5 Werkstofftechnik
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Dislocations are the carriers of plastic deformation. As such, their characterization offers important information on the properties they affect. In this contribution, a new tool is presented, which is incorporated in Amira ZIB Edition and allows for three-dimensional (3D) imaging and quantification of dislocations substructures from thick regions an electron-transparent specimen. In the tool, the dislocation segments are traced on diffraction contrast images that are obtained in the transmission electron microscope (TEM). The uncertainties related to the experimental setup and to the proposed method are discussed on the base of a tilt series.
Ni-base superalloy single crystals have been used in turbine blades for hot sections of gas turbines for over four decades. In order to increase the efficiency of the turbines, a continuous increase in the inlet temperature of combustion gases into the turbine has driven the design of turbine blades to complicated shapes and the presence of a complex pattern of cooling channels. These three-dimensional shapes, together with the inhomogeneous distribution of stresses along the blade, induce an also complicated triaxial stress state, which does not compare to uniaxial tests that are performed to characterize high temperature properties such as creep. A round notch on a test piece represents a simple configuration that generates a quasi-isostatic stress state across the notch. In the present contribution, the effect of a sharp round notch on the microstructural micromechanisms within the notched region cylindrical bars, loaded along [001] at 1020 °C and 160 MPa net stress, is studied. To this end, a series of interrupted creep tests is conducted on plain and notched bars and the microstructure is compared. Results are discussed in terms of degree microstructural coarsening, and dislocation activity. The effect of notch generation via grinding is also discussed in these terms. The presence of carbides evolving in from residual carbon is also shown and discussed. .Funding by the German Research Association (DFG) [grant number AG 191/1] is acknowledge
Im Rahmen der Erstellung einer fraktographischen online-Datenbank an der BAM wurden systematisch Schwingversuche an einem Sinterstahl vorgenommen, dessen Sinterdichte variiert wurde. Die erzeugten Bruchflächen wurden analysiert, mit der Literatur verglichen und Datensätze in die Datenbank eingefügt.
Im Rahmen der DGM/DVM AG Fraktographie wird an der BAM eine fraktographische online-Datenbank aufgebaut. Während von metallischen Werkstoffen viele Beispiele vorliegen, die auch gut verstanden sind, sind die Brüche von Kunststoffen bislang weniger prominent vertreten. Eine teils ungeklärte Frage ist, in welcher Form sich an Kunststoffen klassische Schwingbrüche nachweisen lassen, wie sie von metallischen Werkstoffen bekannt sind. Der Vortrag zeigt einige Beispiele im Detail und stellt diese zur Diskussion.
Thermoelectric materials can convert waste heat directly into electrical power by using the Seebeck effect. Calcium cobaltite Ca3Co4O9 is a promising p-type oxide thermoelectric material for applications between 600 °C and 900 °C in air. The properties and morphology of Ca3Co4O9 are strongly anisotropic because of its crystal structure of alternating layers of CoO2 and Ca2CoO3. By aligning the plate-like grains, the anisotropic properties can be assigned to the component. Pressure-assisted sintering (PAS), as known from large-scale production of low temperature co-fired ceramics, was used to sinter multilayers of Ca3Co4O9 green tape at 900 °C with different pressures and dwell times. In-situ shrinkage measurements, microstructural investigations and electric measurements were performed. Pressure-less sintered multilayers have a 2.5 times higher electrical conductivity at room temperature than dry pressed test bars with randomly oriented particles. The combination of tape casting and PAS induces a pronounced alignment of the anisotropic grains. Relative density increases from 57 % after free sintering for 24 h to 94 % after 2 h of PAS with 10 MPa axial load. By applying a uniaxial pressure of 10 MPa during sintering, the electrical conductivity (at 25°C) improves by a factor of 15 compared to test bars with randomly oriented particles. The high temperature thermoelectric properties show the same dependencies. The smaller the applied axial load, the lower the relative densities, and the lower the electrical conductivity. Longer dwell times may increase the density and the electrical conductivity significantly if the microstructure is less densified as in the case of a small axial load like 2 MPa. At higher applied pressures the dwell time has no significant influence on the thermoelectric properties. This study shows that PAS is a proper technique to produce dense Ca3Co4O9 panels with good thermoelectric properties similar to hot-pressed tablets, even in large-scale production.
Thermoelektrische Materialien können durch die Nutzung des Seebeckeffektes einen Temperaturunterschied direkt in eine Spannung umwandeln. Calciumcobaltit (p-typ) und Calciummanagant (n-typ) sind 2 der vielversprechendsten oxidischen thermoelektrischen Materialien. Für die Entwicklung von kostengünstigen Multilayergeneratoren ist das Co-sintern dieser beiden Materialien notwendig und deshalb eine Anpassung der Sintertemperatur nötig. Calciummangant wird herkömmlicherweise zwischen 1200°C und 1350°C gesintert. Calciumcobaltit erfährt einen ungewünschte Phasenumwandlung bei 926°C, es kann allerding bei 900°C unter 7.5MPa zu 95% dicht gesintert werden. Demzufolge, ist eine Co-sintertemperatur von 900°C anzustreben. Aus diesem Grund wurden mehrere Strategien zur Absenkung der Sintertemperatur von Calciummanaganat untersucht. Zum einen die Zugabe niedrigschmelzender Additive, zum anderen die Zugabe von Additiven, die eine eutektische Schmelze bilden. Es konnte gezeigt werden, dass für Calciummanganat die Verwendung von eutektischen Schmelzen besser geeignet ist als die Verwendung von niedrigschmelzenden Additiven um die Sintertemperatur zu senken.“
Lowering the sintering temperature of calcium manganate CaMnO3 for thermoelectric applications
(2018)
Thermoelectric materials can convert waste heat directly into electrical power by utilizing the Seebeck effect. Calcium cobaltite (p-type) and calcium manganate (n-type) are two of the most promising oxide thermoelectric materials. The development of cost-effective multilayer thermoelectric generators requires the co-firing of these materials and therefore the adjustment of sintering temperatures. Calcium manganate is conventionally sintered between 1200 °C and 1350 °C. Calcium cobaltite exhibits an undesired phase transition at 926 °C but can be sintered to high relative density of 95 % at 900 °C under axial pressure of 7.5 MPa. Hence, co-firing at 900 °C would be favourable. Therefore, strategies for lowering the sintering temperature of calcium manganate have been investigated. Basically, two approaches are common: i) addition of low melting additives like Bi2O3-ZnO-B2O3-SiO2 (BBSZ) glass or Bi2O3, and ii) addition of additives that form low-melting eutectics with the base material, for example CuO. In this study, several low melting additives including BBSZ glass and Bi2O3, as well as CuO were tested regarding their effect on calcium manganate densification. Bi2O3 did not improve the densification, whereas BBSZ glass led to 10 % higher relative density at 1200 °C. An addition of 4 wt% CuO decreases the temperature of maximum sinter rate from above 1200 °C to 1040 °C. By reducing the particle size of the raw materials from 2 μm to 0.7 μm the maximum sinter rate could be further shifted 20 K towards lower temperatures and the sinter begin decreased from 920 °C to 740 °C. It is shown that eutectic phase formation is more effective in lowering sintering temperature and accelerating densification than low-melting additives.
Calciumcobaltit und Calciummanganat gehören zu den vielversprechendsten thermoelektrischen Oxiden im Temperaturbereich zwischen 600 °C und 800 °C an Luft. Mittels thermoelektrischer Generatoren kann ein Temperaturgradient direkt in elektrische Leistung umgewandelt werden. Für die kostengünstige Pulverherstellung von Funktionsmaterialien wird im industriellen Maßstab meist die Festphasenreaktion (bzw. Kalzinierung) verwendet. Da es sich dabei um einen Hochtemperaturprozess handelt, ist diese Kalzinierung sehr energieintensiv. In der Literatur werden sehr unterschiedliche Prozessbedingungen zur Pulversynthese thermoelektrischer Oxide genutzt. Soweit dem Autor bekannt, ist keine systematische Untersuchung des Einflusses der Pulversynthesebedingungen auf die thermoelektrischen Eigenschaften publiziert.
Deshalb wurde eine systematische Untersuchung des Einflusses der Pulversynthesebedingungen (Temperatur, Haltezeit, Partikelgröße, Wiederholungen) auf die thermoelektrischen Eigenschaften von Calciumcobaltit und Calciummanganat durchgeführt.
Es konnte gezeigt werden, dass sich ein höherer Energieeintrag während der Kalzinierung negativ auf die thermoelektrischen Eigenschaften auswirkt.
Es wird eine neu entwickelte Methode zur Thermographiebasierten Rissmessung vorgestellt. Darüber hinaus wird eine numerische Vorarbeit präsentiert, die zeigt, dass anhand der gemeisamen Auswertung der Versuchsdaten aus unterschiedlicher Sensorik die Möglichkeit besteht, die unter Ermüdungsbelastung in Bohrlochproben auftretenden Risse in Geometriekategorien zu unterteilen.
A constitutive model for the mechanical behaviour of single crystal Ni-base superalloys under high temperature conditions has been developed in the framework of a Cooretec project in cooperation with Siemens AG, MTU Aero Engines AG and University Bayreuth. In addition to the conventional material properties e.g. elastic constants, the model requires the parameters of the initial microstructure as an input. Thus, the γ’-precipitate size and the channel width of the γ-matrix were obtained from SEM micrographs. The model uses the slip system theory and describes the movement, multiplication and annihilation of dislocations in the channels. Furthermore, the cutting of precipitates is another mechanism contributing to the plastic flow. The evolution of the morphology due to rafting and its effects on the deformation have been implemented according to. The kinematic hardening is introduced as a stress tensor to realistically represent the strain hardening of arbitrary oriented single crystals.
The mechanical behaviour of single crystal specimens has been experimentally investigated in tension tests at different strain rates and in creep tests under various loads. The constitutive model has been calibrated based on the experimental data for temperatures of 950°C and 850°C and the [001] and [111] crystallographic orientations.
Finally, a micromechanical model was created to simulate the creep response of additive manufactured polycrystalline structures. An EBSD image is taken to obtain the grain geometry and their respective orientation. The grain boundaries are discretised using cohesive elements, whereas the single crystal model was applied to each grain in the representative volume. The polycrystal model is generated using Dream3D, NetGen and other software previously developed at the BAM.
The first documentation of fuel biodeterioration dates back to the late 19th century. However, extensive studies concerning the microbial fuel contamination started in 1980’s. Polymeric fuel storage tanks containing diesel and biodiesel provide environmental conditions for microbial growth. Several studies demonstrated that bacteria, which were found in contaminated fuel systems, can use fuels as macronutrient; but such bacteria can also cause microbiologically influenced corrosion and fouling.
The aim of this study is to investigate the initial attachment behavior of bacteria, isolated from a diesel contamination, on neat and photooxidized high-density polyethylene (PE-HD). Two common PE-HD’s, less- and biodiesel-stabilized, were radiated to UV light representing a tank exposed to sunlight. The effect of photooxidiation on PE-HD’s surface were characterized chemically by Fourier-transform infrared spectroscopy (FTIR). The attached bacteria Pseudomonas aeruginosa and Bacillus subtilis on the polymer surface were evaluated by fluorescence microscopy and colony-forming unit tests (CFU).
PE-HD as a polymeric fuel storage tank material: Photooxidation, fuel sorption and long-term storage
(2018)
High-density polyethylene (PE-HD) is a commodity thermoplastic polymer which is typically used for packing of dangerous goods. Its good resistance against photooxidation, fuels, chemicals and other environmental factors in addition to low production costs makes PE-HD attractive for fuel storage applications. Typical engine fuels stored in polymer tanks are petrol, diesel and biodiesel that receives increasing attention as proper alternative to fossil fuels. One of the major problems with biodiesel is its susceptibility to oxidize due to its chemical composition of unsaturated fatty acids which also can cause polymer degradation.
The aim of this study is to investigate the influence of different environmental factors, UV radiation and commonly stored fuels, on the mechanical, physical and chemical properties of two types of PE-HD polymers (stabilized and non-stabilized). The influence on the mechanical properties was tested by Charpy and tensile tests, chemical and physical properties were evaluated by Fourier-transform infrared spectroscopy (FTIR) and by dynamical mechanical analysis (DMA) tests. Samples were characterized after varying exposure time of UV radiation and after fully and partially immersion in biodiesel. In addition, similar experiments were conducted using diesel for comparison.
Virtual-lab-based determination of a macroscopic yield function for additively manufactured parts
(2018)
This work presents a method for the yield function determination of additively manufactured parts of S316L steel. A crystal plasticity model is calibrated with test results and used afterwards to perform so-called virtual experiments, that account for the specific process-related microstructure including crystallographic and morphological textures. These simulations are undertaken on a representative volume element (RVE), that is generated from EBSD/CT-Scans on in-house additively manufactured specimen, considering grain structure and crystal orientations. The results of the virtual experiments are used to determine an anisotropic Barlat yield function, that can be used in a macroscopical continuum-sense afterwards. This scale-bridging approach enables the calculation of large-scale parts, that would be numerically too expensive to be simulated by a crystal plasticity model.
The creep behavior of single-crystals of the nickel-base superalloy CMSX-4 was investigated at 1288°C, which is the temperature of the hot isostatic pressing (HIP) treatment applied to this superalloy in the industry. It was found that at this super-solvus temperature, where no Gamma’-strengthening occurs, the superalloy is very soft and rapidly deforms under stresses between 4 and 16 MPa. The creep resistance was found to be very anisotropic, e.g. the creep rate of [001] crystals was about 11 times higher than that of a [111] crystal. The specimens of different orientations also showed a very different necking behavior. The reduction of the cross-section area psi of [001] crystals reached nearly 100%, while for a [111] crystal psi=62%. The EBSD analysis of deformed specimens showed that despite such a large local strain the [001] crystals didn’t not recrystallize, while a less deformed [111] crystal totally recrystallized within the necking zone. From the shape of deformed specimens and TEM investigations it was concluded that the main strain contribution resulted from <011> {111} octahedral slip.