5 Werkstofftechnik
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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.
Lightweighting as a cross-cutting technology contributes significantly to achieve the European Green Deal goals. Based on, but not limited to, advanced materials and production technologies, the demand for natural resources and CO2 emmissions are reduced by lightweighting during production, as well as use phase. Therefore, lightweighting is a crucial transformation technology assisting in decoupling economic growth from resource consumption. In this manner, lightweighting contributes significantly as a key technology of relevance for many industrial sectors such as energy, mobility, and infrastructure, towards resource efficiency, climate action and economic strength, as well as a resilient Europe. To strengthen international partnerships, addressing global issues of today at the edge of science with high performance lightweight material based on carbon fibers, an overview about the BAM expertise in carbon fiber reinforced materials is given.
In order to be able to manipulate ceramic powder compacts and ceramic suspensions (slurries) in their volume with light, a minimum transparency of the materials is required. Compared to polymers and metals, ceramic materials are characterized by the fact that they have a wide electronic band gap and therefore a wide optical window of transparency. The optical window generally ranges from less than 0.3 µm to 5 µm wavelength. Therefore, to focus light into the volume of a ceramic powder compact, its light scattering properties need to be tailored. In this study, we present the physical background and material development strategies for the application of two-photon polymerization (2PP), Xolography and selective volumetric sintering for the additive manufacturing of structures in the volume of ceramic slips and green compacts.
Instead of foreseeing and preparing for all possible scenarios of machine failures, accidents, and other challenges arising in space missions, it appears logical to take advantage of the flexibility of additive manufacturing for “in-space manufacturing” (ISM). Manned missions into space rely on complicated equipment, and their safe operation is a great challenge. Bearing in mind the absolute distance for manned missions to the Moon and Mars, the supply of spare parts for the repair and replacement of lost equipment via shipment from Earth would require too much time. With the high flexibility in design and the ability to manufacture ready-to-use components directly from a computer-aided model, additive manufacturing technologies appear to be extremely attractive in this context. Moreover, appropriate technologies are required for the manufacture of building habitats for extended stays of astronauts on the Moon and Mars, as well as material/feedstock. The capacities for sending equipment and material into space are not only very limited and costly, but also raise concerns regarding environmental issues on Earth. Accordingly, not all materials can be sent from Earth, and strategies for the use of in-situ resources, i.e., in-situ resource utilization (ISRU), are being
envisioned. For the manufacturing of both complex parts and equipment, as well as for large infrastructure, appropriate technologies for material processing in space need to be developed.
Glass-fibre-reinforced plastics (GFRP) are commonly used for the construction of pressure vessels and tanks for example in automotive and aerospace industries. Especially for pressure vessels used for the storage of natural gas or hydrogen with operation pressures up to 700 bar, an early material fatigue detection is of great interest. Measuring the distributed strain profile of GFRP structures helps to understand and detect material fatigue. In this article, we demonstrate the great potential of swept wavelength interferometry (SWI) based distributed strain sensing for the monitoring of pressure vessels made from GFRP. A resin transfer molding (RTM) process was used to manufacture GFRP-tube specimens. Commercial optical fibres with polyimid coating were glued to the surface externally in circumferential and axial direction. A cyclic load of up to 150 bar was applied to the samples using a servo-hydraulic test bench. Comparing the loaded and unloaded test conditions, we determined up to 2 % elongation in circumferential direction. We demonstrate reliable distributed strain measurements with sub-centimetre spatial resolution. By monitoring these high-resolution strain profiles, we were able to detect local material degradation that manifested itself as localized strain changes. Crucially, the material Degradation could be detected already after 75 % of dat the fatigue life before a crack appeared that led to leakage.
Characteristics of environmental stress cracking of PE-HD induced by biodiesel and diesel fuels
(2024)
In the context of the increasing effect of carbon dioxide emissions on the global climate biodiesel produced from renewable sources has emerged as a promising contender replacing fossil fuels, especially in long-range transport vehicles, using existing engines and infrastructure.
High-density polyethylene is one of the prevailing materials for pipe and container applications for storage and transport of such fuels, both, from fossil and renewable resources. The contact with the respective fuels raises questions concerning material compatibility as biodiesel exhibits significant differences compared to conventional diesel fuel affecting its sorption and plasticization behavior in polyethylene. In this study, its behavior with respect to environmental stress cracking, considered one of the most frequent damage mechanisms leading to failure of polymer parts and packaging, was evaluated using the well-established Full Notch Creep Test. This
approach allows for a detailed fracture surface analysis using imaging techniques, such as optical and laser scanning microscopy, as well as infrared spectroscopy. Comparing the environmental stress cracking behavior in standard surfactant solutions with that in biodiesel and diesel, respective crack propagation rates, showing different levels of acceleration, were determined and details of the underlying mechanisms could be revealed.
Furthermore, the specific infrared absorption of the biodiesel’s ester functionality allows its semi-quantitative determination on the fracture surface of the tested specimens after failure. Thus, a preferred uptake of sorptive fluids in the fracture zone due to local morphological changes of the polyethylene could be directly evidenced by infrared spectroscopy.
Characterization of early crystallization stages in surface-crystallized diopside glass-ceramics
(2019)
Structure formation in glass-ceramics by means of surface crystallization is a challenging open question and remains elusive to definite answers. In several glass-ceramic systems, oriented crystal layers have been observed at the immediate surface, including diopside and some fresnoite systems. However, it is still open to debate, whether oriented surface crystallization is the result of oriented nucleation or growth selection effects. In the same vein, there is still discussion whether surface nucleation is governed by surface chemistry effects or by defects serving as active nucleation sites.
In order to help answer these questions, annealing experiments at 850°C have been performed on a MgO·CaO·2SiO2 glass, leading to the crystallization of diopside at the surface. Different annealing durations and surface treatment protocols (i.a. lapping with diamond slurries between 16 µm and 1 µm grain size) have been applied. Particular focus has been put on earliest crystallization stages, with crystal sizes down to about 200 nm. The resultant microstructure has been analyzed by electron backscatter diffraction (EBSD) and two different kinds of textures have been observed, with the a- or b-axis being perpendicular to the sample surface and the c-axis lying in the sample plane. Even at shortest annealing durations, a clear texture was present in the samples. Additionally, selected samples have been investigated with energy-dispersive x-ray spectroscopy in the scanning transmission electron microscope (STEM-EDX). The diopside crystals have been found to exhibit distinguished submicron structure variations and the glass around the crystals was shown to be depleted of Mg.
Introduction
Lithium-ion batteries (LIBs) are one key technology to overcome the climate crisis and energy transition challenges. Demands of electric vehicles on higher capacity and power drives research on innovative cathode and anode materials. These high energy-density LIBs are operated at higher voltages, leading to increased electrolyte decay and the current collectors' degradation. Even though this fundamental corrosion process significantly affects battery performance, insufficient research is being done on the aluminum current collector. Fast and convenient analytical methods are needed for monitoring the aging processes in LIBs.
Methods
In this work glow-discharge optical emission spectrometry (GD-OES) was used for depth profile analysis of aged cathode material. The measurements were performed in pulsed radio frequency mode. Under soft and controlled plasma conditions, high-resolution local determination (in depth) of the elemental composition is possible. Scanning electron microscopy (SEM) combined with a focused ion beam (FIB) cutting and energy dispersive X-ray spectroscopy (EDX) was used to confirm GD-OES results and obtain additional information on elemental distribution.
Results
The aging of coin cells manufactured with different cathode materials (LCO, LMO, NMC111, NMC424, NMC532, NMC622, and NMC811) was studied. GD-OES depth profiling of new and aged cathode materials was performed. Quantitative analysis was possible through calibration with synthetic standards and correction by sputter rate. Different amounts of aluminum deposit on the cathode surface were found for different materials. The deposit has its origin in the corrosion of the aluminum current collector. The results are compatible with results from FIB-EDX. However, GD-OES is a faster and less laborious analytical method. Therefore, it will accelerate research on corrosion processes in high energy-density batteries.
Innovative aspects
- Quantitative depth profiling of cathode material
-Monitoring of corrosion processes in high energy-density lithium-ion batteries
- Systematic investigation of the influence of different cathode materials
Low-temperature co-fired ceramics (LTCC) are used to fabricate robust multilayer circuits. Typically, thick-film technology is applied for metallization. For specific sensor applications, thin films are deposited directly on the as-fired LTCC-surface. These deposited thin films are structured either by lift-off or by etching. The latter is less error-prone and thus preferred in industry provided the selected materials allow it.
200 nm Ni-thin films were deposited on three different commercial constrained-sintered LTCC (CT708, CT800 and DP951) by electron beam physical vapour deposition. The thin-films were structured by covering corresponding sections with a UV-curable photo resisn and subsequent etching of the uncovered surface, leaving behind the desired structure. The etched Ni-thin film showed high difference in failure rate and sheet resistance regarding the used LTCC-material. DP951 had the lowest sheet resistance and no failure, whereas the CT800 had a failure rate of 40 %. The LTCC with high failure rate showed a strong chemical attack by the used etching medium. To address this phenomenon, the chemical resistance of the three different commercial LTCC (CT708, CT800 and DP951) against four different commonly used etching media (sulphuric acid, phosphoric acid, aqua regia, and hydrofluoric acid) is investigated. The dissolved ions are analyzed by ICP-OES to correlate the LTCC-composition and its chemical resistance.
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.
Quenching a metallic liquid sufficiently fast can give rise to an amorphous solid, typically referred to as a metallic glass. This out-of-equilibrium material has a long suite of remarkable mechanical and physical properties but suffers from property deterioration via structural relaxation. As a function of time, relaxation may indeed constitute significant threads to safe applications. Consequently, relaxation of glasses has a long history across different amorphous materials and typical characterization methods promote a picture of gradually evolving and smooth relaxation, as for example obtained from mechanical spectroscopy. However, the true structural dynamics and underlying mechanisms remain far from understood and have hampered a physically informed atomic-scale picture of transport and physical aging of glasses.
Here we exploit the ability to track atomic-scale dynamics with x-ray photon correlation spectroscopy (XPCS) and resolve an unprecedented spectrum of short- and long-term relaxation time scales in metallic glasses. Conducted across temperatures and under the application of stress, the results reveal anything else than smooth aging and gradual energy minimization. In fact, temporal fluctuations persist throughout isothermal conditions over several hundred thousand of seconds, demonstrating heterogeneous dynamics at the atomic scale. In concert with microsecond molecular dynamic simulations, we identify possible mechanisms of correlated atomic-scale dynamics that can underly the temporal fluctuations and structural decorrelations. Despite temporally heterogeneous, the Kohlrausch-Williams-Watts functions is well suited to capture the average intermediate relaxation time regime, but at very long time scales an asymptotic power-law emerges. This indicates anomalous diffusion and gives overall strong evidence for temporal fractional diffusion in metallic glasses. We discuss these results in terms of the structural fast and slow relaxation modes as well as a true microstructure in metallic glasses.
Within the perspective of increasing reliability of AM processes, real-time monitoring allows part inspection while it is built and simultaneous defect detection. Further developments of real-time monitoring can also bring to self-regulating process controls. Key points to reach such a goal are the extensive research and knowledge of correlations between sensor signals and their causes in the process.
Several recent studies have revealed that the phase decomposition in medium- and high-entropy alloys is triggered by solute segregation at grain boundaries. The chemically complex nature of these alloys already clues that such segregation in materials should be something more than the interaction between solutes and grain boundary, but also affected by the solute-solute interactions during the segregation. In fact, experiments indicate the significance of such solute-solute interaction. Yet, the mechanisms of co-segregation in multi-component alloys are rather challenging to explore and rarely studied quantitatively. Recently, a CALPHAD-integrated density-based phase-field model has been proposed for studying grain boundary phenomena. Several applications of this model have shown its expansive capacity for investigating grain boundary segregation and phase behavior. In this talk, the applications of this model to studying co-segregation phenomena and grain boundary phase diagrams in multi-component alloys are presented ––the term ‘co-segregation’ here refers to co-evolution and any mutual interplay among the solutes and grain boundary during the segregation. In particular, the iron-based ternary and quaternary alloys are discussed. I show how a grain boundary may have its own miscibility gap and how this immiscibility can influence the co-segregation behavior. As an alternative to grain boundary phase diagrams, rather suited for binary and ternary alloys, a new concept of co-segregation maps for screening and segregation design in multi-component alloys is presented. Applying the co-segregation maps, the nonlinear Mn and Cr co-segregation in Fe-Co-Mn-Cr is discussed.
Carbon Capture Utilization and Storage (CCUS) is a promising technology to reach the target for reduction of CO2 emissions. Crucial points for a sustainable and future-proof CCUS system are reliability and cost efficiency of the whole process chain, including separation of CO2 from the source, compression of CO2, its subsequent transportation to the injection site and injection into geological formations, e.g. aquifers. Recent studies have shown that even at a very low concentration of impurities, condensation of sulfuric and nitric acids in dense phase CO2 are possible and observable. Thus, impact of impure CO2 stream toward corrosion susceptibility of materials to be used in CCUS system need to be considered. In this talk, basing on results achieved from two German long-term projects (COORAL and CLUSTER), the dominating impurities of the CO2 stream and corrosion mechanisms are addressed. Investigations cover the whole CCUS process chain and provide a material recommendation for certain parts.
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.
Depending on the CO2 generating and the capture process as well as on consecutive purification steps applied, CO2 streams from different emitters may differ in their composition. When CO2 streams with different compositions are fed into a larger pipeline network, there are several aspects that must be considered: i) chemical reactions, such as acid formation, may occur within the joint CO2 stream; ii) there may be a variation of mass flow rate and CO2 stream composition within the pipeline network if the feed-in behavior of different CO2 sources changes with time. Potential impacts of changing CO2 stream compositions and mass flow rates in CCS cluster systems were investigated in the collaborative project "CLUSTER" (see also www.bgr.bund.de/CLUSTER). In this presentation, we focus on the experimental investigations of formation and condensation of strong acids and their impacts on the corrosion of pipeline steels. When SO2, NO2, O2 and H2O are present simultaneously in CO2 streams chemical cross-reactions may occur leading to the formation of strong acids such as sulfuric and nitric acid. To prevent this acid formation the concentration of at least one of these four impurities must be kept very low (e.g., Rütters et al., 2016). At temperatures below the acid dew point temperature, acids will condense, e.g., on pipeline steel surfaces. In turn, these acid condensates may trigger steel corrosion. To better understand the process of acid formation and condensation and its implications for steel corrosion, exposure tests were performed on pipeline steel X70 in dense CO2 with varying SO2, NO2 and O2 concentration under high pressure and at 278 K in an observable autoclave, in which water was added as droplets or as vapor. Further, electrochemical tests were carried out with X70 specimens immersed in 500 mL CO2-saturated synthetic condensate solution or in droplets of the same solution on the specimen’s surface. Depending on impurity concentrations in the CO2 streams, condensates consisting of different relative amounts of nitric and sulfuric acid were formed. In condensates containing both nitric and sulfuric acid, corrosion rates were higher than the sum of those of the individual acids. In addition, corrosion products and forms depended on the condensate composition. Investigations of water droplets on steel surfaces in impurity-containing dense-phase CO2 revealed the diffusion of SO2 and NO2, followed by cross-reactions forming corresponding acids. An increase in droplet size (from 1 to 5 µl) lead to higher corrosion rates. However, in comparison to measurements in bulk solution, corrosion reactions in droplets resulted in thick, high-resistance corrosion products and observed droplet corrosion rates were significantly lower. In addition, the possibility of acid droplet formation and growth in impure liquid CO2 is influenced by the wetting behavior of the acid droplet on the steel surface. Thus, the contact angle between a water droplet and the surface steel specimens in a CO2 atmosphere was investigated in a high pressure view cell following the sessile drop method. The contact angle wasand found to be larger at higher CO2 pressures (studied from 5 to 20 MPa) and at higher temperatures (e.g. 278 K to 333 K). Further, measured contact angles were larger on rough than on smooth metal surfaces. In addition, acid formation reduced the contact angle, i.e. lead to better wetting, thereby stimulating condensation that was followed by a corrosion process. These detailed insights on the complex interplay of acid formation, condensation, wetting behavior and corrosion allow a better assessment of material suitability for pipeline transportation of impure CO2 streams
Trace elements W and Hf have different influence on the microstructure and the mechanical properties when added to the Al10Co25Cr8Fe15Ni36Ti6 compositionally complex alloy. The addition of both can thus merge both element’s beneficial influences when combined with the appropriate heat treatment: Hf enhances the cubicity of the γ’ particles in the γ matrix while the W reduces the negative influence of the Heusler phase: this phase can be completely dissolved when W is present in the alloy.
Low-temperature co-fired ceramics (LTCC) are used to fabricate multilayer circuits which are robust in harsh environments. Thick-film technology is well established for the metallization of circuit boards and microsystems. For specific sensor applications, the combination of LTCC and thin-film technology is advantageous to reach higher structure resolutions. Due to the high roughness of as-fired LTCC surfaces compared with silicon-wafers, the deposition of low-defect- films with narrowly specified properties is challenging. There is spare literature about thin films on commercial LTCC comparing different material systems or sintering techniques. For developing thin film sensors on multilayer circuits it is crucial to identify thin-film-compatible commercial LTCC material as well as the crucial surface properties. In this work we evaluate the thin-film capability of different LTCC surfaces.
The as-fired surfaces of free-sintered, constrained-sintered (sacrificial tape), and pressure-assisted sintered commercial LTCCs (DP951, CT708, CT800), as well as respective polished surfaces, were analyzed by tactile and optical roughness measurements and scanning electron microscopy. The thin-film capability of the LTCC surfaces was assessed by sheet resistance and temperature coefficient of resistance (TCR) of deposited Ni thin-film layers. Contrary to the expectations, no correlation between roughness and thin-film capability was found. Ni thin films on constrained sintered DP951 show the lowest sheet resistance and highest TCR within the experimental framework of the as-fired surfaces. The influence of surface morphology on the film properties is discussed.
Reliable characterization of materials at the nanoscale regarding their physio-chemical properties is a challenging task, which is important when utilizing and designing nanoscale materials. Nanoscale materials pose a potential toxicological hazard to the environment and the human body. For this reason, the European Commission amended the REACH Regulation in 2018 to govern the classification of nanomaterials, relying on number-based distribution of the particle size.
Suitable methods exist for the granulometric characterization of monodisperse and ideally shaped nanoparticles. However, the evaluation of commercially available nanoscale powders is problematic. These powders tend to agglomerate, show a wide particle size distribution and are of irregular particle shape.
Zinc oxide, aluminum oxide and cerium oxide with particle sizes less than 100 nm were selected for the studies and different preparation methods were used comparatively.
First, the nanoparticles were dispersed in different dispersants and prepared on TEM-supported copper grids. Furthermore, individual powders were deposited on carbon-based self-adhesive pads. In addition, the samples were embedded by hot mounting and then ground and polished.
The prepared samples were investigated by scanning electron microscopy (including the transmission mode STEM-in-SEM) and Dynamic Light scattering. The software package ImageJ was used to segment the SEM images and obtain the particle sizes and shapes and finally the number-based particles size distribution with size expressed as various descriptors.
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
Additively Manufactured (AM) parts are still far from being used in safety-relevant applications, mainly due to a lack of understanding of the feedstock-process-propertiesperformance relationship. This work aims at providing a characterization of the fatigue behavior of the additively manufactured AISI 316L austenitic stainless steel and a direct comparison with the fatigue performance of the wrought steel. A set of specimens has been produced by laser powder bed fusion (L-PBF) and a second set of specimens has been machined out of hot-rolled plates. The L-PBF material shows a higher fatigue limit and better finite life performance compared to the wrought material, accompanied by an extensive amount of cyclic softening.
The phenomenon of expelling nanomaterial from microparticles of different materials, such as Au, WO3 or B2O3 under the influence of a convergent electron beam (CB) of a transmission electron microscope (TEM) was reviewed by Ignacio Gonzalez-Martinez [1]. Converging the e-beam in a TEM means that a high amount of energy enters the microparticle at a very local place and interact with the matter. Obviously, during the convergent beam protocol, no imaging with the electron beam is possible, but at the end, nanoparticles with different appearances lie down next to the microparticle while its size is reduced.
Hence, there is a blind spot in the observation, which we want to fill, as we want to help clarify the nature of the expelling phenomenon. One hypothesis that explains the phenomenon is the so-called damage (of the microparticle) induced by an electric field (DIEF). Within this theory, the material is ionized and expelled in form of ionic waves. Our aim is therefore to fabricate specimens with artificial microlandscapes, as schematically exemplified in figure 1a), using the focused ion beam (FIB) and micromanipulators, as experimental setups to follow the paths of the expelled material.
As a first step towards the fabrication of such specimen, we make experimental feasibility studies for each fabrication method, FIB structuring with Ga+ ion beam and micromanipulated microparticle deposition. Bridges (gray regions in Fig. 1) are created by milling a commercially available electron transparent membrane (silicon oxide or carbon) of a Cu-TEM grid. Platinum or carbon walls (blue features in Fig. 1) are built to stand on those bridges. Microparticles (yellow sphere in Fig. 1) of gold or other material are deposited in the center of the bridges.
Figure 2a) shows four square holes (black area) and between them the residual silicon oxide membrane bridges (dark grey). On top of the bridges, walls (light grey) are deposited. The width of the bridges is different, the walls overlap the holes as well as the distance between the walls is very small, so these and other parameters need to be optimized. Figure 2b) shows a square hole (black) with bridges (white) on the right side on top of a carbon membrane (grey). There are still some obstacles which needs to be eliminated. For instance, the deposition process of the walls is not reliable as visible at the wall on top where a hole arises instead of a wall.
These studies are still in progress and the results are further discussed in terms of the applicability for the DIEF experiment in the TEM.
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.
Non-equilibrium microstructure evolution in additive manufacturing (AM) is a major barrier for establishing a safe and sustainable application of AM in industrial processes. The constant heat source in the AM continuously affects the just-solidified grains beneath the melting pool, leading to directional grain growth (DGG). While real-time measurements of the non-equilibrium microstructure evolution is challenging, here developing a computational framework to systematically explore DGG becomes imperative.
We have advanced a comprehensive approach, integrating mean-field modeling and phase-field simulations, to elucidate the dynamics of DGG under an external driving force. Our simulations unveil a steady-state power-law grain growth kinetics during DGG, characterized by the interplay between curvature-driven dynamics at grain boundary junctions and directional driving forces.
The durability of concrete structures and its performance over the lifetime is strongly influenced by many interacting phenomena such as e.g. mechanical degradation due to fatigue loading, loss of prestress, degradation due to chemical reactions or creep and shrinkage. Failure due to cyclic loading is generally not instantaneous, but characterized by a steady damage accumulation.
Many constitutive models for concrete are currently available, which are applicable for specific loading regimes, different time scales and different resolution scales. A key limitation is that the models often do not address issues related to fatigue on a structural level. Very few models can be found in the literature that reproduce deterioration of concrete under repeated loading-unloading cycles.
The objective of this paper is the presentation of numerical methods for the simulation of concrete under fatigue loading using a temporal multiscale method.
First, a continuum damage model for concrete is developed with a focus on fatigue under compressive stresses. This includes the possibility to model stress redistributions and capture size effects. In contrast to cycle based approaches, where damage is accumulated based on the number of full stress cycles, a strain based approach is developed that can capture cyclic degradation under variable loading cycles including different amplitudes and loading frequencies. Second, a multiscale approach in time is presented to enable structural computations of fatigue failure with a reduced computational effort. The damage rate within the short time scale corresponding to a single cycle is computed based on a Fourier based approach. This evolution equation is then solved on the long time scale using different time integration schemes.
Considerations for nanomaterial identification of powders using volume-specific surface area method
(2019)
The EC’s recommendation for a definition of nanomaterial (2011/696/EU) should allow the identification of a particulate nanomaterial based on the number-based metric criterion according to which at least 50% of the constituent particles have the smallest dimension between 1 and 100 nm. However, it has been recently demonstrated that the implementation of this definition for regulatory purposes is conditioned by the large deviations between the results obtained by different sizing methods or due to practical reasons such as high costs and time-consuming.
For most measurement methods for particle size determination it is necessary to initially disperse the particles in a suitable liquid. However, as the particle size decreases, the adhesion forces increase strongly, making it more difficult to deagglomerate the particles and to assess accurately the result of this process. Therefore, the success of the deagglomeration process substantially determines the measurement uncertainty and hence, the comparability between different methods.
Many common methods such as dynamic light scattering (DLS), centrifugal liquid sedimentation (CLS) or ultrasound attenuation spectroscopy (US) can give good comparable results for the size of nanoparticles, if they are properly separated and stabilized (e.g. in reference suspensions).
In order to avoid the use of hardly available and expensive methods such as SEM / TEM for all powders, an agglomeration-tolerant screening method is useful.
One of the measurement methods well suited to probe the size of particulate powder is the determination of the volume-specific surface area (VSSA) by means of gas adsorption as well as skeletal density. The value of 60 m2/cm3 corresponding to spherical, monodisperse particles with a diameter of 100 nm constitutes the threshold for decisioning if the material is a nano- or non-nanomaterial. The identification of a nanomaterial by VSSA method is accepted by the EU recommendation.
However, the application of the VSSA method was associated also with some limitations. The threshold of 60 m2/cm3 is dependent on the particle shape, so that it changes considerably with the number of nano-dimensions, but also with the degree of sphericity of the particles. For particles containing micro-pores or having a microporous coating, false positive results are induced. Furthermore, broad particle size distributions made necessary to additionally correct the threshold. Based on examples of commercially available ceramic powders, the applicability of the VSSA approach was tested in relation with SEM and TEM measurements. The introduction of a correction term for deviations from sphericity and further additions improved the applicability of VSSA as a screening method.
The commercial usage of latent thermal energy storages primarily depends on the development of a suitable phase change material (PCM). For industrial high temperature applications above 400 °C multicomponent chloride eutectics are promising and therefore discussed seriously. The profound thermodynamic investigation of such eutectics requires a much greater amount of specimen material than conventional calorimeter can handle. Therefore, a special adiabatic calorimeter was developed and designed. With a specimen mass of > 100 g the typical thermodynamic measurements with a commercial calorimeter can be extended by cycle stability measurements, which are often decisive for practical application of PCM. Furthermore, by implementing corrosion specimens inside the calorimeter high temperature corrosion experiments according to ISO 21608 can be performed inside the calorimeter. Adiabatic measuring conditions can be provided by using two separate heating systems. Therefore, the outer “protective system” follows the temperature curve of the inner “measuring system” minimizing the temperature difference between the heating systems and simultaneously preventing heat losses from the measuring systems.
Powder bed technologies are amongst the most successful Additive Manufacturing (AM) techniques. 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 enabling 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. Not only very fine, submicron powders can be processed with low organics, but also the dense powder bed provides excellent support to the parts built. The LSD technology can be combined with binder jetting to develop the so-called “LSD-print” process. LSD-print combines the high-speed printing of binder jetting with the possibility of producing a variety of high-quality ceramics with properties comparable to traditional processing.
The latest development of this technology shows that it is possible to print ceramic parts in a continuous process by depositing a layer onto a rotating platform, growing a powder bed following a spiral motion. The unique mechanical stability of the layers in LSD-print allows to grow a powder bed several centimeters thick without any lateral support. The continuous layer deposition allows to achieve a productivity more than 10X higher compared to the linear deposition, approaching a build volume of 1 liter/hour.
In order to observe the effect of the aggregate phases between 2 mm and 16 mm without overlap with rheological effects induced by the cement hy-dration and without interactions with a threshold fine sand particle size that affects both, paste and aggregates, rheological experiments were conducted on a limestone filler based paste mixed with aggregates up to 16 mm. Vari-ous aggregate fractions were blended and mixed with the replacement paste in different volumetric ratios.
The dry aggregates’ flow coefficients were determined and compared to yield stress and plastic viscosity values at different aggregate volume fractions. The results indicated that the flow coefficient is not a suitable parameter to predict the performance of the aggregates in the paste. It was shown that the yield stress of pastes is largely determined by the blend of different aggregate fractions, while the plastic viscosity to large extend depends upon the coars-est aggregate fraction.
Based on the results, ideal aggregate composition ranges for minimised yield stress are presented. For the plastic viscosity no such grading curves to achieve minimum values could be found, but high viscosity curves are identified.
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.
Static immersion tests of potential injection pipe steels 42CrMo4, X20Cr13, X46Cr13, X35CrMo4, and X5CrNiCuNb16-4 at T = 60 °C and ambient pressure, as well as p = 100 bar were performed for 700–8000 h in a CO₂-saturated synthetic aquifer environment similar to CCS sites in the Northern German Basin (NGB). Corrosion rates at 100 bar are generally lower than at ambient pressure. The main corrosion products are FeCO₃ and FeOOH with surface and local corrosion phenomena directly related to the alloy composition and microstructure. The appropriate heat treatment enhances corrosion resistance. The lifetime reduction of X46Cr13, X5CrNiCuNb16-4, and duplex stainless steel X2CrNiMoN22-5-3 in a CCS environment is demonstrated in the in situ corrosion fatigue CF experiments (axial push-pull and rotation bending load, 60 °C, brine: Stuttgart Aquifer and NGB, flowing CO₂: 30 L/h, +/- applied potential). Insulating the test setup is necessary to gain reliable data. S-N plots, micrographic-, phase-, fractographic-, and surface analysis prove that the life expectancy of X2CrNiMoN22-5-3 in the axial cyclic load to failure is clearly related to the surface finish, applied stress amplitude, and stress mode. The horizontal grain attack within corrosion pit cavities, multiple fatigue cracks, and preferable deterioration of austenitic phase mainly cause fatigue failure. The CF life range increases significantly when a protective potential is applied.
Static immersion tests of potential injection pipe steels 42CrMo4, X20Cr13, X46Cr13, X35CrMo4, and X5CrNiCuNb16-4 at T = 60 °C and ambient pressure, as well as p = 100 bar were performed for 700–8000 h in a CO2-saturated synthetic aquifer environment similar to CCS sites in the Northern German Basin (NGB). Corrosion rates at 100 bar are generally lower than at ambient pressure. The main corrosion products are FeCO3 and FeOOH with surface and local corrosion phenomena directly related to the alloy composition and microstructure. The appropriate heat treatment enhances corrosion resistance. The lifetime reduction of X46Cr13, X5CrNiCuNb16-4, and duplex stainless steel X2CrNiMoN22-5-3 in a CCS environment is demonstrated in the in situ corrosion fatigue CF experiments (axial push-pull and rotation bending load, 60 °C, brine: Stuttgart Aquifer and NGB, flowing CO2: 30 L/h, +/− applied potential). Insulating the test setup is necessary to gain reliable data. S-N plots, micrographic-, phase-, fractographic-, and surface analysis prove that the life expectancy of X2CrNiMoN22-5-3 in the axial cyclic load to failure is clearly related to the surface finish, applied stress amplitude, and stress mode. The horizontal grain attack within corrosion pit cavities, multiple fatigue cracks, and preferable deterioration of austenitic phase mainly cause fatigue failure. The CF life range increases significantly when a protective potential is applied.
During capture and storage technology (CCS) as well as in geothermal energy production Steels need to withstand the corrosive environment such as: heat, pressure, salinity of the aquifer and CO2-partial pressure. 1.4542 shows unusual corrosion phenomena, but is still sufficiently resistant in corrosive environments. To better understand its behaviour differently heat treated coupons of 1.4542 and for comparison X20Cr13 and X46Cr13 were kept in the artificial brine of the Northern German Basin at T=60 °C. Ambient pressure as well as p=100 bar for 700 h - 8000 h in water saturated supercritical CO2 and CO2-saturated synthetic aquifer Environment was applied. Fatigue tests were performed via push-pull tests with a series of 30 specimens from 150 MPa to 500 MPa (sinusoidal dynamic test loads, R=-1; resonant frequency ~ 30 Hz). FeCO3 and FeOOH are corrosion products also after dynamic corrosion tests. Martensitic microstructure offers good corrosion resistance in geothermal environment. The S-N-curve showing no typical fatigue strength and very steep slopes of possible fatigue strength for finite life. Possible influencing artefacts, such as Al-inclusions could not be correlated to early rupture despite specimens containing inclusions at the fracture surface and cross section reached lower number of cycles. Applied potential proofed to enhance fatigue life tremendously.
This contribution provides current findings regarding materials susceptibility for carbon capture, utilization and storage (CCUS) applications. Basing on results gathered in 2 German long-term projects (COORAL and CLUSTER) suitable materials are introduced as well as dominating impurities of the CO2-stream and corrosion mechanisms. Investigations cover the whole CCUS process chain and provide material recommendations for certain parts.
This contribution provides current findings regarding materials susceptibility for carbon capture, utilization and storage (CCUS) applications. Basing on results gathered in 2 German long-term projects (COORAL and CLUSTER) suitable materials are introduced as well as dominating impurities of the CO2-stream and corrosion mechanisms. Investigations cover the whole CCUS process chain and provide material recommendations for certain parts.
The ferritic steel 13CrMo4-5 due to good properties with relation to attractive price is frequently use in power plants industry. According EN10028-2 this steel can be used up to 570 °C because of its creep behavior but its corrosion resistance limits the use frequently to lower temperatures, depending on gas temperature and slag formation. The corrosion test were performed in environment containing mixture of gases like: O2, COx, SOx and ashes, with elements e.g. Na, Cl, Ca, Si, C, Fe, Al. Exposure time was respectively 240 h, 1000 h and 4500 h in temperature 600 °C. The oxide scale on the 13CrMo4-5 steel was significant thicker than for In686 coating and the difference increase according for longer exposure time.
The microstructure, chemical and phase composition of the oxide scales were investigated by means of a light microscope, the electron scanning and transmission microscopes (SEM,TEM) equipped with the EDS detectors.
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.
While a lage amount of research on high entropy alloys is oriented towards mechanical properties and the microstructural improvement it is also necessary to keep an eye on the environment that potential application materials will be submitted to. The Co-Cr-Fe-Ni based high entropy family has shown great potential over the years of high entropy research and some candidate alloys are chosen for an insight into their corrosion behaviour. Several atmospheres are studied, i.e. O2, H2O, SO2 and a mix thereof in argon as well as synthetic air. Just as for classic alloys, the chromium is the most important element in terms of protection agains further corrosion. The addition of manganese, as in case of the “Cantor alloy” CrMnFeCoNi, overpasses Cr when it comes to oxygen affinity and thus counteracts the layer formation of Cr2O3. Even without Mn, a temperature chosen too high will also affect the formation of the chromium oxide layer and spall it off, annulling its protective potential. We can also observe how trace elements influence the layer formation. These effects and their mechanisms will be discussed for the alloys CrFeNi, CoCrNi, CrMnFeCoNi and variations of Al10Co25Cr8Fe15Ni36Ti6 using a combination of electron microscopy, thermodynamic calculations and x-ray diffraction.
To apply high-entropy alloys (HEA) of the CrMnFeCoNi family in challenging atmospheres, their degradation behavior under harsh environments needs to be investigated. Oxidation studies to HEAs have not been extensively investigated and most of them are concentrated on environments like synthetic air, laboratory air, CO/CO2, O2 and H2O atmospheres. Main corrosion products which were identified after aging times of up to 100 h are Mn2O3 (≤800°C) and Mn3O4 (≥800°C).
Another corrosive medium in high temperature applications is SO2, which preferentially forms sulfides on commercial steels for example. These can be occurred both in the oxide layer and at the oxide/metal interface. For instance, on Fe-Cr based alloys sulfides (Cr5S6) were detected along grain boundaries and their number increases with exposure time and Cr-content in the alloy. These sulfides show an increased hardness, compared to the bulk alloy, and cause an embrittlement of the grain boundaries. This is a serious material degradation phenomenon, now addressed for the case of HEAs.
In the present study metal sulfides were identified after corrosion of the HEA CrMnFeCoNi alloy in an Ar-0.5vol.%SO2 atmosphere at 800°C for 24 h, 48 h, 96 h and 192 h exposure time. After all three duration times, a thin non-protective Cr2O3 layer has formed at the oxide/alloy interface. At the gas side a thick Mn3O4 layer with local voids containing sulfur could be detected by SEM-EDS analysis. Furthermore, S precipitates could be detected in the bulk material near the surface. These sulfides were characterized in detail by scanning and transmission electron microscopy. Based on these results, a model for grain boundary sulfidation of high-entropy alloy CrMnFeCoNi is discussed.
Alkali and alkaline earth chlorides are discussed as heat storage media and are characterized by their low price and high availability. Disadvantages are a high corrosion rate and formation of Cr6+ ions in the melt, as observed in various binary chlorine salt melts. In our work the system NaCl-KCl-MgCl2 is considered. The storage capacity in this salt system is between 2 and 3 MWh per 10 t salt, depending on composition, melting temperature and working temperature. At the same time the system offers a eutectic line, which allows a high variance of the composition and possibly different corrosion rates can be observed. Corrosion tests in melts were carried out and the corrosion layers investigated. The tests with chloride melts on 12% Cr steel show an inner corrosion zone of up to 40 µm depth after 96 hours. The corrosion mechanisms and potential solutions are discussed.
This contribution provides current findings regarding materials susceptibility for CCUS applications. Basing on results gathered in 2 German long-term projects (COORAL and CLUSTER) suitable materials are introduced as well as dominating impurities of the CO2 stream and corrosion mechanisms. Investigations cover the whole CCUS process chain and provide the following recommendations for certain parts. 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.
Fiber-reinforced-polymers (FRPs) are in current research focus in the lightweight construction industry, because of their extraordinary characteristics (stiffness and strength-to-density relation). The structure of polymer matrix and the interaction with reinforcement are crucial for optimization of the mechanical and thermal properties of FRPs. Due to the macromolecular chain structure, the mechanical properties of a polymer strongly vary with temperature: Below the glass transition, the chain segments of a polymer are “frozen”. Regarding fracture, the total changed energy during fracture if only dissipates for the generation of the new surfaces. However, in the region of the glass transition, the polymer chain segments start to get “unfrozen”, and the energy is not only required for generating new surfaces, but also for irreversibly deformation. This irreversible deformation is affected by the global temperature and the local temperature near the crack tip, which is affected by the local strain rate and crack propagation velocity.
Hence, in this research project, the irreversible deformation of neat and reinforced polymers will be controlled by changing the global temperature as well as the local temperature. With using different fracture experiments, the amount of energy required for creating new surfaces and for the irreversible deformation will be separated. The fracture tests include the conventional tensile test, the macroscopic peel test and the single fiber peel – off test.
Crack propagation in polymers: Separation of surface energy and irreversible deformation energy
(2019)
Fiber-reinforced-polymers (FRPs) are in current research focus in the lightweight construction industry, because of their extraordinary characteristics (stiffness and strength-to-density relation). The structure of polymer matrix and the interaction with reinforcement are crucial for optimization of the mechanical and thermal properties of FRPs. Due to the macromolecular chain structure, the mechanical properties of a polymer strongly vary with temperature: Below the glass transition, the chain segments of a polymer are “frozen”. Regarding fracture, the total changed energy during fracture if only dissipates for the generation of the new surfaces. However, in the region of the glass transition, the polymer chain segments start to get “unfrozen”, and the energy is not only required for generating new surfaces, but also for irreversibly deformation. This irreversible deformation is affected by the global temperature and the local temperature near the crack tip, which is affected by the local strain rate and crack propagation velocity.
Hence, in this research project, the irreversible deformation of neat and reinforced polymers will be controlled by changing the global temperature as well as the local temperature. With using different fracture experiments, the amount of energy required for creating new surfaces and for the irreversible deformation will be separated. This poster is the summary of the first part of the whole project. In the first part, the basic crack propagation theory for neat polymers is established and the special fracture experiment sample is prepared and tested at room temperature. In addition, the fracture experiment at room temperature is validated numerically.
Following the new paradigm of materials development, design and optimization, digitalization is the main goal in materials sciences (MS) 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. For storage, processing, and querying of data in contextualized form, Semantic Web Technologies (SWT) are used since they allow for machine-actionable and human-readable knowledge representations needed for data management, retrieval, and (re)use.
In this respect, the motivation for digital transformation in materials sciences stemming from the need to handle the ever-increasing volume and complexity of data will be elaborated on. By embracing digital tools and methodologies, researchers can enhance the efficiency, accuracy, and reproducibility of their work. The benefits of digital transformation in materials sciences are manifold, including improved data management, enhanced collaboration, and accelerated innovation. Being a core component of this transformation, ensuring data reliability and reproducibility is critical for the advancement of the field, enabling researchers to build on each other's work with confidence. Implementing FAIR data principles facilitates this by making data more accessible and usable across different platforms and studies. Furthermore, Semantic Web technologies (SWT) and ontologies play a crucial role in achieving these goals. Ontologies, typically consisting of the T-Box (terminological component) and A-Box (assertional component), provide a structured framework for representing knowledge. This presentation will outline the path of ontology creation and the formal transformation procedure, highlighting the various ontology levels that organize data into meaningful hierarchies.
Real-world use cases presented, such as the Tensile Test Ontology (TTO) and the Orowan Demonstrator, illustrate the practical applications of these technologies. These examples will demonstrate how ontologies can be leveraged to standardize data and facilitate interoperability between different systems and research groups. Finally, in this presentation, Ontopanel is introduced, a tool designed to aid in the creation and management of ontologies. Ontopanel simplifies the process of developing and maintaining ontologies, making it accessible to researchers and practitioners in the field. By integrating these technologies and principles, the materials science community can move towards a more digital, interconnected, and efficient future making the knowledge and education on these topics very valuable.
The aim of the task area Materials Data Infrastructure (TA-MDI) of the consortium Materials Science and Engineering (MatWerk) of National Research Data Infrastructure (NFDI) is to shape scientific datasets obtained through the Participant Projects (PPs) from a data management perspective conforming to the FAIR principles, making use of the FAIR Digital Object (FAIR DO) concept, including structured metadata and storage solutions. As an example, they apply PP18 (BAM) as a use case to demonstrate the proposed technical workflow.
Creep and fracture behavior of conventionally and additively manufactured stainless steel 316L
(2020)
A critical task within the frame of establishing process-structure-property-performance relationships in additive manufacturing (AM) of metals is producing reliable and well-documented material behavior’s data and knowledge regarding the structure-property correlation, including the role of defects. After all, it represents the basis for developing more targeted process optimizations and more reliable predictions of performance in the future. Within this context, this contribution aims to close the actual gap of limited historical data and knowledge concerning the creep behavior of the widely used austenitic stainless steel 316L, manufactured by Laser-Powder-Bed-Fusion (L-PBF). To address this objective, specimens from conventional hot-rolled and AM material were tested under application-relevant conditions according to existing standards for conventional material, and microstructurally characterized before and after failure. The test specimens were machined from single blocks from the AM material. The blocks were manufactured using a standard scan and build-up strategy and were subsequently heat-treated. The creep behavior is described and comparatively assessed based on the creep lifetime and selected creep curves and characteristic values. The effect of defects and microstructure on the material’s behavior is analyzed based on destructive and non-destructive evaluations on selected specimens. The AM material shows shorter creep lives, reaches the secondary creep stage much faster and at a lower strain, and features lower creep ductility compared to its conventional counterpart. The creep damage behavior of the AM material is more microstructure than defect controlled and is characterized by the formation and accumulation of single intergranular damage along the whole volume. Critical features identified are the grain morphology and the grain-boundary as well as the dislocation’s density. Micro-computed tomography (µCT) proves to be an alternative to metallography to analyze the creep damage.
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.
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.
Metal additive manufacturing (Metal AM) continues to gain momentum. Many companies explore the manufacturing of innovative products, including components for safety critical applications. Despite the intensive research of recent years, a fundamental understanding of the process‑structure‑property relationships remains challenging due to, i.a., the inherently complex and highly hierarchical microstructures arising from the wide range of build process parameter variability. This contribution presents the resu lts of an experimental study on the creep behavior of an austenitic 316L stainless steel produced by laser powder bed fusion (PBF LB/M/316L) with an emphasis on understanding the effects of microstructure on creep mechanisms. Hot tensile tests and constant force creep tests at 600 °C and 650 °C, X ray computed tomography, as well as optical and electron microscopy were performed. The produced PBF LB/M/316L exhibits a low void population 0.01 %) resulting from the manufacturing parameters used and which a llowed us to understand the effects of other microstructural aspects on creep behavior, e.g., grain morphology and dislocation substructure. A hot‑rolled variant of 316L hwas also tested as a reference. The produced PBF LB/M/316L possesses shorter primary and secondary creep stages and times to rupture and smaller creep stress exponents than the hot‑rolled variant. Overall, the creep damage is more extensive in the PBF LB/M/316L and is characterized as predominantly intergranular. It is considered that the damage behavior is mainly impacted by the formation of precipitates at the grain boundaries combined with their unfavorable orientation. The dislocation substructure and local elemental segregation appear to have a decisive impact on the overall creep behavior.
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.
The development of refractory CCAs has been explored for potential use in high temperature applications. An example of this is the AlMo0.5NbTa0.5TiZr alloy, which resembles the well-known γ/γ’ microstructure in Ni-Base superalloys with cuboidal particles embedded in a continuous matrix. The aim of this work is to evaluate the alloy’s mechanical behavior under tension in the temperature range 800-1000°C, by applying creep tests under vacuum (excluding oxidation effects). Some little temperature influence on minimum creep rate @ 1000 and 1100 °C was found and at a first glance, and Norton plots shows that deformation is probably both diffusion and dislocation controlled. However, further work is needed to stablish deformation and degradation micro mechanisms in the studied creep regime.
The elastic constants are the most basic mechanical properties of a material and are needed for any structural analysis of a component. For example, they have a major influence on the eigenfrequencies of vibrating parts. Single crystals of Ni-base superalloys are strongly anisotropic, which means that the observed properties are orientation dependent. Tensor algebra is then required to mathematically formulate the elastic properties and their relations to the crystal orientation. Hence, this chapter first summarizes some basic definitions and calculation rules for Rotation matrices, including the definition of the Euler angles, which are most commonly used to define the relative orientations of the crystal and the component. Parts of this chapter closely follow the lines of the excellent exposition of the topic by Olschewski.
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.
High-temperature corrosion is a widespread problem in various industries.
As soon as a hot and reactive gas (CO2, O2, H2O, SO2, NOx, etc.) is in contact with a solid, physico-chemical processes at the surface and interfaces lead to material degradation. The processes are dynamic and controlled by thermodynamic and kinetic boundary conditions. Whether a reaction product is protective or not depends on various factors, such as chemical composition of the solid and the reactive media, surface treatment as well as diffusion and transport paths of cations and anions. Resulting chemical and structural inhomogeneities with the corrosion layers are characterized by off stoichiometry within cationic and anionic sub lattices. The competitive processes can be studied by various techniques of applied crystallography.
This chapter gives an overview on the challenges of chemical-structural Analysis of reaction products by crystallographic methods such as X-ray diffraction and X-ray near-edge structure spectroscopy and scanning electron microscopy electron backscatter diffraction (SEM-EBSD) for corrosion science.
This presentation is a summary of the work from the past 20 years’ development of PMC-testing at the BAM-FB 5.3 with respect to safety-relevant design of advanced light weight structures in aircraft, wind turbine and automotive applications. The talk begins with wood as an example from nature, and emphasizes that load case, fiber architectural design and the production process and quality have to go hand in hand to generate an advanced light weight structure. Since PMC-relevant basic findings of mankind span across hundreds of years, high-performance composite applications today are based more on long term experiences than on breakthrough inventions of modern days.
In the second part of the talk, future plans and projects of FB-5.3 are presented, specifically addressing H2-safety, circular economy, recycling by design and digitalization of PMC-technologies.
Cyclic fatigue behavior of glass fiber reinforced epoxy resin at ambient and elevated temperatures
(2018)
The fatigue behavior of ±45° glass fiber reinforced epoxy resin under cyclic mechanical and constant thermal loading is investigated in this study. Tests at three different temperature levels in the range 296 K to 343 K have been performed in order to create S-N curves for each temperature level. The specimen damage is measured in-situ using optical grayscale analysis. The characteristic damage state (CDS) is evaluated for each specimen. It is shown that the point of CDS is suitable as a failure criterion to compare the resulting S-N curves. With micromechanical formulations, the temperature-dependent matrix effort is calculated for each stress-temperature level. In terms of matrix effort, the longest fatigue life is reached at high temperatures, while, in terms of stress, the lowest fatigue life is reached at the highest temperatures.
Cyclic fatigue behavior of glass fiber reinforced epoxy resin at ambient and elevated temperatures
(2018)
The fatigue behavior of ±45° glass fiber reinforced epoxy resin under cyclic mechanical and constant thermal loading is investigated in this study. Tests at three different temperature levels in the range 296 K to 343 K have been performed in order to create S-N curves for each temperature level. The specimen damage is measured in-situ using optical grayscale analysis. The characteristic damage state (CDS) is evaluated for each specimen. It is shown that the point of CDS is suitable as a failure criterion to compare the resulting S-N curves. With micromechanical formulations, the temperature-dependent matrix effort is calculated for each stress-temperature level. In terms of matrix effort, the longest fatigue life is reached at high temperatures, while, in terms of stress, the lowest fatigue life is reached at the highest temperatures.
9-12% Cr ferritic-martensitic stainless steels are widely used as high temperature construction materials in power plants due to their excellent creep and oxidation resistance. The growing share of renewable energy sources in power generation forces many of these plants into more flexible operation with frequent load shifts or shutdowns. These cyclic operation profiles constitute a major lifetime issue. The present contribution reports on current findings obtained in a multidisciplinary project which combines cyclic mechanical and cyclic oxidation testing of different 9-12% Cr grades with detailed microstructural analyses.
Mechanical analyses are carried out on P92 and P91 steel grades to give an overview of softening phenomena and lifetimes obtained in isothermal cyclic loading (low cycle fatigue, LCF), non-isothermal cyclic loading (thermo-mechanical fatigue, TMF), and service-like combinations of creep and fatigue periods.
Complementary microstructural investigations by scanning and transmission electron microscopy plus EBSD are used for phase identification, substrate/oxide interface characterization and quantification of the microstructure evolution under cyclic conditions.
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.
Cyclic mechanical performance and microstructure evolution of P92 under LCF and TMF conditions
(2019)
9-12% Cr ferritic-martensitic stainless steels are widely used as high temperature construction materials in fossil fueled power plants due to their excellent creep and oxidation resistance, but changes in electricity markets during the last two decades have considerably changed the typical working conditions of these facilities. The growing contribution of renewable energy sources in power generation forces most of these plants into flexible operation with frequent load shifts or shutdowns. These cyclic operation profiles constitute a major lifetime issue, raising the question which fundamental processes govern the reaction of ferritic-martensitic steels to cyclic load and temperature variations.
The present contribution reports on current findings obtained in a multidisciplinary project funded by German Ministry of Education and Research (BMBF) which combines cyclic mechanical and cyclic oxidation testing of different 9-12% Cr grades with detailed microstructural analyses and related micromechanical modeling.
In this contribution, an overview will be given on the results obtained in the mechanical testing programme of the project. Mechanical analyses were carried out on P91 and (mainly) P92 steel grades, particularly looking at softening phenomena and lifetimes obtained in isothermal cyclic loading (low cycle fatigue, LCF), non-isothermal cyclic loading (thermo-mechanical fatigue, TMF), and service-like combinations of fatigue and creep/relaxation periods. For this purpose, cylindrical specimens were extracted from thick-walled steam pipes, orthogonal to the pipe axis, and subjected to strain controlled cyclic loading (± 0.2 to ±0.5 % mechanical strain). Temperature intervals of TMF tests were chosen as either 300-620°C or 500-620°C, resembling so-called warm or hot start conditions of a power plant.
The test results will be presented and discussed with a focus on the impact of hold periods during testing (combined creep/relaxation-fatigue conditions) on mechanical softening, lifetime and formation of cracks. The findings will be complemented by results on the modification of the hierarchical ferritic-martensitic microstructure under different loading scenarios.
9-12% Cr ferritic-martensitic stainless steels are widely used as high temperature construction materials in fossil fueled power plants due to their excellent creep and oxidation resistance, but changes in electricity markets during the last two decades have considerably changed the typical working conditions of these facilities. The growing share of renewable energy sources in power generation forces most of these plants into flexible operation with frequent load shifts or shutdowns. These cyclic operation profiles constitute a major lifetime issue, raising the question which fundamental processes govern the reaction of ferritic-martensitic steels to cyclic load and temperature variations.
The present contribution reports on current findings obtained in a multidisciplinary project funded by German Ministry of Education and Research (BMBF) which combines cyclic mechanical and cyclic oxidation testing of different 9-12% Cr grades with detailed microstructural analyses and related micromechanical modeling.
In the present first part of our contribution, an overview will be given on the results obtained in the mechanical testing programme of the project. Mechanical analyses were carried out on P91 and (mainly) P92 steel grades, particularly looking at softening phenomena and lifetimes obtained in isothermal cyclic loading (low cycle fatigue, LCF), non-isothermal cyclic loading (thermo-mechanical fatigue, TMF), and service-like combinations of creep and fatigue periods. For this purpose, cylindrical specimens were extracted from thick-walled steam pipes, orthogonal to the pipe axis, and subjected to strain controlled cyclic loading (± 0.2 to ±0.5 % mechanical strain) to different degrees of softening at temperatures up to 620 °C.
The test results will be presented and discussed with a focus on the impact of hold periods (i.e. combined creep-fatigue conditions) on mechanical softening, lifetime and crack formation. Details on the microstructural evolution and their representation in a micromechanical model will be given in a second, complementary contribution to this conference.
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, both of which are presented in “Part 2: Microstructural Evolution during Cyclic Loading and its Representation in a Physically-based Micromechanical Model“.
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.
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.
1. Introduction
A normally unwanted process that can arise when converging an electron beam onto, e.g. microparticles, has been called "damage induced by electric field" (DIEF) [1]. By DIEF, the convergent electron beam (CEB) imparts a high amount of energy to the microparticle locally and strongly interacts with its atoms. At a specific current density J, which can be controlled by the convergence angle α, the irradiated material begins to transform. The phenomenon of expelling nanomaterial from microparticles under the influence of a convergent electron beam (CB) in a transmission electron microscope (TEM) has been largely studied [2]. Several types of nanoparticles (NPs) have been observed for different metallic materials and metal oxides after specific CB protocols (P) in the TEM. Thus, DIEF can be used as a promising synthesis method controlled changes of micrometric material to create new nanometric material compositions and morphologies.
While these reactions have been observed in situ at the high acceleration voltages associated with TEM, it remains unclear whether the SEM can also be used to fabricate NPs via DIEF. In contrast to TEM there is no possibility to statically convert the electron beam to a range of α to reach the needed J as in TEM. Instead, the scanning parameters and the magnification can be manipulated so as to find an integrated J. Considering that the scanning electron microscope (SEM) is easier to use, more accessible and cheaper than a TEM, here we explore the possibility to transfer the concepts of DIEF known to operate in the TEM for in situ NP generation SEM.
2. Objectives
The main goal is to determine whether DIEF can be translated to the SEM perform to controlled in situ fabrication of nanoparticles from microparticles, using gold microparticles on amorphous SiO substrate as precursors. We determine what experimental parameters must be taken into account to create SEM-based CBPs for NP creation in the SEM with these materials.
3. Materials & methods
Gold microparticles with diameter of around 1 to 3 µm were deposited on electron transparent amorphous SiO/SiO2 substrate. Using a convergent electron beam protocol (CBP) in a scanning electron microscope (SEM) at an acceleration voltage of 30 kV, the gold microparticles were irradiated until a production of NPs takes place as shown in figure 1. The beam current varied between 16 and 23 nA.
4. Results
Depending on the CBP parameters, either only Au NPs or a mixture of Au and Si NPs are produced. The particle size ranges from a few nm up to 100 nm, and it depends on the distance of the NP to the initial position of the microparticle. Further beam parameters such as the dwell time, the effective irradiated volume and particle size determine whether NPs are produced or if the microparticles only are expelled from the substrate without reacting.
5. Conclusion
The SEM can be used as an instrument for synthesizing nanomaterials via DIEF. Different CBP protocols can be applied for obtaining either gold nanoparticles or silicon + gold nanoparticles
Damage induced by electric field (DIEF) that happens in the transmission electron microscope (TEM) when converging the electron beam (e-beam) on microparticles (MPs) can be used to synthesis new nanomaterial and nanomaterial compositions. The research questions are to clarify the limits and possibilities of the method regarding materials that can be produced, systems to which it is applicable and working beam parameters. Synthesis of nano-objects from microparticles using DIEF in TEM could be shown for different materials. Additionally, DIEF using the e-beam in a scanning electron microscope (SEM) can also be used to synthesis nano-objects. A deeper material analysis of this nano-objects was done using TEM and shows that the material of the nanoparticles (NPs) can be gold or/and silicon. Furthermore, the size of the NPs depends on the distance to the center of DIEF whereby the larger NPs are closer to the center. The areas of gold NPs are promising candidates for plasmonic or photonic devices for energy storage or transport.
Wind turbine rotor blades, made of fiber reinforced polymers (FRP), often 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 [1]. A potential repair alternative is to locally patch these areas of the blades with adhesively bonded structural repairs. However, the effects of such repair methods of the outer shell region on the structural integrity of the rotor blades are still largely unknown, and are thus investigated in this project.
The shell components of rotor blades are made of FRP composite material sandwiching a lightweight core, often a rigid foam or Balsa wood. The repair methods involve replacing the lost load path with a new material that is joined to the parent structure [2]. Repairs in this project focus on the scarf method, which allow for a smoother load distribution across the joint, aiming to study the damage mechanism of glass FRP scarf repairs for wind turbine blade shell applications. Namely, the source and path of the damage initiation and propagation, role of the interface between parent and patch material, and the role of the fiber orientation mismatch at this interface are examined. Biaxial ±45° and 0/90° FRP specimens are produced with the vacuum-assisted resin infusion (VARI) process using E-glass non-crimp fabric. The patch layers are then joined using VARI with a scarf ratio of 1:50, using glass FRP fabric with half the areal weight of the parent side to allow for better drapability. The methods and practices in specimen production are based on common industry practice in rotor blade shell manufacturing and repairs.
The specimens are tested under uniaxial tensile load, during which they are periodically monitored for damage onset. A comparison of the ±45° and 0/90° specimens allows 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. Although failure in both orientations begins as delamination at the joint edge, the difference in the mechanisms at play in the two different specimen types leads ultimately to different fracture paths. Namely, in the inter fiber failure mechanism of the ±45° specimens, the higher interlaminar strength compared to the intralaminar strength of the laminate leads to intralaminar failure of the ±45° scarf joint specimens. Alternatively, the competition in the 0/90° specimens lies between the interlaminar strength and fiber failure strength, and here we experience failure primarily across the scarf joint length. The scarf joint in the 0/90° specimens disrupts the continuity of the load-carrying 0° layers, directing the failure path to remain primarily along the scarf joint. Experimental results are compared to finite element analyses of scarf patch repairs on glass FRP sandwich specimens with the same respective layup orientations, where the damage initiation regions are identified and correlated to fiber orientation, serving as a bridge to future work which will experimentally examine the scarf repair patches on sandwich shell specimens.
Currently, the Full Notch Creep Test (FNCT) [1] method is used by material suppliers and end users in industry for the approval of container and pipe materials based on high-density polyethylene (PE-HD). The resistance to environmental stress cracking (ESC) of the material is evaluated using the time to failure of the specimen in an aqueous solution of a detergent [2, 3]. Usually specimens made of sheets with isotropic material properties, manufactured by hot pressing, are employed in order to obtain intrinsic properties of the material in terms of ESC failure. In contrast, the processes used in manufacturing to form containers and pipes, such as extrusion blow molding or extrusion, impose anisotropic properties to the material. These are mostly due to a microstructural orientation (polymer chains or crystallites) [4]. Furthermore, the different cooling conditions significantly affect the size distribution of crystallites as well as the overall morphology. It is therefore essential to understand the influence of process-induced material characteristics on failure due to ESC.
A large number of studies on material properties as a function of microstructural preferential orientation have already been conducted [5-7]. However, effects on ESC as the major failure mechanism of containers and pipes are still rather unexplored [8, 9]. The most important factor is whether primarily intramolecular high-strength covalent bonds or the substantially weaker intermolecular van der Waals forces are predominantly loaded.
In addition to the widely established classification by time to failure, the strain or crack opening displacement (COD) provides valuable information about the evolution and progression of damage as a function of time [10, 11]. Optical strain measurement using digital image correlation allows the differences in COD for isotropic and different angles of orientation of anisotropic specimens to be discussed. Also, a post-fracture surface analysis provides clarification on the craze-crack mechanism of the ESC. These different ESC-related properties of extruded and hot-pressed specimens have been investigated at different environmental medium temperatures and different initial stresses to provide a broad characterization of the fracture behavior of PE-HD.
Damage tolerance counts as one of the most widespread approach to fatigue assessment and surely as one of the most promising in understanding the process-structure-property-performance relationships in additively manufactured metallic materials. Manufacturing defects, surface roughness, microstructural features, short and long crack fatigue propagation, residual stresses and applied loads can be taken into consideration in a fracture mechanics-based fatigue assessment. Many aspects are crucial to the reliable component life prediction. Among those a prominent role is played by an accurate measurement and modelling of the short crack fatigue behavior, and reliable statistical characterization of defects and residual stresses.
This work aims at addressing the issues related to both experimental testing, fatigue and fatigue crack propagation, and fracture mechanics-based modelling of fatigue lives. Examples will be provided on an additively manufactured AISI 316 L.
This contribution contains the raw data used to compare experimental results with thermodynamic calculations using the CALPHAD method, which is related to the research article “The AlMo0.5NbTa0.5TiZr refractory high entropy superalloy: experimental findings and comparison with calculations using the CALPHAD method” [1] , and therefore this article can be used as a basis for interpreting the data contained therein. The AlMo0.5NbTa0.5TiZr refractory superalloy was characterized in the cast and annealed condition (1400 °C for 24 h) in order to measure grain size and to identify and measure the size and area fraction of the phases present. The raw data of this article include X-ray diffraction (XRD) measurements, microstructural characterization by scanning and transmission electron microscopy (SEM and TEM), and elemental analysis by energy dispersive X-ray spectroscopy (EDX). XRD includes the determination of phases and the lattice parameters (A2, B2, and hexagonal structure). Microstructural analysis by scanning and transmission electron microscopy includes (1) identification of composition, size, and volume fraction of the present phases and (2) determination of grain size. Based on these experimental data, it is possible to identify similarities and discrepancies with the data calculated using the CALPHAD method for the alloy under study in Ref. [1] , which provides the basis for better and more efficient development of reliable databases.
As part of a joint project involving the Fraunhofer Institute for Silicate Research (ISC), the Friedrich Schiller University of Jena, the Clausthal University of Technology and the Federal Institute for Materials Research and Testing (BAM), digital tools are to be created for the development of new types of glass materials. Current processes for the production of glasses with improved properties are usually very cost- and energy-intensive due to the low degree of automation and are subject to long development cycles. The use of robotic synthesis processes in combination with self-learning machines is intended to overcome these problems in the long term. The development of new types of glass can then not only be accelerated considerably, but also be achieved with much less effort.
In this talk, data generation via a robotic high-throughput glass melting system is presented, which should be the experimental basis for the ontology developed within the project GlasDigital.
The dataset provided in this repository comprises data obtained from a series of full-notch creep tests (FNCT) performed on selected high-density polyethylene (PE-HD) materials (for further details, see section 1 Materials in this document) in accordance with the corresponding standard ISO 16770.
The FNCT is one of the mechanical testing procedures used to characterize polymer materials with respect to their environmental stress cracking (ESC) behavior. It is widely applied for PE-HD materials, that are predominantly used for pipe and container applications. It is based on the determination of the time to failure for a test specimen under constant mechanical load in a well-defined and temperature controlled liquid environment. The test device used here also allows for continuous monitoring of applied force, specimen elongation and temperature.
The dataset contains 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.
Further information on data and data acquisition, analysis, and experimental details are given in “Experimental Data from Service-Like Creep-Fatigue Experiments on Grade P92 Steel”, submitted to Data in Brief. Additional analyses of these datasets, as well as experimental findings and discussions are presented in “Creep-Fatigue of P92 in Service-Like Tests with Combined Stress- and Strain-Controlled Dwell Times”, submitted to International Journal of Fatigue.
This paper investigates fast and inexpensive measurement methods for defect detection in parts produced by Additive Manufacturing (AM) with special focus on lattice parts made of ceramics. By Lithography-based Ceramic Manufacturing, parts were built both without defects and with typical defects intentionally introduced. These defects were investigated and confirmed by industrial X-ray Computed Tomography. Alternative inexpensive methods were applied afterwards on the parts such as weighing, volume determination by Archimedes method and gas permeability measurement. The results showed, that defects resulting in around 20% of change in volume and mass could be separated from parts free of defects by determination of mass or volume. Minor defects were not detectable as they were in the range of process-related fluctuations. Permeability measurement did not allow to safely identify parts with defects. The measurement methods investigated can be easily integrated in AM process chains to support quality control.
The Topic of the presentationis a discussion on defects which can cause failure in cyclically loaded metallic components. Although also touching Features such as material defects such as pores or micro-shrinkages, etc. and geometric defects such as surface roughness and secondary notches (which are not considered in the design process) which origin in manufacturing, and others the presentation concentrates on non-metallic inclusions. It is prefaced by an introduction to the life cycle of a fatigue crack from initiation up to fracture. Special emphasis is put on the fact that only cracks which are not arrested during one of their distinct Propagation stages can grow to a critical size.
At high temperatures and in harsh environments ceramic springs are often superior to metallic springs and allow for innovative solutions. A recently proposed application involves ceramic springs with metallized surfaces as capacitive force sensor. A strictly linear stress-strain characteristic of the spring is a precondition for such a sensor.
Helical ceramic springs with rectangular cross-section have been produced from sintered hollow cylinders. Alumina, ATZ, Y-TZP, and Ce-TZP springs with identical dimensions were characterized and compared regarding deformation behavior.
Spring deformation was investigated under various load scenarios.
Dynamic compression was performed with deformation speeds from 0.3 to 30 mm/min. Spring constants of alumina springs are strain rate independent. By contrast, Y-TZP spring constant increases by approximately 3 % within the experimental framework.
A high-precision test facility was developed to characterize spring displacement in nm range under static tensile load over long periods of time. Spring elongation with asymptotic course was observed for zirconia containing materials at room temperature. This effect is particularly strong in the case of Y-TZP. Up to 0.3 % time-dependent elongation was measured after 24 h under constant load. Deformation is completely reversible after unloading. Alumina springs do not show any time-dependent deformation under identical test conditions.
Contrary to alumina springs, a non-linear stress-strain behavior of TZP springs at room temperature was proved in both test series. It is supposed, that pseudo-elasticity caused by stress-induced phase transformation from tetragonal to monoclinic is responsible for this special behavior of TZP springs.
Degradation of AISI 630 exposed to CO2-saturated saline aquifer at ambient pressure and 100 bar
(2018)
In general high alloyed steels are suitable as pipe steels for carbon capture and storage technology (CCS), because they provide sufficient resistance against the corrosive environment of CO2-saturated saline aquifer which serves as potential CCS-site in Germany. High alloyed martensitic steel AISI 630 has been proven to be sufficient resistant in corrosive environments, e.g. regarding heat, pressure, salinity of the aquifer, CO2-partial pressure), but reveals a distinct corrosion pattern in CCS environment. Therefore coupons of AISI 630 heat treated using usual protocols were kept at T=60 °C and ambient pressure as well as p=100 bar up to 8000 h in an a) water saturated supercritical CO2 and b) CO2-saturated synthetic aquifer environment similar to on-shore CCS-sites in the Northern German Basin. AISI 630 precipitates a discontinuous ellipsoidal corrosion layer after being exposed for more than 4000 hours. Best corrosion resistance in the CO2-saturated synthetic aquifer environment phase is achieved via normalizing prior to exposure. In water saturated supercritical CO2 tempering at medium temperatures after hardening gives lowest corrosion rates. Corrosion fatigue via push-pull tests with a series of 30 specimens was evaluated at stress amplitudes between 150 MPa and 500 MPa (sinusoidal dynamic test loads, R=-1; resonant frequency ~ 30 Hz). The endurance limit of AISI 630 is reduced by more than 50% when exposed to CCS environment (maximum number of cycles (10 x 106) at a stress amplitude of 150 MPa).
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.
Regarding feedstocks for the additive manufacturing (AM) of ceramics, two features are most critical in classical powder based AM processes: a high particle packing density (typically >50% TD) must be achieved with very fine particles (typically submicron) in order to ensure sufficient sintering activity. Three innovative approaches will be introduced to overcome this problem:
1. Layer wise slurry deposition: The use of water based ceramic slurries as feedstock for the additive manufacture of ceramics has many advantages which are not fully exploit yet. In the layerwise slurry deposition (LSD) process a slurry with no or low organic content is repetitively spread as thin layers on each other by means of a doctor blade. During the deposition, the ceramic particles settle on the previously deposited and dried material to form thin layers with a high packing density (55-60%). The LSD therefore shares aspects both of tape casting and slip casting. The LSD differentiates from the classical powder-based AM layer deposition, which typically achieves with a flowable coarse grained powder a low packing density (35-50%) only, consequently hindering the ability of sintering ceramic parts to full density. The LSD is coupled with the principles of selective laser sintering (SLS) or binder jetting, to generate novel processes which take advantage of the possibility of achieving a highly dense powder-bed.
2. Laser induced slip casting: Contrary to the LSD process, which requires drying of each individual layer, the direct interaction of ceramic slurries with intense laser radiation, for the laser induced slip casting (LIS), is a promising approach for the additive manufacture of voluminous parts.
3. Gas flow assisted powder deposition: By the application of a vacuum pump a gas flow is realized throughout the powder bed. This gas flow stabilizes the powder bed and results into an enhanced flowability and packing density of the powder during layer deposition.
The presentation will provide a detailed discussion of potentialities and issues connected to the mentioned technologies and will describe the most recent developments in their application to technical ceramics.
Many of the most successful and precise additive manufacturing (AM) technologies are based on the deposition layer-by-layer of a flowable powder. Since the first pioneering work at the end of the 1980th many developments have been introduced, greatly extending the use of different materials, improving the physical properties of the components built and enhancing the accuracy of the process. Still very important issues remain nowadays, hampering a completely autonomous production of parts and even restricting the freedom of design by means of these technologies. One of the major issues is the low density and stability of the parts during the building process, which implies the need of support structures: The powder bed surrounding the part has an essential role, since it should support the structure during building, until it’s ready for removal. Moreover, the microstructure of the powder bed is a template for the microstructure of the part produced. In this context, the use of submicron ceramic powders is still a challenge. Three approaches for the stabilization and densification of powder beds will be presented: The Layerwise Slurry Deposition process LSD, the gas flow assisted powder deposition and the Laser Induced Slipcasting (LIS) of ceramic powder compacts.
Grain boundary (GB) chemical and structural variations can significantly influence materials performance. The former is generally ascribed to the structural gradient between the grain and GB. While GB segregation may be accompanied by chemical and structural variations, clear insights about the GB’s thermodynamic phase behaviour upon coupling between its chemistry and structure is lacking. Using the CALPHAD integrated density-based phase field model, we study the co-evolution of GB’s structure and segregation in Fe-Mn alloys. We found that the GB segregation transition is amplified if its structure can respond to chemical variation. Additionally, the coupling between GB structural and segregation evolution was found to enable co-existence of the spinodally formed low- and high-Mn phases within the GB. In the light of atomistic simulations, we expand on investigating the correlation between the parameters that characterise the GB density map with GB properties.
Systematic microstructure design requires reliable thermodynamic descriptions and phase diagrams of each and all microstructure elements. While such descriptions are well established for most bulk phases, thermodynamic assessment of crystal defects is greatly challenged by their individualistic aspects. In this talk, we present a density-based thermodynamic concept to describe defects based on available bulk thermodynamic data. Here dealing with grain boundaries (GBs), we apply this concept to compute GB (phase) diagram. Applications to segregation engineering of GBs in bulk and nanocrystalline alloys will be presented. We further develop this model to include the effect of elastic interactions due to atom size mismatch and obtain the corresponding GB (phase) diagram for the ternary Al-Cu-Li system.
Ceramic springs offer versatile possibilities for load bearing or sensor applications in challenging environments. Although it may appear unexpected, a wide range of spring constants can be implemented by material selection and especially by the design of the spring. Based on a rectangular cross-section of the windings, it is possible to design a spring geometry that generates the desired spring constant simply by choosing appropriate diameter, height, widths, and number of windings. In a recent research project the calculation of helical compression springs made of rectangular steel (German standard DIN 2090) was applied for the design of ceramic springs. A manufacturing technology has been worked out to fabricate such springs from hollow cylinders of several highly dense technical ceramics by milling. Ceramic springs with precise rectangular section, without edge damage, and mean surface roughness smaller than 0.2 µm were produced after parameter optimization. Tolerances of less than 10 µm were achieved regarding spring diameter, height, and width of cross section. It is shown that the calculations outlined in the standard are valid for a variety of ceramic materials as well. Demonstrator springs with a wide range of spring constants have been fabricated, including zirconia springs with 0.02 N/mm, alumina springs with 1 N/mm and Si3N4 springs with 5 N/mm. A reproducibility study of six zirconia springs with a constant of 0.3 N/mm showed a relative difference in spring constants of less than +/- 1 %. This combination of a valid calculation approach for spring geometry and a reliable manufacturing technology allows for purposeful development and fabrication of ceramic springs with precise mechanical properties and superior chemical stability.
Destructive and non-destructive 3D-characterization of inner metal structures in ceramic packages
(2023)
Ceramic multilayer packages provide successful solutions for manifold
applications in telecommunication, microsystem, and sensor technology. In such packages, three-dimensional circuitry is generated by combination of structured and metallized ceramic layers by means of tape casting and multilayer technology. During development and for quality assurance in manufacturing, characterization of integrity, deformation, and positioning of the inner metal features is necessary.
Visualization with high resolution and material contrast is needed.
Robot-assisted 3D-materialography is a useful technique to characterize such multimaterial structures. In that, many sections of the specimen are polished and imaged automatically. A three-dimensional representation of the structure is created by digital combination of the image stack. A quasi non-destructive approach is to perform X-ray computer tomography (CT) with different beam energies. The energies are chosen to achieve a good imaging of either the metal features, or the ceramic matrix of the structure. The combination of the respective tomograms results in a high contrast representation of the entire structure. Both methods were tested to characterize Ag and Ag/Pd conductors in a ceramic multilayer package. The results were compared in terms of information content, effort, and applicability of the methods.
The presence of large quantities of plastic waste and its fragmentation in various environmental compartments are an important subject of current research. In the environment, (photo ) oxidation processes and mechanical abrasion lead to the formation of microplastics. However, until now, there are no established quality assurance concepts for the analysis of microplastic (<5 mm) in environmental compartments, including sampling, processing and analysis.
The aim of the present work is the development of suitable examination methods and protocols (sampling, sample preparation and detection) to qualify and quantify microplastic in urbane water management systems. At first a fractional filtration system for sampling and the analytical tool, the so-called TED-GC-MS (thermal desorption gas chromatography mass spectrometry) were developed. The TED-GC-MS method is a two-step analytical procedure which consists of a thermal extraction where the sample is annealed and characteristic decomposition products of the polymers are collected on a solid phase. Afterwards these products are analysed using GC-MS. The developed fractional filtration for sampling and the TED-GC-MS for detection were used for quantitative analysis to screen the waste water influent and effluent of a Berlin waste water treatment plant for the most relevant polymers, polyethylene (PE), polypropylene (PP), polystyrene (PS), polyethylene terephthalate (PET) and polyamide (PA).
The results of the study revealed that the polymeres PE, PS and PP were detected in the effluent, and PE and PS were find in the raw waste water of the sewage treatment plant in Ruhleben, Berlin. Differences in polymer types and amounts were detected at different sampling dates and within different sieve fractions. Much higher amounts of polymers were observed in the raw waste water. The peak areas of the decomposition products, used for quantification of the polymers, were adjusted using so-called response factors since the TED-GC-MS method is more sensitive for PP and PS than for PE. It has been shown that PE is the most dominant polymer in the samples. Comparing the masses of polymers in the effluent and in the raw sewage, a removal of 99 % of the polymers in the water treatment plant can be assumed. These results are consistent with the literature where removal rates between 98-99 % were described.
Determination of Distribution Function used in MCS on Safety Analysis of Hydrogen Pressure Vessel
(2019)
The test data of static burst strength and load cycle strength of composite pressure vessels are often described by GAUSSian normal or WEIBULL distribution function to perform safety analyses. The goodness of assumed distribution function plays a significant role in the inferential statistics to predict the population properties by using limited test data. Often, GAUSSian and WEIBULL probability nets are empirical methods used to validate the distribution function; Anderson-Darling and KolmogorovSmirnov tests are the mostly favorable approaches for Goodness of Fit. However, the different approaches used to determine the parameters of distribution function lead mostly to different conclusions for safety assessments. In this study, six different methods are investigated to show the variations on the rates for accepting the composite pressure vessels according to GTR No. 13 life test procedure. The six methods are: a) NormLog based method, b) Least squares regression, c) Weighted least squares regression, d) A linear approach based on good linear unbiased estimators, e) Maximum likelihood estimation and f) The method of moments estimation. In addition, various approaches of ranking function are considered. In the study, Monte Carlo simulations are conducted to generate basic populations based on the distribution functions which are determined using different methods. Then the samples are extracted randomly from a population and evaluated to obtain acceptance rate. Here, the “populations” and “samples” are corresponding to the burst strength or load cycle strength of the pressure vessels made from composite material and a plastic liner (type 4) for the storage of hydrogen. To the end, the results are discussed, and the best reliable methods are proposed.
Determination of Distribution Function used in MCS on Safety Analysis of Hydrogen Pressure Vessel
(2019)
The test data of static burst strength and load cycle strength of composite pressure vessels are often described by GAUSSian normal or WEIBULL distribution function to perform safety analyses. The goodness of assumed distribution function plays a significant role in the inferential statistics to predict the population properties by using limited test data. Often, GAUSSian and WEIBULL probability nets are empirical methods used to validate the distribution function; Anderson-Darling and Kolmogorov-Smirnov tests are the mostly favorable approaches for Goodness of Fit. However, the different approaches used to determine the parameters of distribution function lead mostly to different conclusions for safety assessments. In this study, six different methods are investigated to show the variations on the rates for accepting the composite pressure vessels according to GTR No. 13 life test procedure. The six methods are: a) Norm-Log based method, b) Least squares regression, c) Weighted least squares regression, d) A linear approach based on good linear unbiased estimators, e) Maximum likelihood estimation and f) The method of moments estimation. In addition, various approaches of ranking function are considered. In the study, Monte Carlo simulations are conducted to generate basic populations based on the distribution functions which are determined using different methods. Then the samples are extracted randomly from a population and evaluated to obtain acceptance rate. Here, the “populations” and “samples” are corresponding to the burst strength or load cycle strength of the pressure vessels made from composite material and a plastic liner (type 4) for the storage of hydrogen. To the end, the results are discussed, and the best reliable methods are proposed.
Development and characterization of starch film and the incorporation of silver nanoparticles
(2020)
Starch is one of the biopolymers being used for bioplastic synthesis. For production, starch can be combined with different plasticizers, starches from different plant sources and even with nanomaterials to improve or to add film properties. The challenge of adding these, e.g. in the form of silver nanoparticles (AgNp) is to determine the concentration so as to avoid impairing the properties of the film, agglomeration or altering the visual characteristics of the film. In this study, a starch film synthesis route and the incorporation of silver nanoparticles has been proposed in order not to alter the properties of the film while maintaining the transparency and a clear colour of the starch film. The results showed that the proposed synthesis route is promising, efficient, reproducible, fast and the film has good mechanical properties.
Development and characterization of starch film and the incorporation of silver nanoparticles
(2020)
Starch is one of the biopolymers being used for bioplastic synthesis. For production, starch can be combined with different plasticizers, starches from different plant sources and even with nanomaterials to improve or to add film properties. The challenge of adding these, e.g. in the form of silver nanoparticles (AgNp) is to determine the concentration so as to avoid impairing the properties of the film, agglomeration or altering the visual characteristics of the film. In this study, a starch film synthesis route and the incorporation of silver nanoparticles has been proposed in order not to alter the properties of the film while maintaining the transparency and a clear colour of the starch film. The results showed that the proposed synthesis route is promising, efficient, reproducible, fast and the film has good mechanical properties.
Many microstructural features exhibit non-trivial geometries, which can only be derived to a limited extent from two-dimensional images. E.g., graphite arrangements in lamellar gray cast iron have complex geometries, and the same is true for additively manufactured materials and three-dimensional conductive path structures. Some can be visualized using tomographic methods, but some cannot be due to weak contrast and/or lack of resolution when analyzing macroscopic objects. Classic metallography can help but must be expanded to the third dimension. The method of reconstructing three-dimensional structures from serial metallographic sections surely is not new. However, the effort required to manually assemble many individual sections into image stacks is very high and stands in the way of frequent application. For this reason, an automated, robot-supported 3D metallography system is being developed at BAM, which carries out the steps of repeated preparation and image acquisition on polished specimen.
Preparation includes grinding, polishing and optionally etching of the polished surface. Image acquisition comprises autofocused light microscopic imaging at several magnification levels. The image stacks obtained are then pre-processed, segmented, and converted into 3D models, which in the result appear like microtomographic models, but with high resolution at large volume. Contrasting by classical chemical etching reveals structures that cannot be resolved using tomographic methods. The integration of further imaging and measuring methods into this system is underway. Some examples will be discussed in the presentation.