-entropy alloys (HEAs) contain five or more principal elements, which broaden chemical complexity and with it a realm of synergistic mechanisms. The AlMo0.5NbTa0.5TiZr HEA initiated a subclass of Al-containing refractory (r)HEAs that has recently drawn attention [2]. The alloy has a superalloy-resembling B2/bcc nanostructure, which inspired its name refractory high entropy superalloy (RSA). With high-temperature (HT) compressive strengths beyond conventional Ni-based superalloys, this nanostructure could be used for improved HT structural applications. However, in the application-relevant HT regime the Al-Zr-rich B2 phase decomposes to form a hexagonal Al-Zr-based intermetallic (Al4-xZr5; x: 0..1) [3,4]. This work explores the fascinating yet fatal micromechanisms associated to this phase transformation, in the context of creep, annealing and oxidation experiments performed between 800 and 1200 °C.
The material was produced by arc-melting and heat treatment in argon, which lead to grain boundaries decorated with up to 7%. Interrupted constant-load creep tests were performed under vacuum (at 10-4 Pa), at 900–1100 °C with external tensile stresses of 30–120 MPa. Oxidation experiments were separately conducted for 24 hours at 800 and 1000 °C in both dry (21% O2 + 79% N2) and humid (8% O2 + 74% N2 + 18% H2O) air. After the experiments, the samples were characterized by X-ray diffraction, scanning electron microscopy and transmission electron microscopy to reveal degradation mechanisms. Crystallographic texture, orientation relationships and stabilization of an oxygen-containing iso structure (Al4-xZr5(Ox-y); y: 0..x) of the Al-Zr-rich intermetallic are found and discussed.