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Due to the diversity of materials and the processes associated with their production and use, the complexity of the lifecycles of materials and the multitude of academic and industrial researchers participating in generation of data for material design impose a huge challenge. The topical goal of digitalizing materials and processes can only be adequately addressed by consolidating the efforts of all stakeholders in this field. There are many scattered activities, but there is a demand for an elimination of redundancies as well as an advance in acceptance and a common basis in the digitalization of materials. Furthermore, data analysis methods play an important role in both, the experimental and simulation-based digital description of materials, but they have been poorly structured so far.
Therefore, the two joint projects Platform Material Digital (PMD, materialdigital.de) and Materials open Laboratory (Mat-o-Lab, matolab.de) aim to contribute to a standardized description of data processing methods in materials research. Besides stimulating the formation of a collaborative community in this respect, their main technical goals are the quality assurance of the processes and the output data, the acquisition and definition of their accuracy as well as the interoperability between applications. In this regard, data management in accordance with the FAIR (findability, accessibility, interoperability, reuseability) principles is addressed. There is a common agreement in the scientific community following current discussions that data is supposed to be conform to these principles. This includes storage, processing and querying of data in a preferably standardized form.
To meet the challenge to contextualize material data in a way that is consistent with all stakeholders, all necessary information on the condition of the material including production and application-related changes have to be made available via a uniform, machine-readable description. For this purpose, ontologies are to be used since they allow for machine-understandable knowledge representations and conceptualizations that are needed for data management and the digitalization in the field of materials science.
As first efforts in PMD and Mat-o-Lab, application ontologies are created to explicitly describe processes and test methods. Thereby, the well-known tensile test of metals at room temperature was described ontologically in accordance with the respective ISO standard 6892-1:2019-11.
The efforts in creating this tensile test application ontology are shown in this presentation. Especially, the path of ontology development based on standards to be pursued is focused, which is in accordance with the generic recommendations for ontology development and which is supposed to be exemplary for the creation of other application ontologies.
Carbon Capture Utilization and Storage (CCUS) is a promising technology to reach the target for reduction of CO2 emissions, e.g. from fossil-fuel operated power plants or cement mills. Crucial points for a sustainable and future-proof CCUS procedure 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.
Most components that are in contact with CO2-stream consist of steel. Depending on the operating conditions (e.g. temperature, pressure, and CO2-stream composition) specific suitable steels should be used. The compressed CO2-stream is likely to contain process specific impurities; small amounts of SO2 and NO2 in combination with oxygen and water are most harmful.
One approach, as currently preferred by pipeline operators, is to clean the CO2-stream to such levels, acceptable for carbon steel, commonly used as pipeline material. Another consideration would be, to use more corrosion resistant alloys for CO2-streams with higher amounts of impurities.
Due to the absence of certified benchmarks for upper limits, systematic experiments with impurities in the CO2-stream were carried out reflecting mainly transport and injection conditions.
Within the COORAL project (German acronym for “CO2 purity for capture and storage”) levels of impurities in the CO2-stream, being acceptable when using specific steels, were evaluated. Material exposure to dense or multiphase carbon dioxide (CO2) containing specific amounts of water vapor, oxygen (O2) sulfur dioxide (SO2), nitrogen dioxide (NO2), carbon monoxide (CO) can be a challenge to steels. In some situations, condensation of impurities and reaction products from the CO2 stream can occur.
CO2 saturated brine is supposed to rise in the well when the injection process is interrupted. The material selection shall ensure that neither CO2 nor brine or a combination of both will leak out of the inner tubing.
This COORAL-work was extended by a follow-up project, called CLUSTER. Here the additional influence of impurities was investigated when merging CO2 streams from different sources, combined within a “so-called” cluster.
Results are summarized within the following table regarding suitability for different parts of the process chain.
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.
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.
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.
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.
Bei der Untersuchung von Bruchflächen werden zunächst Beobachtungen gemacht, d.h. makroskopische und mikroskopische Merkmale analysiert und in Bildern dokumentiert. Im zweiten Schritt werden anhand der gefundenen Merkmale Rissverlauf und Bruchmechanismen ermittelt. Abschließend sollen diese Ergebnisse in einem Bericht oder Gutachten zusammengefasst werden. Hierbei ist eine skizzenhafte Darstellung der fraktographischen Befunde hilfreich für das Verständnis des Lesers. Ein vorgefertigter fraktographischer Symbolsatz würde dies erheblich vereinfachen.
Skizzen von fraktographischen Befunden sind in der Literatur recht häufig zu finden, z.B. in der VDI 3822 oder dem ASM Handbook Fractography, allerdings gibt es hierzu keine umfassende Systematik, wie sie z.B. aus der Meteorologie (Wetterkarten), Geographie (Landkarten, Seekarten) oder Geologie (Bodenkarten) seit langer Zeit bekannt sind. Deshalb wird hier der Versuch unternommen, einen Symbolsatz zu entwickeln und zur Verfügung zu stellen, mit dessen Hilfe fraktographische Befunde in eindeutiger und übersichtlicher Weise veranschaulicht werden können. Der fraktographische Symbolsatz ("Fracto Graphics") befindet sich in Entwicklung, ist offen zur Diskussion sowie für Verbesserungen.
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.
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.
Molecular orientation has a significant effect on the material properties of polymers. Preferential orientation of the microstructure (polymer chains or crystallites) in a specific direction or plane often enhances the material properties, especially if the high-strength covalent bonds are primarily exposed to loads instead of the weaker van der Waals bonds. However, the orientation-dependent microstructure and its mechanical behavior is in general already well understood by many scientific studies [1-3]. Isotropic materials are frequently required for an intrinsic material characterization without prevailing processing-induced properties, as is the case for Full Notch Creep Test (FNCT) [4] addressing environmental stress cracking (ESC) in high-density polyethylene (PE-HD) [5, 6]. Since ESC is one of the major limiting issues for long-term performance of PE-HD pipes and containers [7], which in contrast have a production-related preferential orientated microstructure due to extrusion or extrusion blow molding, it is important to additionally investigate the ESC resistance of such anisotropic microstructure.
Investigations of the slow crack growth (SCG) with respect to the molecular orientation generally obtain a factor of 1.2 up to 4.7 between crack growth perpendicular to the extrusion direction and crack growth parallel to the extrusion direction 8. Based on FNCT investigations with an aqueous detergent solution as environmental medium, hot pressed sheets with isotropic morphology are compared with extruded sheets from which specimens with different orientation angles are taken. However, the time to failure obtained by FNCT is also significantly influenced by the different cooling conditions under which the final morphology is formed. The tendency of the specimen to fail due to ESC is investigated as a function of environmental medium temperature. For a more detailed analysis of the affecting parameters in the manufacturing process, the ESC resistance is discussed considering the differences in crystallinity as revealed by thermal analysis.
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 refractory chemically complex alloy (rCCA) AlMo0.5NbTa0.5TiZr, with a density of 7.4 g/cm3, shows a compressive ultimate strength of 772 MPa at 1000 °C, comparatively surpassing Ni-base and other rCCAs. Its dual-phase microstructure, with a high volume fraction (≈ 62%) of cuboidal and plate-like particles coherently embedded in a continuous matrix, resembles the well-known pattern of the γ/γ" in Ni-base superalloys. Its developers have thus implied that it could stand as structural alloy for high temperature (HT) applications. Here, we report the HT creep properties and the underlying microstructural changes of the rCCA AlMo0.5NbTa0.5TiZr to propose deformation and degradation micromecanisms for this regime. The material was produced by arc-melting and subsequently heat treated in argon: at 1400 °C for 24 h plus a hot isostatic pressure treatment at 1370 °C and 170 MPa for 4 h, with a cooling rate of 10 K/min. Miniaturized tensile specimens (≈ 28 x 7 x 2 mm) were cut and polished to a quality of 1 μm. Creep tests were conducted in vacuum in the respective temperature and stress range 800-1200 °C and 30-120 MPa. For observation, thin slices were extracted from the gauge length, away from the fracture surface, grinded to a thickness of 100 μm, and electropolished to electron transparency. The microstructure was observed on the electropolished specimens using scanning (S) as well as transmission (T) electron microscopy (EM). The Norton plot gives Norton exponents of about 3.1 and 3.2 for temperatures of 1000 and 1100 °C, respectively. Curiously, creep rate minima are very close for a stress level of 30. The starting microstructure reflects a macroscopically lean coarse grain structure and a microscopically fine-meshed basketweave structure with coherency dislocations only around coarsened particles usually close to subgrain boundaries. Results are discussed on the base of variations of this starting microstructure after interrupted and ruptured creep tests.
A set of some unexpected and interesting microstructures has put the so-called complex concentrated alloys (CCAs) in the eye of the scientific community. The AlMo0.5NbTa0.5TiZr refractory (r)CCA, aimed at substituting Ni-base superalloys in gas turbine applications, belongs to this alloy family. After a two-stage heat treatment, this rCCA morphologically resembles the typical a two-phase microstructure of the latter. The objective of this work consists in determining the effect of the two stages of the heat treatment on the microstructure of the AlMo0.5NbTa0.5TiZr alloy to eventually improve it in terms of homogeneity and porosity.
Ti-6Al-4V alloy is intensively used in the aerospace industry because of its high specific strength. However, the application of Laser Powder Bed Fusion (LPBF) Ti-6Al-4V alloy for structurally critical load-bearing components is limited. One of the main limiting factors affecting the structural integrity, are manufacturing defects. Additionally, the high cooling rates associated with LPBF process result in the formation of large residual stress (RS) with complex fields. Such RS can cause cracking and geometrical distortions of the part even right after production. Also, the microstructure of LPBF Ti-6Al-4V in the as-built condition is significantly different from that of the conventionally produced alloy. All these factors affect the mechanical behavior of the material. Therefore, to improve the material performance it is important to evaluate the individual effect of RS, defects, and microstructure on fatigue life. To this aim Ti-6Al-4V LPBF material in as-built condition and subjected to different post-processing, including two heat treatments (for stress relief and microstructural modification) and Hot Isostatic Pressing (HIP, for densification), were investigated.
Prior to fatigue tests at elevated temperature, the microstructure, the mesostructure, and subsurface RS on the fatigue samples were investigated. It was found that the fatigue performance of HIPped samples is similar to that of conventionally produced Ti-6Al-4V. The tensile RS found at the surface of as-built samples decreased the fatigue life compared to heat-treated samples. Additionally, the modification of the microstructure (by heat treatment) did not affect the fatigue performance in the regime of mostly elastic strain. This shows that in the absence of tensile RS the manufacturing defects solely control the failure of LPBF components and densification has the strongest effect on the improvement of the mechanical performance.
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.
The relaxation of macroscopic residual stresses in laser powder bed fused stainless steel 316L
(2021)
The processing of stainless steel 316L using the additive manufacturing process Laser Powder Bed Fusion (LPBF) can widen its field of application due to a strong increase in Yield strength, without making major compromises on the ductility nor its outstanding corrosion and oxidation properties. Furthermore, improved designs that either reduce the weight or optimise the function of a part can be obtained using LPBF. These benefits are however counterbalanced by the proneness of LPBF to inducing high Residual Stresses (RS) during manufacturing. The characterisation and monitoring of these RS are of paramount importance for the wider acceptance of the LPBF process. This study focuses on the relaxation of the initial macroscopic RS present in an LPBF 316L as-built prism that undergoes various routes of manufacturing steps to achieve different specimen geometries and stress relieving treatments. The RS are determined using Angle-Dispersive (AD) and Time-of-Flight (TOF) neutron diffraction. The results reveal high tensile RS close to the surfaces and compressive RS near the centre of the as-built parts. The reduction in size and change of geometry heavily impact the stress ranges of the remaining RS, with lower stress ranges in cylindrical shaped compared to rectangular shaped specimens. Also, the application of different stress relieving heat treatments showed that heat-treating temperatures above 800 °C are necessary to obtain a strong relaxation in LPBF 316L.
High- and medium-entropy alloys (HEAs and MEAs) constitute a new class of materials. Those with a face-centered cubic (fcc) structure from the Cr-Mn-Fe-Co-Ni system have excellent mechanical properties and are considered for high-temperature applications since diffusion in these alloys was reported to be sluggish. However, their corrosion resistance at high temperatures must still be evaluated to further qualify them for such kinds of applications. Various groups studied the oxidation behavior of HEAs and MEAs under (dry) laboratory and artificial air as well as CO2/CO mixtures in different temperature ranges. Adomako et al. carried out oxidation tests in dry air between 800 °C and 1000 °C for 24 h in equiatomic CrCoNi, CrMnCoNi, and CrMnFeCoNi alloys. The authors showed that CrCoNi exhibits the best corrosion resistance at 800 °C due to the formation of a protective Cr2O3 layer. The matrix below the oxide scale was reported to be correspondingly depleted in Cr. It was further shown that the addition of Mn and Fe to CrCoNi changes the phase composition of the oxide scale at 800 °C. A Mn2O3 layer was grown during oxidation on CrMnCoNi and CrMnFeCoNi and a Cr2O3 scale was formed at the matrix/oxide scale interface. Beneath these oxide layers, Mn- and Cr-depleted zones were detected. These phase morphologies demonstrate the inward diffusion of oxygen and outward diffusion of Cr and Mn resulting in the formation of Cr2O3 and Mn2O3. In the present study, the corrosion resistance of CrMnFeCoNi and CrCoNi were confirmed and additionally characterized under further oxidizing atmospheres at 800 °C including Ar-2 Vol.% O2, Ar-2 Vol.% H20, and Ar-2 Vol.% SO2 mixtures.
In CCS environment (carbon capture and storage) pipes are loaded statically and/or cyclically and at the same time exposed constantly to the highly corrosive hot thermal water. Experimental procedures such as ambient pressure immersions tests, in-situ corrosion fatigue experiments using a flexibly designed corrosion chamber at ambient pressure and a specially designed corrosion chamber at high pressure. Experimental set-ups for push/pull and rotation bending load are introduced. The corrosion behavior and lifetime reduction of high alloyed steels (X46Cr13, 1.4043), (X5CrNiCuNb16-4, 1.4542) and (X2CrNiMoN22-5-3, 1.4462) is demonstrated (T=60 °C, geothermal brine: Stuttgart Aquifer flow rate: 9 l/h, CO₂).
Immersion tests of potential injection pipe steels 42CrMo4, X20Cr13, X46Cr13, X35CrMo4 and X5CrNiCuNb16-4 at T=60 °C and ambient pressure and p=100 bar were performed for 700 h - 8000 h in a CO₂-saturated synthetic aquifer environment similar to CCS-sites in the Northern-German-Basin. Main corrosion products are FeCO₃ and FeOOH. Highest surface corrosion rates at ambient pressure are 0.8 mm/year for 42CrMo4 and lowest 0.01 mm/year for X5CrNiCuNb16-4. Corrosion rates at 100 bar (max. 0.01 mm/year for 42CrMo4, X20Cr13, X46Cr13) are generally lower than at ambient pressure (<0.01 mm/year for X35CrMo4, X5CrNiCuNb16-4). Heat treatment to martensitic microstructure offers good corrosion resistance.
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.