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Seit Beginn der Luftfahrt Anfang des letzten Jahrhunderts ist die Menschheit auf der Suche nach neuen Materialien, die das Abenteuer Fliegen sicherer, angenehmer, schneller und rentabler gestalten. Hochentropielegierungen sind solche vielversprechenden Materialien. Die richtige Analytik hilft dabei, besser zu verstehen, wie deren Zusammensetzung und atomare Anordnung die makroskopischen Eigenschaften beeinflusst.
A new race for high performance structural materials has started since the discovery of high entropy alloys at the beginning of the 21st century. The possible combination of several elements in an, until then, unknown composition space opened the ground for discovering new materials. Solid solution strengthening remains the most prominent mechanisms that is active in this family of materials, but it is supported by all other strengthening mechanism on the path to better and better performing materials. Chemical, thermal and mechanical approaches are combined to optimize these alloys. Optimum performances can be reached by using a high number of different strengthening mechanisms, induced both by composition and processing. The most prominent with composition induced mechanism is precipitation hardening, and on the processing side it is cold working such as cold-rolling, torsion or extrusion. The contribution uses tensile test data at room temperature solely for comparison – high temperature and cryogenic data are omitted because it would lead beyond the scope of this manuscript.
Uniaxial mechanical properties of face‑centered cubic singleand multiphase high‑entropy alloys
(2022)
Since the high entropy concept was proposed at the beginning of the millennium, the research focus of this alloy family has been wide ranging. The initial search for single-phase alloys has expanded with the aim of improving mechanical properties. This can be achieved by several strengthening mechanisms such as solid-solution hardening, hot and cold working and precipitation hardening. Both single- and multiphase high- and medium-entropy alloys can be optimized for mechanical strength via several processing routes, as is the case for conventional alloys with only one base element, such as steels or Ni-based superalloys.
Early material damage in equimolar CrMnFeCoNi in mixed oxidizing/sulfiding hot gas atmosphere
(2022)
The challenges to use more varied fuels at medium and high temperatures above 500 °C need to be addressed by tuning the materials toward a better resistance against increased corrosion. As a first step the corrosion processes need to be better understood, especially in the case of the unavoidable and highly corrosive sulfur-based gases. Herein, oxidation/sulfidation of an equimolar CrMnFeCoNi high-entropy alloy is studied at an early stage after hot gas exposure at 600 °C for 6 h in 0.5% SO2 and 99.5% Ar. The oxidation process is studied by means of X-ray diffraction, scanning and transmission electron microscopy, and supported by thermodynamic calculations. It is found that the sulfur does not enter the bulk material but interacts mainly with the fast-diffusing manganese at grain boundary triple junctions at the alloy surface. Submicrometer scaled Cr–S–O-rich phases close to the grain boundaries complete the sulfur-based phase formation. The grains are covered in different Fe-, Mn-, and Cr-based spinels and other oxides.
Superalloy inspired Al10Co25Cr8Fe15Ni36Ti6 compositionally complex alloy is known for its gamma-gamma' microstructure and the third Heusler phase. Variations of this alloy, gained by replacing 0.5 or 1 at. pct Al by the equivalent amount of Mo, W, Zr, Hf or B, can show more phases in addition to this three-phase morphology. When the homogenization temperature is chosen too high, a eutectic phase formation can take place at the grain boundaries, depending on the trace elements: Mo and W do not form eutectics while Hf, Zr and B do. In order to avoid the eutectic formation and the potential implied grain boundary weakening, the homogenization temperature must be chosen carefully by differential scanning calorimetry measurements. A too low homogenization temperature, however, could impede the misorientation alignment of the dendrites in the grain. The influence of grain boundary phases and incomplete dendrite re-orientation are compared and discussed.
Hierarchical microstructures are created when additional γ particles form in γ’ precipitates and they are linked to improved strength and creep properties in high-temperature alloys. Here, we follow the formation and evolution of a hierarchical microstructure in Ni86.1Al8.5Ti5.4 by in situ synchrotron X-ray diffraction at 1023 K up to 48 h to derive the lattice parameters of the γ matrix, γ’ precipitates and γ particles and misfits between phases. Finite element method-based computer simulations of hierarchical microstructures allow obtaining each phase's lattice parameter, thereby aiding peak identification in the in situ X-ray diffraction data. The simulations further give insight into the heterogeneous strain distribution between γ’ precipitates and γ particles, which gives rise to an anisotropic diffusion potential that drives the directional growth of γ particles. We rationalize a schematic model for the growth of γ particles, based on the Gibbs-Thomson effect of capillary and strain-induced anisotropic diffusion potentials. Our results highlight the importance of elastic properties, elastic anisotropy, lattice parameters, and diffusion potentials in controlling the behavior and stability of hierarchical microstructures.
Early Material Damage in Equimolar CrMnFeCoNi in Mixed Oxidizing/Sulfiding Hot Gas Atmosphere
(2022)
The challenges to use more varied fuels at medium and high temperatures above 500 °C need to be addressed by tuning the materials towards a better resistance against increased corrosion. As a first step the corrosion processes need to be better understood, especially in the case of the unavoidable and highly corrosive sulfur-based gases. In this work oxidation/sulfidation of an equimolar CrMnFeCoNi high entropy alloy is studied at an early stage after hot gas exposure at 600 °C for 6 h in 0.5% SO2 and 99.5% Ar. The oxidation process is studied by means of x-ray diffraction, scanning and transmission electron microscopy and supported by thermodynamic calculations. It is found that the sulfur does not enter the bulk material but interacts mainly with the fast-diffusing manganese at grain boundary triple junctions at the alloy surface. Sub-micrometer scaled Cr-S-O rich phases close to the grain boundaries complete the sulfur-based phase formation. The grains are covered in different Fe, Mn and Cr based spinels and other oxides.
Spurenelemente spielen eine wichtige Rolle bei der Verfeinerung der Eigenschaften von komplexen Materialien. Diese Arbeit zeigt die Korrelation zwischen der Mikrostruktur, der Gitterfehlpassung und den Kriecheigenschaften. Die Legierung Al10Co25Cr8Fe15Ni36Ti6 (in at. %) mit komplexer Zusammensetzung wurde mit den Elementen Hf und W verstärkt. Die Zugabe von Hf bewirkt eine eckigere Form der würfelförmigen gamma'-Ausscheidungen und einen erhöhten Anteil der Heusler-Phase. Die Zugabe von W wiederum formt die Würfelchen rundlicher und löst die Heusler-Phase auf. Eine Mischung der beiden Spurenelemente zeigt einen Übergang zwischen den beiden Extremen, sowohl in Hinsicht auf die Form der Ausscheidungen als auch in Bezug auf die Gitterfehlpassung und die Kriecheigenschaften.
Early Material Damage in Equimolar CrMnFeCoNi in Mixed Oxidizing/Sulfiding Hot Gas Atmosphere
(2022)
The use of more and more varied fuels implies an increased list of criteria that need to be addressed when choosing a material for a combustion chamber and its supply pipes. The materials must be very resistant against corrosion, especially when the process takes place at temperatures above 500°C. In this work the influence of SO2 on the surface of the “Cantor alloy” is investigated.
Trace elements play an important role in the fine-tuning of complex material properties. This study focuses on the correlation of microstructure, lattice misfit and creep properties. The compositionally complex alloy Al10Co25Cr8Fe15Ni36Ti6 (in at. %) was tuned with high melting trace elements Hf and W. The microstructure consists of a γ matrix, γ' precipitates and the Heusler phase and it is accompanied by good mechanical properties for high temperature applications. The addition of 0.5 at.% Hf to the Al10Co25Cr8Fe15Ni36Ti6 alloy resulted in more sharp-edged cubic γ′ precipitates and an increase in the Heusler phase amount. The addition of 1 at.% W led to more rounded γ′ precipitates and the dissolution of the Heusler phase. The shapes of the γ' precipitates of the alloys Al9.25Co25Cr8Fe15Ni36Ti6Hf0.25W0.5 and Al9.25Co25Cr8Fe15Ni36Ti6Hf0.5W0.25, that are the alloys of interest in this paper, create a transition from the well-rounded precipitates in the alloy with 1% W containing alloy to the sharp angular particles in the alloy with 0.5% Hf. While the lattice misfit has a direct correlation to the γ' precipitates shape, the creep rate is also related to the amount of the Heusler phase. The lattice misfit increases with decreasing corner radius of the γ' precipitates. So does the creep rate, but it also increases with the amount of Heusler phase. The microstructures were investigated by SEM and TEM, the lattice misfit was calculated from the lattice parameters obtained by synchrotron radiation measurements.
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.
Unlike conventional alloys, high entropy alloys are characterized by one or more solid solution phase(s) without a clearly defined solvent, all element contribute to the matrix in a way that is still not entirely understood. In addition, it is not known to what extent classic thermodynamic rules can be applied to these multi-element alloys, especially concerning the question about what factor incites the matrix to undergo a phase transformation.
This work tackles directly some of these aspects on a chosen alloy, Al8Cr17Co17Cu8Fe17Ni33 (at.%), which presents a high temperature single-phase γ state and a two-phase state with γ′ precipitates, above and below 900 ◦C, respectively. A combined investigation via microstructural observations, hardness testing, X-ray absorption and photoelectron spectroscopy was carried out above the γ′ formation temperature. Hardness values are independent of the annealing temperatures, microstructural analysis shows no phase formation and X-ray absorption spectroscopy does not reveal observable changes in neither local atomic nor electronic structure, indicating that approaching γ′ formation temperature is not influenced by atomic or electronic rearrangements.
Interestingly, short-range chemical order remains quantitatively compatible at any annealing temperature in the single-phase γ state, and the observed preferred pairs Al–Cu and Al–Ni in the γ state match with the γ’ precipitates composition below 900 ◦C.
The Gibbs free energy of a grain boundary is a complex thermodynamic function of temperature, pressure, and composition. These complexities add to the intrinsic crystallographic and chemical constraints imposed by the adjacent bulk phase. Recently we have proposed a density-based model for assessing grain boundary thermodynamics that enables a CALPHAD-informed description of the grain boundary. As such, the Gibbs free energy of the grain boundary is directly linked with available CALPHAD thermodynamic data. In this talk, new aspects of interfacial segregation and phase transformation are revealed by benchmarking the current model for various experimental cases, including several steels, high-entropy alloys and aluminum alloys. The effects of elastic interactions on the grain boundary segregation and the application of the model to a nanocrystalline Pt-Au alloy, with numerous grain boundaries of various characters, will be discussed.