5 Werkstofftechnik
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Laser powder bed fusion (LPBF) is an additive manufacturing process for materials which inherently tends to yield various degrees of metastable hierarchical microstructures, defects and high residual stresses in the as-built condition depending on the process parameters. The understanding of the evolution of these typical features during heat treatment and subsequent thermal and mechanical ageing is crucial for the wider acceptance for safety critical structures. A multi-disciplinary research project at BAM studying the development of the microstructure, defects, residual stresses typical of LPBF 316L and their evolution during thermal and mechanical ageing has led to insights into the stability of these inherent features. This presentation aims to give a broad overview of the project with a few specific cases of investigation. Firstly, the formation of residual stresses, the nature of the initial microstructure, the tensile properties and a modelling approach to understand the anisotropy will be presented. This will be followed by examples of studies of their evolution during heat treatment, long term thermal exposure, and room temperature and high temperature mechanical testing compared to a baseline of conventional wrought variant of the same alloy.
Porosity in single-crystal nickel-base superalloys is removed by hot isostatic pressing (HIP) at temperatures above gamma’-solvus where the material is very soft and ductile. For example, single-crystal nickel-base superalloy CMSX-4 is HIPed at temperature 1288 °C, which is slightly higher than the gamma’-solvus temperature of this alloy equal to about 1280 °C. It is assumed that pore shrinking during HIP is mostly due to dislocation creep. Such a modelling of HIP of CMSX-4 was started in our group on the base of results of creep tests of [001] single-crystals at 1288 °C [1]. However, it was found later [2] that the alloy CMSX-4 shows very strong creep anisotropy at 1288 °C. Therefore, for calibration of the creep law, creep tests of different orientations under different stress levels are required at the HIP temperature. This was the main task of present work. Single-crystals of CMSX-4 of axial orientations [001], [011], [123] and [111] were cast by VIAM Moscow and tested by BAM Berlin under creep conditions at 1288 °C and stress levels between 4 MPa and 16 MPa. At all stress levels, the creep rate increases by an order of magnitude when changing the orientation from [001] to [111] with [011] and [123] orientations in between. Such a character of creep anisotropy corresponds to the orientation dependence of the Schmid factor for octahedral glide.
The crystal viscoplasticity model developed in [1] was improved to better represent the time induced softening observed during creep. The creep tests for different stresses and orientations as well as pore closure were simulated. The results of pore closure simulation are compared with measurements of porosity decrease during Hiping.
From molecular dynamics simulations and the capillary fluctuation method, the solid-liquid interfacial free energy has been computed for the B2-liquid interface in the Cu-Zr system. Consistent with previous results for the FCC-liquid interface in Cu-Zr and Al-Sm but atypical of most alloys, was found to increase as the temperature is lowered. In addition, the temperature dependence was obtained for model Lennard-Jones B2-liquid alloys. In all cases the unusual temperature dependence of is correlated with an atomic structure of the interfacial region characterized by a misalignment of the number density peaks between solvents and solutes. In cases where the number density peaks are aligned, the typical temperature dependence is observed. The results are discussed in terms of the Gibbs theory of the thermodynamics of interfaces. It is proposed that the unique interfacial structure and the atypical temperature dependence of are hallmarks of an easy glass forming alloy.
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.
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.
Due to the diversity of materials and the processes associated with their production and use, the complexity of the lifecycles of materials and the multitude of academic and industrial researchers participating in generation of data for material design impose a huge challenge. The topical goal of digitalizing materials and processes can only be adequately addressed by consolidating the efforts of all stakeholders in this field. There are many scattered activities, but there is a demand for an elimination of redundancies as well as an advance in acceptance and a common basis in the digitalization of materials. Furthermore, data analysis methods play an important role in both, the experimental and simulation-based digital description of materials, but they have been poorly structured so far.
Therefore, the two joint projects Platform Material Digital (PMD, materialdigital.de) and Materials open Laboratory (Mat-o-Lab, matolab.de) aim to contribute to a standardized description of data processing methods in materials research. Besides stimulating the formation of a collaborative community in this respect, their main technical goals are the quality assurance of the processes and the output data, the acquisition and definition of their accuracy as well as the interoperability between applications. In this regard, data management in accordance with the FAIR (findability, accessibility, interoperability, reuseability) principles is addressed. There is a common agreement in the scientific community following current discussions that data is supposed to be conform to these principles. This includes storage, processing and querying of data in a preferably standardized form.
To meet the challenge to contextualize material data in a way that is consistent with all stakeholders, all necessary information on the condition of the material including production and application-related changes have to be made available via a uniform, machine-readable description. For this purpose, ontologies are to be used since they allow for machine-understandable knowledge representations and conceptualizations that are needed for data management and the digitalization in the field of materials science.
As first efforts in PMD and Mat-o-Lab, application ontologies are created to explicitly describe processes and test methods. Thereby, the well-known tensile test of metals at room temperature was described ontologically in accordance with the respective ISO standard 6892-1:2019-11.
The efforts in creating this tensile test application ontology are shown in this presentation. Especially, the path of ontology development based on standards to be pursued is focused, which is in accordance with the generic recommendations for ontology development and which is supposed to be exemplary for the creation of other application ontologies.
Thermal cycling of a Ni-excess NiTi alloy was conducted between 50 °C and liquid nitrogen temperature to induce martensitic transformations and to reverse them after. The starting point was an annealed and slowly cooled state, the end point a sample thermally cycled 1500 times. Positron annihilation lifetime spectra and Coincidence Doppler Broadening profiles were obtained in various states and at various tem- peratures. It was found that the initial state was low in defects with positron lifetimes close to that of bulk NiTi. Cycling lead to a continuous build-up of a defect structure up to 20 0 −50 0 cycles after which saturation was reached. Two types of defects created during cycling were identified, namely pure dislo- cations and vacancies attached to dislocations.
Ti-6Al-4V alloy is intensively used in the aerospace industry because of its high specific strength. However, the application of Laser Powder Bed Fusion (LPBF) Ti-6Al-4V alloy for structurally critical load-bearing components is limited. One of the main limiting factors affecting the structural integrity, are manufacturing defects. Additionally, the high cooling rates associated with LPBF process result in the formation of large residual stress (RS) with complex fields. Such RS can cause cracking and geometrical distortions of the part even right after production. Also, the microstructure of LPBF Ti-6Al-4V in the as-built condition is significantly different from that of the conventionally produced alloy. All these factors affect the mechanical behavior of the material. Therefore, to improve the material performance it is important to evaluate the individual effect of RS, defects, and microstructure on fatigue life. To this aim Ti-6Al-4V LPBF material in as-built condition and subjected to different post-processing, including two heat treatments (for stress relief and microstructural modification) and Hot Isostatic Pressing (HIP, for densification), were investigated.
Prior to fatigue tests at elevated temperature, the microstructure, the mesostructure, and subsurface RS on the fatigue samples were investigated. It was found that the fatigue performance of HIPped samples is similar to that of conventionally produced Ti-6Al-4V. The tensile RS found at the surface of as-built samples decreased the fatigue life compared to heat-treated samples. Additionally, the modification of the microstructure (by heat treatment) did not affect the fatigue performance in the regime of mostly elastic strain. This shows that in the absence of tensile RS the manufacturing defects solely control the failure of LPBF components and densification has the strongest effect on the improvement of the mechanical performance.
A γ-analogue of the superalloy CMSX-4 that does not contain the strengthening γ′ -phase and only consists of the γ-solid solution of nickel has been designed, solidified as single-crystals of different orientations, and tested under creep conditions in the temperature range between 1150 and 1288 °C. The tests have revealed a very high creep anisotropy of this alloy, as was previously found for CMSX-4 at supersolvus temperature of 1288 °C. This creep anisotropy could be explained by the dominance of 〈011〉{111} octahedral slip. Furthermore, the analysis of the creep data has yielded a high value of the creep activation energy, Qc≈442 kJ/mol, which correlates with the high activation energy of Re diffusion in Ni. This supports the hypothesis that dislocation motion in the γ-matrix of Re-containing superalloys is controlled by the diffusion of the Re atoms segregating at the dislocation core. The Norton stress exponent n is close to 5, which is a typical value for pure metals and their alloys. The absence of γ′ -reprecipitation after high-temperature creep tests facilitates microstructural investigations. It has been shown by EBSD that creep deformation results in an increasing misorientation of the existing low angle boundaries. In addition, according to TEM, new low angle boundaries appear due to reactions of the a/2 〈011〉 mobile dislocations and knitting of new networks.
The phase-like behavior of grain boundaries (GBs), recently evidenced in several materials, is opening up new possibilities in the design of alloy microstructures. In this context, GB phase diagrams are contributing to a predictive description of GB segregation and (interfacial) phase changes. The influence of chemo-mechanical solute-GB interactions on the GB phase diagram remains elusive so far. This is particularly important for multi-component alloys where the elastic interactions among solute atoms, of various sizes and bonding energies, can prevail, governing a complex co-segregation phenomenon. Recently, we developed a density-based model for GB thermodynamics that intrinsically accounts for GB elasticity in pure elements. In this work, we incorporate the homogeneous and heterogeneous elastic energies associated with the solutes into the density-based framework. We derive the multi-component homogeneous elastic energy by generalizing the continuum misfitting sphere model and extend it for GBs. The density-based free energy functional directly uses bulk CALPHAD thermodynamic data. The model is applied to binary and ternary Al alloys. We reveal that the elastic energy can profoundly affect the GB solubility and segregation behavior, leading to Cu segregation in otherwise Cu-depleted Al GBs. Consequently, GB segregation transition, i.e., a jump in the GB segregation as a function of alloy composition, is revealed in Al-Cu and Al-Cu-Mg alloy systems with implications for subsequent GB precipitation in these alloys. CALPHAD-informed elasticity-incorporated GB phase diagrams enable addressing a broader range of GB phenomena in engineering multi-component alloys.
Data analysis methods play an important role in both the experimental and simulation-based digital description of materials but have so far been poorly structured. The platform Material Digital (PMD) is supposed to contribute to a standardized description of data processing methods in materials research. The goal is the quality assurance of the processes and the output data, the acquisition and definition of their accuracy as well as the interoperability between applications.
Therefore, application ontologies are created to explicitly describe processes and test methods. In this presentation, the first efforts within the joint project PMD in creating a tensile test application ontology in accordance with the ISO standard 6892-1:2019-11 are shown. Especially, the path of ontology development to be pursued based on standards was focused. Furthermore, the presentation includes a live demonstration of queries possibly performed to query data that was uploaded in the PMD triple store.
For more than half a century, spinodal decomposition has been a key phenomenon in considering the formation of secondary phases in alloys. The most prominent aspect of the spinodal phenomenon is the lack of an energy barrier on its transformation pathway, offering an alternative to the nucleation and growth mechanism. The classical description of spinodal decomposition often neglects the influence of defects, such as grain boundaries, on the transformation because the innate ability for like-atoms to cluster is assumed to lead the process. Nevertheless, in nanocrystalline alloys, with a high population of grain boundaries with diverse characters, the structurally heterogeneous landscape can greatly influence the chemical decomposition behavior. Combining atom-probe tomography, precession electron diffraction and density-based phase-field simulations, we address how grain boundaries contribute to the temporal evolution of chemical decomposition within the miscibility gap of a Pt-Au nanocrystalline system. We found that grain boundaries can actually have their own miscibility gaps profoundly altering the spinodal decomposition in nanocrystalline alloys. A complex realm of multiple interfacial states, ranging from competitive grain boundary segregation to barrier-free low-dimensional interfacial decomposition, occurs with a dependency upon the grain boundary character.
Initially, as-cast and homogenized single crystals of nickel-base superalloy CMSX-4 are subjected to hot isostatic pressing at 1288 °C. Two series of experiments are conducted: under the same pressure of 103 MPa but with different durations, between 0.5 and 6 h, and under different pressures, between 15 and 150 MPa, but for the same time of 0.5 h. The porosity annihilation is investigated metallographically and by high-resolution synchrotron X-ray tomography. The obtained experimental results are compared with the predictions of the vacancy model proposed recently in the group. Herein, the model is further refined by coupling with X-ray tomography. The model describes the evolution of the pore arrays enclosed in the 3D synchrotron tomograms during hot isostatic pressing and properly predicts the time and stress dependences of the pore annihilation kinetics. The validated model and the obtained experimental results are used for selecting the optimal technological parameters such as applied pressure and processing time
This presentation shows some experimental results of the characterization of the creep behavior of LPBF 316L, which has been poorly studied and understood to date. The presentation includes results regarding the mechanical properties, the initial microstructural state and its evolution under loading, and the damage mechanism. This work was done within the BAM focus area materials project AGIL. As a benchmark to assess the material properties of the LPBF 316L, a conventionally manufactured variant was also tested.
The underlying cause of mechanical anisotropy in additively manufactured (AM) parts is not yet fully understood and has been attributed to several different factors like microstructural defects, residual stresses, melt pool boundaries, crystallographic and morphological textures.
To better understand the main contributing factor to the mechanical anisotropy of AM stainless steel 316L, bulk specimens were fabricated via laser powder bed fusion (LPBF).
Tensile specimens were machined from these AM bulk materials for three different inclinations relative to the build plate. Dynamic Young's modulus measurements and tensile tests were used to determine the mechanical anisotropy. Some tensile specimens were also subjected to residual stress measurement via neutron diffraction, porosity determination with X-ray micro-computed tomography, and texture analysis with electron backscatter diffraction (EBSD). A crystal plasticity model was used to analyze the elastic anisotropy and the anisotropic yield behavior of the AM specimens, and it was able to capture and predict the experimental behavior accurately. Overall, it was shown that the mechanical anisotropy of the tested specimens was mainly influenced by the crystallographic texture.
The cyclic crack tip opening displacement ΔCTOD is a promising loading Parameter to quantify the crack propagation under thermomechanical fatigue (TMF). In this work, suitable techniques are investigated and compared for an accurate calculation of ΔCTOD under TMF loading using a viscoplastic temperature dependent material model.
It turned out that collapsed special crack tip elements give the best results. An efficient FEM-technique is developed to simulate the incremental crack growth by successive remeshing, whereby the deformations and internal state variables are mapped from the old mesh onto the new one. The developed techniques are demonstrated and discussed for two-dimensional examples like TMF-specimens. Recommendations are made regarding important numerical control parameters like optimal size of crack tip elements, length of crack growth increment in relation to plastic zone size and ΔCTOD value.
The cyclic crack tip opening displacement ΔCTOD is a promising loading Parameter to quantify the crack propagation under thermomechanical fatigue (TMF). In this work, suitable techniques are investigated and compared for an accurate calculation of ΔCTOD under TMF loading using a viscoplastic temperature dependent material model.
It turned out that collapsed special crack tip elements give the best results. An efficient FEM-technique is developed to simulate the incremental crack growth by successive remeshing, whereby the deformations and internal state variables are mapped from the old mesh onto the new one. The developed techniques are demonstrated and discussed for two-dimensional examples like TMF-specimens. Recommendations are made regarding important numerical control parameters like optimal size of crack tip elements, length of crack growth increment in relation to plastic zone size and ΔCTOD value.
The discovery of the high entropy concept at the beginning of the 3rd millennium lead to a worldwide increase in metallurgical research, as the possible element combinations seemed nearly endless and the range of applications wide. In the early years of research, one of the main goals was the discovery of a single-phase high entropy alloy. As research evolved, it was found that properties could be enhanced by opening the HE-concept towards multiphase alloys, and from the wide area of possibilities our group chose a tuning of the properties towards high temperature application.
Compositionally complex Al10Co25Cr8Fe15Ni36Ti6 alloy, which is single-phase at high temperature, around 1200°C, shows a three phase morphology at intermediate temperatures, around 800°C. A high temperature homogenization procedure has to be applied in order to decrease the segregation induced by the dendritic growth. Subsequent annealing promotes the formation of the strengthening γ' precipitates. The alloy shows a positive lattice misfit between the γ and the γ' phase, which can be an indicator for good creep properties.
The microstructure can be optimized by adding trace elements such as Mo and Hf, known as γ and γ' strengtheners in Ni-based superalloys, respectively. Atom probe measurements show that Mo segregates into the γ matrix, and Hf prefers the γ' precipitates, where it increases the lattice parameter and thus also the lattice misfit, by about 50%. The alloy family shows interesting mechanical properties, especially the Al9.5Co25Cr8Fe15Ni36Ti6Hf0,5 alloy – its tensile properties are better than those of commercial Alloy 800H and IN617 at temperatures up to 700°C.