5 Werkstofftechnik
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Following the new paradigm of materials development, design and optimization, the digitalization of materials and processes is the main goal which imposes a huge challenge. In this respect, the quality assurance of processes and output data as well as the interoperability between applications following FAIR (findability, accessibility, interoperability, reusability) principles are to be ensured. This includes storage, processing and querying of data in a preferably standardized form, also addressing the incorporation of standardization bodies. 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 semantic conceptualizations that are needed for data management and the digitalization in the field of materials science.
With respect to this currently ever-growing topic of integration and reuse of data and knowledge from synthesis, production and characterization of materials, this presentation shows the efforts taken within the project Platform MaterialDigital (PMD, materialdigital.de) to store tensile test data in accordance with a standard-compliant ontological representation. The includes the path from developing an ontology in accordance with the respective standard, converting ordinary and arbitrarily selected data gained from standard tests into the interoperable RDF format, up to connecting the ontology and data, respectively. Finally, such data can be queried from a triple store.
In the field of material science and engineering (MSE), most mechanical test methods are standardized which serves as a valid basis for ontology development. Therefore, the well-known tensile test of metals at room temperature (DIN EN ISO standard 6892-1:2019-11) was selected to be considered as one of the first use cases in PMD. This consideration within the PMD features both, the ontological representation of such a tensile test in accordance with the standard as well as exemplary data generation. The semantic connection of the ontology and data leads to interoperability and an enhanced ability of querying.
The mechanical strength of wrought high-strength aluminum alloys is essentially based on precipitation hardening, possibly in combination with prior forming, e. g. by stretching. Important parameters for achieving an optimum combination of hardness, strength, ductility, toughness, and further properties such as corrosion resistance are age-hardening temperature and time.
During thermal (mechanical) treatment, nucleation and growth of precipitates takes place, leading to the desired degree of hardening. In aluminum alloys, precipitation sequences are usually passed through, i. e. a sequence of metastable precipitates is formed before the stable phase can precipitate. The optimum combination of properties is therefore based on a certain (optimum) microstructure, which can, however, change during the use of a component, since the microstructure is not stable. This happens in particular when the operating temperatures are close to the aging temperature and/or the operating times are sufficiently long. An external mechanical load may accelerate the processes. The presentation gives some examples for this.
The presentation shows the results of high cycle fatigue (HCF) tests from the aluminium alloy EN AW-2618A. This study investigates the mean stress influence in the T61 condition and the effect of overaging. For this purpose, axial HCF tests were carried out at room temperature and different stress ratios (R=-1, R=0.1) as well as with overaged conditions (T61+10h@230°C, T61+1000h@230°C). After completion of the tests, the fracture surfaces were examined to study crack initiation.
Thermal spraying enables a fast and propelling way to additively deposit various ceramics as electric insulators, which are used in conditions where polymers are not suitable. Alumina (Al2O3) is among the most employed materials in the coating industry since it exhibits good dielectric properties, high hardness, high melting point while still being cost-effective. Various parameters (e.g. feedstock type, plasma gas mixture, plasma power) significantly influence the resulting coating in terms of microstructure, porosity, crystallinity, and degree of un-or molten particles. As a consequence, these parameters need to be investigated to estimate the impact on the electrical insulating properties of thermally sprayed alumina. This study focuses on the development of a novel electric insulation coating from Al2O3 feedstock powders deposited via atmospheric plasma spray (APS). The microstructure, porosity, and corresponding crystallographic phases have been analyzed with optical microscopy, XRD, and SEM images. To achieve an understanding of the parameters influencing the electrical insulation performance of the manufactured coatings, an in-depth analysis of the fundamental dielectric parameters e.g., DC resistance, breakdown strength, dielectric loss tangent, permittivity is presented.
Multilayer thermoelectric generators are a promising perspective to the conventional π-type generators. Ceramic multilayer technology is well established for production of microelectronics and piezo-stacks. Key features of ceramic multilayer technology are full-automation, cost-effectiveness, and the co-firing of all materials in one single step. This requires similar sintering temperatures of all used materials. The development of multilayer thermoelectric generators is a subject of current research due to the advantages of this technology. One of the challenges is the compatibility of the different materials with respect to the specific design.
The presented study compares three different designs of multilayer generators based on a given set of material properties. Dualleg, unileg and transverse multilayer generators are compared to conventional π-type generators., the designs are evaluated regarding the expected maximum output power and power density using analytical calculations and FEM simulations. Additionally, the complexity of the production process and material requirements are assessed and design optimizations to simplify production are discussed.
Besides the theoretical aspects, unileg multilayer generator prototypes were produced by tape-casting and pressure-assisted sintering. These prototypes are compared to other multilayer generators from literature regarding the power factors of the used material system and the power density. Improvements of the power output by design optimizations are discussed
The interest to additively manufacture Nickel-based superalloys has substantially grown within the past decade both academically and industrially. More specifically, additive manufacturing processes such as laser powder bed fusion (LPBF) offer the ability to produce dense parts within a single manufacturing step. In fact, the exceptional freedom in design associated with the layer-based nature of the processes is of particular interest for the complex shapes typically required in turbine applications. In certain cases, the overall part performance can be achieved by tailoring the microstructure and the crystallographic texture to the specific application. However, these advantages must be paid at a price: the large local temperature gradients associated with the rapid melting and solidification produce parts that inherently contain large residual stress in the as-manufactured state. In addition, the presence of pores in the final part may further affect the in-service part failure. As among Nickel-based alloys Inconel 718 exhibits excellent weldability, this alloy has been widely studied in open research in the domain of LPBF. However, significant microsegregation of the heavier alloying elements such as Niobium and Molybdenum accompanied by dislocation entanglements may preclude the application of conventional heat treatment schedules. Therefore, different post processing heat treatments are required for laser powder bed fused Inconel 718 as compared to conventional variants of the same alloy.
In this study, we investigated two different heat treatment routes for LPBF Inconel 718. In a first routine, the samples were stress relieved and subsequently subjected to hot isostatic pressing (HIP) followed by a solution heat treatment and a two-step age (referred to as FHT). In a second routine, the samples were subjected to a single-step direct age post stress relieving heat treatment (referred to DA). We investigated the consequences of such heat treatment schedules on the microstructure, texture, and mechanical behavior. We show that by applying a DA heat treatment the typical columnar microstructure possessing a crystallographic texture is retained, while an equiaxed untextured microstructure prevails in case of an FHT heat treatment. We further evaluate how these heat treatments affect the mechanical behaviour on the macroscopic and microscopic scale.
The fracture surface of slow and continuous crack propagation during environmental stress cracking of a semicrystalline polyethylene exhibits isotropic roughness exponents at the local scale but resolved across the macroscopic fracture surface a clear position dependence is found. The spatially resolved roughness exponent admits values in the range between 0.1 and 0.4, demonstrating nontrivial exponents in the small length-scale regime. Instead, they vary across the fracture surface according to the stress-state distribution, which suggests that the exponents are intimately linked to the locally dominating dissipation processes during craze cracking.
Currently, calcium manganate CaMnO3 and calcium cobaltite Ca3Co4O9 are being investigated as n-type resp. p-type semiconducting materials as oxidation- and temperature-resistant thermoelectric materials for oxide multilayer thermoelectric generators (TEGs). In order to manufacture multilayer TEGs, pressure-assisted sintering processes at high temperatures are necessary to achieve optimal thermoelectric material properties. To realize TEGs in planar film technology, another method to obtain dense ceramic layers directly from the synthesized starting powders without a subsequent high temperature step is emerging recently: the powder aerosol deposition (PAD) method. In the present work, it is investigated whether PAD is suitable to produce dense ceramic films from Sm-doped CaMnO3 and Ca3Co4O9 powders. The resulting thermoelectric properties are characterized as a function of temperature.
CaMnO3 powder could successfully be processed by PAD with resulting layer thicknesses of 5- 6 µm without any high-temperature sintering steps of the films. The electrical conductivity and the Seebeck coefficient of the films were determined in-plane from room temperature to 600 °C in air. The results show a Seebeck coefficient of around -200 µV/K, which is comparable to results of pressed and sintered bars. At 400 °C, the electrical conductivity corresponds to the conductivity of the bar. At higher temperatures the conductivity is better than with the reference. Below 400°C, the electrical conductivity is somewhat lower than that of the reference sample, a mild thermal treatment of the PAD layer improves it. It is expected that the thermal conductivity of the PAD film will be lower compared to the bars due to the nano-crystalline film morphology. This should result in a significantly increased ZT value for the PAD layers and a higher efficiency of the TEG.
The work shows that both CaMnO3 and Ca3Co4O9 can be successfully processed by PAD, and the PAD films show comparable thermoelectric properties.
Melting of Na2CO3-ZnO-B2O3 batches containing up to 16.8 wt% AgNO3 (5 mol% Ag2O in the target glass composition) was observed in situ by means of hot stage microscopy. In all batches metallic silver precipitation took place as most of the silver nitrate was reduced to metallic silver before Ag+ ions could be dissolved in the evolving borate melts. In turn, only traces of Ag+ (<300 ppmw) were dissolved in the sodium zinc borate glass melts under study. It is assumed that the oxidation to Ag+ was limited due to poor availability of reducible oxygen in the glass melts and presence of Na2O being a stronger base than Ag2O. Thus, the precipitated metallic silver formed droplets of different sizes. The larger droplets (d > 20 µm) were already settled at the bottom of the container and remained constant in size upon dwelling for 1 h at 1050 °C of about one hour and the subsequent cooling (45 K/min) to room temperature, whereas the smaller droplets (d < 20 µm) were mobile in the borate melt due to Marangoni and Stokes motion. For the latter droplets, coalescence was observed in situ. A growth of larger droplets at the expense of smaller ones, i.e., Ostwald ripening was also expected but could not be studied with the used experimental equipment.
Liquid phase sintering of glass bearing silver pastes used in photovoltaics and microelectronics is poorly understood. In particular, the role of different network modifiers acting in the glass component and the question of the most suitable atmospheric oxygen level during sintering are still under considerable debate. To tackle these issues, low-melting and lead-free X2O-ZnO-B2O3 glasses with X = Li, Na, K and Rb (LZB, NZB, KZB and RZB) were prepared. Infrared spectroscopy showed that the glass structure was similar to each other, while an increase of tetrahedrally coordinated boron with increasing field strength of the alkali was evident. In turn, the glass transition temperature (from differential thermal analysis) increased in the order: RZB (449 °C) < KZB (460 °C) < NZB (465 °C) < LZB (472 °C). Powders of each glass were mixed with organics to receive silver-glass-pastes containing 30 vol% glass and these were subjected to heating microscopy in air. Although similar onset temperatures of sintering were recorded for Ag-NZB and Ag-LZB glass pastes, and for Ag-RZB paste and KZB-Ag-paste, respectively, differences in the crystallization behavior and final densification were observed between the former and the latter group. These were translated in terms of differences in silver dissolution and reprecipitation among the two groups. Further, running the experiments in nitrogen gas showed that sintering of all pastes was considerably hampered. The slow-down of the sinter kinetics was found to be in line with the assumed lower oxidation and dissolution of silver ions into the glass-forming liquid.
To reveal the corrosion resistance of casing steel/mortar interface in CO2 injection condition, sandwich samples were prepared and exposed up to 20 weeks in aquifer fluid under 10 MPa and 60 °C. Cross section analysis revealed the crevice corrosion as main mechanism instead of pitting corrosion, which would be expected to happen in the extremely high Chloride concentration. Detailed analysis using EDS line scan shown the slow diffusion of Chloride, suggesting why pitting did not happen after 20 weeks. To mimic the passivated steel surface, the steel coupon was passivated in simulated pore solution having pH 13.5 for 42 days. The passivated coupon was further exposed to NGB solution for 28 days. Electrochemical characterization was performed along the exposure processes to reveal the change in impedance, indicating the corrosion resistance of steel casing/mortar interface.
Fully-reversed fatigue behavior of scarf joint repairs for wind turbine blade shell applications
(2022)
Due to manufacturing imperfections which can propagate to damage under in-service loads, wind turbine rotor blades, made primarily of glass fiber reinforced polymers (GFRP), often fail significantly before their design life. To enable a quick and cost-effective return to service, localized repairs can be executed by technicians in the field, directly accessing the blades by suspended roping. Scarf joint repairs, shown to be highly efficient with a smooth load transition across angled joint walls and a restored aerodynamic profile, are the focus of this study. The damage mechanisms of these structures were examined under fully-reversed mechanical cyclic loading with a load ratio R = -1, which was made possible on the coupon scale by a custom designed anti-buckling support. The number of cycles to failure were compared across load levels. While the scarf joint ratio was held constant at 1:50, known from industry and literature to be a good compromise between restored mechanical properties and repair size, the layup sequence was varied between small-to-large and large-to-small. Hereby the effect of the presence of resin pockets and fiber orientation mismatch between the parent and repair structure on the failure mechanism as well as fatigue strength of ±45° GFRP scarf joint repair structures was studied. Strain development across the joint length was measured to assess stiffness degradation in addition to the fatigue strength recovery of scarf joint structures with respect to pristine reference specimens. Grayscale analysis was used to monitor the damage state leading to fracture across the specimens. Post-mortem fractography analysis with light microscopy described the global failure mechanisms as well as local damage distribution within the structure, all of which provided insight to critical variables in scarf joint GFRP structures under fully-reversed mechanical cyclic loading, allowing for the tailoring of such repairs on wind turbine blade shells for maximum restoration of service life.
To reveal the corrosion resistance of casing steel/mortar interface in CO2 injection condition, sandwich samples were prepared and exposed up to 20 weeks in aquifer fluid under 10 MPa and 60 °C.
Cross section analysis revealed the crevice corrosion as main mechanism instead of pitting corrosion despite very high concentration of Cl in NGB.
EDS element line scan analysis of the 20-week-exposed metal/mortar coupon showed Chloride distribution, which still not reached the metal/mortar interface, explaining no pitting was observed.
It was confirmed that FeCO3 cannot protect the steel surface in CO2 saturated NGB.
To verify the protective possibility of passivation happened on casing steel/mortar interface, simulated pore solution was synthesized and used to passivate the steel for 42 days. OCP and EIS confirmed the formation of passive layer.
The 42 day passivated layer was broken during the first minute of exposure in CO2 saturated NGB.
However, due to high concentration of Ca2+, a new carbonate CaCO3 dense layer was formed, increased the corrosion resistance of steel surface.
Glasses in the systems Me2O-ZnO-B2O3 with Me = Li, Na, K, Rb (MeZB), Na2O-ZnO-CuO-B2O3 (NZCuB), CaO-ZnO-B2O3 (CaZB), and Li2O-PbO-B2O3 (LPbB) as a reference, were studied by differential thermal analysis, dilatometry, rotational viscometry, and heating microscopy. A decrease of viscosity and sintering range was found with decreasing number of fourfold coordinated boron. The viscosity of the alkali zinc borate glasses varies only slightly. LPbB and CaZB stand out by their reduced and increased viscosities, respectively. Sodium, potassium, and calcium zinc borate glasses possess a fragility above 76. All glasses were sintered to full density before crystallization. Mostly binary zinc borate phases govern crystallization. A ternary crystalline phase was detected only in the potassium containing sample. The Weinberg glass stability parameter ranges between 0.07 and 0.12. This is caused by the presence of several crystalline phases and varying melting points of even the same crystalline phase in different glass matrices.
Low melting Li2O-PbO-B2O3, Me2O-ZnO-B2O3, Me = Li, Na, K, Rb and CaO-ZnO-B2O3 glasses were studied with Raman and infrared spectroscopies to advance the structural understanding of zinc borate glasses as potential candidates for substitution of lead containing glasses. Although the effect of type of alkali ions on the number (N4) of fourfold coordinated boron (B4) in the glasses is small, the alkali ions direct the type of borate groups, i.e., pentaborate in lithium, sodium, and calcium zinc borate glasses, as well as diborate in potassium and rubidium containing ones. Both groups were simultaneously found in Li2O-PbO-B2O3. Alkali ions are mainly responsible for the formation of B4-units and metaborate. Zinc ions favorably compensate non-bridging oxygen and partially form ZnO4. With decreasing N4 and field strength of the alkali ions the atomic packing density, glass transition temper ature and Young’s Modulus also decrease. The coefficient of thermal expansion increases with decreasing N4.
BAM is currently building up a platform of novel nanoRMs relying on iron oxide nanoparticles of different shape, size and surface chemistry. Iron oxide was chosen as a core material because of its relevance to the material and life sciences.
As a first candidate of this series, we present cubic iron oxide nanoparticles with a nominal edge length of 8 nm. These particles were synthesized by thermal decomposition of iron oleate in high boiling organic solvents adapting well-known literature procedures. After dilution to a concentration suitable for electron microscopy (TEM and SEM) as well as for small-angle X-ray scattering (SAXS) measurements, the candidate nanoRM was bottled and assessed for homogeneity and stability by both methods following the guidelines of ISO 17034 and ISO Guide 35.
The particle sizes obtained by both STEM-in-SEM and TEM are in excellent agreement with a minimum Feret of 8.3 nm ± 0.7 nm. The aspect ratio (AR) of the iron oxide cubes were extracted from the images as the ratio of minimum Feret to Feret resulting in an AR of 1.18 for TEM to 1.25 for SEM. Alternatively, a rectangular bounding box was fitted originating from the minimum Feret and the longest distance through the particle in perpendicular direction. This led to AR values of 1.05 for TEM and 1.12 for SEM, respectively. The results confirm the almost ideal cubic shape.
The manufacturability of metallic alloys using laser-based additive manufacturing methods such as laser powder bed fusion has substantially improved within the last decade. However, local melting and solidification cause hierarchically structured and crystallographically textured microstructures possessing large residual stress. Such microstructures are not only the origin of mechanical anisotropy but also pose metrological challenges for the diffraction-based residual stress determination. Here we demonstrate the influence of the build orientation and the texture on the microstructure and consequently the mechanical anisotropy of as-built Inconel 718. For this purpose, we manufactured specimens with [001]/[011]-, [001]- and [011]/[111]-type textures along their loading direction. In addition to changes in the Young’s moduli, the differences in the crystallographic textures result in variations of the yield and ultimate tensile strengths. With this in mind, we studied the anisotropy on the micromechanical scale by subjecting the specimens to tensile loads along the different texture directions during in situ neutron diffraction experiments. In this context, the response of multiple lattice planes up to a tensile strain of 10% displayed differences in the load partitioning and the residual strain accumulation for the specimen with [011]/[111]-type texture. However, the relative behavior of the specimens possessing an [001]/[011]- and [001]-type texture remained qualitatively similar. The consequences on the metrology of residual stress determination methods are discussed.
This study combines three different approaches to lower the sintering temperature of Sm-doped CaMnO3 to save energy in production and facilitate co-firing with other low-firing oxides or metallization. The surface energy of the powder was increased by fine milling, sintering kinetics were enhanced by additives, and uniaxial pressure during sintering was applied. The shrinkage, density, microstructure, and thermoelectric properties were evaluated. Compared to micro-sized powder, the use of finely ground powder allows us to lower the sintering temperature by 150 K without reduction of the power factor. By screening the effect of various common additives on linear shrinkage of CaMnO3 after sintering at 1100 ○C for 2 h, CuO is identified as the most effective additive. Densification at sintering temperatures below 1000 ○C can be significantly increased by pressure-assisted sintering. The power factor at room temperature of CaMnO3 nano-powder sintered at 1250 ○C was 445 μW/(m K2). Sintering at 1100 ○C reduced the power factor to 130 μW/(m K2) for CaMnO3 nano-powder, while addition of 4 wt.% CuO to the same powder led to ∼290 μW/(m K2). The combination of fine milling, CuO addition, and pressureassisted sintering at 950 ○C resulted in a power factor of ∼130 μW/(m K2). These results show that nano-sized powder and CuO addition are successful and recommendable strategies to produce CaMnO3 with competitive properties at significantly reduced temperatures and dwell times.
Influence of the dispersant on the parts quality in slurry-based binder jetting of SiC ceramics
(2022)
Binder jetting is establishing more and more in the ceramic industry to produce large complex shaped parts. A parameter with a great impact on the quality of the parts is the binder–powder interaction. The use of ceramic slurries as feedstock for this process, such as in the layerwise slurry deposition–print technology, allows a great flexibility in the composition. Such slurries are typically composed of ceramic powder, water, and small amounts of various additives. The understanding of the effect of these components on the printing quality is thus essential for the feedstock development. Four models were developed regarding the impact of additives, such as dispersants on printing. These models were confirmed or rebutted by experiments performed for an SiC slurry system with two different concentrations of a dispersant and a commercial phenolic resin used as a binder. It is shown that for this system the influence of the dispersant on the curing behavior and the clogging of the pores by dispersant can be neglected. The redispersion of the dispersant after the curing of the resin has no or only a minor effect. However, the wetting behavior determined by the surface energies of the system seem to be most crucial. In case the surface energy of the slurry additive is significantly lower than the surface energy of the binder, the strength of the green parts and the printing quality will be low. This was shown by inverse gas chromatography, contact angle measurement, rheological characterization, and mechanical tests with casted samples.
Powder bed technologies are amongst the most successful Additive Manufacturing (AM) techniques. Powder bed fusion and binder jetting especially are leading AM technologies for metals and polymers, thanks to their high productivity and scalability.
The application of these techniques to most ceramics has been difficult so far, because of the challenges related to the deposition of homogeneous powder layers when using fine powders.
In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method which enables the use of powder bed AM technologies also for advanced ceramic materials. The layerwise slurry deposition consists of the layer-by-layer deposition of a ceramic slurry by means of a doctor blade, in which the slurry is deposited and dried to achieve a highly packed powder layer. This offers high flexibility in the ceramic feedstock used, especially concerning material and particle size.
The LSD technology can be combined with binder jetting to develop the so-called “LSDprint” process for the additive manufacturing of ceramics.
The LSDprint technology combines the high-speed printing of binder jetting with the possibility of producing a variety of high-quality ceramics with properties comparable to those achieved by traditional processing.
In this presentation, the LSD process will be introduced and several examples of application ranging from silicate to high-performance ceramics will be shown.
Recent developments towards the scale-up and industrialization of this process will be discussed, alongside future perspectives for the multi-material additive manufacturing.