5 Werkstofftechnik
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Performing mechanical tests at high temperatures is a nontrivial issue: Compared to room temperature testing, additional phenomena like time-dependent Deformation processes and oxidation effects raise the complexity of the material’s response, while more sophisticated test setups and additional control parameters increase the number of potential sources of error. To a large extent, these complications can be overcome by carefully following all recommendations given in the respective high temperature testing standards, but more comprehensive background information helps to identify points of specific importance in particular test campaigns. In this chapter, an overview is given on general high temperature testing issues like the appropriate choice of experimental equipment and key aspects of temperature measurement. In subsequent sections, the major static and dynamic high temperature test methods are reviewed and their Special features, as compared to testing at room temperature, are highlighted based on example data sets. Influences of specimen size and environmental effects are shortly outlined in a concluding section. In the whole chapter, a focus is set on testing of “classical” metallic high temperature materials, but many considerations are equally valid for testing of intermetallics, composites, and high temperature ceramics.
The possibility to produce dense monolithic ceramic parts with additive manufacturing is at the moment restricted to small parts with low wall thickness. Up to now, the additive manufacturing of voluminous ceramic parts is realized by powder bed based processes which, however, generate parts with residual porosity. Via infiltration these parts can be processed to dense parts like for example SiC but this is not possible for all ceramics like for example Si3N4. There is a lack of methods for the additive manufacturing of dense voluminous parts for most ceramics.
We have developed a new additive manufacturing technology, the Laser Induced Slip casting (LIS), based on the layerwise deposition of slurries and their local drying by laser radiation. Laser Induced Slip casting generates ceramic green bodies which can be sintered to dense ceramic components like traditional formed ceramic powder compacts. We will introduce the LIS technology, green bodies and sintered parts will be shown and their microstructure and mechanical properties will be discussed.
Today, more than 12% of the primary energy is lost in the form of waste heat. Thermoelectric generators (TEGs) can convert waste heat directly into electrical power by utilizing the Seebeck effect. The performance of such a generator is defined by a dimensionless figure of merit ZT of the thermoelectric pairs and the resistance R of the metallic contacts between these pairs. The figure of merit of thermoelectric oxides is considerably smaller compared to semiconductors. Still, thermoelectric oxides like calcium cobaltite (Ca3Co4O9) are attractive for applications at elevated temperatures in air. In contrast to the established π-type architecture of common TEGs, tape casting and multilayer technology may be applied for cost-effective manufacturing of oxide TEGs. Promising demonstrations of multilayer TEGs have been published in the last years. Still, the development of reliable and scalable manufacturing processes and proper material combinations is necessary. The aim of our project is to evaluate the feasibility of low temperature co-fired ceramics (LTCC) technology for a practical manufacturing of oxide multilayer TEGs of Ca3Co4O9 (p-type) and calcium manganate (CaMnO3, n-type). Ca3Co4O9 exhibits an undesired phase decomposition at 926 °C. Because of that, the application of sintering strategies and interconnect concepts well known from LTCC technology is a promising approach. We present results of pressure-assisted sintering of Ca3Co4O9 multilayer at 900 °C and axial pressures of up to 7.5 MPa. Ca3Co4O9 was produced by solid state reaction of CaCO3 and cobalt(II,III)oxide at 900 °C. Green tapes were prepared by a doctor-blade process, manually stacked and laminated by uniaxial thermocompression. Sintering was conducted in a LTCC sintering press between SiC setter plates. The thickness shrinkage was recorded by an in-situ technique. After sintering under 7.5 MPa, the microstructure of the single phase material shows a high density of 95 % and an advantageous alignment of the platelet grains. This results in good electrical conductivity and a comparatively high ZT of 0.018 at room temperature. However, the lowering of CaMnO3 sintering temperature from above 1200 °C to below 920 °C remains a challenge. To select a proper metal paste for interconnections of an oxide TEG, several pastes have been investigated regarding contact resistance of internal and external (soldered) connections in a preliminary study. Commercial pastes containing Ag, Au, Au/Pt, Ag/Pd, and Ag/Pd/Bi were manually applied and post-fired on sintered test bars of Ca3Co4O9 and CaMnO3 at 900 °C for 2 h. All tested pastes formed mechanically stable metallization after firing. For resistance measurement, 4-wire method and a custom-made probe head were used. The contacts on Ca3Co4O9 exhibit significantly (2-sample t-test, α = 5%) higher resistance compared to contacts on CaMnO3. Pure silver paste exhibits the lowest resistance for internal contacts on both materials, lower than 5 mΩ on CaMnO3. Ag/Pd/Bi paste resulted in conspicuously high variance of resistance. EDX analyses clarified an enrichment of Bi in the thermoelectric material near the interface and thereby the formation of an oxide layer with probably high electrical resistance. The thickness of that layer varies with the thickness of metallization. In conclusion, the use of Bi containing pastes is not advisable. Pure Ag paste shows the best results regarding resistance and solderability.
Helical springs with a rectangular cross-section have been machined from sintered and grinded hollow cylinders with high geometrical precision and good reproducibility. Such springs made from tetragonal zirconia polycrystal (TZP) ceramic show excellent edge quality because of high fracture toughness and bending strength of the starting material. Hence, springs with desired geometric dimension and tailored spring constant can be manufactured for highly demanding applications at high temperatures and in harsh environments.
Prior to any practical use, application limits of springs under mechanical and thermal load have to be analyzed. Therefore, different displacement experiments were carried out on the helical TZP springs.
- Dynamic displacement tests at various temperatures from -15°C to +60°C using a piezo actor to load/unload springs with frequencies between 1 and 40 Hz: Springs remained undamaged and the spring constants were not altered, even after more than one million cycles of compression loading.
- Long-time displacement measurements under static tensile loading at room temperature with a high-precision interferometer test facility: Significant spring elongation under constant strain was surprisingly proved over a period of many hours already at room temperature.
- Creeping experiments for 48 h under static compression load at different temperatures up to 1000 °C: After cooling down and load removing no permanent length reduction of springs was observed for test temperatures up to 700 °C. However, reshaping of TZP springs by plastic deformation is possible at higher temperatures and opens up additional possibilities for spring design and manufacturing.
In diesem Forschungsvorhaben wurde ein Verfahren entwickelt, um die Genauigkeit der Lebensdauerbewertung für Abgasturbolader (ATL)-Verdichterräder aus der ausscheidungs-härtbaren Aluminiumlegierung EN AW-2618A zu verbessern. Dies umfasst insbesondere die Berücksichtigung der Werkstoffalterung, mit der beim Einsatz dieser Bauteile unter entsprechender Betriebsbeanspruchung (Temperatur, Zeit, Spannung) gerechnet werden muss. Zunächst wurde eine solide experimentelle Datenbasis für den untersuchten Werkstoff geschaffen. Dies umfasste sowohl eine mechanische als auch eine mikrostrukturelle Charakterisierung des Ausgangszustands (T61) sowie von ausgelagerten Zuständen bis zu 25.000 h bei betriebsrelevanten Temperaturen (160 °C, 180 °C, 190 °C). Bei den Untersuchungen zur Mikrostruktur wurde der Fokus auf die Entwicklung der Radien der stäbchen-förmigen aushärtenden Phase gelegt, die während der Alterung vergröbern. Der Zusammenhang zwischen Auslagerungstemperatur, -zeit und ggfs. mechanischer Belastung wurde erstmals in diesem Umfang quantifiziert und entsprechende Gesetzmäßigkeiten zur Beschreibung der Vergröberung ermittelt. Vergleichend dazu wurde der Einfluss der Alterung auf die Härte, die Festigkeit, das Kriechverhalten und die Ermüdungslebensdauer (LCF, TMF) bestimmt, so dass eine Korrelation zur Mikrostruktur vorliegt.
Die Ergebnisse der Kriechversuche wurden zur Kalibrierung eines modifizierten Sinus-hyperbolicus-Kriechmodells verwendet. Ein zeit- und temperaturabhängiges Verformungsmodell nach Chaboche, welches die wesentlichen Phänomene der Hochtemperaturverformung und der Wechselplastizität beschreibt, wurde erweitert und berücksichtigt nun die Werkstoffalterung, indem die Festigkeit nicht nur als Funktion der Temperatur, sondern auch des Alterungszustands (d. h. des mittleren Radius der Ausscheidungen) dargestellt wird. Für die Erweiterung des Modells zur Bewertung der Ermüdungslebensdauer wurde analog verfahren. Die berechnete Lebensdauer der im Verlauf des Vorhabens durchgeführten LCF- und TMF-Versuche stimmt gut mit den experimentellen Ergebnissen überein. Lediglich ein LCF-Versuch mit einer Haltezeit von 900 s im Zug weicht deutlich vom Mittelwert ab und zeigt die Grenzen des zeitunabhängigen Schädigungsmodells auf. Versuche mit kürzeren Haltezeiten bis zu 60 s liegen im Streuband, ebenso die verschiedenen Alterungszustände. Eine Schädigungsakkumulation unter Berücksichtigung der fortschreitenden Alterung über der Lebensdauer wurde entwickelt und implementiert. Neben der Berücksichtigung der Alterung in der Verformungs- und Lebensdaueranalyse besteht auch die Möglichkeit, komplexe Belastungszyklen in einem Postprozessing zu bewerten, indem Rainflow-Klassierungen typischer komplexer Belastungszyklen vorgenommen werden.
Die Methodik und die Modelle wurden in die Finite-Elemente-Programme Abaqus und Ansys implementiert und stehen für die rechnerische Bewertung von Bauteilen zur Verfügung.
Cyclic fatigue behavior of glass fiber reinforced epoxy resin at ambient and elevated temperatures
(2018)
The fatigue behavior of ±45° glass fiber reinforced epoxy resin under cyclic mechanical and constant thermal loading is investigated in this study. Tests at three different temperature levels in the range 296 K to 343 K have been performed in order to create S-N curves for each temperature level. The specimen damage is measured in-situ using optical grayscale analysis. The characteristic damage state (CDS) is evaluated for each specimen. It is shown that the point of CDS is suitable as a failure criterion to compare the resulting S-N curves. With micromechanical formulations, the temperature-dependent matrix effort is calculated for each stress-temperature level. In terms of matrix effort, the longest fatigue life is reached at high temperatures, while, in terms of stress, the lowest fatigue life is reached at the highest temperatures.