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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.
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.
Mit Beginn der Covid-19 Pandemie und dem damit verbundenen ausschließlichen Lehren im online-Format war die Hoffnung verbunden ein Blended Learning Lehrformat für die Studieeingangsphase ohne viel konzeptionelle Änderungen übertragen zu können. Der Kurs Werkstofftechnik als Grundlagenfach für den Maschinenbau baut sich auf inverted classroom Lehrszenarien auf, deren Lerngrundlage hierfür eigens produzierte und auf das Lernziel abgestimmte Lehrfilme und Lightboard-Vorlesungen darstellen. Im Kontext der Studieneingangsphase bieten audiovisuell stimulierende Lehrfilme umfassende Lernmedien, wenn sie analog der Lerninhalte einem technischen und didaktischen Qualitätsanspruch genügen. In der Praxis des SS2020 und WS2020/21 hat sich gezeigt, dass die Moderation und Durchführung eines online-Kurses sich deutlich von dem eins blended learning-Kurses unterscheidet. Um denselben Lernerfolg bei Studierenden zu erzielen, müs-sen Anforderungen viel genauer und detaillierter verfasst werden, Studierende enger und persönlicher begleitet werden und Lehrfilme und Lernmedien in einen Gesamtzusammenhang gestellt werden. Im Folgenden werden aus persönlicher Erfahrung heraus niederschwellige, zum Teil ungewöhnliche praktische Erfahrungen zur erfolgreichen Umsetzung von Lehrfilm-basierten inverted classroom Lehrszenarien zusammengefasst und im Hinblick auf die online-Lehre bewertet.
Flipping the classroom is a method to let students study on their own and then take time to discuss their questions and do extended hands-on lectures or exercises in class – or in the case of the covid-19 pandemic during plenary online sessions. First year mechanical engineering students use different teaching materials (mainly lecture videos, lightboard videos and micromodule lectures) to study from a distance and comprehend the principle underlying science in theory. Then the online plenary lectures offer the opportunity to apply their knowledge and transfer different scientific aspects of the course to get the bigger picture. Exercises, worked solutions, selfassessed tests and peer-instruction during present time help students to check on their learning progress. However, the self-study periods and (online) plenary sessions need to be guided carefully. To meet the course learning outcome and overcome the diversity of a first year class various practical leads have to be fulfilled to turn flipped classroom teaching into success.
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.
The development of refractory chemically complex alloys (rCCAs) has been explored for potential use in high temperature applications. An example of this is the AlMo0.5NbTa0.5TiZr alloy. It was named as “high entropy superalloy” as it resembles the well-known γ/γ’ microstructure in Ni-Base superalloys with cuboidal particles embedded in a continuous matrix. However, the continuous phase in Ni Base alloys is an fcc solution and the cuboidal γ’ precipitates present the L12 intermetallic structure. On the opposite, this CCA has a reversed microstructure where the continuous matrix is formed by an ordered B2 phase which contains cuboidal precipitates of a disordered BCC phase. Some of the most importat results of microstructural analysis, creep test and oxidation are presented in the following work. The as-cast sample shows a bcc/B2 structure with hexagonal phase precipitates in amorphous state whereas the annealed sample also shows a combination of these phases but with larger bcc precipitates and a fully crystallized hexagonal intermetallic. It was found that porosity was higher in the annealed samples (Kinkerdall effect) and the hardness was higher in samples with faster cooling rate due smaller nanostructure. Norton plots show both diffusion and dislocation controlled deformation, and it was found different kinetics between dry and humid air oxidation with the presence of spallation.
Diese Untersuchung beschäftigt sich mit der Charakterisierung von Kurzrisswachstum in mittels Laser-Pulverbett-Verschmelzen (LPBF - Laser Powder Bed Fusion) hergestelltem rostfreien austenitischen Stahl. Spezifischer wird die Ermittlung zyklischer R-Kurven untersucht. Diese beschreiben den Aufbau des Widerstands gegen Ermüdungsrisswachstum - d.h. des Schwellenwertes - aufgrund von Rissschließeffekten bei physikalisch kurzen Rissen. Mit Hilfe der zyklischen R-Kurven kann die Fähigkeit eines Bauteils, physikalisch kurze Risse zu arretieren, charakterisiert werden. Wir verfügen damit über eine Schnittstelle zwischen klassischer Ermüdung und Bruchmechanik. Das ist gerade auch für additiv gefertigte (AM – Additive Manufacturing) Materialien von Interesse. Diese weisen prozessintrinsische Defekte auf, die als Initiierungsstellen kurzer Ermüdungsrisse agieren. Im Rahmen der experimentellen Untersuchungen wurden zyklische R-Kurven für konventionellen und LPBF AISI-316L-Stahl ermittelt. Insbesondere wurde der Einfluss verschiedener Wärmebehandlungen (WB1: 450°C, WB2: 800°C und WB3: 900°C) auf das Wachstumsverhalten physikalisch kurzer Risse im LPBF-Material untersucht. Aufgrund hoher Eigenspannungen war die Ermittlung des Kurzrisswachstumsverhaltens bei WB1 nicht möglich. Für WB2 und WB3 ergaben sich sehr unterschiedliche zyklische R-Kurven. Untersuchungen der Eigenspannungen, der Bruchfläche (insbesondere der Rauheit) und der Mikrostruktur sollen die Ursachen für das unterschiedliche Verhalten erklären. Die Ergebnisse werden mit den Verhältnissen in konventionellem Material verglichen.
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.
The chemically complex alloys (CCAs) that contain mostly refractory elements (rCCAs), may be highly resistant to heat and load, which makes them attractive candidates for use at extremely high temperatures associated with many technological applications, e.g. aeroengine turbines. However, the field of CCAs, especially their resistance in harsh (oxidative) and hot environment is still young and not much experimental evidence for the understanding mechanisms in this regime is available, which the proposed study addresses. For safe use in structural applications, in addition to their mechanical performance, the environmental resistance of this alloy is also critical. Surface degradation can significantly decrease the mechanical resistance during high temperature exposure, leading to premature failure. The AlMo0.5NbTa0.5TiZr rCCA only contains Al as a protection candidate and it is composed of a coherent B2/bcc nanoscopic cube-on-cube interweave and an hexagonal phase. The evaluation of the oxidation process in the AlMo0.5NbTa0.5TiZr rCCA in the heat-treated state has not been assessed yet. The proposed study focusses on a deeper understanding of the formation mechanism and growth kinetics of oxides at high temperature in the AlMo0.5NbTa0.5TiZr rCCA using synchrotron radiation. Due to the envisaged high temperature structural applications, the alloy is evaluated in an oxidation environment specifically between 800°C and 1000°C.
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.
Zur Bewältigung der Herausforderung bei der Digitalisierung von Materialien und Prozessen ist eine mit allen Stakeholdern konsistente Kontextualisierung von Materialdaten anzustreben, d.h. alle erforderlichen Informationen über den Zustand des Materials einschließlich produktions- und anwendungsbezogener Änderungen müssen über eine einheitliche, maschinenlesbare Beschreibung verfügbar gemacht werden. Dazu werden Wissensrepräsentationen und Konzeptualisierungen ermöglichende Ontologien verwendet. Erste Bemühungen in den beiden Projekten Plattform Material Digital und Materials-open-Laboratory führten zur Erstellung von Anwendungsontologien, die Prozesse und Testmethoden explizit beschreiben. Dabei wurde u.a. der Zugversuch an Metallen bei Raumtemperatur nach DIN EN ISO 6892-1 ontologisch beschrieben. Diese als Beispiel dienende Ontologieentwicklung wird in dieser Präsentation vorgestellt.
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.
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.
The discovery of the high entropy concept at the beginning of the 3rd millennium lead to a worldwide increase in metallurgical research, as the possible element combinations seemed nearly endless and the range of applications wide. In the early years of research, one of the main goals was the discovery of a single-phase high entropy alloy. As research evolved, it was found that properties could be enhanced by opening the HE-concept towards multiphase alloys, and from the wide area of possibilities our group chose a tuning of the properties towards high temperature application.
Compositionally complex Al10Co25Cr8Fe15Ni36Ti6 alloy, which is single-phase at high temperature, around 1200°C, shows a three phase morphology at intermediate temperatures, around 800°C. A high temperature homogenization procedure has to be applied in order to decrease the segregation induced by the dendritic growth. Subsequent annealing promotes the formation of the strengthening γ' precipitates. The alloy shows a positive lattice misfit between the γ and the γ' phase, which can be an indicator for good creep properties.
The microstructure can be optimized by adding trace elements such as Mo and Hf, known as γ and γ' strengtheners in Ni-based superalloys, respectively. Atom probe measurements show that Mo segregates into the γ matrix, and Hf prefers the γ' precipitates, where it increases the lattice parameter and thus also the lattice misfit, by about 50%. The alloy family shows interesting mechanical properties, especially the Al9.5Co25Cr8Fe15Ni36Ti6Hf0,5 alloy – its tensile properties are better than those of commercial Alloy 800H and IN617 at temperatures up to 700°C.
CALM is software for determining the Bravais lattice type and the resulting lattice parameters from a single Kikuchi pattern. It requires the definition of 4 bands and a single bandwidth from which all other band positions as well as bandwidths are derived. For band detection, it uses the Funk transform, which allows detection of twice as many bands as usual. CALM works for any symmetry and requires low-noise patterns of at least 320x240 pixels. The resulting errors are <2% even for such small patterns, assuming good quality. The relative errors are <0.5%. However, this requires a projection centre position best derived from a sample of a cubic phase in CALM. However, this must have been recorded under identical conditions. Hundreds of Kikuchi patterns of phases with different symmetries were examined.
The main deference between high entropy alloys and conventional alloys is the solid solution strengthening effect, which moves from a single element to a multi-element matrix. Little is known about the effectiveness of this effect at high temperatures. Investigation of temperature dependent solid solution strengthening in single phase multicomponent alloys with medium and high entropy using creep testing was performed. Creep tests carried out on single phase SX CrCoNi , CrMnFeCoNi and pure Ni from 700 to 1200 °C excluding oxidation, grain boundaries and multiphase effects. It was found that the influence of solid solution strengthening of CrCoNi and CrMnFeCoNi increases by decreasing temperature (1200 to 700 °C), and dislocation forests occur in CrCoNi and CrMnFeCoNi in comparison to pure Ni.
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.
Die „auffälligen großen Streifen“ sind von echten Schwingstreifen nur sehr schwer zu trennen, weil sie parallel zu den Schwingstreifen verlaufen und meistens ebenfalls nicht sehr groß sind. Die im Labor getesteten Proben zeigten, dass diese großen Streifen zusammen mit Verreibungen auftraten und „tire tracks“ („Reifenspuren“) verursachten. Dies wurde durch eine hochauflösende REM-Untersuchung bestätigt, die „tire tracks“ auf den „großen Streifen“ zeigte. Ein weiterer Hinweis ist die Änderung des R-Werts von -1 auf 0,1, was zu einer Bruchfläche ohne große Streifen und „tire tracks“ führt.
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.
As more industrial interests focusing on using salt caverns and repurposed gas or petroleum reservoirs for alternative fuel storage, i.e. CO2/H2, the question raises whether microorganisms may impact the infrastructure, gas purity and storage condition over time.
Environments with high salinity (> 1.5 Meq of NaCl) are resided by halophiles (salt-loving microorganisms). To compensate for the intensive osmotic stress, they have resorted to two main adaptation strategies: 1) production of compatible solutes and 2) accumulation of intracellular KCl. Microbial community analysis of several high salinity environments revealed a number of recurring genera, including Halomonas and Halanaerobium. However, the impact of halophiles on the overall integrity and stability of the storage facilities remain largely unknown.
To evaluate the suitability and stability of saline storage facilities, several model halophilic microorganisms, such as members of Halomonas, will be selected as testing subjects. First, the impact of halophiles on the infrastructure will be determined using an integrative approach by combining a number of techniques, including electrochemistry, TOF-SIMS, SEM/FIB/EDS and FIB-TEM. Second, the abilities of halophiles to alter the fuel composition (i.e. increase/decrease the fractions of H2) will be monitored using gas chromatography by growing them under high pressure.
As a result of climate change and the accompanying mandatory shift to renewable energy resources, microorganisms will continue to play an important role in the energy sector, both to their benefit and detriment. Thus, it is important to achieve a certain level of understanding regarding the activities and mechanisms of halophiles prior to large-scaled excursions.
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.
Study of Polyaniline/Silicon Dioxide based Coating on Carbon Steel in Artificial Geothermal Brine
(2021)
By using the available resources in Indonesia, such as silicon dioxide and marine coating base, the PANI/SiO2 modified alkyd coating was able to protect carbon steel in a deaerated artificial geothermal water. The screening of coatings shows that the modification by adding individual pigment was not sufficient to protect carbon steel even during a short-term exposure, indicated by the discoloration after only seven days of exposure. Electrochemical tests indicated that there was no significant change in the Ecorr between the coated and uncoated carbon steel at room temperature. At 150 °C, the coated carbon steel has a lower potential than that of carbon steel, indicating that the coating is protecting carbon steel cathodically or slowing down the corrosion reaction. Finally, a long-term exposure test confirmed that the PANI/SiO2 modified coating successfully protects the carbon steel in the Sibayak artificial geothermal water up to 150 °C for 6 months.
Commercially available carbon steels are suitable for compression and pipelines as long as moisture content and impurities are limited. (water 50 to 100 ppmv, SO2 and NO2 ca. 100 ppmv).
Corrosion rates increase with increasing water content.
(0.2 – 20 mm/a).
Condensation of acids and therefore droplet formation is always possible, even at low water contents.
A low SO2 content within the CO2-stream might be more important than a low water content.
Cr13-steels showed a general susceptibility to shallow pitting and pitting. So, they seem to be not suitable for CCUS applications.
Low alloyed steels showed better corrosion behavior. (predictable uniform corrosion)
For direct contact with saline aquifer fluids only high alloyed steels shall be used.
Die Analyse von Bruchflächen wird in der Schadensanalyse meist auf der Basis von Erfahrungswissen vorgenommen, welches aus vorliegenden Untersuchungen, eigenen Vergleichsversuchen und aus der Literatur stammt. Durch Vergleiche mit bereits vorliegenden Bildern werden qualitativ Bruchmechanismen ermittelt. Grundlage sind zumeist zweidimensionale Bilder aus licht- und elektronenoptischen Verfahren. Quantitative Aussagen beziehen sich bislang beispielsweise auf makroskopische Anteile von Bruchmechanismen oder die Ausmessung von Schwingstreifen. In jüngerer Zeit gibt es vermehrt Ansätze, Computer-Algorithmen einzusetzen, die in der Lage sind, unterschiedlich strukturierte Bruchmerkmale zu finden und zu klassifizieren. Im hier vorgestellten IGF-Vorhaben „iFrakto“, IGF Vorhaben Nr.: 21477 N, werden licht- und elektronen-optisch Topographie-Bilder erzeugt und die gewonnenen 3D-Informationen zusammen mit den klassischen 2D-Bildern ausgewertet. Analytische Algorithmen und Machine Learning werden eingesetzt, um Bruchmerkmale zu analysieren, zu bewerten und mit Informationen aus einer fraktographischen Datenbank zu verknüpfen. Ziel ist die Bereitstellung von Software zur Unterstützung der Fraktographie in der Schadensanalyse. In diesem Beitrag werden erste Ergebnisse des Vorhabens vorgestellt.
Latente Wärmspeicher auf der Basis von NaCl-KCl-MgCl2 Mischungen stellen eine kostengünstige Option für die Energiespeicherung von Prozesswärme dar. Der Beitrag gibt einen Überblick über die materialwissenschaftlichen Herausforderungen im System Salz-Legierung, welche gelöst werden müssen, um diese Speichertechnologie industriell zu etablieren.
In this study, nanoscopic particles of magnesium Fluoride (MgF2) and calcium fluoride (CaF2) also known as nano metal fluorides (NMFs), were evaluated for their potential to improve wood durability. Even though these fluorides are sparingly soluble, their synthesis in the form of nano-sized particles turns them into promising candidates for wood preservation. Their distinct property of low-water solubility is proposed to maintain long-lasting protection of treated wood by reducing the leaching of fluoride. Analytical methods were used to characterize the synthesized NMFs and their distribution in treated wood specimens. Transmission electron microscopy images showed that these fluoride particles are smaller than 10 nm. In nano metal fluoride (NMF) treated specimens, aggregates of these particles are uniformly distributed in the wood matrix as confirmed with scanning electron microscopy images and their corresponding energy-dispersive X-ray spectroscopy maps. The fluoride aggregates form a protective layer around the tracheid walls and block the bordered pits, thus reducing the possible flow path for water absorption into wood. This is reflected in the reduced swelling and increased hydrophobicity of wood treated with NMFs. The biocidal efficacy of NMFs was tested against brown-rot fungi (Coniophora puteanaand Rhodonia placenta), white-rot fungus (Trametes versicolor), and termites (Coptotermes formosanus). The fungal and termite tests were performed in accordance with the EN 113 (1996) and EN 117 (2012) standards, respectively. Prior to fungal tests, the NMF treated wood specimens were leached according to the EN 84 (1997)standard. Compared to untreated specimens, the NMF treated wood specimens have a higher resistance to decay caused by brown-rot fungi, white-rot fungus, and termites. Although all NMF treatments in wood reduce the mass loss caused by fungal decay, only the combined treatment of MgF2 and CaF2 has efficacy against both brown-rot fungi and white-rot fungus. Similarly, wood treated with the combined NMF formulation is the least susceptible to attack by C. formosanus.It is proposed that combining MgF2 and CaF2changes their overall solubility to promote the release of fluoride ions at the optimal concentration needed for biocidal efficacy against fungi and termites. In this thesis, it was proven that even after leaching, sufficient fluoride was present to protect NMF treated wood from fungal decay. This shows that NMFs are robust enough for above ground contact outdoor applications of wood, where permanent wetness cannot be avoided according to Use Class 3.2, as per the EN 335 (2013) standard. Also, they pose a low risk to human health and the environment because they are sparingly soluble. Since NMFs significantly reduce the decay of wood, the CO2 fixed in it will be retained for longer than in unpreserved wood. Overall, the novel results of this study show the potential of NMFs to increase the service life of building materials made from non-durable wood.
The publicly available document encapsulates the first version of the Catalogue of Services of the future EC4Safenano Centre (CoS 2019).
The CoS 2019 is structured in 12 Service Categories and 27 Service Topics, for each of the 12 categories considered. This architecture configures a 12 x 27 matrix that allows ordering the potential EC4Safenano offer in 324 types of services/groups of services.
Each type of service/group of services is described, in a simple and friendly way, by means of a specific service sheet: the EC4Safenano - Service Data Sheet (EC4-SDS). These EC4-SDSs allow structuring and summarizing the information of each service, providing the customer with a concise view of characteristics of the service and also the contact details with the service provider.
The CoS 2019 deploys a map of services consisting of a set of 100 EC4-SDSs, covering 7 of the 12 Service Categories and 17 of the 27 Service Topics.
The harmonization of services is visualized as a future necessary step in EC4Safenano, in order to strengthen the offer and provide added value to customers with a growing offer of harmonized services in future versions of the CoS.
The information contained in this document is structured in 3 main sections, as follows:
• Catalogue structure. This section describes in short the main characteristics of the CoS 2019.
• Catalogue content. This section represents the core part of the document and encapsulates the set of 100 SDSs displaying the offer proposed by the CoS 2019.
• Online Catalogue. This section describes the resources implemented by EC4Safenano to facilitate the on-line consultation of the CoS 2019 by customers and other interested parties.
Thermoelectric generators can be used as energy harvesters for sensor applications. Multilayer thermoelectric generators (ML-TEGs) are a promising alternative to conventional π-type generators due to their high filling factor, high capability of automated production and the texturing potential during the production process. Calcium cobaltite is a promising thermoelectric oxide (p-type) with highly anisotropic properties. The following study shows the development of a textured unileg ML-TEG using ceramic multilayer technology.
Tape-casting and pressure assisted sintering are applied to fabricate textured calcium cobaltite. Compared to conventional sintering, pressure assisted sintering increases the strength by the factor 10. Thermoelectric properties can be tuned either towards maximum power factor or towards maximum figure of merit depending on the pressure level.
As electrical insulation material, a screen-printable glass-ceramic with high resistivity and adapted coefficient of thermal expansion is developed. From various commercial pastes a metallization with low contact resistance is chosen. The unileg ML-TEG is co-fired in one single step. The demonstrators reach 80% of the simulated output power and the power output is highly reproducible between the different demonstrators (99%). These results provide the first proof-of-concept for fabricating co-fired multilayer generators based on textured calcium cobaltite with high power factor, high density, and high strength.
Thermoelectric generators can be used for energy harvesting by directly transforming a temperature gradient into a voltage. Multilayer generators based on low-temperature co-fired ceramics technology (LTCC) are an interesting alternative to conventional π-type generators. They exhibit several advantages like high filling factor, possibility of texturing, co-firing of all materials in one single-step, and reduction of production costs due to the high possible degree of automation. Pressure-assisted sintering enables the theoretical possibility of co-firing two promising oxide thermoelectric materials: Ca3Co4O9 (p-type) and CaMnO3 (n-type). Due to the large difference in sintering temperature (300 K) the process is very challenging.
In this work we show the material development of Ca3Co4O9, CaMnO3, insulation and metallization for multilayer generators co-fired under pressure at 900 °C. The materials are tailored regarding their sintering behavior, electrical performance and coefficients of thermal expansion. Different generator designs (unileg and pn-type) were fabricated and analyzed regarding crack formation, interaction layers and thermoelectric performance. Simulated stresses during cooling in the multilayers are compared with actual crack formation for different sintering conditions. This study shows that a lower pressure level and a lower level of complexity are beneficial for co-firing and performance.
Texturing of calcium cobaltite for thermoelectric applications by pressure assisted sintering
(2021)
Thermoelectric materials can convert waste heat directly into electrical power by using the Seebeck effect. Calcium cobaltite (CCO) is considered as a promising thermoelectric p-type oxide for energy harvesting applications at temperatures above 500 °C. The properties and morphology of single-crystal CCO are strongly anisotropic because of its crystal structure of alternating layers of CoO2 and Ca2CoO3. By aligning the plate-like grains, the anisotropic properties of the grains can be assigned to the poly-crystalline parts.
In this study, the combination of tape casting and pressure-assisted sintering is used to texture and densify large scale components (50 cm²). Thereby, the influence of powder preparation and applied pressure during sintering on texturing and thermoelectric properties is investigated.
The analysis of XRD pole figures revealed that tape casting already leads to highly textured CCO. By pressure variation during sintering, the microstructure of CCO can be tailored either toward maximum power factor as required for energy harvesting or toward maximum figure of merit as required for energy recovery. Low pressure lead to a porous microstructure and maximum figure of merit and higher pressure to full densification and maximum power factor. The electrical and thermal conductivity of CCO seem depending on both texture and sinter density.
The insulation system of high voltage electrical devices like generators and electrical motors has to withstand thermal, electrical, ambient and mechanical influences (TEAM) during operation. Especially the dielectric properties have to satisfy the requirements also under elevated temperatures and extreme environments. To provide this high quality, the conventional fabrication process uses partly manually applied insulation tapes combined with a cost-intensive and under safety concerns at least problematic vacuum pressure impregnation step (VPI). In order to reduce process costs by increasing the degree of automation and avoiding the VPI process, additively manufactured (AM) insulations were studied. This study focuses on the fabrication of ceramic/polymer compounds via AM technique. The AM technology used a rotating screw extrusion print head with air pressure to supply the paste. Plate-like samples with dimensions of 55 mm x 55 mm x1mm thickness were produced. This work focuses on the homogeneously high viscous paste with 12.5 to 50 volume % ratio of filler particles. Three types of mica powders as ceramic filler materials with different particle sizes from micro to mm scale were evaluated. The controlled volume % ratio of particles affects the paste viscosity which enables stacking of paste layers with a viscosity close to clay pastes. The mixed pastes were cured by heating and UV light to increase mechanical properties. A TG/DTA was performed, and electrical properties were investigated. First experiments with respect to the dielectric properties such as volume resistance, permittivity and dielectric strength revealed promising results and the possibility to use AM techniques for the fabrication of high voltage insulations for electrical machines.
Ceramic springs combine attractive properties for applications in machinery, metrology, and sensor technology. They are electrically insulating, non-magnetic, provide a linear stress-strain behavior, and are stable at high temperatures and in corrosive environments. Generally, the precise dimensioning of a ceramic spring with respect to the spring constant is challenging. Different models are described, but many of these calculations do not match the actual spring properties. We demonstrate a reliable approach for the dimensioning and manufacturing of helical compression springs with a rectangular winding cross-section. Based on the German standard DIN 2090, which is referring to metallic springs, the spring constant can be calculated based on shear modulus, diameter, height, widths, and number of windings. Different ceramic springs were produced by milling of sintered hollow cylinders of zirconia, alumina and silicon nitride. The experimental spring constants are in very good agreement with the calculated values. Spring constants of zirconia springs were varied over three orders of magnitude between 0.02 N/mm and 5 N/mm by purposeful adaption of the spring geometry. The combination of dimensioning based on DIN 2090 and precise hard machining offers a reliable technology for the fabrication of tailored ceramic springs for special applications.
The dielectric breakdown strength of ceramics strongly depends on the test conditions. Thus, standardized test procedures and thorough documentation are indispensable. However, during dielectric strength testing the breakdown often occurs near the electrode edge or even outside the specified electrode area. This behavior is similarly observed for printed and cylindrical electrodes. The aim of the presented study was to calculate the electric field strength distribution in a ball-on-plate testing setup for metallized samples and to correlate the field distribution with the observed breakdown locations. Small misalignments in the test setup were also considered in the simulations. Furthermore, the field strength at the breakdown Location should be compared to the experimentally determined dielectric strength. Therefore, Finite Element Models of several test conditions with varying printed electrode areas and sample thicknesses were created and electrostatic calculations of the electric field Distribution were performed. The simulation results were compared to experimental data. Alumina (96 %) was used as test material. The calculations show that the electric field strength maxima match the experimentally observed locations of breakdown. Without any fitting of the model, the maximum calculated field strength is in reasonable agreement with the experimental dielectric strength. The FE analysis is a helpful tool to understand the observations in experimental dielectric strength testing.
Ceramic multilayer technology is an attractive approach for the cost-effective fabrication of thermoelectric generators. Therefore, efforts are being made to co-sinter two promising thermoelectric oxides, namely calcium cobaltite and calcium manganate. In this study, calcium cobaltite, calcium manganate and release tapes were pressure assisted sintered. A major challenge here is the cracking of calcium manganate during cooling. A relationship between the properties of the release tape used in pressure-assisted sintering and the cracking behavior was observed experimentally.
To understand the origin of failure, formed reaction layers in the multilayer were analyzed by EDX and grazing incident XRD. Based on this analysis, bulk samples were prepared, and thermal expansion and Young's modulus and were determined thereon, if they were not known from the literature. The biaxial strength of the thermoelectric oxides was determined by the ball on three ball method.
The thermal stresses during cooling of different multilayer designs were estimated by finite element simulations. The stresses caused by the reaction layers turned out to be negligible. The FEM study indicated further, and a validation experiment proved, that the thickness of the release tape has the main effect on thermal stresses during cooling in single material. For best performance, the design of a thermoelectric multilayer generator needs to consider thermoelectric performance and thermal stresses during cooling.
The underlying cause of mechanical anisotropy in additively manufactured (AM) parts is not yet fully understood and has been attributed to several different factors like microstructural defects, residual stresses, melt pool boundaries, crystallographic and morphological textures. To better understand the main contributing factor to the mechanical anisotropy of AM stainless steel 316L, bulk specimens were fabricated via laser powder bed fusion (LPBF). Tensile specimens were machined from these AM bulk materials for three different inclinations: 0◦, 45◦, and 90◦ relative to the build plate. Dynamic Young’s modulus measurements and tensile tests were used to determine the mechanical anisotropy. Some tensile specimens were also subjected to residual stress measurement via neutron diffraction, porosity determination with X-ray micro-computed tomography (μCT), and texture analysis with electron backscatter diffraction (EBSD). These investigations revealed that the specimens exhibited near full density and the detected defects were spherical. Furthermore, the residual stresses in the loading direction were between −74 ± 24 MPa and 137 ± 20 MPa, and the EBSD measurements showed a preferential ⟨110⟩ orientation parallel to the build direction. A crystal plasticity model was used to analyze the elastic anisotropy and the anisotropic yield behavior of the AM specimens, and it was able to capture and predict the experimental behavior accurately. Overall, it was shown that the mechanical anisotropy of the tested specimens was mainly influenced by the crystallographic texture.
Results of an extended TMF test program on grade P92 steel in the temperature range of 620 °C - 300 °C, comprising in-phase (IP) and out-of-phase (OP) tests, partly performed with symmetric dwells at Tmax/Tmin, are presented. In contrast to previous studies, the low-strain regime is also illuminated, which approaches flexible operation in a power plant with start/stop cycles. At all strain amplitudes, the material performance is characterized by continuous cyclic softening, which is retarded in tests at lower strains but reaches similar magnitudes in the course of testing. In the investigated temperature range, the phase angle does not affect fatigue life in continuous experiments, whereas the IP condition is more detrimental in tests with dwells. Fractographic analyses indicate creep-dominated and fatigue-dominated damage for IP and OP, respectively. Analyses of the (micro)hardness distribution in the tested specimens suggest an enhanced microstructural softening in tests with dwell times for the low- but not for the high-strain regime. To rationalize the obtained fatigue data, the fracture-mechanics-based D_TMF concept, which was developed for TMF life assessment of ductile alloys, was applied. It is found that the D_TMF parameter correlates well with the measured fatigue lives, suggesting that subcritical growth of cracks (with sizes from a few microns to a few millimeters) governs failure in the investigated range of strain amplitudes.
Additive manufacturing (AM) processes allow a high level of freedom in designing and producing components for complex structures. They offer the possibility of a significant reduction of the process chain. However, the large number of process parameters influence the structure and the behavior of AM parts. A thorough understanding of the interdependent mechanisms is necessary for the reliable design and production of safe AM parts.
In this presentation we discuss the online monitoring of metallic AM parts produced by the Laser Powder Bed Fusion (LPBF) process by using optical, thermographic and electromagnetic methods. In a first approach we present the detection of defects generated during the process and discuss how to improve these methods for the optimization of design and production of metallic AM parts.
Undetected and undesired microstructural variations in components produced by laser powder bed fusion are a major challenge, especially for safety-critical components. In this study, an in-depth analysis of the microstructural features of 316L specimens produced by laser powder bed fusion at different levels of volumetric energy density and different levels of inter layer time is reported. The study has been conducted on specimens with an application relevant build height
(>100 mm). Furthermore, the evolution of the intrinsic preheating temperature during the build-up of specimens was monitored using a thermographic in-situ monitoring set-up. By applying recently determined emissivity values of 316L powder layers, real temperatures could be quantified. Heat accumulation led to preheating temperatures of up to about 600 °C. Significant differences in the preheating temperatures were discussed with respect to the individual process parameter combinations, including the build height. A strong effect of the inter layer time on the heat accumulation was observed. A shorter inter layer time resulted in an increase of the preheating temperature by more than a factor of 2 in the upper part of the specimens compared to longer inter layer times. This, in turn, resulted in heterogeneity of the microstructure and differences in material properties within individual specimens. The resulting differences in the microstructure were analyzed using electron back scatter diffraction and scanning electron microscopy. Results from chemical analysis as well as electron back scatter diffraction measurements indicated stable conditions in terms of chemical alloy composition and austenite phase content for the used set of parameter combinations. However, an increase of the average grain size by more than a factor of 2.5 could be revealed within individual specimens. Additionally, differences in feature size of the solidification cellular substructure were examined and a trend of increasing cell sizes was observed. This trend was attributed to differences in solidification rate and thermal gradients induced by differences in scanning velocity and preheating temperature. A change of the thermal history due to intrinsic preheating could be identified as the main cause of this heterogeneity. It was induced by critical combinations of the energy input and differences in heat transfer conditions by variations of the inter layer time. The microstructural variations were directly correlated to differences in hardness.
Laser powder bed fusion (LPBF) is an additive manufacturing process for materials which inherently tends to yield various degrees of metastable hierarchical microstructures, defects and high residual stresses in the as-built condition depending on the process parameters. The understanding of the evolution of these typical features during heat treatment and subsequent thermal and mechanical ageing is crucial for the wider acceptance for safety critical structures. A multi-disciplinary research project at BAM studying the development of the microstructure, defects, residual stresses typical of LPBF 316L and their evolution during thermal and mechanical ageing has led to insights into the stability of these inherent features. This presentation aims to give a broad overview of the project with a few specific cases of investigation. Firstly, the formation of residual stresses, the nature of the initial microstructure, the tensile properties and a modelling approach to understand the anisotropy will be presented. This will be followed by examples of studies of their evolution during heat treatment, long term thermal exposure, and room temperature and high temperature mechanical testing compared to a baseline of conventional wrought variant of the same alloy.
The relationship between fracture toughness and Yttria content in modern zirconia ceramics was revised. For that purpose, we evaluated here 10 modern Y2O3-stabilized zirconia (YSZ) materials currently used in biomedical applications, namely prosthetic and implant dentistry. The most relevant range between 2-5 mol% Y2O3 was addressed by selecting from conventional opaque 3 mol% YSZ up to more translucent compositions (4-5 mol% YSZs). A technical 2YSZ was used to extend the range of our evaluation. The bulk mol% Y2O3 concentration was measured by X-Ray Fluorescence Spectroscopy. Phase quantification by Rietveld refinement considered two tetragonal phases or an additional cubic phase. A first-account of the fracture toughness (KIc) of the pre-sintered blocks is given, which amounted to 0.4 – 0.7 MPa√m. In the fully-densified state, an inverse power-law behavior was obtained between KIc and bulk mol% Y2O3 content, whether using only our measurements or including literature data, challenging some established relationships. A linear relationship between KIc and the fraction of the transformable t-phase was established within the range of 30–70 vol%.
Glass-ceramic composites as insulation material for thermoelectric oxide multilayer generators
(2021)
Thermoelectric generators can be used as energy harvesters for sensor applications.
Adapting the ceramic multilayer technology, their production can be
highly automated. In such multilayer thermoelectric generators, the electrical insulation material, which separates the thermoelectric legs, is crucial for the performance of the device. The insulationmaterial should be adapted to the thermoelectric regarding its averaged coefficient of thermal expansion α and its sintering temperature while maintaining a high resistivity.
In this study, starting from theoretical calculations, a glass-ceramic Composite material adapted for multilayer generators fromcalciummanganate and Calcium cobaltite is developed. The material is optimized towards an α of 11 × 10−6 K−1 (20–500◦C), a sintering temperature of 900◦C, and a high resistivity up to 800◦C.
Calculated and measured α are in good agreement. The chosen glass-ceramic composite with 45 vol.% quartz has a resistivity of 1 × 107 Ωcm and an open porosity of <3%. Sintered multilayer samples from tape-cast thermoelectric oxides and screen-printed insulation show only small reaction layers. It can be concluded that glass-ceramic composites are a well-suited material class for insulation layers as their physical properties can be tuned by varying glass composition or dispersion phases.
In many late-breaking research fields as in photovoltaics, microelectronics, nuclear waste glasses or at least mirror glasses silver diffusion in glasses is relevant to the issues of high-level functionality and recycling. The present study is focused on silver diffusion in innovative, low-melting alkali zinc borate glasses (X2O-ZnO-B2O3, X = Li, Na, K, Rb) potentially usable for silver metallization-pastes in solar cells. The glasses were coated with a thin metallic silver layer and heat treatments in air and nitrogen close to Tg at 470 °C for 2 h were performed. After heat treatment under air and nitrogen atmospheres the coating thickness, measured by a white light interferometer, was about 1.8 µm thick. Silver depth profiles determined by means of secondary neutral mass spectrometry (SNMS) indicate the fastest silver diffusion to a depth of 3.5 µm for Li2O-ZnO-B2O3 (LZB) glass. Nevertheless, the influence of the different alkali ions on the silver diffusion is small. The oxygen availability determines the silver diffusion into the glasses. The oxygen promotes the oxidation of the silver layer enabling Ag+ to diffuse into the glass and to precipitate as Ag0. Both species were detected by x-ray absorption spectroscopy (XAS). The precipitated metallic silver particles in Na2O-ZnO-B2O3 (NZB) glass have a mean size of 5.9 nm ± 1.2 nm diameter, which was determined using transmission electron microscopy (TEM). Phase separation in zinc-rich and zinc-poor phases with a mean diameter of 75 nm ± 20 nm occurred in NZB glass after heat treatment. Ion diffusion of the glasses into the silver layer was suggested by EDX-line scans.
A new patented dynamic mechanical analysis (DMA) is presented, where the tensile, bending- or torsional stiffness of a media can be characterized in-situ during the phase transition from liquid to solid. An epoxy system, e.g. Hexion L285/H287, is filled into an elastomer container, such as a silicone tube. This can be mounted into a conventional DMA and, based on a linear viscoelastic approach, the storage modulus (E’;G’), the loss modulus (E’’;G’’) and the loss angle tan(delta) can be measured at constant temperature as a function of time in order to investigate the liquid to sol-gel to solid transition. With this new method, the stiffness increase as a result of the cure process can be directly measured more precisely than with a rheometer in a shear plate set-up, because using an elastomer container gives a defined cross section for calculating the Young’s modulus.
Sintering, crystallization, and foaming of 44.8SiO2–2.5P2O3–36.5CaO–6.6Na2O–6.6K2O–3.0CaF2 (F3) and 54.6SiO2–1.7P2O3–22.1CaO–6.0Na2O–7.9K2O–7.7MgO (13–93) bioactive glass powders milled in isopropanol and CO2 were studied via heating microscopy, differential thermal analysis, vacuum hot extraction (VHE), Infrared spectroscopy, and time-of-flight secondary ion mass spectrometry. Full densification was reached in any case and followed by significant foaming.
VHE studies show that foaming is driven by carbon gases and carbonates were detected by Infrared spectroscopy to provide the major foaming source. Carbonates could be detected even after heating to 750◦C, which hints on a thermally very stable species or mechanical trapping. Otherwise, dark gray compact colors for milling in isopropanol indicate the presence of residual carbon as well. Its significant contribution to foaming, however, could not be proved and might be
limited by the diffusivity of oxygen needed for carbon oxidation to carbon gas.
Recently, additive manufacturing of ceramics has achieved the maturity to be transferred from scientific laboratories to industrial applications. At the same time, research is progressing to expand the boundaries of this field into the territory of novel materials and applications. This feature issue addresses current progress in all aspects of additive manufacturing of ceramics, from parts design to feedstock selection, from technological development to characterization of printed components.
In typical material oriented research projects numerous types and sources of data need to get connected to form the final outcome. The data-structures have to be described in a manner semantically concise enough so that all participants share the meaning and at the same time flexible enough to allow connecting findings and facts that have not been connected before.
The present contribution describes the approach that is being taken in a public funded research project with two cooperating research institutes. The aim of the data-management solution is to describe and interlink three main entity types: material entities like a test specimen that is under observation, immaterial entities like a fatigue life model and processes that generate and transform the immaterial and material entities.
The shared understanding of what is described by the data is achieved by referring to existing linked data resources. In addition a common thesaurus that is subject to ongoing discussion is used for concepts and terms that need precision beyond publicly available concept descriptions. The data associated with the entities and processes and entities is rather small and well structured. The entities and processes covered by the vocabularies are typical to laboratories performing fatigue testing and microstructure analysis. Through the interlinking of the entities and processes it becomes possible to intuitively understand the knowledge that is accumulating in the database. For example it is easy to trace the history of a creep test specimen starting from the chemical composition that has been analyzed for the heat, continuing with the heat treatment of the material, going into the creep test itself with the associated creep data and finally finding the transmission electron microscopy images that have been taken from the crept sample.
The presented approach is prototypical way to tackle the sustainable management of structured open research data. Open questions remain for example with the management of attributions, the acceptance of an increased effort in data creation and the access control to specific regions of the data. On the other hand the approach sketches what added value can be created, if the community adopts and contributes to the linked data principles.
Laser powder-based directed energy deposition (DED-L) is a technology that offers the possibility for 3D material deposition over hundreds of layers and has thus the potential for application in additive manufacturing (AM). However, to achieve broad industrial application as AM technology, more data and knowledge about the fabricated materials regarding the achieved properties and their relationship to the manufacturing process and the resulting microstructure is still needed. In this work, we present data regarding the low-cycle fatigue (LCF) behavior of Ti-6Al-4V. The material was fabricated using an optimized DED-L process. It features a low defect population and excellent tensile properties. To assess its LCF behavior two conventionally manufactured variants of the same alloy featuring different microstructures were additionally tested. The strain-controlled LCF tests were carried out in fully reversed mode with 0.3 % to 1.0 % axial strain amplitude from room temperature up to 400°C. The LCF behavior and failure mechanisms are described. For characterization, optical microscopy (OM), scanning electron microscopy (SEM), and micro-computed tomography (µCT) were used. The low defect population allows for a better understanding of the intrinsic material’s properties and enables a fairer comparison against the conventional variants. The fatigue lifetimes of the DED-L material are nearly independent of the test temperature. At elevated test temperatures, they are similar or higher than the lifetimes of the conventional counterparts. At room temperature, they are only surpassed by the lifetimes of one of them. The principal failure mechanism involves multiple crack initiation sites.
In this study, the influence of aging and mean stress on fatigue of the aluminium-alloy EN AW-2618A is investigated. Therefore axial fatigue tests are carried out on smooth specimens. The experiments show that the fatigue life decreases with increasing mean stress. Furthermore, the tests with the overaged specimens demonstrate that the number of cycles to failure is decreasing with increasing aging time.