5 Werkstofftechnik
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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.
Powder based Additive Manufacturing (AM) processes are widely used for metallic and polymeric materials, but rarely commercially used for ceramic materials, especially for technical ceramics. This seemingly contradicting observation is explained by the fact that in powder based AM, a dry flowable powder needs to be used. Technical ceramics powders are in fact typically very fine and poorly flowable, which makes them not suitable for AM. The layerwise slurry deposition (LSD) is an innovative process for the deposition of powder layers with a high packing density for powder based AM. In the LSD process, a ceramic slurry is deposited to form thin powder layers, rather than using a dry powder This allows the use of fine powders and achieves high packing density (55-60%) in the layers after drying. When coupled with a printing head or with a laser source, the LSD enables novel AM technologies which are similar to *Denotes Presenter 42nd International Conference & Exposition on Advanced Ceramics & Composites 127 Abstracts the 3D printing or selective laser sintering, but taking advantage of having a highly dense powder bed. The LSD -3D printing, in particular, offers the potential of producing large (> 100 mm) and high quality ceramic parts, with microstructure and properties similar to traditional processing. This presentation will give an overview of the milestones in the development of this technology, with focus on the latest results applied both to silicate and to technical ceramics.
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.“
Die Bundesanstalt für Materialforschung und -prüfung (BAM) ist eine Ressortforschungseinrichtung, die zum Schutz von Mensch, Umwelt und Sachgüter, forscht, prüft und berät. Im Fokus aller Tätigkeiten in der Materialwissenschaft, der Werkstofftechnik und der Chemie steht dabei die technische Sicherheit von Produkten und Prozessen. Dazu werden Substanzen, Werkstoffe, Bauteile, Komponenten und Anlagen sowie natürliche und technische Systeme erforscht und auf sicheren Umgang oder Betrieb geprüft und bewertet. Schwerpunkt des Vortrages sind multimodale Polymeranalytik, nanoskalige Sensormaterialien und die Charakterisierung von technischen Eigenschaften von Polymeren sowie ihre Alterung und Umweltrelevanz.
Dry pressing of ceramic materials requires homogeneously soft granules with good flowability to allow rapid die filling and to avoid packing defects. Spray-drying granulation appears to be the best method for obtaining granules with high flowability in industrial scale. But, strength reducing internal microstructural defects caused by spray-dried granules with hollow and hard shells are often observed using nano and/or multi-component starting powders.
Using the example of a ZTA composite, the potential of slurry optimization, ultrasound atomization and infrared drying for better granule properties and compaction behavior were investigated. Starting granules produced in a conventional spray dryer (Niro, Denmark) with a two fluid nozzle showed typical defects like large central pores and dimples.
The early step of slurry preparation already possesses an essential optimization possibility in the form of stability adjustments. Granule compaction was clearly improved upon a specific reduction in slurry stability. The second optimization opportunity to improve the granule quality was the atomization step. Implementation of an ultrasound atomizing unit into the conventional spray dryer positively affected granule size distribution and therefor flowability and as well granule yield. But, a combination of both process optimizations delivered the best sinter bodies with highest density and strength due to further reduction in maximum size and fraction of pores.
As last step of a spray drying process, the drying is the focus of further investigations. A current setup implying a spray dryer prototype utilizes stacked infrared heater in a countercurrent setup delivering a further increase in granule yield and enduring spraying process stability.
Dielectric strength testing of ceramics is simple and yet challenging. The execution of a breakthrough voltage measurement of a given sample is fast and straightforward. ASTM D149 describes the standardized procedure. But, there are versatile effects of test conditions and sample properties that affect the result of such a measurement. As one example, ASTM D149 allows different sizes of test electrodes and does not unambiguously prescribe the condition of the electrodes. Thus, different electrode configurations are used in the field. We conducted several test series on alumina samples to comprehensively quantify the effect of test conditions and sample properties on dielectric strength results. In our study, testing of alumina substrates using different electrode configurations resulted in differences of mean values of up to 20%. Further test series on alumina focused on the effect of voltage ramp rate. The results are complemented by calculations of failure probability at different voltage levels and corresponding withstand voltage tests. We conclude that a communication and comparison of single dielectric strength values is insufficient and may be misleading. A meaningful comparison of dielectric strength studies from different sources requires a thorough consideration of test conditions.