5 Werkstofftechnik
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The current competitive situation on electricity markets forces power plants into cyclic operation regimes with frequent load shifts and starts/shutdowns. In the present work, the cyclic mechanical behavior of ferritic-martensitic 9-12 % Cr steels under isothermal and thermomechanical loading was investigated for the example of grade P92 material. A continuous softening was observed under all loading conditions. The introduction of hold periods to the applied cycles reduced material lifetime, with most prominent effects at technologically relevant small strain levels. The microstructural characterization reveals a coarsening of the original “martensitic” lath-type microstructure to a structure with polygonal subgrains and reduced dislocation density. The microstructural data forms the input for a physically-based modelling approach.
Shear testing can contribute to a better understanding of the plastic deformation of Ni-base superalloy single crystals. In the present study, shear testing is discussed with special emphasis placed on its strengths and weaknesses. Key mechanical and microstructural results which were obtained for the high-temperature (T ≈ 1000 °C) and low-stress (τ ≈ 200 MPa) creep regime are briefly reviewed. New 3D stereo STEM images of dislocation substructures which form during shear creep deformation in this regime are presented. It is then shown which new aspects need to be considered when performing double shear creep testing at lower temperatures (T < 800 °C) and higher stresses (τ > 600 MPa). In this creep regime, the macroscopic crystallographic [11−2](111) shear system deforms significantly faster than the [01−1](111) system. This represents direct mechanical evidence for a new planar fault nucleation scenario, which was recently suggested (Wu et al. in Acta Mater 144:642–655, 2018). The double shear creep specimen geometry inspired a micro-mechanical in-situ shear test specimen. Moreover, the in-situ SEM shear specimen can be FIB micro-machined from prior dendritic and interdendritic regions. Dendritic regions, which have a lower γ′ volume fraction, show a lower critical resolved shear stress.
Subsurface characterization of high-strength high-interstitial austenitic steels after impact wear
(2018)
The microstructure of the subsurface after impact wear of three high-strength high interstitial austenitic steels has been analysed using transmission electron microscopy (TEM) in alloys with C and N as interstitial elements. In all cases, a nanocrystalline region followed by a transition zone and a cold-worked area are present. Additionally, microhardness and nano-scratching tests were conducted to study the wear-related properties of the impact subsurface and the base material. The results of the microstructural analysis reveal that the following mechanisms are involved during impact wear: abrasion (ploughing), microcrack formation associated with contact fatigue, entrapment and adhesion of SiO2 particles. The analysis of the wear-related properties indicates that the subsurface acts as a self-protective layer that prevents the deterioration of the substrate.
A great amount of material properties is strongly influenced by dislocations, the carriers of plastic deformation. It is therefore paramount to have appropriate tools to quantify dislocation substructures with regard to their features, e.g., dislocation density, Burgers vectors or line direction. While the transmission electron microscope (TEM) has been the most widely-used equipment implemented to investigate dislocations, it usually is limited to the two-dimensional (2D) observation of three-dimensional (3D) structures. We reconstruct, visualize and quantify 3D dislocation substructure models from only two TEM images (stereo pairs) and assess the results. The reconstruction is based on the manual interactive tracing of filiform objects on both images of the stereo pair. The reconstruction and quantification method are demonstrated on dark field (DF) scanning (S)TEM micrographs of dislocation substructures imaged under diffraction contrast conditions. For this purpose, thick regions (> 300 nm) of TEM foils are analyzed, which are extracted from a Ni-base superalloy single crystal after high temperature creep deformation. It is shown how the method allows 3D quantification from stereo pairs in a wide range of tilt conditions, achieving line length and orientation uncertainties of 3% and 7°, respectively. Parameters that affect the quality of such reconstructions are discussed.
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.
Ni-base superalloy single crystals have been used in turbine blades for hot sections of gas turbines for over four decades. In order to increase the efficiency of the turbines, a continuous increase in the inlet temperature of combustion gases into the turbine has driven the design of turbine blades to complicated shapes and the presence of a complex pattern of cooling channels. These three-dimensional shapes, together with the inhomogeneous distribution of stresses along the blade, induce an also complicated triaxial stress state, which does not compare to uniaxial tests that are performed to characterize high temperature properties such as creep. A round notch on a test piece represents a simple configuration that generates a quasi-isostatic stress state across the notch. In the present contribution, the effect of a sharp round notch on the microstructural micromechanisms within the notched region cylindrical bars, loaded along [001] at 1020 °C and 160 MPa net stress, is studied. To this end, a series of interrupted creep tests is conducted on plain and notched bars and the microstructure is compared. Results are discussed in terms of degree microstructural coarsening, and dislocation activity. The effect of notch generation via grinding is also discussed in these terms. The presence of carbides evolving in from residual carbon is also shown and discussed. .Funding by the German Research Association (DFG) [grant number AG 191/1] is acknowledge
The current competitive situation on electricity markets forces conventional power plants into cyclic operation regimes with frequent load shifts and starts/shutdowns. In the present work, the cyclic mechanical behavior of ferritic-martensitic 9-12 % Cr steels under isothermal and thermomechanical loading was investigated for the example of grade P92 material. A continuous softening was observed under all loading conditions. The introduction of hold periods to the applied cycles reduced material lifetime, with most prominent effects at technologically relevant small strain levels. The microstructural characterization reveals a coarsening of the original “martensitic” lath-type microstructure to a structure with polygonal subgrains and reduced dislocation density. The microstructural data forms the input for a physically-based modelling approach.
Thermodynamic study of a refractory complex concentrated alloy (rCCA) using the CALPHAD method
(2019)
Multi-principal-element alloys (MPEAs), have recently come to the attention of the scientific community due to their potential for improving properties such as, e.g. mechanical strength and oxidation resistance in high temperature structural applications. The AlMo0.5NbTa0.5TiZr refractory (r)CCA is one such candidate, showing a two-phase microstructure after a two-stage heat treatment under argon atmosphere at a controlled cooling rate. Since the application conditions intended for this alloy require a long-term high temperature (> 700 °C) mechanical and oxidation resistance, it becomes necessary to assess the possible phase development in this regime. The diagrams reveal that two BCC-based phases could form during alloy solidification, where one phase would be enriched with Mo, Nb and Ta while the other phase, with Al, Ti and Zr. Activity oxides diagrams show that a stable form of aluminum oxide (α-Al2O3, Pearson symbol: hR10, corundum) can be formed.
Understanding the interaction between boehmite and epoxy and the formation of their interphases with different mechanical and chemical structures is crucial to predict and optimize the properties of epoxy-boehmite nanocomposites. Probing the interfacial properties with atomic force microscopy (AFM)-based methods, especially particle-matrix long-range interactions, is challenging. This is due to size limitations of various analytical methods in resolving nanoparticles and their interphases, the overlap of interphases, and the effect of buried particles that prevent the accurate interphase property measurement. Here, we develop a layered model system in which the epoxy is cured in contact with a thin layer of hydrothermally synthesized boehmite. Different microscopy methods are employed to evaluate the interfacial properties. With intermodulation atomic force microscopy (ImAFM) and amplitude dependence force spectroscopy (ADFS), which contain information about stiffness, electrostatic, and van der Waals forces, a soft interphase was detected between the epoxy and boehmite. Surface potential maps obtained by scanning Kelvin probe microscopy (SKPM) revealed another interphase about one order of magnitude larger than the mechanical interphase. The AFM-infrared spectroscopy (AFM-IR) technique reveals that the soft interphase consists of unreacted curing agent. The long-range electrical interphase is attributed to the chemical alteration of the bulk epoxy and the formation of new absorption bands.
The current trend towards cyclic, “flexible” operation of fossil-fueled power plants constitutes a major issue regarding lifetime and operational safety of the respective installations and their components, as was outlined in our complementary contribution (Part 1). The present contribution reports on the investigation of the microstructure evolution in cyclically loaded ferritic-martensitic steels and its representation in a physically-based micromechanical model.
For this purpose, specimens of P92 steel grade from the mechanical test programme outlined in our companion contribution (Part 1) were analyzed by scanning electron microscopy (SEM), including backscattered diffraction (EBSD) mapping, and transmission electron microscopy (TEM). A novel method was implemented to improve angular resolution of EBSD scans. Additionally, a correlative microscopy approach was developed and used to correlate EBSD and TEM measurements on the same locations of thick regions of electron transparent specimens. By applying these techniques, a detailed quantitative microstructure description of the as-received material condition, namely in terms of subgrain morphology and dislocation density/distributions, was established. Comparisons of as-received and cyclically loaded conditions from tests interrupted at different stages of lifetime indicate a rapid redistribution of in-grain dislocations with a strong interaction between mobile dislocations and low angle grain boundaries (LABs).
The proposed micromechanical model is formulated in a viscoplastic self-consistent (VPSC) scheme, which is a mean-field approach that allows us to include the crystal details at the level of slip systems while avoiding the considerable computational costs of full-field approaches (such as the classical crystal plasticity finite element analysis). Being physically-based, the model uses dislocation densities and includes the interaction between dislocations, e.g. annihilation of mobile dislocations, and evolution of microstructure, e.g. the grain coarsening. Particularly, the constitutive laws for dislocation evolution and interaction between dislocations and low angle boundaries are calibrated based on two-dimensional discrete dislocation dynamic (2D DDD) simulations, which are performed at a micro-/meso-scale. The results of the beforementioned EBSD experiments are considered as a direct input, involving e.g. the amount of geometrically necessary dislocations, average misorientations and grain characteristics.