TY - RPRT A1 - Rabe, Torsten A1 - Schulz, Bärbel A1 - Salehi, M. T1 - Alterungsbeständige keramische Federsensoren durch nanostrukturierte Werkstoffe, Präzisionsbearbeitung und hochdielektrische Nanosuspensionen N2 - Das Ziel des Gesamtvorhabens bestand darin, einen neuartigen kapazitiven Sensortyp zur hochauflösenden Bestimmung von Masse- und Gravitationskraftänderungen zu entwickeln. Bisherige Technologien nutzten dafür Federn oder Biegebalken aus gehärteten metallischen Werkstoffen, deren Alterungsverhalten die Präzision der Kräftemessung begrenzen. Grundprinzip des neuen Sensortyps ist es, eine auf die keramische Feder einwirkenden Änderung der Gewichts- oder Gravitationskraft durch eine Erfassung der Kapazitätsänderung am Sensor zu bestimmen. Dazu muss die durch Stauchung oder Dehnung der Feder entstehende Kapazitätsänderung mit hoher Auflösung reproduzierbar gemessen werden. Neben einem geeigneten Sensordesign waren Lösungen für Messsignalerfassung und -auswertung (Elektronik/Software) und die Systemintegration zu entwickeln. Die wichtigsten im Rahmen des BAM-Teilvorhabens erzielten Ergebnisse sind: - Ausgehend von kommerziellen High-end Keramikpulvern wurden durch Optimierung der keramischen Technologie nahezu porenfreie Al2O3, ZrO2 und Si3N4-Werkstoffe hergestellt und bezüglich Gefüge und Phasenbestand sowie mechanischen, thermischen und elektrischen Eigenschaften bewertet. Insbesondere die defektfreie Herstellung von nanostrukturierten Werkstoffen erforderte umfangreiche Variationen der Prozessparameter. Geeignete Werkstoffvarianten wurden für die Federherstellung ausgewählt. - Gemeinsam mit den Projektpartnern wurden Layoutvarianten für Schraubendruckfedern mit rechteckigem Windungsquerschnitt und für die Federeinbindung in das Sensorsystem erarbeitet. - 4 Federvarianten wurden an der BAM durch Hartbearbeitung von gesinterten Hohlzylindern umgesetzt. Fertigungstoleranzen von < ±10 µm für Windungsbreite, Windungshöhe und Windungsabstand und dünnfilm-kompatible innere Windungsflächen (Ra < 0,2 µm) wurden erreicht. Al2O3- und ZrO2-Federn können rissfrei und mit sehr guter Kantenqualität gefertigt werden, bei Si3N4-Federn konnten Kantenschädigungen nicht vollständig verhindert werden. - Mit der entwickelten Herstellungstechnologie können sowohl „harte“ als auch sehr „weiche“ Federn produziert werden. Federkonstanten zwischen 0,02 N/mm und 10 N/mm wurden realisiert. Die Reproduzierbarkeit der Federfertigung ist gegeben, innerhalb einer Charge unterschieden sich die Federkonstanten der gefertigten Federn nur um etwa +/- 1%. - An einem speziell entwickelten Versuchsstand wurden die Federn unter zyklischer Druckbelastung im Temperaturbereich von -20 bis +80 °C untersucht. An den Al2O3- und ZrO2-Federn wurden keine Schädigungen beobachtet, die Federkonstante wird durch die zyklische Langzeitbelastung nicht verändert. - Die Eignung der keramischen Federn für den Applikationsfall wurde mit zahlreichen Spannungs-Dehnungs-Experimenten, teilweise an speziell aufgebauten Versuchsapparaturen, untersucht. An Al2O3- und Si3N4-Federn wurde – wie erwartet – gefunden, dass die Federkonstante unabhängig von der Belastungsgeschwindigkeit ist und unter konstanter Last auch über lange Zeiträume keine Verformung auftritt. Überraschenderweise zeigten ZrO2 (TZP)-Federn ein zeitabhängiges Verhalten unter Last. Dieses ist besonders stark bei Y-stabilisierten Werkstoffvarianten ausgebildet, wurde aber mit Hochpräzisionsmessungen auch bei Ce-stabilsierten Werkstoffen nachgewiesen. Die Deformation ist reversibel, eine vollständige Relaxation wird erst nach Tagen erreicht. Aufgrund der zeitabhängigen Verformung können ZrO2 (TZP)-Federn, trotz ihrer hervorragenden Festigkeit und Bruchzähigkeit, nicht für die konzipierten Sensorfedern eingesetzt werden. - Das durch die Fa. Siegert TFT entwickelte Metallisierungs-Schichtsystem, bestehend aus aufgesputterten Ti-, Pt- und Au-Schichten verstärkt durch eine galvanisch aufgebrachte Au-Schicht, wurde an der BAM umfassend bewertet. Die Schichten sind untereinander und mit der Keramik weitgehend defektfrei verbunden, die lokale Schichtdicke schwankt jedoch bedingt durch Abschattungseffekte während der Beschichtungsvorgang. Es wurden Schichtwiderstände zwischen 50 und 90 Ohm und damit die Zielvorgabe des Projektes (< 100 Ohm) erreicht. In statischen und dynamischen Belastungstests wurden keine Veränderungen der Leitungswiderstände festgestellt. - Zur Erhöhung der Kapazität des Kondensators kann der Raum zwischen den Federwindungen statt mit Luft mit einer Flüssigkeit mit hoher Dielektrizitätskonstante gefüllt werden. Als geeignete Flüssigkeit wurde Propylencarbonat mit einer Dielektrizitätskonstante von 65, einem hohen Siedepunkt und einer geringen Viskosität identifiziert. Um eine noch höhere Dielektrizitätskonstante zwischen den Federwindungen zu erreichen. wurden Suspensionen aus Silikonöl und nanokristallinem Bariumtitanat hergestellt und bezüglich ihrer Langzeitstabiltät charakterisiert. - Gemäß den Anforderungen des Projektpartners KOMPASS wurden maßgeschneiderte Al2O3-Federn mit einer Federkonstante < 0,1 N/mm hergestellt und für den Aufbau des finalen Demonstrator eingesetzt. Die prinzipielle Funktionsfähigkeit des neuen Sensorkonzeptes auf Basis keramischer Federn wurde mit dem im Projekt aufgebauten Demonstrator nachgewiesen. Die Umsetzung der F+E-ergebnisse in eine industrielle Nutzung zur Herstellung von Gravimetern wird vom Projektpartner KOMPASS angestrebt und ist bereits mit detaillierten Zeitplänen untersetzt. KW - Langzeitstabilität KW - Sensorik KW - Keramikfeder KW - Spannungs-Dehnungs-Verhalten PY - 2019 UR - https://www.gbv.de/dms/tib-ub-hannover/1681417375.pdf UR - https://www.tib.eu/de/suchen/id/TIBKAT%3A1681417375/Alterungsbest%C3%A4ndige-keramische-Federsensoren-durch/ SP - 1 EP - 64 PB - Bundesanstalt für Materialforschung und -prüfung CY - Berlin AN - OPUS4-50742 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matz, R. A1 - Rabe, Torsten A1 - Töpfer, J. A1 - Ziesche, S. T1 - Circuit-Board-Integrated Transformers Design and Manufacture N2 - Transformers couple two sections of a circuit by electromagnetic induction. They are widely used to either transform alternating voltage levels or to transmit power or signals across galvanic isolation. Both of these functions are essential for the operation of sensors and controllers. Covering all aspects from idea to circuit performance and from design to manufacture, this paper presents the first comprehensive description of the making of miniaturized, rugged, up-to-100W transformers for embedding into multilayer circuit boards. For circular coils, the well-manageable Ampere-Laplace law is shown to yield reliable designs, predicting correctly the performance of manufactured hardware. This enables fast design without lengthy finite element modelling. In the low-power linear regime, basic relations describe how the device’s characteristics evolve from the material properties and device structure. While scattering Parameters are useful for the analysis of isolated transformers with their intrinsic parasitics, the interaction with the components of the final circuit and the aspects of power and efficiency are addressed by chain matrixes. While these design rules are similar for multilayer boards of different material (like epoxy, Teflon, ceramics), the manufacturing of ceramic board transformers is considered here in detail. Low-temperature-cofired ceramic (LTCC) boards being sintered at 900 °C are particularly suited for harsh environments with chemical or thermal stress as frequently found at sensor positions. The transformer performance usually benefits from or even requires an integrated ceramic core of higher permeability, a ferrite, to shape the magnetic flux. Methods to sinter ferrites inside a dielectric ceramic multilayerandto measure their performance are therefore described in detail.Asthe sintering behaviour of dielectricandmagnetic ceramics differs considerably, their simultaneous sintering is challenging.However, the sintering temperatures of the usefulMnZnand NiZnCu ferrites can be lowered to that of the dielectric material with only moderate loss of permeability by glass additives. Furthermore, thermal mismatch between materials causes catastrophic failure or at least stress and loss of magnetic performance during cooling to room temperature after sintering. This is avoidable by either adjusting the thermal expansion coefficient of the ferrite or by enclosing the ferrite between stressreleasing separation layers.We present the state of the art in materials development according to the first approach as well as fully functional devices made with the second technique. Other applications not directly addressed but well related to this work are characterized by low load resistance in relation to the coil resistance of the transformer. Efficient power transmission then requires that technological solutions are applied to achieve the lowest possible resistive loss inside the coils by an enlarged conductor cross-section. As this is particularly challenging for LTCC boards, a technique is discussed to fabricate conductor traces with a thickness larger than their width. KW - Multilayer ceramic technology KW - LTCC KW - Transformer PY - 2020 DO - https://doi.org/10.4416/JCST2019-00071 SN - 2190-9385 VL - 11 IS - 1 SP - 44 EP - 61 PB - Göller Verlag CY - Baden-Baden AN - OPUS4-50751 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn A1 - Rabe, Torsten T1 - Design and fabrication of ceramic springs N2 - Ceramic springs offer versatile possibilities for load bearing or sensor applications in challenging environments. Although it may appear unexpected, a wide range of spring constants can be implemented by material selection and especially by the design of the spring. Based on a rectangular cross-section of the windings, it is possible to design a spring geometry that generates the desired spring constant simply by choosing appropriate diameter, height, widths, and number of windings. In a recent research project the calculation of helical compression springs made of rectangular steel (German standard DIN 2090) was applied for the design of ceramic springs. A manufacturing technology has been worked out to fabricate such springs from hollow cylinders of several highly dense technical ceramics by milling. Ceramic springs with precise rectangular section, without edge damage, and mean surface roughness smaller than 0.2 µm were produced after parameter optimization. Tolerances of less than 10 µm were achieved regarding spring diameter, height, and width of cross section. It is shown that the calculations outlined in the standard are valid for a variety of ceramic materials as well. Demonstrator springs with a wide range of spring constants have been fabricated, including zirconia springs with 0.02 N/mm, alumina springs with 1 N/mm and Si3N4 springs with 5 N/mm. A reproducibility study of six zirconia springs with a constant of 0.3 N/mm showed a relative difference in spring constants of less than +/- 1 %. This combination of a valid calculation approach for spring geometry and a reliable manufacturing technology allows for purposeful development and fabrication of ceramic springs with precise mechanical properties and superior chemical stability. T2 - EUROMAT 2019 CY - Stockholm, Sweden DA - 01.09.2019 KW - Ceramic spring KW - Hard machining KW - Spring constant PY - 2019 AN - OPUS4-48870 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gili, A. A1 - Bischoff, B. A1 - Simon, U. A1 - Schmidt, Franziska A1 - Kober, D. A1 - Görke, O. A1 - Bekheet, M. A1 - Gurlo, A. T1 - Ceria-based dual-phase membranes for high-temperature Carbon dioxide separation: Effect of iron doping and pore generation with MgO template N2 - Dual-phase membranes for high-temperature carbon dioxide Separation have emerged as promising technology to mitigate anthropogenic greenhouse gases emissions, especially as a pre- and post-combustion separation technique in coal burning power plants. To implement These membranes industrially, the carbon dioxide permeability must be improved. In this study, Ce_(0.8) Sm_(0.2) O_(2-d) (SDC) and Ce_(0.8)Sm_(0.19)Fe_(0.01)O_(2-d) (FSDC) ceramic powders were used to form the skeleton in dual-Phase membranes. The use of MgO as an environmentally friendly pore generator allows control over the membrane porosity and microstructure in order to compare the effect of the membrane’s ceramic phase. The ceramic powders and the resulting membranes were characterized using ICP-OES, HSM, gravimetric analysis, SEM/EDX, and XRD, and the carbon dioxide flux density was quantified using a high-temperature membrane permeation setup. The carbon dioxide permeability slightly increases with the addition of iron in the FSDC membranes compared to the SDC membranes mainly due to the reported scavenging effect of iron with the siliceous impurities, with an additional potential contribution of an increased crystallite size due to viscous flow sintering. The increased permeability of the FSDC system and the proper microstructure control by MgO can be further extended to optimize carbon dioxide permeability in this membrane system. KW - Samarium doped ceria KW - SDC KW - FSDC KW - CO2 separation membranes KW - Scavenging effect of iron KW - Permeability PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-488612 DO - https://doi.org/10.3390/membranes9090108 SN - 2077-0375 VL - 9 IS - 9 SP - 108, 1 EP - 15 PB - MDPI AN - OPUS4-48861 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabe, Torsten A1 - Schulz, Bärbel A1 - Paulick, C. T1 - Development of ceramic helical springs for sensor applications N2 - At high temperatures and in harsh environments ceramic springs are often superior to metallic ones and allow for innovative solutions. A further application was proposed by using ceramic springs as capacitive force sensor. Lower and upper coil surfaces are coated by electrically conducting layers. Deformation of such spring results in a change of capacity. Sensor application calls for helical springs with rectangular cross-section, a linear stress-strain characteristic over entire deformation range and low manufacturing tolerances relating to inner and outer diameter, coil cross section and spring pitch. Furthermore, complex spring design with integrated connecting elements has to be realized. Alumina, zirconia (Y-TZP) and silicon nitride springs were produced by hard machining starting from sintered hollow cylinders. After external and internal cylindrical grinding the hollow cylinders were filled with hard wax, followed by multi-stage cutting of spring coils with custom-made cutting discs. Finally, hard wax was removed by melting and burnout. Best surface and edge qualities of springs were reached using Y-TZP material and hot isostatic pressed alumina. Y-TZP springs produced with material-specifically selected cutting discs and optimized process parameters show sharp coil edges without spallings and mean roughness values of inner surfaces < 0.2 μm. Manufacturing tolerances of spring diameters, spring pitch, height and width of coil cross section are in the range of ± 10 microns. Good reproducibility of spring geometry by optimized hard machining technology allows for production of Y-TZP springs with spring constants differing less than ± 1 % within a series. According to DIN 2090 spring constant for rectangular coil cross section is proportional to the square of height and width of coil cross section and indirectly proportional to number of active coils and to the cube of the mean spring diameter. Hence, spring constants can be tailored over a range of many orders of magnitude by changing the spring dimensions. Good agreement was reached between calculated target spring constants and measured values on produced springs. Alumina and zirconia springs were characterized relating to deformation behavior under dynamic compression load with various deformation speeds and under static tensile loads over long periods of time. Contrary to alumina springs, a non-linear stress-strain behavior of TZP springs was proved in both test series. It is supposed, that pseudoelasticity caused by stress-induced transformation of tetragonal to monoclinic phase is responsible for this special feature of TZP springs. Therefore, TZP material cannot be used for capacitive spring sensors. T2 - European Ceramic Society Conference (ECerS) CY - Torino, Italy DA - 16.06.2019 KW - Ceramic spring KW - Sensor KW - Spring constant KW - Failure test KW - Microstructure PY - 2019 AN - OPUS4-48610 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabe, Torsten A1 - Schulz, Bärbel A1 - Kalinka, Gerhard T1 - Deformation behavior of alumina and zirconia springs at room temperature N2 - At high temperatures and in harsh environments ceramic springs are often superior to metallic springs and allow for innovative solutions. A recently proposed application involves ceramic springs with metallized surfaces as capacitive force sensor. A strictly linear stress-strain characteristic of the spring is a precondition for such a sensor. Helical ceramic springs with rectangular cross-section have been produced from sintered hollow cylinders. Alumina, ATZ, Y-TZP, and Ce-TZP springs with identical dimensions were characterized and compared regarding deformation behavior. Spring deformation was investigated under various load scenarios. Dynamic compression was performed with deformation speeds from 0.3 to 30 mm/min. Spring constants of alumina springs are strain rate independent. By contrast, Y-TZP spring constant increases by approximately 3 % within the experimental framework. A high-precision test facility was developed to characterize spring displacement in nm range under static tensile load over long periods of time. Spring elongation with asymptotic course was observed for zirconia containing materials at room temperature. This effect is particularly strong in the case of Y-TZP. Up to 0.3 % time-dependent elongation was measured after 24 h under constant load. Deformation is completely reversible after unloading. Alumina springs do not show any time-dependent deformation under identical test conditions. Contrary to alumina springs, a non-linear stress-strain behavior of TZP springs at room temperature was proved in both test series. It is supposed, that pseudo-elasticity caused by stress-induced phase transformation from tetragonal to monoclinic is responsible for this special behavior of TZP springs. T2 - D-A-CH Keramiktagung CY - Leoben, Austria DA - 06.05.2019 KW - Phase transformation KW - Ceramic spring KW - Force-distance diagram KW - Deformation behavior PY - 2019 AN - OPUS4-48026 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zocca, Andrea A1 - Lima, P. A1 - Diener, S. A1 - Katsikis, N. A1 - Günster, Jens T1 - Additive manufacturing of SiSiC by layerwise slurry deposition and binder jetting (LSD-print) N2 - The current work presents for the first time results on the Additive Manufacturing of SiSiC complex parts based on the Layerwise Slurry Deposition (LSD) process. This technology allows to deposit highly packed powder layers by spreading a ceramic slurry and drying. The capillary forces acting during the process are responsible for the dense powder packing and the good joining between layers. The LSD process can be combined with binder jetting to print 2D cross-sections of an object in each successive layer, thus forming a 3D part. This process is named LSD-print. By LSD-print and silicon infiltration, SiSiC parts with complex geometries and features down to 1mm and an aspect ratio up to 4:1 could be demonstrated. The density and morphology were investigated for a large number of samples. Furthermore, the density and the mechanical properties, measured by ball-on-three-balls method, were in all three building directions close to isostatic pressed references. KW - Silicon Carbide KW - Additive Manufacturing KW - 3D printing KW - Layerwise slurry deposition KW - LSD print PY - 2019 DO - https://doi.org/10.1016/j.jeurceramsoc.2019.05.009 VL - 2019 IS - 39 SP - 3527 EP - 3533 PB - Elsevier Ltd. AN - OPUS4-48546 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul A1 - Abram, Sarah-Luise A1 - Kuchenbecker, Petra A1 - Würth, Christian A1 - Rühle, Bastian A1 - Resch-Genger, Ute A1 - Hodoroaba, Vasile-Dan T1 - Fine iron oxide nanoparticles as a candidate reference material for reliable measurement of particle size N2 - Background, Motivation and Objective Nanomaterials are at the core of some of the 21st century’s most promising technologies. In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important. Furthermore, the European Commission has taken measures via the REACH Regulations to control the classification of nanomaterials. REACH Annexes which entered into force in January 2020 require manufacturers to register nanomaterials that are traded in larger quantities (at least 1 ton). Every powder or dispersion where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as a nanomaterial. This creates a need for both industrial manufacturers and research and analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is working on developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution, but also targeting other key parameters such as shape, structure (including porosity) and functional properties. Thus, candidate materials are considered to complement the already available spherical and monodisperse silica, Au and polystyrene reference nanoparticles, e.g. iron oxide and titanium oxide, with an average atomic number between those of silica and gold. Particularly for the imaging by electron microscopies, new nanoparticles of well-defined size in the range of 10 nm are decisive for the accurate particle segmentation by setting precise thresholds. Statement of Contribution/Methods Synthesis: Highly monodisperse iron oxide nanoparticles can be synthesized in large quantities by thermal decomposition of iron oleate or iron acetylacetonate precursors in high boiling solvents such as octadecene or dioctyl ether in the presence of oleic acid and oleylamine as capping agents. Scanning Electron Microscope: An SEM of type Supra 40 from Zeiss has been used including the dedicated measurement mode transmission in SEM (STEM-in-SEM) with a superior material contrast for the nanoparticle analysis. The software package ImageJ has been used for the analysis of the STEM-in-SEM images and to determine the particle size distribution. Dynamic Light scattering (DLS): Particles in suspension were measured in comparison by means of Zetasizer Nano (Malvern Panalytical; cumulants analysis) and NanoFlex (Microtrac; frequency power spectrum). Results/Discussion In this study iron oxide nanoparticles synthesized at BAM and pre-characterized by DLS, SEM (including the transmission mode STEM-in-SEM) are presented. The particles are spherical and highly monodisperse with sizes slightly larger than 10 nm. T2 - Nanosafe 2020 CY - Online meeting DA - 16.11.2020 KW - Reference nanomaterials KW - Imaging techniques KW - Size and size distribution KW - Reliable characterization KW - Iron oxide nanoparticles PY - 2020 AN - OPUS4-51767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Praktische Erfahrungen zur Granulometrie von Pulvern im Submikron- und Nanobereich N2 - Der Vortrag beleuchtet insbesondere die Herausforderungen die sich bei der Dispergierung der Nanopulver aufgrund der hohen Adhäsivkräfte ergeben. Die Bewertung der Probenpräparation ist nur indirekt zugänglich, aber essentiell für die Zuverlässigkeit der Messergebnisse. Anhand von Beispielen werden Lösungsvorschläge aufgezeigt. Der Vortrag schließt mit einem Vorschlag zur Strategie der Herangehensweise bei der Partikelgrößenbestimmung von Nanopulvern. T2 - Sitzung des Fachausschusses "Material- und Prozessdiagnostik" der Deutschen Keramischen Gesellschaft: Zuverlässige granulometrische Charakterisierung von Mikro- und Nanopulvern – Voraussetzung für optimierte Keramikwerkstoffe in der Energietechnik CY - Online meeting DA - 19.11.2020 KW - Nano-powder KW - particle size determination KW - dispersion KW - sample preparation PY - 2020 AN - OPUS4-51665 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hmood, F. A1 - Schmidt, Franziska A1 - Görke, O. A1 - Günster, Jens T1 - Investigation of chemically modified ICIE16 bioactive glass, part II N2 - Chemically modified bioactive glasses based on ICIE16 were prepared with the melt-quenching method using water as a quenching medium. The sinterability of these bioactive glasses was investigated and is discussed in this article. The sintering experiments were conducted with different sintering temperatures, sintering times and heating rates. Those parameters are crucial for dense glass with an amorphous structure. The particle size (d50) of the starting glass powder was determined at 88 μm and kept constant. The pre-pressed glass pellets were cold-isostatically pressed at 300 MPa to a green density of around 63 %. Density development, phase identification, shrinkage behavior and the microstructure were investigated to determine the sinterability of the developed glasses. The glass powders were sintered at different temperatures inside the processing window while crystallization was monitored. The results have shown that the sinterability of the developed glasses strongly dependsonthe proposed chemical additions. The highest density reached was 96 %, which belongs to BP1 glass with sintering conditions of 20 K/min heating rate for 60 min at 750 °C. KW - Bioactive glass KW - Viscous sintering KW - Crystallization KW - Processing window KW - Grain boundary PY - 2019 DO - https://doi.org/10.4416/JCST2019-00031 VL - 11 IS - 1 SP - 1 EP - 9 PB - Göller Verlag AN - OPUS4-49913 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Orlov, N. K. A1 - Evdokimov, P. V. A1 - Milkin, P. A. A1 - Garshev, A. V. A1 - Putlayev, V. I. A1 - Grebenev, V. V. A1 - Günster, Jens T1 - Phase equilibria in CaNaPO4-CaKPO4 system and their influence on formation of bioceramics based on mixed Ca-K-Na phosphates N2 - An investigation of the two-component phase diagram of the CaNaPO4- CaKPO4system performed using various analysis techniques is reported. The continuous solid solution series of α-CaMPO4 existing above 700 °C undergoes eutectoid decomposition during cooling to β-CaMPO4-based solid solutions enriched with Na and K, and to an intermediate nonstoichiometric compound with an ideal composition of CaK0.6Na0.4PO4. All three compounds exhibit significant volumetric effects associated with first-order phase transitions, with positive volume changes under cooling for the intermediate compound. Increased K content in ceramics based on CaKyNa1-yPO4 compositions enhances the strength properties of those ceramics, including their fracture toughness, which is associated with increased density. Increased K content also has a smaller effect of inducing phase transformations accompanied by strong volume changes. KW - Phase transformations KW - Bioceramics KW - Mixed Ca-K-Na phosphates KW - Na and K rhenanites KW - Phase diagram PY - 2019 DO - https://doi.org/10.1016/j.jeurceramsoc.2019.07.044 VL - 39 IS - 16 SP - 5410 EP - 5422 PB - Elsevier Ltd. AN - OPUS4-49621 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Orlov, N. K. A1 - Milkin, P. V. A1 - Evdokimov, P. A. A1 - Putlayev, V. I. A1 - Günster, Jens T1 - Sintering of sodium and potassium tcp based ceramic for bone grafting application N2 - Biomaterials for bone replacement and grafting should possess sufficient strength, be bioresorbable and demonstrate osteoconductive and osteoinductive properties. However, resorption of modern materials for bone grafting (hydroxyapatite (HA) and tricalcium phosphate (TCP)) is reported, in some cases, to be not enough, this is why the search for more soluble compounds compared to HA and TCP looks very perspective. A possible way to increase ceramics solubility leads to partial substitution of Ca2+ -ions in Ca3(PO4)2 by alkali cations, like Na+ or/and K+. Improvement of solubility stems from decreasing lattice energy of a substituted phase, as well as the increase in hydration energy of the ions releasing from the phase to ambient solution. From this viewpoint, bioceramics based on compositions from Ca3(PO4)2 - CaKPO4 - CaNaPO4 ternary system seems to be prospective for bone replacement and grafting in the sense of resorption properties. At the same time, one should bear in mind that solubility level (resorbability) is governed not only by reduction of lattice energy but also by microstructure features. Grain sizes and porosity contribute much to dissolution rate making the study of sintering of the ceramics mentioned above highly important. To control Ca3(PO4)2 - CaKPO4 - CaNaPO4 based ceramic microstructure it is necessary to know possible phase transformations in the system and the way to manage microstructure by sintering schedule or sintering process. In this work, an isothermal section for phase diagram of Ca3(PO4)2 - CaKPO4 - CaNaPO4 ternary system is studied with several techniques. According to the XRD of quenched samples, this phase triangle has four single-phase areas at 1200˚C (Figure 1). It was shown that single-phase CaK0.6Na0.4PO4 cannot be sintered to full-dense ceramics by conventional sintering regardless time-temperature schedule. Two-step sintering technique, beneficial in the case of HA-ceramics, was unsuccessful in all cases of calcium-alkali phosphate compositions. However, field-assisted sintering techniques like, e.g. Spark Plasma Sintering (SPS), can overcome this problem due to significant impact on grain boundary diffusion. In connection with this fact, grains grow much slower retaining sintering process in a pore control regime. In this work CaK0.6Na0.4PO4 low-porous ceramics was also fabricated by FAST-methods of sintering. Moreover, other alternative sintering techniques, such as reaction sintering, may be useful in accelerating ions diffusion but stopping excessive grain growth.Strength properties of ceramics were evaluated by B3B-testing, micro- and nanoindentation techniques. Fracture toughness also becomes higher with potassium content increase, guiding porosity level. Resorption properties of sintered ceramics were studied in different solutions with pH=5 and 7.4. Acknowledgements. The research of sintering processes in calcium phosphate materials were funded by RFBR according to the research project № 18-33-00974. T2 - XVI ECerS Conference 2019 CY - Turin, Italy DA - 16.06.2019 KW - Phase transformations KW - Bioceramics KW - Mixed Ca-K-Na phosphates KW - Na and K rhenanites KW - Phase diagram PY - 2019 AN - OPUS4-49622 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Günster, Jens A1 - Zocca, Andrea T1 - Dense Powder Beds for the Additive Manufacturing of Ceramics N2 - Many of the most successful and precise additive manufacturing (AM) technologies are based on the deposition layer-by-layer of a flowable powder. Since the first pioneering work at the end of the 1980th many developments have been introduced, greatly extending the use of different materials, improving the physical properties of the components built and enhancing the accuracy of the process. Still very important issues remain nowadays, hampering a completely autonomous production of parts and even restricting the freedom of design by means of these technologies. One of the major issues is the low density and stability of the parts during the building process, which implies the need of support structures: The powder bed surrounding the part has an essential role, since it should support the structure during building, until it’s ready for removal. Moreover, the microstructure of the powder bed is a template for the microstructure of the part produced. In this context, the use of submicron ceramic powders is still a challenge. Three approaches for the stabilization and densification of powder beds will be presented: The Layerwise Slurry Deposition process LSD, the gas flow assisted powder deposition and the Laser Induced Slipcasting (LIS) of ceramic powder compacts. T2 - 43rd International Conference and Exposition on Advanced Ceramics and Composites (ICACC 2019) CY - Daytona Beach, FL, USA DA - 27.01.2019 KW - Ceramics KW - Additive Manufacturing PY - 2019 AN - OPUS4-49627 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Günster, Jens T1 - Powder-based Additive Manufacturing at Micro-Gravity N2 - Are we ready for putting a human footprint on Mars? Obviously, it is possible to send technologically challenging missions to our earth neighbors with a high level of complexity, such as enabling autonomous planetary mobility. As humanity contemplates mounting manned missions to Mars, strategies need to be developed for the design and operation of hospitable environments safely working in space for years. Humans require water and air provided by complicated equipment. Its safe operation is a great challenge and implies being prepared for all eventualities. Instead of foreseeing and preparing for all possible scenarios of machine failures and accidents, it appears logic taking advantage of the flexibility of humans and providing essential equipment for the reaction on critical situations. The supply of spare parts for repair and replacement of lost equipment would be one key pillar of such a strategy. Bearing in mind the absolute distance and flight trajectories for manned missions to Mars, supplying spare parts from Earth is impossible. Thus, in space manufacturing remains the only option for a timely supply. With a high flexibility in design and the ability to manufacture ready to use components directly from a computer aided model, additive manufacturing technologies appear extremely attractive. For metal parts manufacturing the Laser Beam Melting process is the most widely used additive manufacturing process in industrial application. However, envisioning the handling of metal powders in the absence of gravitation is one prerequisite for its successful application in space. A gas flow throughout the powder bed has been successfully applied to compensate for missing gravitational forces in micro gravity experiments. The so-called Gas Flow Assisted Powder Deposition is based on a porous building platform acting as a filter for the fixation of metal particles in a gas flow driven by a pressure difference maintained by a vacuum pump. T2 - 1st Sino-German Workshop on 3D Printing in Space CY - Beijing, China DA - 20.02.2019 KW - Zero-g KW - Additive Manufacturing KW - µ-gravity PY - 2019 AN - OPUS4-49628 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Günster, Jens T1 - Powder-based Additive Manufacturing at Micro-Gravity N2 - Are we ready for putting a human footprint on Mars? Obviously, it is possible to send technologically challenging missions to our earth neighbors with a high level of complexity, such as enabling autonomous planetary mobility. As humanity contemplates mounting manned missions to Mars, strategies need to be developed for the design and operation of hospitable environments safely working in space for years. Humans require water and air provided by complicated equipment. Its safe operation is a great challenge and implies being prepared for all eventualities. Instead of foreseeing and preparing for all possible scenarios of machine failures and accidents, it appears logic taking advantage of the flexibility of humans and providing essential equipment for the reaction on critical situations. The supply of spare parts for repair and replacement of lost equipment would be one key pillar of such a strategy. Bearing in mind the absolute distance and flight trajectories for manned missions to Mars, supplying spare parts from Earth is impossible. Thus, in space manufacturing remains the only option for a timely supply. With a high flexibility in design and the ability to manufacture ready to use components directly from a computer aided model, additive manufacturing technologies appear extremely attractive. For metal parts manufacturing the Laser Beam Melting process is the most widely used additive manufacturing process in industrial application. However, envisioning the handling of metal powders in the absence of gravitation is one prerequisite for its successful application in space. A gas flow throughout the powder bed has been successfully applied to compensate for missing gravitational forces in micro gravity experiments. The so-called Gas Flow Assisted Powder Deposition is based on a porous building platform acting as a filter for the fixation of metal particles in a gas flow driven by a pressure difference maintained by a vacuum pump. T2 - 2nd Sino-German Workshop on 3D Printing in Space CY - Berlin, Germany DA - 28.10.2019 KW - µ-gravity KW - Additive Manufacturing KW - Zero-g PY - 2019 AN - OPUS4-49629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabe, Torsten T1 - Alternative Verfahren zur Strukturierung von Grünfolien und Laminaten N2 - Die Strukturierung keramischer Grünfolien und Laminate ist ein wesentlicher Prozessschritt in der keramischen Multilayer-Technologie und begründet die funktionelle Vielfalt keramischer Multilayer. Benötigt wird die Grünbearbeitung für die Herstellung elektrischer und thermischer Vias sowie innerer Kavitäten und Kanäle für Transport und Lagerung von Gasen und Flüssigkeiten in hochintegrierten Schaltungsträgern, Sensoren und Reaktoren. Standardverfahren in der industriellen Fertigung sind Heißschneiden, Stanzen und Laserbearbeitung. Darüber hinaus werden auch Bohren, Fräsen, Sägen und Heißprägen verwendet. Über die Erprobung weiterer Verfahren wie Wasserstrahlschneiden, Dampfstrahlätzen und Powder Blasting wird in der Literatur berichtet. Im Vortrag werden spezifische Vor- und Nachteile der eingesetzten Verfahren beleuchtet. Abschließend werden die Kriterien für die Auswahl des optimalen Strukturierungsverfahrens diskutiert. Zusammensetzung und Gefüge sowie die dadurch bedingten mechanischen und thermomechanischen Eigenschaften sowie das Absorptionsverhalten von Grünfolien sind sehr unterschiedlich. Daraus resultieren unterschiedliche optimale Bearbeitbarkeitsparameter. T2 - DKG-Seminar "Foliengieß- und Schlitzdüsenverfahen" CY - Hermsdorf, Germany DA - 05.11.2019 KW - Stanzen KW - Keramische Folien KW - Laserbearbeitung KW - Grünfolieneigenschaften PY - 2019 AN - OPUS4-49742 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Orlov, Nikolai A1 - Kiseleva, A. K. A1 - Milkini, P. A. A1 - Evdokimov, P. V. A1 - Putlayev, V. I. A1 - Günster, Jens T1 - Potentialities of Reaction Sintering in the Fabrication of High-Strength Macroporous Ceramics Based on Substituted Calcium Phosphate N2 - Calcium alkali metal (potassium and sodium) double and triple phosphates have been synthesized in different ways. Was for the first time used reaction sintering to produce ceramics based on calcium alkali metal mixed phosphates and investigated the densification behavior of mixed phosphate-based multiphase materials during sintering by this method. Was presented the microstructure of polished surfaces of sintered samples differing in phase composition and determined the density of ceramics prepared using reaction mixtures differing in composition. The effect of reaction sintering on the porosity of the ceramics has been assessed. Using stereolithographic printing and reaction sintering, was produced macroporous mixed Calcium phosphate-based ceramic implants. Their compressive strength has been determined to be 0.78 ± 0.21 MPa for two-phase samples and 1.02 ± 0.13 MPa for three-phase samples. KW - Reaction Sintering KW - Bio Ceramics PY - 2020 DO - https://doi.org/10.1134/s0020168520120146 VL - 56 IS - 12 SP - 1298 EP - 1306 PB - Pleiades Publishing LTD AN - OPUS4-52004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kuchenbecker, Petra T1 - Granulometry of Nano Powders - a Challenge Especially for the Dispersion Process N2 - The use of increasingly finer starting powders up to nanopowders can also be observed in the field of ceramics. Their advantages consist, for example, in their lower activation energy, an increase in strength or unique optical properties. However, handling and characterization of the powders are much more difficult. The main reason for this is the very high adhesive forces between the particles and between particles and other surfaces, too. Therefore, submicron and even more so nanoparticles tend to agglomerate and their separation into primary particles during sample preparation prior to particle sizing is of particular challenge. A representative measurement sample is only obtained when it no longer contains agglomerates. The evaluation of the dispersion process and a decision on whether it was successful thus increases in importance for the reliability of the measurement results of particle sizing. The presentation uses examples to show possible approaches and provides information on possible sources of error. It is shown that successful granulometric characterisation of fine powders requires both an improved dispersion technique and very often an effective combination of two or more measurement methods. KW - Agglomerates KW - Nano-powder KW - Dispersion process PY - 2021 SN - 0173-9913 VL - 98 IS - 2 SP - 47 EP - 54 PB - Göller Verlag GmbH CY - Baden-Baden AN - OPUS4-52504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stargardt, Patrick T1 - Modeling of the cooling behavior of thermoelectric multilayers N2 - Multilayered designs are an attractive approach towards cost-effective manufacturing of thermoelectric generators. Therefore, efforts are being made to co-fire two promising thermoelectric oxides, namely calcium cobaltite and calcium manganate. In this study, ceramic tapes, multilayer technology, and pressure-assisted sintering (PAS) were used. A major challenge for the PAS of low-sintered calcium manganate was cracking during cooling. A relationship between the properties of the release tape used during PAS and the cracking behavior was experimentally observed. To understand the origin of failure, reaction layers in the multilayer were analyzed and thermal stresses during cooling were estimated by finite element (FE) simulations. Thermal expansion, elastic properties, and biaxial strength of the thermoelectric oxides and selected reaction layers were determined on separately prepared bulk samples. The analysis showed that the reaction layers were not the cause for cracking of calcium manganate. Using the FE model, thermal stresses in different manganate multilayer designs with varying properties of the release tape were studied. The FEM study indicated, and a validation experiment proved that the thickness of the release tape has the main effect on thermal stresses during cooling in separately sintered calcium manganate. T2 - Keramik 2021 / Ceramics 2021 CY - Online Meeting DA - 19.04.2021 KW - Fem KW - Thermoelectric KW - Pressure assisted sintering PY - 2021 AN - OPUS4-52489 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Sample Preparation of Nano-Powders for Particle Size Determination N2 - The use of increasingly finer starting powders up to nanopowders can also be observed in the field of ceramics. Their advantages consist, for example, in their lower activation energy, an increase in strength or unique optical properties. However, handling and characterization of the powders are much more difficult. The main reason for this is the very high adhesive forces between the particles and between particles and other surfaces, too. Therefore, submicron and even more so nanoparticles tend to agglomerate and their separation into primary particles during sample preparation prior to particle sizing is of particular challenge. A representative measurement sample is only obtained when it no longer contains agglomerates. The evaluation of the dispersion process and a decision on whether it was successful thus increases in importance for the reliability of the measurement results of particle sizing. The presentation uses examples to show possible approaches and provides information on possible sources of error. It is shown that successful granulometric characterisation of fine powders requires both an improved dispersion technique and very often an effective combination of two or more measurement methods. T2 - 96. Jahrestagung der Deutschen Keramischen Gesellschaft CY - Online Meeting DA - 19.04.2021 KW - Agglomerates KW - Nano-powder KW - Dispersion process PY - 2021 AN - OPUS4-52503 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -