5 Werkstofftechnik
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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.
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 following work deals with the quantitative fracture surface evaluation in damage analysis. So far, fracture surfaces have almost exclusively been evaluated qualitatively, i.e. the presence of fracture features is documented and their surface proportions are estimated, if necessary. Many years of experience are required, as well as an intensive comparison with defined comparative images from the literature. The aim of this work is the development of classifiers which can recognize fracture mechanisms or fracture features in scanning electron microscope images (SEM). The basis is 46 SEM images, which have been evaluated by fractography experts with regard to fracture features. The existing data set of images is expanded using augmentation methods in order to increase the variability of the data and counteract overfitting. Only convolutional neural networks (CNN) are used to create the classifiers. Various network configurations are tested, with the SegNet achieving the best results.
Thermoelectric generators can be used as energy harvesters for sensor applications. Multilayer thermoelectric generators (ML-TEGs) are a promising alternative to conventional π-type generators due to their high filling factor, high capability of automated production and the texturing potential during the production process. Calcium cobaltite is a promising thermoelectric oxide (p-type) with highly anisotropic properties. The following study shows the development of a textured unileg ML-TEG using ceramic multilayer technology.
Tape-casting and pressure assisted sintering are applied to fabricate textured calcium cobaltite. Compared to conventional sintering, pressure assisted sintering increases the strength by the factor 10. Thermoelectric properties can be tuned either towards maximum power factor or towards maximum figure of merit depending on the pressure level.
As electrical insulation material, a screen-printable glass-ceramic with high resistivity and adapted coefficient of thermal expansion is developed. From various commercial pastes a metallization with low contact resistance is chosen. The unileg ML-TEG is co-fired in one single step. The demonstrators reach 80% of the simulated output power and the power output is highly reproducible between the different demonstrators (99%). These results provide the first proof-of-concept for fabricating co-fired multilayer generators based on textured calcium cobaltite with high power factor, high density, and high strength.
Thermoelectric generators can be used for energy harvesting by directly transforming a temperature gradient into a voltage. Multilayer generators based on low-temperature co-fired ceramics technology (LTCC) are an interesting alternative to conventional π-type generators. They exhibit several advantages like high filling factor, possibility of texturing, co-firing of all materials in one single-step, and reduction of production costs due to the high possible degree of automation. Pressure-assisted sintering enables the theoretical possibility of co-firing two promising oxide thermoelectric materials: Ca3Co4O9 (p-type) and CaMnO3 (n-type). Due to the large difference in sintering temperature (300 K) the process is very challenging.
In this work we show the material development of Ca3Co4O9, CaMnO3, insulation and metallization for multilayer generators co-fired under pressure at 900 °C. The materials are tailored regarding their sintering behavior, electrical performance and coefficients of thermal expansion. Different generator designs (unileg and pn-type) were fabricated and analyzed regarding crack formation, interaction layers and thermoelectric performance. Simulated stresses during cooling in the multilayers are compared with actual crack formation for different sintering conditions. This study shows that a lower pressure level and a lower level of complexity are beneficial for co-firing and performance.
Texturing of calcium cobaltite for thermoelectric applications by pressure assisted sintering
(2021)
Thermoelectric materials can convert waste heat directly into electrical power by using the Seebeck effect. Calcium cobaltite (CCO) is considered as a promising thermoelectric p-type oxide for energy harvesting applications at temperatures above 500 °C. The properties and morphology of single-crystal CCO are strongly anisotropic because of its crystal structure of alternating layers of CoO2 and Ca2CoO3. By aligning the plate-like grains, the anisotropic properties of the grains can be assigned to the poly-crystalline parts.
In this study, the combination of tape casting and pressure-assisted sintering is used to texture and densify large scale components (50 cm²). Thereby, the influence of powder preparation and applied pressure during sintering on texturing and thermoelectric properties is investigated.
The analysis of XRD pole figures revealed that tape casting already leads to highly textured CCO. By pressure variation during sintering, the microstructure of CCO can be tailored either toward maximum power factor as required for energy harvesting or toward maximum figure of merit as required for energy recovery. Low pressure lead to a porous microstructure and maximum figure of merit and higher pressure to full densification and maximum power factor. The electrical and thermal conductivity of CCO seem depending on both texture and sinter density.
CO2 quality specifications are not only a matter of CO2 purity (i.e. CO2 content).
The “rest” also matters, in particular contents of reactive impurities affecting material corrosion (and rock alteration).
Also chemical reactions in CO2 stream needs to be considered, in particular when combining CO2 streams of different compositions.
Al2O3 coatings are often used as protective layers on steels against electrochemical and high-temperature corrosion because they are chemically inert and stable at elevated temperatures. This study presents preliminary work on the possibilities of using Al2O3 sol-gel coatings for corrosion protection of martensitic stainless steels in geothermal environments. Al2O3 sol-gel coatings were applied on UNS S42000, which is known to be susceptible to uniform and localized corrosion. The coated steel specimens were then tested in two types of artificial geothermal water, which simulate the geothermal fluids found in Sibayak (SBY), Indonesia, and North German Basin (NGB), Germany, respectively. SBY has pH 4 and 1.5 g/L of chloride ions, whereas NGB has a pH of 6 and 166 g/L of chloride ions. All experiments were carried out in autoclaves at 150 °C and 1 MPa under the deaerated condition. Evaluations were performed by investigating the surface profiles of both uncoated and coated steels before and after the corrosion test using a Laser Scanning Microscope (LSM) and Scanning Electron Microscope (SEM). Finally, Electrochemical Impedance Spectroscopy (EIS) was performed to compare the corrosion resistance of Al2O3 coated steels in SBY and NGB solutions. It was observed from the corrosion test that Al2O3 coatings are more suitable for use in the geothermal water with a higher pH.
Study of Polyaniline/Silicon Dioxide based Coating on Carbon Steel in Artificial Geothermal Brine
(2021)
By using the available resources in Indonesia, such as silicon dioxide and marine coating base, the PANI/SiO2 modified alkyd coating was able to protect carbon steel in a deaerated artificial geothermal water. The screening of coatings shows that the modification by adding individual pigment was not sufficient to protect carbon steel even during a short-term exposure, indicated by the discoloration after only seven days of exposure. Electrochemical tests indicated that there was no significant change in the Ecorr between the coated and uncoated carbon steel at room temperature. At 150 °C, the coated carbon steel has a lower potential than that of carbon steel, indicating that the coating is protecting carbon steel cathodically or slowing down the corrosion reaction. Finally, a long-term exposure test confirmed that the PANI/SiO2 modified coating successfully protects the carbon steel in the Sibayak artificial geothermal water up to 150 °C for 6 months.
Commercially available carbon steels are suitable for compression and pipelines as long as moisture content and impurities are limited. (water 50 to 100 ppmv, SO2 and NO2 ca. 100 ppmv).
Corrosion rates increase with increasing water content.
(0.2 – 20 mm/a).
Condensation of acids and therefore droplet formation is always possible, even at low water contents.
A low SO2 content within the CO2-stream might be more important than a low water content.
Cr13-steels showed a general susceptibility to shallow pitting and pitting. So, they seem to be not suitable for CCUS applications.
Low alloyed steels showed better corrosion behavior. (predictable uniform corrosion)
For direct contact with saline aquifer fluids only high alloyed steels shall be used.
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.
An investigation of the dislocation substructure and mechanical properties of high-purity niobium single crystals with different initial crystal orientations deformed in tension at strain rates of 10^{-4} to 10^3 s^{-1} is presented. Specimens were cut from a large grain niobium disk used for the manufacturing of SRF cavities. Different crystallographic tensile directions exhibited significantly different softening and hardening behaviors and elongation at fracture. Such anisotropy is reduced at high strain rates. Also, different dislocation substructures were observed with TEM at low and high strain rates. At low strain rates, dislocation cells with a high density of long dislocations were observed. At high strain rates, homogeneously distributed dislocations with a higher dislocation dipole density were observed. The relationship between the differences in dislocation substructures and mechanical properties at low and high strain rates and the potential effects on the superconducting properties are discussed.
Interfacial Spinodals
(2021)
Despite their finite spatial extent, interfaces can have profound impacts on microstructure properties. This is because of their distinct phase-like properties distinguishing them from the adjacent homogeneous bulk structure. When noticed by solute atoms, interfaces can experience their own chemical phase changes. In this talk, we investigate the constrained states of chemically decomposed phases at interfaces. A density-based theory of interfaces is proposed to describe the confined chemical decomposition at general grain boundaries. Here the grain boundary is viewed as a lesser dense, defected structure with reference to the corresponding bulk structure. Using this picture, the thermodynamic origins of interfacial spinodal phenomena are revealed. We also show that transient interfacial spinodals can be activated over a large alloy composition range, enabling kinetic engineering of interfacial chemistry.
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.
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.
The main deference between high entropy alloys and conventional alloys is the solid solution strengthening effect, which moves from a single element to a multi-element matrix. Little is known about the effectiveness of this effect at high temperatures. Investigation of temperature dependent solid solution strengthening in single phase multicomponent alloys with medium and high entropy using creep testing was performed. Creep tests carried out on single phase SX CrCoNi , CrMnFeCoNi and pure Ni from 700 to 1200 °C excluding oxidation, grain boundaries and multiphase effects. It was found that the influence of solid solution strengthening of CrCoNi and CrMnFeCoNi increases by decreasing temperature (1200 to 700 °C), and dislocation forests occur in CrCoNi and CrMnFeCoNi in comparison to pure Ni.
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.
Wind turbine rotor blades commonly fail before their projected 20-year lifespan largely due to defects that originate during manufacturing and are propagated by operational fatigue and environmental conditions. The cost-intensive replacement outcomes lead to a high loss of earnings, and are one of the inhibitors of wind turbine production. A potential repair alternative to restoring the mechanical properties of such lightweight fiber reinforced polymer (FRP) structures is to locally patch these areas with scarf joints. This type of repair allows for a smoother load distribution across the joint, and is favored especially on structures where minor aerodynamic contour changes are key. The effects of such repairs on the structural integrity, however, is still largely unknown. Building upon an understanding of the static load failure mechanism of GFRP scarf joints, presented at the ICCS23 Joint Event in 2020, the influence of the fiber orientation mismatch between parent and repair materials of 1:50 scarf joints on the failure mechanism of monolithic glass FRP specimens under cyclic fatigue load were examined in this study. Specimens with various layups were produced with the vacuum-assisted resin infusion (VARI) process using biaxial E-glass non-crimp fabric (NCF). The patch layers were then joined directly to the parent structure with the VARI using biaxial E-glass NCF with half the areal weight of the parent side to allow for better drapability. This mimics the soft-to-hard patch style utilized in wind turbine blade shell field repairs. The specimens were tested under uniaxial fatigue load, during which they were periodically monitored for damage onset. A comparison of the +45/-45° and 0/90° layups allowed for an understanding of the role of a highly mismatching fiber orientation in the transition zone between parent and patch material on the failure mechanism of the scarf joint. In addition to the tensile strength and stiffness property recovery assessment, a grayscale analysis using in-situ camera images determined the damage state leading to failure in each region across the scarf joint, which varied in the parent material versus scarf joint region, providing insight to the critical regions in this composite structure under cyclic loading.
As a type of high-performance composite material, glass-fiber reinforced plastics (GFRP) are favored for the construction of wind turbine rotor blades due to their high specific strength and stiffness properties (Grasse et al, 2010). During the blade manufacturing process, however, imperfections are often introduced, then further propagated due to harsh environmental conditions and a variety of loads (Caminero et al, 2013; Trappe et al, 2018). This leads to failure significantly before their designed lifespan. Since replacement of entire blades can be a costly potential outcome, localized repairs of the damaged region to restore structural integrity and thus lengthen its lifespan can executed in the field by technicians accessing the blades directly by suspended roping. These methods involve replacing the lost load path with a new material that is joined to the parent structure. In recent years, considerable studies have been conducted to investigate the influence of different repair parameters on the stress distribution, ultimate strength, impact behavior, and residual stresses of bonded repaired structures [Caminero et al, 2013; Trappe et al, 2018; Shufeng et al, 2014; Harman and Rider, 2011; Ahn and Springer, 2000; Lekou and Vionis, 2002). However, there currently do not exist any standardized repair procedures for wind turbine rotor blades. Namely, there is a lack of understanding about the effects of the layup of various repair methods, especially on the damage mechanism and fatigue life of the shells of rotor blades (Caminero et al, 2013; Trappe et al, 2018).
This work therefore aims to begin to enrich this knowledge gap by testing the influence of different variables among repair patches on the mechanical properties of sandwich composite structures. Manufactured with the vacuum-assisted resin infusion (VARI) process, the test specimens are produced as a GFRP structure to represent the outer shell portion of a wind turbine blade, then repaired with a scarf joint. Scarf repairs are favored as the most efficient of the common structural joints, as the removal of the damaged area with angled walls leads to a nearly uniform shear stress distribution along the bond surface and no eccentricity in the load distribution (Caminero et al, 2013; Lekou and Vionis, 2002; Siener, 1992).
The performance of specific layup methods of repair patches, namely a large-to-small versus small-to-large scheme of repair layers, is studied with static and load-controlled fatigue testing, then compared to pristine test specimens as well as to each other in terms of mechanical property restoration. The transition layer between repair and parent material is especially of interest in the performance of the structure. Damage onset, crack development and eventual failure are monitored in-situ with non-destructive testing methods, including thermography with an infrared camera system and a 3D deformation analysis system, to develop a more robust understanding of the effects of these repair concept variables on wind turbine blade shell structures.