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The multi-phase approach has proven to widen the application properties of high entropy alloys. After a decade of testing different alloys in the Al-Co-Cr-Cu-Fe-Ni-Ti family the Al10Co25Cr8Fe15Ni36Ti6 was found to be a solid base for more fine-tuned microstructural optimization. Following the example of superalloys, the Al10Co25Cr8Fe15Ni36Ti6 alloy aims for a γ/γ' microstructures in order to guarantee a good microstructural stability at high temperatures. The shape and volume fraction of the γ' particles is known to influence the mechanical properties of superalloys, and they do so in the high entropy family as well [1]. Shape, misfit and creep properties of several modified versions of the Al10Co25Cr8Fe15Ni36Ti6 alloy are compared and discussed in this talk.
A constitutive model for the mechanical behaviour of single crystal Ni-base superalloys under high temperature conditions has been developed in the framework of a Cooretec project in cooperation with Siemens AG, MTU Aero Engines AG and University Bayreuth. In addition to the conventional material properties e.g. elastic constants, the model requires the parameters of the initial microstructure as an input. Thus, the γ’-precipitate size and the channel width of the γ-matrix were obtained from SEM micrographs. The model uses the slip system theory and describes the movement, multiplication and annihilation of dislocations in the channels. Furthermore, the cutting of precipitates is another mechanism contributing to the plastic flow. The evolution of the morphology due to rafting and its effects on the deformation have been implemented according to. The kinematic hardening is introduced as a stress tensor to realistically represent the strain hardening of arbitrary oriented single crystals.
The mechanical behaviour of single crystal specimens has been experimentally investigated in tension tests at different strain rates and in creep tests under various loads. The constitutive model has been calibrated based on the experimental data for temperatures of 950°C and 850°C and the [001] and [111] crystallographic orientations.
Finally, a micromechanical model was created to simulate the creep response of additive manufactured polycrystalline structures. An EBSD image is taken to obtain the grain geometry and their respective orientation. The grain boundaries are discretised using cohesive elements, whereas the single crystal model was applied to each grain in the representative volume. The polycrystal model is generated using Dream3D, NetGen and other software previously developed at the BAM.
The article covers data on the Brinell hardness of the forged precipitation-hardened aluminum alloy EN AW-2618A in the initial T61 condition (i. e. slightly underaged) and after isothermal aging for up to 25,0 0 0 h at aging temperatures between 160 °C and 350 °C. In addition, the hardness was determined on specimens after creep testing at 190 °C and various stresses. The hardness decreases with increasing ag- ing time due to the microstructural evolution of the harden- ing precipitates. The drop occurs faster the higher the aging temperature. Aging under creep load additionally accelerates the hardness decrease.
A study was made on the effect of creep loading on the precipitate radii evolution of the aluminum alloy 2618A.
The overageing process of the alloy was investigated under load at a temperature of 190 °C with stresses between 79 and 181 MPa and compared to stress free isothermal ageing. The precipitates responsible for strength were characterized using dark-field transmission electron microscopy (DFTEM). This allows the experimental Determination of radii distributions of the rod-shaped Al2CuMg precipitates and the evaluation regarding their mean precipitate radius. It was found that the mean precipitate radius enables the comparison of the different microstructural conditions of crept and uncrept samples. The mean precipitate radii of the samples experiencing creep are significantly higher than those of undeformed samples. It was shown that the acquired radii distributions are viable to determine averaged particle radii for comparison of the aged samples. A ripening process including pipe diffusion along dislocations describes the data on coarsening very well for the creep samples.
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 current lack of quantitative knowledge on processing-microstructure–property relationships is one of the major bottlenecks in today’s rapidly expanding field of additive manufacturing. This is centrally rooted in the nature of the processing, leading to complex microstructural features. Experimentally-guided modeling can offer reliable solutions for the safe application of additively manufactured materials. In this work, we combine a set of systematic experiments and modeling to address creep anisotropy and its correlation with microstructural characteristics in laser-based powder bed fusion (PBF-LB/M) additively manufactured Inconel-738LC (IN738LC). Three sample orientations (with the tensile axis parallel, perpendicular, and 45° tilted, relative to the building direction) are crept at 850 °C, accompanied by electron backscatter secondary diffraction (EBSD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) investigations. A crystal plasticity (CP) model for Ni-base superalloys, capable of modeling different types of slip systems, is developed and combined with various polycrystalline representative volume elements (RVEs) built on the experimental measurements. Besides our experiments, we verify our modeling framework on electron beam powder bed fusion (PBF-EB/M) additively manufactured Inconel-738LC. The results of our simulations show that while the crystallographic texture alone cannot explain the observed creep anisotropy, the superlattice extrinsic stacking faults (SESF) and related microtwinning slip systems play major roles as active deformation mechanisms. We confirm this using TEM investigations, revealing evidence of SESFs in crept specimens. We also show that the elongated grain morphology can result in higher creep rates, especially in the specimens with a tilted tensile axis.
In Germany spent nuclear fuel and high level radioactive waste is stored in interim storage containers with double lid systems. Those lids are equipped with metal seals (e.g. Helicoflex®) that ensure the safe enclosure of the inventory. The used metal seals consist of three components as can be seen in the cross-sectional view in Figure 1. The innermost part is a helical spring that is surrounded by an inner jacket made of stainless steel. The outer jacket that is made of a softer material which in case of assembly in the aforementioned storage containers is silver or aluminum (i.e. Al 99.5). During application the seal is compressed and due to the restoring force of the helical spring, the outer jacket is plastically deformed and adapts to the sealing surface. Hence, leakage paths are closed and the sealing function is generated. In Germany the above-mentioned containers are licensed for up to 40 years of interim storage, which in case extended storage becomes necessary before a final repository is available will have to be extended to even longer periods. Therefore, the evaluation of the long-term behavior of the seals is necessary, taking into account storage conditions, decay heat and possible mechanical loads as well.
At Bundesanstalt für Materialforschung und –prüfung (BAM) long-term investigations are being conducted in which seals are assembled in test flanges and aged at temperatures ranging from room temperature to 150°C for accelerated aging. The aged seals are tested semi-annually (after the first 6 months in which the seals are tested more frequently) regarding the sealing performance, the remaining seal force, and the useable resilience upon decompression. Results of these investigations have been published over the past years (e.g. Grelle, Wolff, Probst, Jaunich, & Völzke, 2017; Völzke, Wolff, Probst, Nagelschmidt, & Schulz, 2014). It was found that the seal force and the useable resilience decrease with time and temperature, which is in agreement with the result of other studies (Sassoulas et al., 2006; Wataru et al., 2016) as well. Geometry change of the outer jacket has been identified as the main reason for this seal behavior. At the prevailing operating temperatures and stresses the aluminum is subjected to creep deformation leading to a thinning of the outer jacket. Since the seal groove depth remains unchanged the helical spring expands, which in turn leads to a decrease of the generated spring and seal force.
Although the main reason for the change of seal parameters over time and temperature is known, a detailed characterization of the seal behavior and a reliable prediction of the parameter development for aging times that exceed the experimental time frame have not been possible, yet.
For deeper understanding of the aging processes, an Investigation program, which is covered in this contribution, is conducted at Bundesanstalt für Materialforschung und –prüfung (BAM) that focusses on the behavior of the aluminum jacket and its influence on the long-term sealing performance. The program investigates properties of material samples as well as the behavior of the seal as a component.
Original sheet material of the same aluminum that is used for manufacturing of the seals is investigated in compression creep tests. For this, a DMA (dynamic mechanical analysis) machine is employed (here used for static tests) that allows for a measurement of the specimens deformation under forces of up to 500 N. The advantage of this method is that the original material can be tested in the same shape as used for the seals which is 0.5 mm thick sheet material. For investigation of tensile creep standard specimens are used, that were machined from surrogate material of the same composition and annealing condition.
Furthermore, aluminum seals that are cut into smaller segments are assembled in flanges and placed in heating chambers at temperatures ranging from 23°C to 150°C. After different periods of time from 3 days to 300 days the segments are taken out of the flanges and are investigated, thus giving information on different states of aging. Measurements of the development of the seal contact width and the aluminum jacket thickness are done with an optical microscope. Further investigations on the segments will include metallography and hardness measurements.
From the detailed material and component behavior including the results of the long-term seal force and useable resilience investigations a better understanding of the overall seal behavior can be gained. The aim is to contribute to the development of material models and analytical approaches for the prediction of the sealing behavior in dependence of time and temperature.
In Germany spent nuclear fuel (SNF) and high level radioactive waste (HLW) are stored in interim storage containers with double lid systems. Those lids are equipped with metal seals (e.g. Helicoflex®) that ensure the safe enclosure of the inventory. Being licensed for up to 40 years of interim storage the evaluation of the long-term behavior of the seals is necessary, taking into account storage conditions, decay heat and possible mechanical loads.
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.
The creep behavior of single-crystals of the nickel-base superalloy CMSX-4 was investigated at 1288°C, which is the temperature of the hot isostatic pressing (HIP) treatment applied to this superalloy in the industry. It was found that at this super-solvus temperature, where no Gamma’-strengthening occurs, the superalloy is very soft and rapidly deforms under stresses between 4 and 16 MPa. The creep resistance was found to be very anisotropic, e.g. the creep rate of [001] crystals was about 11 times higher than that of a [111] crystal. The specimens of different orientations also showed a very different necking behavior. The reduction of the cross-section area psi of [001] crystals reached nearly 100%, while for a [111] crystal psi=62%. The EBSD analysis of deformed specimens showed that despite such a large local strain the [001] crystals didn’t not recrystallize, while a less deformed [111] crystal totally recrystallized within the necking zone. From the shape of deformed specimens and TEM investigations it was concluded that the main strain contribution resulted from <011> {111} octahedral slip.
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 large number of TEM investigations and the regular microstructure
of single-crystal nickel-base superalloys has boosted the development of a number of physically motivated constitutive laws. In contrast to the more phenomenological models discussed in the next chapter, these models use dislocation densities as internal variables. Obvious advantages are that the computed densities can be compared to TEM observations and the Deformation mechanisms can be easier translated into mathematical equations.
In our current view, reference datasets in the MSE domain represent specific material properties, e.g., structural, mechanical, … characteristics. A reference dataset must fulfill high-quality standards, not only in precision of measurement but also in a comprehensive documentation of material, processing, and testing history (metadata). This Infrastructure Use Case (IUC) aims to develop a framework for generating reference material datasets using creep data of a single crystal Ni-based superalloy as a best practice example. In a community-driven process, we aim to encourage the discussion and establish a framework for the creation and distribution of reference material datasets. In this poster presentation, we highlight our current vision and activities and intend to stimulate the discussion about the topic reference datasets and future collaborations and work.
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.
This article refers to the research article entitled “Creep-Fatigue of P92 in Service-Like Tests with Combined Stress- and Strain-Controlled Dwell Times” [1]. It presents experimental mechanical data from complex service-like creep-fatigue experiments performed isothermally at 620 °C and a low strain amplitude of 0.2 % on tempered martensite-ferritic grade P92 steel. The data sets in text file format provide cyclic deformation (min. and max. stresses) and the total (hysteresis) data of all recorded fatigue cycles for three different creep-fatigue experiments: 1) a standard relaxation fatigue (RF) test with symmetrical dwell times of three minutes introduced at minimum and maximum strain, 2) a fully strain-controlled service-like relaxation (SLR) test combining these three-minute peak strain dwells with a 30-minute dwell in between at zero strain, and 3) a partly stress-controlled service-like creep (SLC) test combining the three-minute peak strain dwells with 30-minute dwells at constant stress. Such service-like (SL) tests with additional long-term stress- and strain-controlled dwell times are non-standard, rare, and expensive, making these data very valuable. They may be used to approximate cyclic softening in the technically relevant range, for the design of complex SL experiments, or for detailed analyses of stress-strain hystereses (e.g., for stress or strain partitioning methods, for the determination of hysteresis energies (work), inelastic strain components, etc.). In addition, the latter analyses may supply important input for advanced parametric lifetime modeling of components under creep-fatigue loading or model calibration parameters.