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 - JOUR A1 - Agea, Boris A1 - Walzel, S. T1 - 3D Druck unterstütz die Dekarbonisierung N2 - Suspensionsbasiertes Binder Jetting reduziert die Brennzeiten von technischer Keramik im Vergleich zu anderen 3d-druckverfahren signifikant. dabei wird nicht nur Energie beim Betrieb der Brennöfen gespart, sondern auch die Emission von Kohlendioxid beim Brennvorgang selbst gesenkt. KW - Schlickerdeposition PY - 2021 VL - 6 SP - 26 EP - 28 PB - Keramische Zeitschrift AN - OPUS4-53812 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Entwicklung thermoelektrischer Multilayergeneratoren auf der Basis von Calciumcobaltit N2 - 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. N2 - Thermoelektrische Generatoren können zum „Energy harvesting“ für den autarken Betrieb von bspw. Sensoren eingesetzt werden. Eine interessante Alternative zu den herkömmlichen π-Typ Generatoren sind auf Grund der höheren Leistungsdichte und der guten Automatisierbarkeit thermoelektrische Multilayergeneratoren. Calciumcobaltit ist ein vielsprechendes oxidisches Thermoelektrika (p-Typ) mit stark anisotropen Eigenschaften. Die hier vorgestellte Studie zeigt die Entwicklung von texturierten Unileg-Multilayer-Generatoren mittels keramischer Multilayertechnologie. Calciumcobaltit wird durch Foliengießen und druckunterstützte Sinterung texturiert. Im Vergleich zur konventionellen Sinterung verbessert sich die Festigkeit um den Faktor 10. Die thermoelektrischen Eigenschaften können je nach verwendetem Druckniveau hinsichtlich maximalem Power Factor oder hinsichtlich maximalem Gütefaktor optimiert werden. Ein Glaskeramikkomposit wird als Isolationsmaterial mit hohem Volumenwiderstand und angepasstem Wärmeausdehnungskoeffizienten entwickelt. Der Unileg-Multilayer-Generator wird in einem Schritt co-gesintert. Die hergestellten Demonstratoren erreichen 80% der simulierten Output-Leistung. Diese Ergebnisse stellen den ersten Machbarkeitsnachweis für die Herstellung von co-gesinterten Multilayer-Generatoren aus texturiertem Calciumcobaltit mit hohem Power Factor und hoher Festigkeit dar. T2 - Seminar des Lehrstuhls für Funktionsmaterialien, Universität Bayreuth CY - Online meeting DA - 18.06.2021 KW - Thermoelektrischer Generator KW - Multilayertechnik KW - Energy harvesting PY - 2021 AN - OPUS4-52834 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Rabe, Torsten A1 - Eichler, J. A1 - Picht, G. A1 - Rossner, W. A1 - Stelter, M. A1 - Voigt, I. T1 - Digitalisierung der keramischen Fertigung - Herausforderungen und Chancen N2 - Dieses Strategiepapier zielt darauf ab, Akteuren und Entscheidungsträgern den Status der Digitalisierung in der keramischen Fertigung, erfolgreiche Best-Practice-Beispiele aber auch die Herausforderungen nahezubringen, die es nun anzugehen gilt. Es ist die Vision, die Keramikfertigung durchgehend zu digitalisieren und alle Schritte des Produktkreislaufs lückenlos über die gesamte Wertschöpfungs- und Nutzungskette zu vernetzen: also eine Keramikindustrie 4.0 zu etablieren. Das Strategiepapier erfasst zunächst die Spezifität der keramischen Fertigung und nimmt eine Analyse des gegenwärtigen Standes der Digitalisierung in der keramischen Industrie vor, auch anhand einiger ausgewählter Beispiele aus der industriellen Praxis. Auf Basis der wesentlichen Bausteine für eine Fertigungsdigitalisierung werden schließlich die Chancen für Keramikproduzenten sowie der erforderliche Forschungs- und Entwicklungsbedarf aufgezeigt. KW - Datenmanagement KW - Digitalisierung KW - Fertigungsprozess KW - Keramik KW - Sensorik PY - 2021 SP - 1 EP - 39 PB - Deutsche Gesellschaft für Materialkunde (DGM) und Deutsche Keramische Gesellschaft (DKG) CY - Köln ET - 1000 AN - OPUS4-52708 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Höhne, Patrick T1 - Limits of computer tomography aided characterization of different types of porous ceramic materials N2 - Ceramics with open porosity are attractive materials in many fields of applications covering medicine, catalysis, and filtration. Manifold technologies to produce porous ceramics are available, e.g. foaming and replica processes, resulting in various microstructures. Development and manufacturing of new materials is accelerating, while crucial characterization is becoming increasingly difficult and conventional measurements lack the desired speed. Computed tomography (CT) offers the possibility to three-dimensionally characterize entire samples with minimal sample preparation, while its main advantage is that it is non-destructive. Still, the assessment of quantitative results from CT measurements is not trivial. The poster presents CT characterizations of newly developed as well as commercially available openly porous ceramic samples. Properties such as porosity, permeability or pore characteristics were measured conventionally and compared to results calculated from CT-measurements using the commercial software VG StudioMax. The determined differences between measured and calculated values are presented and application areas as well as limits of the CT characterization are evaluated. T2 - Jahrestagung der Deutschen keramischen Gesellschaft 2021 CY - Online Meeting DA - 19.04.2021 KW - Ceramic KW - Porosity PY - 2021 AN - OPUS4-52724 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 - JOUR A1 - Agea Blanco, Boris A1 - Walzel, S. A1 - Chi, J. A1 - Lüchtenborg, J. T1 - Making Binder Jetting Really Work for Technical Ceramics - Additive Manufacturing of Technical Ceramics N2 - As an alternative shaping method to the traditionally used processes, additive manufacturing (AM) can produce economical ceramic components in small lot sizes and/or with complex geometries. Powder-based additive manufacturing processes like binder jetting are popular in the field of metal AM. One reason is the increased productivity compared to other AM technologies. For ceramic materials, powder-based AM technologies result in porous ceramic parts, provided they are not infiltrated. CerAMing GmbH unites the advantages of powder-based processes with the production of dense ceramic by means of the Layerwise Slurry Deposition. By using a suspension, a high packing density of the powder bed is achieved which leads to high green body densities. Due to this advantage the approach overcomes the problems of other powder-based AM technologies. Furthermore, a very economical debinding time allows the production of parts with high wall thicknesses. KW - Additive Manufacturing KW - Binder Jetting KW - Layerwise Slurry Deposition KW - Lithography-based technologies KW - Technical Ceramics PY - 2021 SP - 49 EP - 52 PB - Göller Verlag CY - Baden-Baden AN - OPUS4-52948 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Bestimmung der Partikelgrößenverteilung mittels Zentrifugen-Sedimentationsverfahren nach ISO 13318-2 (Küvette) N2 - Im Vortrag werden das Messprinzip des Zentrifugen-Sedimentationsverfahrens erläutert und die Anforderungen der zugrundeliegenden Normen diskutiert. Es schließen sich umfangreiche Ausführungen zur praktischen Durchführung der Messung, insbesondere auch zu den vorbereitenden Arbeiten, sowie zur Auswertung der Rohdaten an. Gezeigt werden die Validierung sowie ein Beispiel zur regelmäßigen Verifizierung des Verfahrens. Nach Beispielen und Vergleichen zu Ergebnissen mit anderen Messverfahren, wird das Verfahren in einer Zusammenfassung bewertet. T2 - Seminar Rheologie und Stabilität von dispersen Systemen CY - Potsdam, Germany DA - 09.05.2022 KW - Nano powder KW - Cetrifugal Liquid Sedimentation CLS KW - Particle size determination PY - 2022 AN - OPUS4-54863 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönauer-Kamin, Daniela T1 - Powder-Aerosol deposited (PAD) calcium manganate as n-type thermoelectric material N2 - Currently, calcium manganate CaMnO3 and calcium cobaltite Ca3Co4O9 are being investigated as n-type resp. p-type semiconducting materials as oxidation- and temperature-resistant thermoelectric materials for oxide multilayer thermoelectric generators (TEGs). In order to manufacture multilayer TEGs, pressure-assisted sintering processes at high temperatures are necessary to achieve optimal thermoelectric material properties. To realize TEGs in planar film technology, another method to obtain dense ceramic layers directly from the synthesized starting powders without a subsequent high temperature step is emerging recently: the powder aerosol deposition (PAD) method. In the present work, it is investigated whether PAD is suitable to produce dense ceramic films from Sm-doped CaMnO3 and Ca3Co4O9 powders. The resulting thermoelectric properties are characterized as a function of temperature. CaMnO3 powder could successfully be processed by PAD with resulting layer thicknesses of 5- 6 µm without any high-temperature sintering steps of the films. The electrical conductivity and the Seebeck coefficient of the films were determined in-plane from room temperature to 600 °C in air. The results show a Seebeck coefficient of around -200 µV/K, which is comparable to results of pressed and sintered bars. At 400 °C, the electrical conductivity corresponds to the conductivity of the bar. At higher temperatures the conductivity is better than with the reference. Below 400°C, the electrical conductivity is somewhat lower than that of the reference sample, a mild thermal treatment of the PAD layer improves it. It is expected that the thermal conductivity of the PAD film will be lower compared to the bars due to the nano-crystalline film morphology. This should result in a significantly increased ZT value for the PAD layers and a higher efficiency of the TEG. The work shows that both CaMnO3 and Ca3Co4O9 can be successfully processed by PAD, and the PAD films show comparable thermoelectric properties. T2 - 18th European Conference on Thermoelectrics CY - Barcelona, Spanien DA - 14.09.2022 KW - Film depositition KW - Calcium cobaltite PY - 2022 AN - OPUS4-55771 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Junge, P. A1 - Stargardt, Patrick A1 - Kober, D. A1 - Greinacher, M. A1 - Rupprecht, C. T1 - Thermally Sprayed Al2O3 Ceramic Coatings for Electrical Insulation Applications N2 - Thermal spraying enables a fast and propelling way to additively deposit various ceramics as electric insulators, which are used in conditions where polymers are not suitable. Alumina (Al2O3) is among the most employed materials in the coating industry since it exhibits good dielectric properties, high hardness, high melting point while still being cost-effective. Various parameters (e.g. feedstock type, plasma gas mixture, plasma power) significantly influence the resulting coating in terms of microstructure, porosity, crystallinity, and degree of un-or molten particles. As a consequence, these parameters need to be investigated to estimate the impact on the electrical insulating properties of thermally sprayed alumina. This study focuses on the development of a novel electric insulation coating from Al2O3 feedstock powders deposited via atmospheric plasma spray (APS). The microstructure, porosity, and corresponding crystallographic phases have been analyzed with optical microscopy, XRD, and SEM images. To achieve an understanding of the parameters influencing the electrical insulation performance of the manufactured coatings, an in-depth analysis of the fundamental dielectric parameters e.g., DC resistance, breakdown strength, dielectric loss tangent, permittivity is presented. T2 - International Thermal Spray Conference and Exposition 2022 CY - Vienna, Austria DA - 04.05.2022 KW - Thermal Spray KW - Alumina KW - Dielectric properties PY - 2022 SP - 1 EP - 8 AN - OPUS4-55821 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Oxidkeramische Werkstoffe und Folien für thermoelektrische Multilayergeneratoren N2 - Thermoelektrische Effekte beschreiben die direkte Verknüpfung von thermischer Energie und elektrischer Energie in Festkörpern. Durch Thermodiffusionsströme entsteht direkt, ohne beweg¬liche Teile, ein elektrisches Feld als Folge einer Temperaturdifferenz. Diese Material-eigenschaft wird durch den Seebeckkoeffizienten beschrieben. Je nach Art der Ladungs¬träger sind die indu¬zierte Spannung und der Seebeckkoeffizient positiv (p-Typ) oder negativ (n-Typ). Thermo¬elek¬trische Effekte lassen sich beispielsweise in Thermo¬elementen zur Temperatur-messung, in Pel¬tierelementen zum Kühlen oder Heizen und in thermo¬elektrischen Generatoren zur Umwandlung von thermischer Energie in elektrische Energie nutzen. In thermoelektrischen Generatoren werden Schenkel aus p-Typ- und n-Typ-Materialien elek-trisch in Reihe und thermisch parallel verschaltet. Konventionell werden einzelne Schenkel aus Bismut¬tellurid auf ein metallisiertes Substrat gelötet. Man spricht vom π-Typ-Design. Aufgrund auf¬wendiger Fertigung und nicht optimaler Flächennutzung stellt dieses Design nicht die best-mög¬liche Lösung dar. Neben Telluriden gibt es noch andere vielversprechende thermoelektrische Material¬systeme wie die oxidischen Thermoelektrika. Im Temperatur¬bereich oberhalb von 700 °C können oxidische thermoelektrische Materialien mit nichtoxidischen konkurrieren. Zudem sind sie oxidationsbeständig und können aus weniger toxischen und besser verfügbaren Rohstoffen her¬ge¬stellt werden. Da es sich um keramische Materialien handelt, können unter Nutzung der Multi¬layer¬technologie (auch Vielschicht- oder Mehrlagentechnik) Generatoren im Multilayer¬design hergestellt werden. Keramische Multi¬layer¬generatoren sind aufgrund der höheren Leis¬tungs¬dichte, der Möglichkeit der gezielten Texturierung und des hohen möglichen Auto¬mati¬sierungs¬grades des Herstellungs¬prozesses eine viel¬versprechende Alternative zu konven¬tionellen π-Typ-Generatoren. Alle Lagen werden in einem Schritt co-gesintert. Die beiden zum jetzigen Zeit¬punkt wohl viel¬versprechendsten oxi¬dischen Thermoelektrika sind Calcium-cobaltit Ca3Co4O9 als p-Typ und Calciummanganat CaMnO3 als n-Typ. Die Sinter¬tem¬peratur von Ca3Co4O9 ist durch eine Phasenumwandlung bei 926 °C beschränkt. Texturiertes, dichtes Ca3Co4O9 mit einer hohen Festigkeit kann nur über Hei߬pressen hergestellt werden. Das Co-Sintern von Ca3Co4O9 und CaMnO3 war wegen der Tem¬pera¬tur¬differenz von 350 K zwischen den jeweiligen Sinterintervallen bisher nicht möglich. Ziel dieser Arbeit war deshalb die Ent¬wick¬lung von kompatiblen oxidkeramischen Werkstoffen und Folien für thermoelektrische Multilayer-generatoren auf der Basis von Ca3Co4O9 und CaMnO3. Daraus resultieren vier wesentliche Arbeitspakete. Zunächst die Materialentwicklungen von Ca3Co4O9 (p-Typ) und CaMnO3 (n-Typ) für ein Co-Sintern bei 900 °C mit akzeptablen thermoelek¬trischen Eigenschaften, dann die Entwicklung der weiteren im Generator benötigten Kompo¬nenten wie der Isolationsschicht und abschließend die Fertigung und Bewertung von Demonstra¬toren im Multi¬layer¬design. Foliengießen und druckunterstütztes Sintern ermöglichen die Herstellung von dichtem, tex-turier¬tem Ca3Co4O9 mit hoher Festigkeit und hohem Leistungsfaktor. Letzterer ist das Produkt der elek¬trischen Leitfähigkeit und dem Quadrat des Seebeckkoeffizienten. Für die elektrische Leit¬fähigkeit zeigte sich in dieser Arbeit ein kombinierter Einfluss von Sinterdichte und Textur. Die thermo¬elektrischen Eigen¬schaften lassen sich somit über die Einstellung der Mikrostruktur gezielt steuern. Durch die Optimierung der Pulversynthese, die Einführung des Sinteradditives CuO und die Kombi¬nation mit dem druckunterstützten Sintern (7,5 MPa) konnte die Sintertemperatur des CaMnO3 bei gleichbleibendem Leistungsfaktor von 1250 °C auf 950 °C gesenkt werden. Druck-unter¬stütztes Sintern von CaMnO3 ist bei 900 °C möglich, führt aber zu einem Werkstoff mit geringerem Leistungsfaktor, geringerer Dichte und ungenügender Festigkeit. Zur elektrischen Isolation der beiden thermoelektrischen Materialien wurde ein Glas-Keramik-Kompo¬sit mit hohem Volumenwiderstand und angepasstem Wärmeausdehnungs¬koef¬fizienten ent¬wickelt. Aus den zu Folien vergossenen thermoelektrischen Materialien, der siebgedruckten Iso¬lations-schicht und der siebgedruckten Metallisierung wurden mittels Multilayertech¬nologie De¬mons-tratoren hergestellt. Neben dem pn-Generator aus Ca3Co4O9 und CaMnO3 wurden auch Unileg-generatoren aus Ca3Co4O9 gefertigt. Bei Unileggeneratoren wird die Komplexität des Aufbaus durch die Verwendung von nur einem thermoelektrischen Material verringert. Die Simulation der Demonstratoren zeigte, dass der pn-Generator aus Ca3Co4O9 und CaMnO3 keine höheren Leis-tungsdichten erbringt als der aus nur Ca3Co4O9 bestehende Unileg¬generator. Auf¬grund des ge-ringen Leistungsfaktors und der geringen Festigkeit des bei 900 °C gesinterten CaMnO3 er¬scheint die Fertigung von pn-Multilayer¬generatoren aus Ca3Co4O9 und CaMnO3 derzeit nicht sinn¬voll. Die Unileg¬generatoren aus Ca3Co4O9 erreichen mit sehr hoher Reproduzier¬barkeit 2 mW/cm² bei einer Temperaturdifferenz von 230 K, dies entspricht 80 % der simulierten elektrischen Leistung. Es handelt sich hierbei um den ersten Machbarkeits¬nachweis zur Herstellung von Multilayer-generatoren auf Basis von texturiertem Ca3Co4O9 mit hohem thermoelektrischem Leistungsfaktor, hoher Dichte und hoher Festigkeit. Solch thermoelektrische Multilayergeneratoren könnten zukünftig Systeme mit geringen elek-trischen Leistungsanforderungen wie Sensoren autark und nachhaltig mit elektrischer Energie ver¬sorgen. T2 - Promotionskolloquium CY - Bayreuth, Germany DA - 25.04.2022 KW - Calciumcobaltit KW - Calciummanganat KW - Foliengießen KW - Sintertemperatur PY - 2022 AN - OPUS4-54726 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönauer-Kamin, D. T1 - Powder Aerosol deposited (PAD) calcium cobaltite as textured p type thermoelectric material N2 - Oxide thermoelectric semiconducting materials like p-type calcium cobaltite Ca3Co4O9 are investigated as oxidation- and temperature-resistant thermoelectric materials for thermoelectric generators (TEGs). To realize TEGs in planar film technology, the powder aerosol deposition (PAD) method is emerging recently. PAD is a method to obtain dense ceramic films directly from the synthesized starting powders without a subsequent high temperature step. In the present work, Ca3Co4O9 (CCO) powders are processed by PAD to ceramic films at room temperature. The thermoelectric properties of the films (film thickness 10 – 20 µm) are characterized from room temperature to 900°C. Additionally, the layer morphology and texture of the films will be investigated. As result, the Seebeck coefficient of the CCO-PAD film is comparable to pressed and sintered CCO-bulk materials during the 1st heating cycle to 900°C. The morphology of the films after the thermal treatment shows strong aligned crystallites resulting in a strong texture of the films. The electrical conductivity increases strongly during the 1st heating cycle to 900°C and stays almost constant afterwards. Compared to CCO-bulks, the films provide higher electrical conductivity which could be explained by the oriented crystal growth in-plane direction of the film. The relationship between thermoelectric properties and layer morphology as a function of thermal annealing parameters will be further investigated. T2 - KERAMIK 2023 / 98. DKG-Jahrestagung CY - Jena, Germany DA - 27.03.2023 KW - Layer depostion KW - Texture KW - Heat treatment PY - 2023 AN - OPUS4-57285 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Höhne, Patrick T1 - Optimized spray granules for dry pressing by means of slurry destabilization and ultrasonic atomization N2 - The homogeneous introduction of organic additives is a prerequisite for good processability of ceramic powders during dry pressing. The addition of organic additives by wet route via ceramic slurries offers advantages over dry processing. The organic content can be reduced and a more homogeneous distribution of the additives on the particle surface is achieved. In addition to the measurements of zeta potential and viscosity, sedimentation analysis by optical centrifugation was also tested and successfully used to characterize the ceramic slurries and accurately evaluate of the suitability of different types, amounts, and compositions of organic additives. Spray drying of well-stabilized slurries usually results in mostly hollow granules with a hard shell leading to sintered bodies with defects and reduced strength and density. By purposefully degrading the slurry stability after dispersion of the ceramic powder, the drying behavior of the granules in the spray drying process and thus the granule properties can be influenced. Destabilization of the slurry and thus partial flocculation was quantified by optical centrifugation. Spray drying of the destabilized alumina slurries resulted in "non-hollow" granules without the detrimental hard shell and thus improved granule properties. Further improvement of the granules was achieved by installing ultrasonic atomization in the spray dryer. A narrower granule size distribution was achieved, which had a positive effect on, among other things, the flowability of the granules. Specimens produced from this granules had fewer defects of smaller size, leading to better results for the density and strength of the sintered bodies. The observations made for alumina could be transferred to zirconia and as well to ZTA with 20 wt% zirconia. T2 - Ceramics in Europe 2022 CY - Krakau, Poland DA - 10.07.2022 KW - Ultrasound KW - Spray drying KW - Slurry PY - 2022 AN - OPUS4-56171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Junge, P. A1 - Greinacher, M. A1 - Kober, D. A1 - Stargardt, Patrick A1 - Rupprecht, C. T1 - Metastable Phase Formation, Microstructure, and Dielectric Properties in Plasma-Sprayed Alumina Ceramic Coatings N2 - The need for new solutions for electrical insulation is growing due to the increased electrification in numerous industrial sectors, opening the door for innovation. Plasma spraying is a fast and efficient way to deposit various ceramics as electrical insulators, which are used in conditions where polymers are not suitable. Alumina (Al2O3) is among the most employed ceramics in the coating industry since it exhibits good dielectric properties, high hardness, and high melting point, while still being cost-effective. Various parameters (e.g., feedstock type, spray distance, plasma power) significantly influence the resulting coating in terms of microstructure, porosity, and metastable phase formation. Consequently, these parameters need to be investigated to estimate the impact on the dielectric properties of plasma-sprayed alumina coatings. In this work, alumina coatings with different spray distances have been prepared via atmospheric plasma spray (APS) on copper substrates. The microstructure, porosity, and corresponding phase formation have been analyzed with optical microscopy, X-ray diffraction (XRD), and scanning electron microscopy (SEM). Moreover, we present an in-depth analysis of the fundamental dielectric properties e.g., direct current (DC) resistance, breakdown strength, dielectric loss tangent, and permittivity. Our results show that decreasing spray distance reduces the resistivity from 6.31 × 109 Ωm (130 mm) to 6.33 × 108 Ωm (70 mm), while at the same time enhances the formation of the metastable δ-Al2O3 phase. Furthermore, space charge polarization is determined as the main polarization mechanism at low frequencies. KW - Alumina KW - Plasma spray KW - Dielectric properties PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564394 DO - https://doi.org/10.3390/coatings12121847 SN - 2079-6412 VL - 12 SP - 1 EP - 15 PB - MDPI CY - Basel AN - OPUS4-56439 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Lena T1 - Additive Fertigung unter Mikrogravitationsbedingungen für Anwendungen im Weltraum N2 - Präsentation der Aktivitäten an der BAM im Bereich Additive Fertigung unter Mikrogravitationsbedingungen für Anwendungen im Weltraum beim Arbeitsgruppentreffen der AG Werkstoffe & Prozesse vom Netzwerk Space2Motion. T2 - Arbeitsgruppentreffen beim Netzwerk Space2Motion CY - Online meeting DA - 09.11.2022 KW - Additive Fertigung KW - Mikrogravitation PY - 2022 AN - OPUS4-56353 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saber, Yassin A1 - Clague, Leighton T1 - Automated Fused Filament Fabrication of Ceramics and Metals - Remote and in Space N2 - Component manufacturing in remote (i.e., geographically isolated) settings poses significant challenges where access to conventional manufacturing facilities is limited or non-existent. Fused Filament Fabrication (FFF) enables the rapid manufacturing of plastic, metallic and ceramic components with complex geometries. Ceramic and metallic parts formed by FFF require subsequent debinding and sintering to reach full density. Debinding and sintering are typically executed in separate steps with different equipment, necessitating extensive human handling which hinders process automation and may be challenging for the operator in isolated environments. Here an innovative approach is presented: the integration of all process steps into a single, fully automated system, streamlining the process and minimizing human involvement. Our system combines a dual extrusion filament printer with a porous and heat-resistant ceramic print bed. The porous print bed enables mechanical interlocking of the first printed layers, ensuring adhesion and structural integrity during FFF. Ceramic and metallic parts are printed onto thin sacrificial rafts, which are built using an interface material with the same binder as the loaded filament. After the print is completed, the heat-resistant print bed with all parts is transferred seamlessly with a carrier system into a high-temperature furnace for debinding and sintering. During sintering the sacrificial raft is disintegrated, allowing for unconstrained sintering and easy removal of the finished parts. In conclusion, our integrated approach enables significant advancements in the fabrication of complex ceramic or metallic components in remote environments with increased efficiency and minimal human handling. T2 - AM Forum 2025 CY - Berlin, Germany DA - 17.03.2025 KW - Fused Filament Fabrication KW - Ceramics KW - Metalls KW - Process automation PY - 2025 AN - OPUS4-62745 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Siefke, Lennart A1 - Linden, Anna T1 - Towards a robust automated surface inspection method for CT-scanned cannulas N2 - For certain cardiovascular diseases, cannulas are implanted into the blood circuit. To match the patients individual anatomy of the heart, there is research for cannulas to be custom-designed and manufactured aided by 3D printing. However, cannulas have to hold very high standards with regard to the smoothness of their surfaces, as rough patches can lead to formation of blood clots. Therefore, this work uses computer vision to detect such patches as part of quality assurance. First, the produced cannula is scanned using a precise CT scanner and transformed into a 3D mesh object. Rough patches in an otherwise smooth but curved surface are detected by using cosine similarity between neighboring faces and a statistical evaluation. In the end, this method is able to raise a warning when curved surfaces are not smooth enough and visualizes the problematic patches. However, there is just limited access to test data currently and the scanner used needs to be upgraded. T2 - 3D in Science & Applications (3D-iSA) 2024 CY - Berlin, Germany DA - 26.11.2024 KW - Algorithm KW - Additive manufacturing KW - Surface evaluation PY - 2025 UR - https://www.gfai.de SN - 978-3-942709-34-7 SP - 66 EP - 70 AN - OPUS4-63057 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 - 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 - TY - JOUR A1 - Hildebrand, G. A1 - Sänger, Johanna Christiane A1 - Schirmer, U. A1 - Mantei, W. A1 - Dupuis, Y. A1 - Houbertz, R. A1 - Liefeith, K. T1 - Process Development for Additive Manufacturing of Alumina Toughened Zirconia for 3D Structures by Means of Two-Photon Absorption Technique N2 - Additive manufacturing is well established for plastics and metals, and it gets more and more implemented in a variety of industrial processes. Beside these well-established material platforms, additive manufacturing processes are highly interesting for ceramics, especially regarding resource conservation and for the production of complex three-dimensional shapes and structures with specific feature sizes in the µm and mm range with high accuracy. The usage of ceramics in 3D printing is, however, just at the beginning of a technical implementation in a continuously and fast rising field of research and development. The flexible fabrication of highly complex and precise 3D structures by means of light-induced photopolymerization that are difficult to realize using traditional ceramic fabrication methods such as casting and machining is of high importance. Generally, slurry-based ceramic 3D printing technologies involve liquid or semi-liquid polymeric systems dispersed with ceramic particles as feedstock (inks or pastes), depending on the solid loading and viscosity of the system. This paper includes all types of photo-curable polymer-ceramic-mixtures (feedstock), while demonstrating our own work on 3D printed alumina toughened zirconia based ceramic slurries with light induced polymerization on the basis of two-photon absorption (TPA) for the first time. As a proven exemplary on cuboids with varying edge length and double pyramids in the µm-range we state that real 3D micro-stereolithographic fabrication of ceramic products will be generally possible in the near future by means of TPA. This technology enables the fabrication of 3D structures with high accuracy in comparison to ceramic technologies that apply single-photon excitation. In sum, our work is intended to contribute to the fundamental development of this technology for the representation of oxide-ceramic components (proof-of-principle) and helps to exploit the high potential of additive processes in the field of bio-ceramics in the medium to long-term future. KW - Additive manufacturing KW - Ceramics 3D printing KW - Two-photon adsorption KW - Polymer-ceramic mixtures KW - Bio-ceramic engineering PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526672 DO - https://doi.org/10.3390/ceramics4020017 VL - 4 IS - 2 SP - 224 EP - 239 PB - MDPI CY - Basel AN - OPUS4-52667 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Bestimmung der Partikelgrößen-verteilung mittels Zentrifugen-Sedimentationsverfahren nach ISO 13318-2 (Küvette) N2 - Im Vortrag werden das Messprinzip einer Photozentrifuge erläutert und die Anforderungen der zugrundeliegenden Normen diskutiert. Die praktische Durchführung der Messung und insbesondere auch die vorbereitenden Arbeiten, sowie die Auswertung der Rohdaten bilden den Schwerpunkt des Vortrags. Gezeigt werden auch die Validierung sowie ein Beispiel zur regelmäßigen Verifizierung des Verfahrens. Nach Anwendungsbeispielen und Vergleichen zu Ergebnissen mit anderen Messverfahren, wird das Verfahren in einer Zusammenfassung bewertet. T2 - Seminar Rheologie und Stabilität von dispersen Systemen CY - Potsdam, Germany DA - 08.05.2023 KW - CLS KW - Particle size KW - Nano PY - 2023 AN - OPUS4-57679 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lindemann, Franziska T1 - Bestimmung der spezifischen Oberfläche mittels Gasadsorption (BET-Verfahren) N2 - Im Rahmen des 2. BAM-Akademie Info-Tages "Nano or not Nano" wurde die OECD TG 124 "Volume Specific Surface Area of Manufactured Nanomaterials" vorgestellt. Der Vortrag beschreibt die Bestimmung der spezifischen Oberfläche von dispersen und/oder porösen Pulvern mittels Gasadsorption nach dem BET-Verfahren. Es wird auf die Anwendbarkeit der Methode eingegangen und es werden praktische Hinweise zur Probenvorbereitung und Messung von Nanomaterialien gegeben. T2 - BAM Akademie II: Info-Tage "Nano or not Nano" CY - Online meeting DA - 25.01.2024 KW - OECD TG 124 KW - Nanopulver KW - VSSA KW - Nano powder KW - BET KW - Spezifische Oberfläche PY - 2024 AN - OPUS4-59623 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Bestimmung der Skelettdichte mittels Gaspyknometrie N2 - Im Rahmen des 2. BAM-Akademie Info-Tages "Nano or not Nano" wurde die OECD TG 124 "Volume Specific Surface Area of Manufactured Nanomaterials" vorgestellt. Der Vortrag beschreibt detailliert das Messverfahren der He-Gaspyknometrie zur Bestimmung der Skelettdichte von Pulvern und geht auf Anwendbarkeit, Besonderheiten bei Nanopulvern und wichtige Einstellparameter für die Messung ein. T2 - BAM Akademie II: Info-Tage "Nano or not Nano" CY - Online meeting DA - 25.01.2024 KW - Pycnometry KW - Density KW - Nano powder PY - 2024 AN - OPUS4-59561 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Einführung: Volume Specific Surface Area (VSSA) N2 - Im Rahmen der 2. BAM-Akademie-Veranstaltung "Nano or not Nano" wurde die OECD TG 124 "Volume Specific Surface Area of Manufactured Nanomaterials" vorgestellt. Der Vortrag enthält ein Einführung zur VSSA mit Definitionen, Vorteilen und Einschränkungen. T2 - BAM Akademie II: Info-Tage "Nano or not Nano" CY - Online meeting DA - 25.01.2024 KW - Nano powder KW - VSSA KW - Specific surface KW - OECD TG PY - 2024 AN - OPUS4-59560 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Herausforderungen bei der Granulometrie von (technischen) Nano-Pulvern N2 - Einführungsvortrag im Rahmen der Veranstaltung der BAM-Akademie zur Anwendung der OECD TG 124 "Volume Specific Surface Area of Manufactured Nanomaterials" zu Herausforderungen bei der Granulometrie von Nanopulvern. Es werden die Einflüsse von Partikelform, Breite der Partikelgrößenverteilung und Agglomeration/ Aggregation auf das Messergebnis sowie die Vergleichbarkeit der Ergebnisse verschiedener Messverfahren dargelegt. T2 - BAM Akademie II: Info-Tage "Nano or not Nano" CY - Online meeting DA - 25.01.2024 KW - Nanopulver KW - Granulometrie KW - Partikelgröße KW - VSSA KW - OECD TG 124 PY - 2024 AN - OPUS4-59558 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Dynamische Lichtstreuung DLS nach ISO 22412:2017 N2 - Einführung in die Partikelgrößenbestimmung von Nano-Materialien mittels Dynamischer Lichtstreuung. Normative Grundlagen (ISO 22412 und OECD TG 125); Messprinzip, Auswertealgorithmen, Informationsgehalt der Daten, Metadaten, Reporting. T2 - BAM Akademie: Info-Tage "NANO OR NOT NANO" CY - Online meeting DA - 16.02.2023 KW - DLS KW - Particle size KW - Nano PY - 2023 AN - OPUS4-57128 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Exkurs Partikelgrößenverteilungen N2 - Einführung in die Darstellung der Ergebnisse von Partikelgrößenbestimmungen: Was ist ein Kugeläquivalenzdurchmesser; welche Bedeutung hat die gemessene Mengenart; welche Parameter werden ausgewiesen. Bezug zu Regularien hinsichtlich der Bewertung "Nano- oder nicht Nano-Material. T2 - BAM Akademie: Info-Tage "NANO OR NOT NANO" CY - Online meeting DA - 16.02.2023 KW - Nano material KW - Particle size KW - Size distribution PY - 2023 AN - OPUS4-57127 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Zentrifugen Sedimentationsverfahren CLS nach ISO 13318 2:2007 N2 - Einführung in die Bestimmung der Partikelgröße von Nano-Materialien mittels Zentrifugen Sedimentationsverfahren CLS nach ISO 13318 2:2007. Normative Grundlagen (einschließlich OECD TG 125), Messprinzip, Auswertung, Vor- und Nachteile der Methode, Metadaten, Reporting. T2 - BAM Akademie: Info-Tage "NANO OR NOT NANO" CY - Online meeting DA - 16.02.2023 KW - CLS KW - Particle size KW - Nano PY - 2023 AN - OPUS4-57129 LA - deu 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 - GEN A1 - Kuchenbecker, Petra A1 - Lindemann, Franziska T1 - Particle size determination of a commercially available CeO2 nano powder - SOPs and reference data N2 - Compilation of detailed SOPs for characterization of a commercially available CeO2 nano powder including - suspension preparation (indirect and direct sonication), - particle size determination (Dynamic Light Scattering DLS and Centrifugal Liquid Sedimentation CLS) with reference data, respectively. For sample preparation and analysis by Scanning Electron Microscopy (SEM) of this powder see related works (submitted, coming soon). KW - Wet dispersion KW - Nano powder KW - Particle size KW - CeO2 KW - Ceria KW - DLS KW - CLS PY - 2023 DO - https://doi.org/10.5281/zenodo.10061079 PB - Zenodo CY - Geneva AN - OPUS4-58785 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kuchenbecker, Petra A1 - Lindemann, Franziska T1 - SOP and reference data for determination of the Volume-specific Surface Area (VSSA) of a commercially available CeO2 nano powder N2 - Detailed SOP and reference data for the determination of the VSSA of a commercially available CeO2 nano powder: specific (BET-) Surface Area by gas adsorption (Ar and N2) skeletal (true solid state) density by gas pycnometry. Estimation of the particle size by VSSA screening method. KW - Nano powder KW - VSSA KW - Volume specific surface area KW - Screening method KW - Ceria KW - CeO2 PY - 2023 DO - https://doi.org/10.5281/zenodo.10061235 PB - Zenodo CY - Geneva AN - OPUS4-58786 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Linden, Anna T1 - AMVAD - Additive manufacturing for ventricular assist devices N2 - Some children are born with a univentricular heart, meaning their heart has only one pumping chamber instead of two. To improve circulation, patients often undergo the Fontan procedure, which reroutes blood flow — but this can put stress on other organs. In some cases, ventricular assist devices, or VADs, are used to support the heart’s pumping function. This involves an artificial pump connected directly to the patient's heart via silicone-based cannulas. Unique anatomical conditions introduce special challenges for cannula geometry. Additive manufacturing offers innovative solutions by enabling the production of personalized medical devices. The aim of the project is to develop the manufacturing workflow for the individualized cannula from digital imaging of the patient and customized design to additive manufacturing. Besides technical feasibility, validating the entire process is crucial for regulatory approval. The selection and testing of suitable additive manufacturing processes and biocompatible materials for individualized silicone cannulas, ensuring compliance with quality standards for high-risk medical products, will be presented. T2 - AMBER Spotlight On: 3D Printing meets Health & Biotech CY - Berlin, Germany DA - 16.09.2025 KW - Additive manufacturing KW - Medical device KW - Liquid silicone rubber PY - 2025 AN - OPUS4-64101 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Clozel, Melanie A1 - Neumann, Christian A1 - Thore, Johannes A1 - Kolbe, Matthias A1 - Yang, Fan A1 - Gutowski, Olof A1 - Dippel, Ann-Christin A1 - Ruschel, Lucas M. A1 - Busch, Ralf A1 - Altenbach, Christoph A1 - Akuata, Chijioke Kenneth A1 - Zander, Daniela A1 - Wilbig, Janka A1 - Meyer, Andreas T1 - Microstructure formation during gas flow-assisted additive manufacturing of a metallic glass powder on ground and in microgravity N2 - We studied bulk metallic glasses produced from gas flow-assisted laser-based powder bed fusion process, which is capable of additive manufacturing metallic parts in microgravity. A Zr-based bulk metallic glass composition Zr₅₉ˏ₃Cu₂₈ˏ₈Al₁₀ˏ₄Nb₁ˏ₅ has been processed on ground and in microgravity in a compact sounding rocket payload MARS-M. Microstructure characterization was performed using electron microscopy and X-ray diffraction computed tomography, which cope with small amounts of sample materials, especially for those fabricated under microgravity conditions. Very similar microstructures and crystalline fractions are observed in sample manufactured on ground and in microgravity, which shows that process parameters of conventional laser powder bed fusion for manufacturing metallic glasses can be transferred to the processes in microgravity. Two different origins of crystallization have been identified in the Zr₅₉ˏ₃Cu₂₈ˏ₈Al₁₀ˏ₄Nb₁ˏ₅ sample. The preferred occurrence of CuZr₂ at the interlayer boundaries is likely a result of recrystallization from the undercooled melt and hence associated with laser scanning strategy. In contrast, the more uniformly distributed Al₃Zr₄ phase is considered to be triggered by the formation of Cu₂Zr₄O. Thus, for the fabrication of fully amorphous builds both on ground and in space, our findings point to higher scanning speeds and lower oxygen contents, while the latter can also be used to tune the crystalline fractions in the sample. KW - Gas flow-assisted laser-based powder bed fusion KW - Microgravity KW - Glass-forming alloys KW - X-ray diffraction tomography PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641253 DO - https://doi.org/10.1007/s40964-025-01275-2 SN - 2363-9512 SP - 1 EP - 14 PB - Springer Science and Business Media LLC CY - Cham, Switzerland AN - OPUS4-64125 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Panzier, Nicole A1 - Zocca, Andrea T1 - Silikatkeramik und Hochleistungskeramik aus dem 3-D-Druck N2 - In diesem Artikel werden die verschiedenen additiven Fertigungsverfahren und ihre Anwendungsmöglichkeiten vorgestellt. Der Fokus liegt hierbei auf Silikatkeramik. Für jedes 3D Druckverfahren werden die Möglichkeiten mit Silikatkeramik, Hochleistungskeramik und Dentalkeramik aufgezeigt. Auf den Nutzen der verschiedenen 3D Druckverfahren für industrielle Anwendungen, den privaten Bereich, sowie die Verwendung für Kunst und Design wird eingegangen. Das Potenzial der Additiven Fertigung wird auch für den Bereich der Keramik in der dentalen Anwendung bewertet. KW - Additive Fertigung KW - 3D Druck KW - Silikatkeramik KW - Hochleistungskeramik PY - 2022 UR - https://www.quintessence-publishing.com/deu/de/article/3634513/quintessenz-zahntechnik/2022/12/silikatkeramik-und-hochleistungskeramik-aus-dem-3-d-druck SN - 0340-4641 VL - 48 IS - 12 SP - 1260 EP - 1268 PB - Quintessence Publ. CY - Berlin AN - OPUS4-56792 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Franchin, G. A1 - Zocca, Andrea A1 - Karl, D. A1 - Yun, H. A1 - Tian, X. T1 - Editorial: Advances in additive manufacturing of ceramics N2 - 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. KW - Additive manufacturing KW - Ceramic PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549361 DO - https://doi.org/10.1016/j.oceram.2022.100277 SN - 2666-5395 VL - 10 SP - 1 EP - 2 PB - Elsevier CY - Amsterdam AN - OPUS4-54936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Salari, Farid A1 - Zocca, Andrea A1 - Bosetti, Paolo A1 - Hlaváček, Petr A1 - Italiano, Antonino A1 - Gobbin, Filippo A1 - Colombo, Paolo A1 - Kühne, Hans-Carsten A1 - Sglavo, Vincenzo M. T1 - Powder-bed 3D printing by selective activation of magnesium phosphate cement: Determining significant processing parameters and their effect on mechanical strength N2 - The present work addresses powder bed binder jetting additive manufacturing by selective magnesium phosphate cement activation. Despite the potential of this technology to aid the digitalization of the construction industry, the effect of processing parameters on the mechanical performance of printed materials has not yet been studied to generate a guideline for the further development of the technology. Statistical methodologies were used to screen the effect of four printing process parameters (printing speed, layer thickness, raster angle, and build direction on flexural and compressive strength). As the exploited technology works with constant fluid pressure, the physical interpretation of the effect of each factor can be considered taking into account the interactions between the binder materials in the powder bed. Analysis of variance (ANOVA) indicated that printing speed and layer thickness significantly affect mechanical performances. Furthermore, the layout of samples for the printing process is preferable to be parallel the printhead movement. An anisotropic behavior was observed, and the samples subjected to compressive forces parallel to the layer plane possessed lower strength values. This effect can be interpreted as a result of a weak area of low density in between layers, leading to a pronounced delamination under compression. Even though the strength of the printed material is not suitable for a structural concrete, it can be marginally improved by design of experiment and optimized for non-structural applications, such as for porous artificial stone. Design of experiment coupled with ANOVA methods can be used in the future to support the development of novel material mixtures, thus expanding the fields of application of this novel additive manufacturing technology. KW - Concrete 3D-printing KW - Particle-bed binder jetting KW - Design of experiment PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601654 DO - https://doi.org/10.1016/j.oceram.2024.100609 VL - 18 SP - 1 EP - 11 PB - Elsevier B.V. AN - OPUS4-60165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xu, F. A1 - Ren, H. A1 - Zheng, M. A1 - Shao, X. A1 - Dai, T. A1 - Wu, Y. A1 - Tian, L. A1 - Liu, Y. A1 - Liu, B. A1 - Günster, Jens A1 - Liu, Y. A1 - Liu, Y. T1 - Development of biodegradable bioactive glass ceramics by DLP printed containing EPCs/BMSCs for bone tissue engineering of rabbit mandible defects N2 - Bioactive glass ceramics have excellent biocompatibility and osteoconductivity; and can form direct chemical bonds with human bones; thus, these ceramic are considered as “Smart” materials. In this study, we develop a new type of bioactive glass ceramic (AP40mod) as a scaffold containing Endothelial progenitor cells (EPCs) and Mesenchymal stem cells (BMSCs) to repair critical-sized bone defects in rabbit mandibles. For in vitro experiments: AP40mod was prepared by Dgital light processing (DLP) system and the optimal ratio of EPCs/BMSCs was screened by analyzing cell proliferation and ALP activity, as well as the influence of genes related to osteogenesis and angiogenesis by direct inoculation into scaffolds. The scaffold showed suitable mechanical properties, with a Bending strength 52.7 MPa and a good biological activity. Additionally, when EPCs/BMSCs ratio were combined at a ratio of 2:1 with AP40mod, the ALP activity, osteogenesis and angiogenesis were significantly increased. For in vivo experiments: application of AP40mod/EPCs/BMSCs (after 7 days of in vitro spin culture) to repair and reconstruct critical-sized mandible defect in rabbit showed that all scaffolds were successfully accurately implanted into the defect area. As revealed by macroscopically and CT at the end of 9 months, defects in the AP40mod/EPCs/BMSCs group were nearly completely covered by normal bone and the degradation rate was 29.9% compared to 20.1% in the AP40mod group by the 3D reconstruction. As revealed by HE and Masson staining analyses, newly formed blood vessels, bone marrow and collagen maturity were significantly increased in the AP40mod/EPCs/BMSCs group compared to those in the AP40mod group. We directly inoculated cells on the novel material to screen for the best inoculation ratio. It is concluded that the AP40mod combination of EPCs/BMSCs is a promising approach for repairing and reconstructing large load bearing bone defect. KW - Three-dimensional Bone tissue engineering KW - Endothelial progenitor cell KW - Bone marrow-derived mesenchymal stem cell KW - Bioactive glass scaffold PY - 2020 DO - https://doi.org/10.1016/j.jmbbm.2019.103532 SN - 1751-6161 VL - 103 SP - 103532 EP - 103532 PB - Elsevier Ltd. AN - OPUS4-50491 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blaeß, Carsten T1 - 3D printing of crystallizing bioactive glasses N2 - Artificial bone replacement by individual customized three-dimensional resorbable bioactive glass has not yet been widely established in the clinical use. This is mainly due to the antagonism of sintering ability and suitable bioactivity. Competitive crystallization often prevents the generation of dense sintered bodies, especially for additive manufactured 3D structures. Previous studies of the fluoride-containing glass F3 have shown its potential to combine both sintering ability and suitable bioactivity. Furthermore, the occurring sintering blockade by surface crystallization of Na2CaSi2O6 was tunable by glass particle size. In this study the glasses F3, F3-Cu with 1 mol% CuO added at the expense of CaO and the well-known 13-93 were chosen to determine the influence of surface crystallization on 3D printed sinter bodies. For this purpose, grain size fractions in range of smaller 32 µm to 315 µm in fraction size of 6-20 µm were sieved from jaw crushed glass frit as well as glass cubes were cut from casted blocks for all glasses. Sintering behavior of both pressed and printed powder compacts was observed via heating microscopy. Crystallization was determined by DTA and crystallization progress was monitored on fractured sinter bodies and polished cubes via electron and laser scanning microscopy as well as with diffractometry. Depending on grain size the formation of crystalline support framework along former grain boundaries shows the capability to stabilize fully densified sinter bodies before softening. Beside of this, the generation of complex hierarchic porosity was possible as well. T2 - ICG Berlin 2022 CY - Berlin, Germany DA - 03.07.2022 KW - Bioactive Glass KW - Crystallization KW - Sintering KW - 3D printing PY - 2022 AN - OPUS4-55253 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller-Elmau, Johanna A1 - Göbel, Artur A1 - Junge, Paul A1 - Müller, Julian A1 - Rousseau, Tom A1 - Görke, Oliver A1 - Nikasch, Christian A1 - Kiliani, Stefan T1 - Thermal cycling of YAG infiltration and plasma sprayed coatings as environmental barrier coating on ceramic heat shields for use in hydrogen operating gas turbines N2 - Environmental barrier coatings (EBC) are intended to protect alumina ceramic tiles in hot water vapor conditions, enabling gas turbines to operate with higher hydrogen content or even pure hydrogen. For these operating conditions, yttrium aluminum garnet (YAG) promises the highest protection against hydrolysis, which can be applied via atmospheric plasmaspraying (APS). To enhance the protection efficiency, the coating is combined with a prior infiltration of the base material. The obtained design acts as in-depth protection even if the coating exhibits cracks. KW - Thermal shock KW - Thermal cycles KW - Environmental barrier coating (EBC) KW - Water vapor corrosion PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639829 DO - https://doi.org/10.1016/j.oceram.2025.100837 VL - 23 SP - 1 EP - 7 PB - Elsevier Ltd. AN - OPUS4-63982 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Kuchenbecker, Petra A1 - Lindemann, Franziska T1 - Final report proficiency test LS BAM-5.5-2021: Measurement of the particle size distribution of ceramic powders by laser diffraction in accordance with ISO 13320 N2 - This is the final report on the proficiency test (PT) „Measurement of the particle size distribution of ceramic powders by laser diffraction”. The PT was organized by the Federal Institute for Materials Research and Testing (BAM), division 5.5 “Advanced technical ceramics”. The measurements took place from 12/2021 to 03/2022. The aim of the interlaboratory comparison was the proficiency assessment of the participating laboratories. Management and realization of PT were performed in accordance with DIN EN ISO/IEC 17043:2010. The basis of the harmonized measuring procedure and the instructions for the interlaboratory comparison was the standard ISO 13320:2020. The statistical analysis was performed in accordance with DIN ISO 13528:2020 by use of the software PROLab Plus (QuoData GmbH, Dresden, Germany). A group of 44 laboratories from 17 countries participated in the PT. Laser diffraction analyzers produced by 7 different manufacturers were used. The three test materials were commercial products. Overall, the measured characteristic values of the particle distributions (d10, d50 and d90) were in the size range between 0.5 and 25 μm. The final report contains all individual results in an anonymous way. KW - Proficiency test KW - Particle size KW - Laser light scattering PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548640 DO - https://doi.org/10.26272/opus4-54864 SP - 1 EP - 33 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-54864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Kuchenbecker, Petra A1 - Lindemann, Franziska T1 - Final report proficiency test LS BAM-5.4-2024 - Measurement of the particle size distribution of ceramic powders by laser diffraction N2 - This publication is the final report on the proficiency test (PT) LS BAM-5.4-2024 „Measurement of the particle size distribution of ceramic powders by laser diffraction”. The PT was organized by the Federal Institute for Materials Research and Testing (BAM), division 5.4 “Advanced Multi-materials Processing”, Germany. The measurements took place from 2024/05 to 2024/07. The aim of the interlaboratory comparison was the proficiency assessment of the participating laboratories. The PT was performed in accordance with DIN EN ISO/IEC 17043:2010. The harmonized measurement procedure was based on ISO 13320:2020The statistical analysis was performed in accordance with DIN ISO 13528:2020 by use of the software PROLab (QuoData GmbH, Dresden, Germany). A group of 35 laboratories from 14 countries participated in the PT. Laser diffraction analyzers produced by 7 different manufacturers were used. The three test materials were commercial ceramic powders. Overall, the measured characteristic values of the particle size distributions (d10,3, d50,3 and d90,3) were in the size range between 1 and 35 μm. The final report contains all individual results in an anonymous form. KW - Proficiency test KW - Particle size determination KW - Laser diffraction PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-610602 DO - https://doi.org/10.26272/opus4-61060 SP - 1 EP - 33 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-61060 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo T1 - Sensoren und Analytik für Sicherheit und Prozesskontrolle in Wasserstofftechnologien N2 - Der Beitrag beinhaltet Themen vom H2Safety@BAM-Kompetenzfeld Sensorik, Analytik und zertifizierte Referenzmaterialien (SensRef) mit Fokus auf Mess- und Prüfverfahren mit verschiedenen Sensortechnologien und Ultraschallwellen: Metrologie zur Wasserstoffspeicherung - Euramet-Vorhaben "MefHySto", Erkennung von freigesetztem Wasserstoff sowie die Bestimmung des Wasserstoff-Luftverhälntisses mit Gassensoren, zerstörungsfreie Fehlstellenerkennung mit integriertem Zustandsüberwachungssystem basierend auf geführten Ultraschallwellen zur Lebensdauerüberwachung von Composite-Behältern (Wasserstoffspeicher) sowie faseroptische Sensorik zur Schadenfrüherkennung von Wasserstoffspeichern aufgrund erkennbarer Dehnungsänderungen an Druckbehältern. T2 - DVGW Kongress H2 Sicherheit CY - Online meeting DA - 23.11.2022 KW - H2Safety@BAM KW - SensRef KW - Faseroptische Sensorik KW - Gassensorik KW - Geführte Ultraschallwellen KW - Leckdetektion KW - Metrologie zur Wasserstoffspeicherung KW - Zerstörungsfreie Prüfung KW - Structural Health Monitoring (SHM) PY - 2022 AN - OPUS4-56683 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo T1 - Sensoren und Analytik für Sicherheit und Prozesskontrolle in Wasserstofftechnologien N2 - Der Beitrag behandelt verschiedene Themen aus dem H2Safety@BAM-Kompetenzfeld Sensorik, Analytik und zertifizierte Referenzmaterialien (SensRef) mit Schwerpunkt auf Mess- und Prüfverfahren, die verschiedene Analyseverfahren, Sensortechnologien und Ultraschallwellen nutzen. Ein Teil davon ist das Euramet-Vorhaben "MefHySto" zur Metrologie der Wasserstoffspeicherung. Des Weiteren werden Verfahren zur Erkennung von freigesetztem Wasserstoff und zur Bestimmung des Wasserstoff-Luftverhältnisses mithilfe von Gassensoren behandelt. Ein weiterer Aspekt ist die zerstörungsfreie Fehlstellenerkennung mit einem integrierten Zustandsüberwachungssystem, das auf geführten Ultraschallwellen basiert und zur Überwachung der Lebensdauer von Composite-Behältern (Wasserstoffspeicher) dient. Zudem wird die Anwendung faseroptischer Sensorik zur Schadenfrüherkennung an Wasserstoffspeichern diskutiert. Dabei werden erkennbare Dehnungsänderungen an Druckbehältern als Indikatoren genutzt. T2 - DVGW-Kongress "H2 Sicherheit" CY - Online meeting DA - 15.03.2023 KW - Faseroptische Sensorik KW - Gassensorik KW - Geführte Ultraschallwellen KW - Leckdetektion KW - Metrologie zur Wasserstoffspeicherung KW - Structural Health Monitoring (SHM) KW - Zerstörungsfreie Prüfung KW - SensRef KW - H2Safety@BAM PY - 2023 AN - OPUS4-57529 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Harald T1 - Tour de table - BAM N2 - Kurzübersicht über die neuen Aktivitäten zu Nanomaterialien in 2021. T2 - Nano-Behördenklausur der Bundesoberbehörden 2021 CY - Online meeting DA - 17.11.2021 KW - Nano KW - Nanomaterial KW - Nanopartikel KW - Bundesoberbehörden PY - 2021 AN - OPUS4-53827 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė A1 - Bustamante, Joana A1 - Mieller, Björn A1 - Stawski, Tomasz A1 - George, Janine A1 - Knoop, F. T1 - High-quality zirconium vanadate samples for negative thermal expansion (NTE) analysis N2 - Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material which exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). The linear thermal expansion coefficient of ZrV2O7 is −7.1×10-6 K-1. Therefore, it can be used to create composites with controllable expansion coefficients and prevent destruction by thermal shock. Material characterization, leading to application, requires pure, homogenous samples of high crystallinity via a reliable synthesis route. While there is a selection of described syntheses in the literature, it still needs to be addressed which synthesis route leads to truly pure and homogenous samples. Here, we study the influence of the synthesis methods (solid-state, sol-gel, solvothermal) and their parameters on the sample's purity, crystallinity, and homogeneity. The reproducibility of results and data obtained with scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning calorimetry, and thermogravimetric analysis (DSC/TGA) were analyzed extensively. The sol-gel method proves superior to the solid-state method and produces higher-quality samples over varying parameters. Sample purity also plays an important role in NTE micro and macro-scale characterizations that explain the impact of porosity versus structural changes. Moreover, we implement ab-initio-based vibrational computations with partially treated anharmonicity (quasi-harmonic approximation, temperature-dependent effective harmonic potentials) in combination with experimental methods to follow and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder, microstructure, and defects. Khosrovani et al. and Korthuis et al., in a series of diffraction experiments, attributed the thermal contraction of ZrV2O7 to the transverse thermal motion of oxygen atoms in V-O-V linkages. In addition to previous explanations, we hypothesize that local disorder develops in ZrV2O7 crystals during heating. We are working on the experimental ZrV2O7 development and discuss difficulties one might face in the process as well as high-quality sample significance in further investigation. The obtained samples are currently used in the ongoing research of structure analysis and the negative thermal expansion mechanism. T2 - TDEP2023: Finite-temperature and anharmonic response properties of solids in theory and practice CY - Linköping, Sweden DA - 21.08.2023 KW - NTE KW - Sol-gel KW - Solid-state KW - Ab-initio KW - TDEP PY - 2023 AN - OPUS4-58135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė A1 - Bustamante, Joana A1 - Mieller, Björn A1 - Stawski, Tomasz A1 - George, Janine A1 - Knoop, F. T1 - High-quality zirconium vanadate samples for negative thermal expansion (NTE) analysis N2 - Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material which exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). The linear thermal expansion coefficient of ZrV2O7 is −7.1×10-6 K-. Therefore, it can be used to create composites with controllable expansion coefficients and prevent destruction by thermal shock. Material characterization, leading to application, requires pure, homogenous samples of high crystallinity via a reliable synthesis route. While there is a selection of described syntheses in the literature, it still needs to be addressed which synthesis route leads to truly pure and homogenous samples. Here, we study the influence of the synthesis methods (solid-state, sol-gel, solvothermal) and their parameters on the sample's purity, crystallinity, and homogeneity. The reproducibility of results and data obtained with scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning calorimetry, and thermogravimetric analysis (DSC/TGA) were analyzed extensively. The sol-gel method proves superior to the solid-state method and produces higher-quality samples over varying parameters. Sample purity also plays an important role in NTE micro and macro-scale characterizations that explain the impact of porosity versus structural changes. Moreover, we implement ab-initio-based vibrational computations with partially treated anharmonicity (quasi-harmonic approximation, temperature-dependent effective harmonic potentials) in combination with experimental methods to follow and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder, microstructure, and defects. Khosrovani et al. and Korthuis et al., in a series of diffraction experiments, attributed the thermal contraction of ZrV2O7 to the transverse thermal motion of oxygen atoms in V-O-V linkages. In addition to previous explanations, we hypothesize that local disorder develops in ZrV2O7 crystals during heating. We are working on the experimental ZrV2O7 development and discuss difficulties one might face in the process as well as high-quality sample significance in further investigation. The obtained samples are currently used in the ongoing research of structure analysis and the negative thermal expansion mechanism. T2 - 4th International Symposium on Negative Thermal Expansion and Related Materials (ISNTE-4) CY - Padua, Italy DA - 04.07.2023 KW - NTE KW - Sol-gel KW - Solid-state KW - Ab-initio KW - TDEP PY - 2023 AN - OPUS4-58132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė A1 - Bustamante, Joana A1 - Mieller, Björn A1 - Stawski, Tomasz A1 - George, Janine A1 - Knoop, F. T1 - High-quality zirconium vanadate samples for negative thermal expansion (NTE) analysis N2 - Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material which exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). The linear thermal expansion coefficient of ZrV2O7 is −7.1×10-6 K-. Therefore, it can be used to create composites with controllable expansion coefficients and prevent destruction by thermal shock. Material characterization, leading to application, requires pure, homogenous samples of high crystallinity via a reliable synthesis route. While there is a selection of described syntheses in the literature, it still needs to be addressed which synthesis route leads to truly pure and homogenous samples. Here, we study the influence of the synthesis methods (solid-state, sol-gel, solvothermal) and their parameters on the sample's purity, crystallinity, and homogeneity. The reproducibility of results and data obtained with scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning calorimetry, and thermogravimetric analysis (DSC/TGA) were analyzed extensively. The sol-gel method proves superior to the solid-state method and produces higher-quality samples over varying parameters. Sample purity also plays an important role in NTE micro and macro-scale characterizations that explain the impact of porosity versus structural changes. Moreover, we implement ab-initio-based vibrational computations with partially treated anharmonicity (quasi-harmonic approximation, temperature-dependent effective harmonic potentials) in combination with experimental methods to follow and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder, microstructure, and defects. Khosrovani et al. and Korthuis et al., in a series of diffraction experiments, attributed the thermal contraction of ZrV2O7 to the transverse thermal motion of oxygen atoms in V-O-V linkages. In addition to previous explanations, we hypothesize that local disorder develops in ZrV2O7 crystals during heating. We are working on the experimental ZrV2O7 development and discuss difficulties one might face in the process as well as high-quality sample significance in further investigation. The obtained samples are currently used in the ongoing research of structure analysis and the negative thermal expansion mechanism. T2 - 16th International conference on materials chemistry (MC16) CY - Dublin, Ireland DA - 03.07.2023 KW - NTE KW - Sol-gel KW - Solid-state KW - Ab-initio KW - TDEP PY - 2023 AN - OPUS4-58134 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė A1 - George, Janine A1 - Mieller, Björn A1 - Stawski, Tomasz T1 - ZrV2O7 negative thermal expansion (NTE) material N2 - Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material that exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). Therefore, it can be used to create composites with controllable expansion coefficients and prevent thermal stress, fatigue, cracking, and deformation at interfaces. We implement interdisciplinary research to analyze such material. We study the influence of the synthesis methods and their parameters on the sample's purity, crystallinity, and homogeneity. Moreover, we implement ab initio-based vibrational computations with partially treated anharmonicity in combination with experimental methods to follow temperature-induced structural changes and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder. T2 - SALSA Make and Measure Conference CY - Berlin, Germany DA - 13.09.2023 KW - NTE KW - Composites KW - TEM PY - 2023 AN - OPUS4-58367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hajian, A. A1 - Konegger, T. A1 - Bielecki, K. A1 - Mieller, Björn A1 - Rabe, Torsten A1 - Schwarz, S. A1 - Zellner, C. A1 - Schmid, U. T1 - Wet chemical porosification with phosphate buffer solutions for permittivity reduction of LTCC substrates N2 - The wireless high-frequency technology requires a robust, cost-effective, and highly integrated substrate technology offering the capability for areas of tailored permittivity. The wet-chemical porosification of low temperature co-fired ceramics (LTCC) substrates offers such an approach by locally embedding air. Porosification of LTCC in both extremely acidic and alkaline media has been investigated in previous works. However, for improving the available knowledge on the porosification of LTCC with H3PO4 as a standard and a widely used etching solution, the impact of solution concentration was systematically investigated and a substantial improvement in the etching performance was achieved. Moreover, in the present study, for the first time, the intermediate pH values, and the impact of pH as a key parameter on the etching process have been investigated. For this purpose, the applicability of phosphate buffer solution (PBS) as a prospective novel etchant mixture for the porosification of a commercially available LTCC tape (Ceramtape GC) was explored. Valuable information about surface morphology, crystalline composition, and the pore structure of the etched LTCCs was gathered employing scanning electron microscopy, transmission electron microscopy, X-ray diffraction analysis, and mercury porosimetry measurements. Based on these findings, the performance of PBS-based etchant systems towards the generation of porous LTCCs combining high depths of porosification with acceptable surface characteristics for subsequent metallization is demonstrated. Based on the obtained results, by application of a 0.2 mol L−1 solution of PBS, the effective relative permittivity of test samples with a thickness of approximately 600 µm and a porosification depth of 186 µm from each side, could be reduced up to 10% of its initial “as fired” value. Also, based on the measurement results and by measuring the depth of porosification, the permittivity of the etched layer was estimated to show a reduction of up to 22% compared to the initial “as fired” value. KW - LTCC KW - Porosification KW - Wet chemical etching KW - Permittivity reduction PY - 2020 DO - https://doi.org/10.1016/j.jallcom.2020.158059 SN - 0925-8388 VL - 863 SP - 158059 PB - Elsevier B.V. AN - OPUS4-51800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Markötter, Henning T1 - Tomographic Imaging Capabilities with hard X-Rays at BAMline (Bessy II) N2 - The BAMline at the synchrotron X-ray source BESSY II (Berlin, Germany) is supporting researchers especially in materials science. As a non-destructive characterization method, synchrotron X-ray imaging, especially tomography with hard X-Rays, plays an important role in structural 3D characterization. The imaging capabilities allow for in-situ and operando experiments. In this presentation the equipment, data handling pipeline as well as various examples from material science are presented. T2 - Correlative Materials Characterization Workshop 2023 CY - Brno, Czech Republic DA - 09.11.2023 KW - Tomography KW - X-ray imaging KW - Li-ion battery PY - 2023 AN - OPUS4-58958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Making materials (digital) - Keramik N2 - Der Vortrag gibt einen Überblick über die Materialklasse Keramik, insbesondere Technische Keramik. Nach einem kurzen Überblick über typische Anwendungen und Werkstoffe wird die keramische Prozesskette erläutert. Am Beispiel von Festigkeit wird der für Keramik typische, enge Zusammenhang zwischen Technologie, Mikrostruktur und Eigenschaften herausgearbeitet. Daraus werden Anforderungen für eine erfolgreiche Digitalisierung abgeleitet. T2 - Workshop "STREAM" - Semantische Repräsentation, Vernetzung und Kuratierung von qualitätsgesicherten Materialdaten CY - Darmstadt, Germany DA - 26.09.2022 KW - Keramik KW - Festigkeit KW - Überblick PY - 2022 AN - OPUS4-55859 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Belli, Renan A1 - Hartmann, Sabine A1 - Lubauer, Julia A1 - Pereira, Raíssa Monteiro A1 - Hurle, Katrin A1 - Yin, Ling A1 - Mieller, Björn A1 - Lohbauer, Ulrich T1 - Improving the chipping resistance of pre-sintered zirconia white-bodies N2 - Objectives: The high occurrence of fractures, cracking and chipping of zirconia pre-sintered blanks and blocks during machining decreases their yield and can transfer lifetime-limiting racks to the final sintered restoration. This study has the objective of characterizing the mechanical and fracture properties of two zirconia compositions while varying temperature and time of pre-sintering, in order to assess the space for possible improvement. Methods: We selected two typical granular powders with 3 mol% (3YSZ, Zpex®, Tosoh) or 5 mol% (5YSZ, Zpex Smile®, Tosoh) yttria-stabilized zirconia and two pre-sintered commercial analogs (IPS e.max® ZirCAD MO, Ivoclar and Katana™ STML, Kuraray). The debinding and pre-sintering stages of the experimental powders were characterized using thermal analyses (differential scanning calorimetry and thermogravimetry), and the crystal phase composition was quantified using X-ray diffraction (XRD). Physical and mechanical properties such as density, hardness, flexural modulus, biaxial flexural strength and fracture toughness were measured for two pre-sintering temperatures (1000 ◦C, 1100 ◦C) and increasing holding times at those temperatures (2 h, 4 h, 6 h). The chipping resistance for those conditions was quantified using the edge chipping test using a Vickers diamond indenter. Results: Thermal analyses revealed that both powders show comparable debinding behavior and contained approx. 3.8 mass % organic binder, which burns-out completely between 300 and 400 ◦C. The crystallographic phase changes occurring during the 2–6 h at 1000 ◦C and 1100 ◦C was not detectable in the DSC signal, but quantifiable by XRD. Namely, a major content of monoclinic phase in both powders transforms completely into the two tetragonal phases, starting below 1000 ◦C and concluding above 1100 ◦C. All physical and mechanical properties increased with holding time for both temperatures, though more steeply for pre-sintering at 1100◦C. Edge chipping resistance response was well aligned with other fracture properties, with a more marked improvement for 3YSZ pre-sintered at 1100 ◦C. For all properties, the 3YSZ zirconia showed statistically-higher values for the same temperature-time conditions, in agreement with the values obtained for the commercial materials as well. Significance: The results demonstrate the weakness of pre-sintered zirconia products concerning fracture properties, but also the potential for improvement as related to type of zirconia and pre-sintering conditions. This study outlines the use of a set of mechanical tests that can characterize chipping resistance and guide future research engaging in optimizing the machining resistance of pre-sintered zirconia products. KW - Zirconia KW - Fracture KW - White body KW - Dental materials KW - Pre-sintering PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653457 DO - https://doi.org/10.1016/j.dental.2025.12.012 SN - 0109-5641 SP - 1 EP - 12 PB - Elsevier Inc. AN - OPUS4-65345 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mrkwitschka, Paul A1 - Abram, Sarah-Luise A1 - Thünemann, Andreas A1 - Rühle, Bastian A1 - Radnik, Jörg A1 - Bresch, Harald A1 - Resch-Genger, Ute A1 - Hodoroaba, Vasile-Dan T1 - The Role of Electron Microscopy in the Development of Monodisperse Cubic Iron Oxide Nanoparticles as Certified Reference Material for Size and Shape N2 - BAM is currently building up a platform of novel nanoRMs relying on iron oxide nanoparticles of different shape, size and surface chemistry. Iron oxide was chosen as a core material because of its relevance to the material and life sciences. As a first candidate of this series, we present cubic iron oxide nanoparticles with a nominal edge length of 8 nm. These particles were synthesized by thermal decomposition of iron oleate in high boiling organic solvents adapting well-known literature procedures. After dilution to a concentration suitable for electron microscopy (TEM and SEM) as well as for small-angle X-ray scattering (SAXS) measurements, the candidate nanoRM was bottled and assessed for homogeneity and stability by both methods following the guidelines of ISO 17034 and ISO Guide 35. The particle sizes obtained by both STEM-in-SEM and TEM are in excellent agreement with a minimum Feret of 8.3 nm ± 0.7 nm. The aspect ratio (AR) of the iron oxide cubes were extracted from the images as the ratio of minimum Feret to Feret resulting in an AR of 1.18 for TEM to 1.25 for SEM. Alternatively, a rectangular bounding box was fitted originating from the minimum Feret and the longest distance through the particle in perpendicular direction. This led to AR values of 1.05 for TEM and 1.12 for SEM, respectively. The results confirm the almost ideal cubic shape. KW - Reference nanoparticles KW - Iron oxide KW - Cubical shape KW - Electron microscopy KW - SAXS KW - Nano CRM KW - Size PY - 2022 DO - https://doi.org/10.1017/S1431927622003610 SN - 1435-8115 VL - 28 IS - Suppl. 1 SP - 802 EP - 805 PB - Cambridge University Press AN - OPUS4-55599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - The Role of Electron Microscopy in the Development of Monodisperse Cubic Iron Oxide Nanoparticles as CRM for Size and Shape N2 - Due to their unique physico-chemical properties, nanoparticles are well established in research and industrial applications. A reliable characterization of their size, shape, and size distribution is not only mandatory to fully understand and exploit their potential and develop reproducible syntheses, but also to manage environmental and health risks related to their exposure and for regulatory requirements. To validate and standardize methods for the accurate and reliable particle size determination nanoscale reference materials (nanoRMs) are necessary. However, there is only a very small number of nanoRMs for particle size offered by key distributors such as the National Institute of Standards and Technology (NIST) and the Joint Research Centre (JRC) and, moreover, few provide certified values. In addition, these materials are currently restricted to polymers, silica, titanium dioxide, gold and silver, which have a spherical shape except for titania nanorods. To expand this list with other relevant nanomaterials of different shapes and elemental composition, that can be used for more than one sizing technique, we are currently building up a platform of novel nanoRMs relying on iron oxide nanoparticles of different shape, size and surface chemistry. Iron oxide was chosen as a core material because of its relevance for the material and life sciences. T2 - Microscopy and Microanalysis 2022 CY - Online meeting DA - 31.07.2022 KW - Certified Referencematerial KW - Cubical Iron Oxide KW - Nanoparticles KW - Electron Microscopy KW - Small-Angle X-ray Scattering PY - 2022 AN - OPUS4-57035 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mrkwitschka, Paul A1 - Rühle, Bastian A1 - Kuchenbecker, Petra A1 - Löhmann, Oliver A1 - Lindemann, Franziska A1 - Hodoroaba, Vasile-Dan T1 - Embedding and cross-sectioning as a sample preparation procedure for accurate and representative size and shape measurement of nanopowders N2 - Reliable measurement of the size of polydisperse, complex-shaped commercial nanopowders is a difficult but necessary task, e.g., for regulatory requirements and toxicity risk assessment. Suitable methods exist for the accurate characterization of the size of non-aggregated, stabilized, spherical and monodisperse nanoparticles. In contrast, industrial nanoscale powders usually require dedicated sample preparation procedures developed for the analysis method of choice. These nano-powders tend to agglomerate and/or aggregate, a behavior which in combination with an innate broad particle size distribution and irregular shape often significantly alters the achievable accuracy of the measured size parameters. The present study systematically tests two commercially available nanoscale powders using different sample preparation methods for correlative analysis by scanning electron microscopy, dynamic light scattering, Brunauer–Emmet–Teller method and differential mobility analysis. One focus was set on the sample preparation by embedding nanoparticles in carbon-based hot-mounting resin. Literature on this topic is scarce and the accuracy of the data extracted from cross sections of these particles is unclearly stated. In this paper systematic simulations on the deviation of the size parameters of well-defined series of nanoparticles with different shapes from the nominal value were carried out and the contributing factors are discussed. KW - Nanopowder KW - Electron microscopy KW - Sample preparation KW - Cross-sectioning KW - Cerium oxide KW - Zinc oxide PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593289 DO - https://doi.org/10.1038/s41598-023-51094-0 SN - 2045-2322 VL - 14 SP - 1 EP - 10 PB - Springer Nature CY - London AN - OPUS4-59328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - López de Ipina, J.-M. A1 - Arevalillo, A. A1 - Martín, A. A1 - Caillard, B. A1 - Marcoulaki, E. A1 - Aguerre- Charol, O. A1 - van Duuren-Stuurman, B. A1 - Hodoroaba, Vasile-Dan A1 - Viitanen, A.-K. A1 - Witters, H. A1 - Vercauteren, S. A1 - Persson, K. A1 - Bard, D. A1 - Evans, G. A1 - Jensen, K.A. A1 - Himly, M. A1 - Scalbi, S. A1 - Papin, A. A1 - Le Bihan, O. A1 - Kanerva, T. A1 - Tirez, K. A1 - Frijns, E. A1 - Niga, P. A1 - Eleftheriadis, K. A1 - Travlos, A. A1 - Geppert, M. A1 - Himly, M. A1 - Radnik, Jörg A1 - Kuchenbecker, Petra A1 - Resch-Genger, Ute A1 - Fraboulet, I. A1 - Bressot, C. A1 - Rissler, J. A1 - Gaucher, R. A1 - Binotto, G. A1 - Krietsch, Arne A1 - Braun, A. A1 - Abenet, S. A1 - Catalan, J. A1 - Verstraelen, S. A1 - Manier, N. A1 - Manzo, S. A1 - Fransman, S. A1 - Queron, J. A1 - Charpentier, D. A1 - Taxell, D. A1 - Säämänen, A. A1 - Brignon, J.-M. A1 - Jovanovic, A. A1 - Bisson, M A1 - Neofytou, P. T1 - EC4Safenano - Catalogue of Services N2 - 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. KW - Nano-safety KW - Analytical services KW - Nanomaterials KW - Catalogue of services KW - EC4SafeNano KW - European Centre PY - 2021 UR - https://ec4safenano.eu-vri.eu/Public/Guidance SP - 1 EP - 72 PB - EU-VRi – European Virtual Institute for Integrated Risk Management CY - Stuttgart, Germany AN - OPUS4-52943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Gibson, N. A1 - Kuchenbecker, Petra A1 - Rasmussen, K. A1 - Hodoroaba, Vasile-Dan A1 - Rauscher, H. ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A.G. T1 - Volume-specific surface area by gas adsorption analysis with the BET method N2 - This chapter first gives an introduction to the concepts of SSA and volume-specific surface area (VSSA) and an outline of the BET method. It continues with a discussion of the relationship between particle size, shape, and the VSSA, followed by an overview of instrumentation, experimental methods, and standards. Finally, sections on the use of the VSSA as a tool to identify nanomaterials and non-nanomaterials and its role in a regulatory context provide some insight on the importance of VSSA in the current Regulation of nanomaterials. KW - Nanomaterials KW - Volume specific surface area PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00017-1 SP - 265 EP - 293 PB - Elsevier CY - Amsterdam AN - OPUS4-49572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pereira, Raíssa Monteiro A1 - Lohbauer, Ulrich A1 - Schulbert, Christian A1 - Göken, Mathias A1 - Wurmshuber, Michael A1 - Campos, Tiago Bastos Moreira A1 - Thim, Gilmar Patrocínio A1 - Mieller, Björn A1 - Belli, Renan T1 - Instantiations of Multiscale Kinship in Pressing‐Defect Distributions in Yttria‐Stabilized Zirconias by Powder Partitioning N2 - Modern dry pressing of ceramic powders using spray‐dried granulates cannot avoid the occurrence of defects related to persisting inter‐ and intra‐granulate interstitial voids. These constitute the parent defect size population limiting the application of polycrystalline ceramics in high‐stress conditions. The mitigation of such defects could widen the range of application in technical and biomedical engineering, reduce the safety range for design, and extend the lifetime of components. Herein, the Weibull size‐effect on strength in size‐partitioned Yttria‐stabilized zirconias (YSZ) feedstocks is used to explore the viability of changing the density distribution of granulate sizes as an effective strategy to obtain a denser particle packing that could reduce the size distribution of strength‐limiting pressing defects. In a direct assessment of critical defect size using multiscale strength testing with a dataset of ≈1300 values, the success of such an approach in increasing the strength reliability for small volume components is demonstrated, along with its ultimate failure in altering the defect size distribution in sintered YSZ ceramics across several length scales. Finally, it is shown that granule morphology (spherical or dimpled) fails to affect the defect density and size distribution in YSZ ceramics. KW - Zirconia KW - Strength KW - Toughness KW - Weibull distribution KW - Defect population PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-602697 DO - https://doi.org/10.1002/adem.202400139 SN - 1438-1656 SP - 1 EP - 17 PB - Wiley VHC-Verlag AN - OPUS4-60269 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paulus, Daniel A1 - Bresch, Sophie A1 - Moos, Ralf A1 - Schönauer-Kamin, Daniela T1 - Powder aerosol deposited calcium cobaltite as textured P-type thermoelectric material with power factors approaching single crystal values N2 - In this work, the thermoelectric material calcium cobaltite Ca3Co4O9 (CCO), a promising p-type conducting thermoelectric oxide with anisotropic properties, was processed by the powder aerosol deposition method (PAD) to form a dense ceramic CCO film with a thickness in the µm range. The prepared films were characterized regarding their microstructure and thermoelectric properties between room temperature and 900 °C. After heat treatment at 900 °C, the CCO PAD film in-plane shows excellent properties in terms of electrical conductivity (280 S/cm at 900 °C) and Seebeck coefficient (220 µV/K at 900 °C). The calculated power factor in-plane (ab) reaches with 1125 µW/(m K2) 40 % of the single crystal value, surpassing the known-properties of CCO bulk ceramics. Examination of the microstructure shows a strong fiber texture of the film as well as a strong coarsening of the grains during the first heat treatment up to 900 °C. KW - thermoelectrics KW - calcium cobaltite KW - thermoelectric oxide KW - aerosol deposition method (ADM) PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-606246 DO - https://doi.org/10.1016/j.jeurceramsoc.2024.116717 SN - 0955-2219 VL - 44 IS - 15 SP - 1 EP - 8 PB - Elsevier BV AN - OPUS4-60624 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mieller, Björn A1 - Hassine, Sahar Ben A1 - Töpfer, Jörg A1 - Priese, Christoph A1 - Bochmann, Arne A1 - Capraro, Beate A1 - Stark, Sebastian A1 - Partsch, Uwe A1 - Fresemann, Carina T1 - Ontology‐based Data Acquisition, Refinement, and Utilization in the Development of a Multilayer Ferrite Inductor N2 - A key aspect in the development of multilayer inductors is the magnetic permeability of the ferrite layers. Here, the effects of different processing steps on the permeability of a NiCuZn ferrite is investigated. Dry pressed, tape cast, and co‐fired multilayer samples are analyzed. An automated data pipeline is applied to structure the acquired experimental data according to a domain ontology based on PMDco (Platform MaterialDigital core ontology). Example queries to the ontology show how the determined process‐property correlations are accessible to non‐experts and thus how suitable data for component design can be identified. It is demonstrated how the inductance of co‐fired multilayer inductors is reliably predicted by simulations if the appropriate input data corresponding to the manufacturing process is used.This article is protected by copyright. All rights reserved. KW - Ontology KW - Ceramic multilayer KW - Data pipeline PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-605483 DO - https://doi.org/10.1002/adem.202401042 SN - 1527-2648 SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim AN - OPUS4-60548 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mieller, Björn A1 - Valavi, Masood A1 - Caldeira Rêgo, Celso Ricardo T1 - An Automatized Simulation Workflow for Powder Pressing Simulations Using SimStack N2 - Automated computational workflows are a powerful concept that can improve the usability and reproducibility of simulation and data processing approaches. Although used very successfully in bioinformatics, workflow environments in materials science are currently commonly applied in the field of atomistic simulations. This work showcases the integration of a discrete element method (DEM) simulation of powder pressing in the convenient SimStack workflow environment. For this purpose, a Workflow active Node (WaNo) was developed to generate input scripts for the DEM solver using LIGGGHTS Open Source Discrete Element Method Particle Simulation code. Combining different WaNos in the SimStack framework makes it possible to build workflows and loop over different simulation or evaluation conditions. The functionality of the workflows is explained, and the added user value is discussed. The procedure presented here is an example and template for many other simulation methods and issues in materials science and engineering. KW - Simulation workflow KW - Discrete element method PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-604791 DO - https://doi.org/10.1002/adem.202400872 SP - 1 EP - 7 PB - Wiley AN - OPUS4-60479 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Reaction sintering and sintering additives for cost-effective production of thermoelectric oxides N2 - Thermoelectric oxides attract much interest recently. Although their thermoelectric properties are inferior to non-oxides, they exhibit distinct advantages. Thermoelectric oxides are stable in air at higher temperatures, their raw materials are less toxic, and more abundant. To enhance attractivity of these materials for industrial applications, production costs need to be reduced. Conventionally, the legs of thermoelectric generators are sintered from green bodies of previously synthesized powder. Reaction-sintering is a fabrication method without a powder synthesis step, as the final phase is formed during the sintering from a raw material mixture. Moreover, the reduction of chemical potential during reaction-sintering is effective as an additional driving force for sintering. We show that reaction-sintering increases the densification of CaMnO3 (n-type, Sm doped). Consequently, the electrical conductivities improved by about 100 % leading to superior power factors (PF = 230 µW/mK² for CaMnO3). Another approach to reduce the production costs is to lower the sintering temperature by adding sinter additives. The addition of 4 wt% CuO to CaMnO3 lowers the sinter temperature from 1250 °C to 1050 °C. The achieved power factor PF = 264 µW/mK is more than two times higher as reported in literature for the same dopant. T2 - Virtual Conference on Thermoelectrics (VCT) CY - Online meeting DA - 21.07.2020 KW - Thermoelectrics KW - Reaction sintering KW - Sintering additives KW - Calcium manganate KW - Calcium cobaltite PY - 2020 AN - OPUS4-51070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul A1 - Mieller, Björn A1 - Rabe, Torsten A1 - Markötter, Henning ED - Petzow, G. ED - Mücklich, F. T1 - Machine learning assisted characterization of a Low Temperature Cofired Ceramic (LTCC) module measured by synchrotron computed tomography N2 - The 5G technology promises real time data transmission for industrial processes, autonomous driving, virtual and augmented reality, E-health applications and many more. The Low Temperature Co-fired Ceramics (LTCC) technology is well suited for the manufacturing of microelectronic components for such applications. Still, improvement of the technology such as further miniaturization is required. This study focuses on the characterization of inner metallization of LTCC multilayer modules, especially on the vertical interconnect access (VIA). Critical considerations for this characterization are delamination, pore clustering in and at the edge of the VIA, deformation, and stacking offset. A LTCC multilayer consisting of a glassy crystalline matrix with silver based VIAs was investigated by synchrotron x-ray tomography (CT). The aim of this study is to propose a multitude of structural characteristic values to maximize the information gained from the available dataset. Data analysis has been done with the open source software ImageJ as well as several additional plugins. The high-resolution CT data was evaluated through 2D slices for accessibility reasons. The segmentation of all 2000 slices to assess the different regions e.g. pores, silver and glass ceramic was done by a supervised machine learning algorithm. A quantitative evaluation of shape, deformation, and porosity of the VIA with respect to its dimensions is presented and the suitability of the characterization approach is assessed. T2 - 54. Metallographie Taagung CY - Online meeting DA - 16.09.2020 KW - Machine Learning KW - LTCC KW - Synchrotron Tomography PY - 2020 SN - 978-3-88355-422-8 VL - 54 SP - 136 EP - 141 PB - Deutsche Gesellschaft für Materialkunde e.V CY - Sankt Augustin AN - OPUS4-51298 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Improved thermoelectric properties of CaMnO3 and Ca3Co4O9 by increasing the driving force for sintering N2 - Thermoelectric materials can convert waste heat directly into electrical power by utilizing the Seebeck effect. Calcium cobaltite (Ca3Co4O9, p-type) and calcium manganate (CaMnO3, n-type) are two of the most promising oxide thermoelectric materials. The performance of these materials is evaluated by the power factor PF = S²∙σ and the figure of merit ZT = (PF ∙ T) / κ, demanding high Seebeck coefficient S, high electrical conductivity σ and low thermal conductivity κ. The latter two are increasing with increasing relative sinter density. According to theory, the relative density of ceramics can be improved by increasing the driving force for sintering. This study investigates different approaches to increase the driving force for sintering of Ca3Co4O9 and CaMnO3 to improve densities and thermoelectric properties. The following approaches were applied: minimizing the energy input during powder synthesis by calcination, fine milling of the powder, using reaction-sintering without a powder synthesis step, and adding a transient liquid phase by sinter additives. All different approaches led to an increased densification and thus higher electrical conductivity and higher PF. Thermal conductivity increased as well but not to the same extent. E.g. reaction-sintering increased the densification of Ca3Co4O9 (p-type) and CaMnO3 (n-type). Consequently, the electrical conductivities improved by about 100 % for both oxides leading to superior power factors (PF = 230 µW/mK² for CaMnO3). Although the thermal conductivity increased as well by 8 %, the figures of merit (ZT) were significantly higher compared to conventionally sintered bars. The addition of 4 wt% CuO as a sinter additive to CaMnO3 lowers the sinter temperature from above 1250 °C to below 1100 °C and increases the relative density. Due to the increased density, both electrical conductivity and PF increased by more than 200 % even though the sintering temperature was 150 K lower. T2 - Electroceramics XVII CY - Online meeting DA - 24.08.2020 KW - Thermoelectrics KW - Reaction sintering KW - Sintering additives PY - 2020 AN - OPUS4-51163 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Practical breakdown voltage calculations using dielectric breakdown strength reference values N2 - Dielectric breakdown is a catastrophic failure of ceramic substrates and insulators. The use of dielectric breakdown strength (DBS) reference values for the dimensioning of such components is not straightforward, as the DBS depends on sample thickness and electrode area. This fact also hampers a valid comparison of data taken from different literature sources. Based on the empirically confirmed proportionality of DBS to the reciprocal square root of sample thickness and an approach to account for the influence of electrode area on the failure probability, a practical equation is derived to calculate the breakdown voltage for arbitrary sample thickness and electrode area from one set of DBS reference data. To validate the equation, the AC DBS of commercial alumina substrates with thicknesses ranging from 0.3 mm to 1.0 mm was performed using different printed electrodes with varying areas. The breakdown voltages comprise a range from 18 kV for thick samples to 8.5 kV for thin samples, resulting in DBS values from 17 kV/mm for 1.0 mm thick samples to 29 kV/mm for 0.3 mm thin samples, all made from the same material. The influence of electrode area is comparatively smaller. The results calculated with the proposed equation are in reasonable accordance with the measured data. Thus, the equation can be applied for a proper comparison of literature DBS data measured in different setups and for a reasonable estimation of breakdown voltages in DBS tests and applications based on reference data. T2 - Electroceramics Conference XVII CY - Online meeting DA - 24.08.2020 KW - Ceramics KW - Dielectric breakdown KW - Weibull distribution PY - 2020 AN - OPUS4-51151 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Machine learning assisted characterization of a Low Temperature Co-fired Ceramic (LTCC) module measured by synchrotron computed tomography. N2 - The 5G technology promises real time data transmission for industrial processes, autonomous driving, virtual and augmented reality, E-health applications and many more. The Low Temperature Co-fired Ceramics (LTCC) technology is well suited for the manufacturing of microelectronic components for such applications. Still, improvement of the technology such as further miniaturization is required. This study focuses on the characterization of inner metallization of LTCC multilayer modules, especially on the vertical interconnect access (VIA). Critical considerations for this characterization are delamination, pore clustering in and at the edge of the VIA, deformation, and stacking offset. A LTCC multilayer consisting of a glassy crystalline matrix with silver based VIAs was investigated by synchrotron x-ray tomography (CT). The aim of this study is to propose a multitude of structural characteristic values to maximize the information gained from the available dataset. Data analysis has been done with the open source software ImageJ as well as several additional plugins. The high-resolution CT data was evaluated through 2D slices for accessibility reasons. The segmentation of all 2000 slices to assess the different regions e.g. pores, silver and glass ceramic was done by a supervised machine learning algorithm. A quantitative evaluation of shape, deformation, and porosity of the VIA with respect to its dimensions is presented and the suitability of the characterization approach is assessed. T2 - 54. Metallographie Tagung CY - Online meeting DA - 16.09.2020 KW - Machine Learning KW - LTCC KW - Synchrotron Tomography PY - 2020 AN - OPUS4-51299 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Mrkwitschka, Paul A1 - Moos, R. A1 - Rabe, Torsten T1 - Glass-ceramic composites as insulation material for thermoelectric oxide multilayer generators N2 - 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. KW - Electrical insulators KW - Glass-ceramics KW - Multilayers KW - Thermal expansion PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538898 DO - https://doi.org/10.1111/jace.18235 SN - 0002-7820 SP - 1 EP - 10 PB - Wiley Online Library AN - OPUS4-53889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Schönauer-Kamin, D. A1 - Moos, R. A1 - Reimann, T. A1 - Giovannelli, F. A1 - Rabe, Torsten T1 - Influence of pressure and dwell time on pressure‐assisted sintering of calcium cobaltite N2 - Calcium cobaltite Ca3Co4O9, abbreviated Co349, is a promising thermoelectric material for high‐temperature applications in air. Its anisotropic properties can be assigned to polycrystalline parts by texturing. Tape casting and pressure‐assisted sintering (PAS) are a possible future way for a cost‐effective mass‐production of thermoelectric generators. This study examines the influence of pressure and dwell time during PAS at 900°C of tape‐cast Co349 on texture and thermoelectric properties. Tape casting aligns lentoid Co349. PAS results in a textured Co349 microstructure with the thermoelectrically favorable ab‐direction perpendicular to the pressing direction. By pressure variation during sintering, the microstructure of Co349 can be tailored either toward a maximum figure of merit as required for energy harvesting or toward a maximum power factor as required for energy harvesting. Moderate pressure of 2.5 MPa results in 25% porosity and a textured microstructure with a figure of merit of 0.13 at 700°C, two times higher than the dry‐pressed, pressureless‐sintered reference. A pressure of 7.5 MPa leads to 94% density and a high power factor of 326 µW/mK2 at 800°C, which is 11 times higher than the dry‐pressed reference (30 MPa) from the same powder. KW - Hot pressing KW - Texture KW - Thermoelectric properties PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515973 DO - https://doi.org/https://doi.org/10.1111/jace.17541 SN - 0002-7820 VL - 104 IS - 2 SP - 917 EP - 927 PB - Wiley Periodicals LLC AN - OPUS4-51597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Höhne, Patrick A1 - Mieller, Björn A1 - Rabe, Torsten T1 - Advancing spray granulation by ultrasound atomization N2 - The influence of the atomization technique on the suitability of granules for dry pressing is the focus of the presented investigations. Therefore, destabilized alumina, zirconia, and zirconia toughened alumina (ZTA) slurries were spray dried and the obtained granules were used to fabricate green and finally sintered bodies for evaluation. Granules made in a laboratory spray dryer with a two-fluid nozzle served as a reference. An ultrasonic atomizer was integrated into the same spray dryer and the influence on the granule properties was evaluated. Untapped bulk density, granule size distribution, and flowability are among the evaluated granule-related properties as well as the granule yield which is used as an indicator of the process efficiency. Yield and flowability as most important granule properties are clearly improved when atomization is realized with ultrasound. The investigated sinter body properties include porosity, sinter body density, and biaxial strength and are as well positively affected by switching the atomization technique to ultrasound. Therefore, the Approach to improve the compressibility of granules by ultrasonic atomization, which leads to an improved microstructure, density, and strength of sintered bodies, has proven to be successful for single-component ceramics (alumina and zirconia) as well as for the multicomponent ceramic ZTA. KW - Alumina KW - Granules KW - Spray drying KW - Ultrasound KW - Zirconia KW - Zirconia-toughened alumina PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510696 DO - https://doi.org/10.1111/ijac.13534 VL - 17 IS - 5 SP - 2212 EP - 2219 AN - OPUS4-51069 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Mieller, Björn A1 - Maiwald, Michael A1 - Kipphardt, Heinrich A1 - Tuma, Dirk A1 - Prager, Jens A1 - Schukar, Marcus A1 - Strohhäcker, J. T1 - Sensoren und Analytik für Sicherheit und Prozesskontrolle in Wasserstofftechnologien N2 - Die Nutzung von Sensortechnologien, insbesondere im Bereich der Gasdetektion mit einem Schwerpunkt auf Wasserstoff, spielt eine entscheidende Rolle in verschiedenen Anwendungsbereichen der Wasserstofftechnologie. Sicherheitsüberwachung, Leckdetektion und Prozesskontrolle gehören zu den prominenten Anwendungsgebieten dieser Sensortechnologien. Ein zentrales Ziel ist die Erkennung von freigesetztem Wasserstoff sowie die genaue Bestimmung des Wasserstoff-Luftverhältnisses mithilfe von Gassensoren. Dies ist von entscheidender Bedeutung, um potenzielle Gefahren frühzeitig zu erkennen und angemessene Maßnahmen zu ergreifen. Ein weiterer Schwerpunkt dieses Beitrags liegt auf der Analytik und der Verwendung zertifizierter Referenzmaterialien in Verbindung mit Metrologie für die Wasserstoffspeicherung. Dies gewährleistet eine präzise und zuverlässige Charakterisierung von Wasserstoff und unterstützt die Entwicklung sicherer Speichertechnologien. Im Rahmen des Euramet-Vorhabens Metrology for Advanced Hydrogen Storage Solutions (MefHySto) wird eine Kurzvorstellung präsentiert. Der Vortrag stellt zwei zerstörungsfreie Prüfverfahren zum strukturellen Zustandsüberwachung (Structural Health Monitoring, SHM) für Wasserstofftechnologien vor. Insbesondere die Fehlstellenerkennung mittels geführter Ultraschallwellen spielt eine bedeutende Rolle bei der Lebensdauerüberwachung von Wasserstoffspeichern. Ein weiterer Aspekt ist die Anwendung faseroptischer Sensorik zur Schadensfrüherkennung von Wasserstoffspeichern. Diese zerstörungsfreien Prüfverfahren ermöglichen eine präzise und frühzeitige Identifizierung von Schäden, was die Sicherheit und Effizienz von Wasserstoffspeichersystemen entscheidend verbessert. T2 - DVGW Kongress H2 Sicherheit CY - Online meeting DA - 15.11.2023 KW - H2Safety@BAM KW - Gassensorik KW - Metrologie KW - zertifizierte Referenzmaterialien KW - Zerstörungsfreie Prüfung KW - Ultraschall KW - Faseroptik PY - 2023 AN - OPUS4-59230 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rabe, T. A1 - Kalinka, Gerhard A1 - Mieller, Björn T1 - Manufacturing and deformation behavior of alumina and zirconia helical springs at room temperature N2 - Ceramic helical springs with identical dimensions were produced by hard machining from alumina, alumina toughened zirconia (ATZ), and tetragonal zirconia polycrystals (TZP) stabilized with different oxides. According to the results of the spring constant determination under deformation rates of 3 mm/min, the deformation behavior of all ceramic springs obeys to Hook’s law. However, variation of the deformation rate, tests under constant load, and spring recovery behavior revealed differences in the deformation behavior of alumina, TZP, and ATZ springs. Alumina springs exhibited time-independent deformation in all tests. In contrast, anelastic deformation at room temperature was demonstrated in all springs containing TZP. This deformation is completely reversible over a period of several days. Anelastic behavior is particularly pronounced in Y-TZP springs, whereas Ce-TZP springs exhibit comparatively very low but still reliably detectable anelasticity. Oxygen vacancies in the TZP ceramic are considered the most likely explanation for the anelastic behavior of TZP springs at room temperature. KW - Alumina KW - Creep KW - Elastic properties KW - Zirconia PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571858 DO - https://doi.org/10.1111/jace.19085 SN - 0002-7820 SP - 1 EP - 14 PB - Wiley-Blackwell CY - Oxford [u.a.] AN - OPUS4-57185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eddah, Mustapha T1 - Synchrotron Multi-energy HDR tomography for LTCC systems N2 - LTCCs (Low-temperature co-fired ceramics) consist of three-dimensionally distributed, hermetically bonded ceramic and metallic components with structure sizes within [10; 100] µm. A non-destructive imaging technique is needed that provides 3D, sharp, high-contrast resolution of these structures, as well as porosity and defect analysis, which is made difficult by the very different X-ray absorption coefficients of the individual components of the microstructure. A HDR method is being developed that allows a combination of different tomograms, each with X-ray energies adapted to individual materials. T2 - Bessy II User Meeting CY - Berlin, Germany DA - 22.06.2023 KW - LTCC KW - Synchrotron tomography KW - Data fusion KW - In-situ tomography PY - 2023 AN - OPUS4-57795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Texturing of calcium cobaltite for thermoelectric applications by pressure assisted sintering N2 - 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. T2 - KERAMIK 2021 / CERAMICS 2021 CY - Online meeting DA - 19.04.2021 KW - Thermoelectrics KW - Hot pressing KW - Pole figures PY - 2021 AN - OPUS4-52490 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Thermoelectric multilayer generators: development from oxide powder to demonstrator N2 - Thermoelectric generators can be used for energy harvesting by directly transforming a temperature gradient into a voltage. Multilayer generators based on ceramic multilayer technology 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. But, co-firing of promising oxide thermoelectric materials, Ca3Co4O9 (p-type) and CaMnO3 (n-type), is very challenging due to the large difference in sintering temperature (300 K). In this work we show the material development of Ca3Co4O9, CaMnO3, and insulation for multilayer generators co-fired under uniaxial pressure at 900 °C. The materials are tailored regarding their sintering behavior, electrical performance and coefficients of thermal expansion. Tape-casting and pressure assisted sintering are applied to fabricate textured Ca3Co4O9. Compared to conventional sintering, pressure assisted sintering increases the strength by the factor 10 and the power factor by the factor of 20. The combination of sintering additives and uniaxial pressure is used to decrease the sintering temperature of CaMnO3 to 900 °C while maintaining acceptable thermoelectric properties. Different generator designs (unileg and pn-type) were fabricated and analyzed regarding microstructure and thermoelectric performance. A lower level of complexity is beneficial for co-firing and performance. The unileg demonstrators reach 80% of the simulated output power and the power output is highly reproducible between the different demonstrators (99%). T2 - Ceramics in Europe 2022 CY - Krakow, Poland DA - 10.07.2022 KW - Thermoelectrics KW - Multilayer technology KW - Co-firing KW - Texture PY - 2022 AN - OPUS4-55357 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Miliūtė, Aistė ED - Bustamante, Joana ED - Karafiludis, Stephanos ED - Zöllner, Moritz ED - Eddah, Mustapha ED - Emmerling, Franziska ED - Mieller, Björn ED - George, Janine ED - Stawski, Tomasz T1 - Synthesis and phase purity of the negative thermal expansion material ZrV2O7 N2 - Synthesis of pure, homogeneous, and reproducible materials is key for the comprehensive understanding, design, and tailoring of material properties. In this study, we focus on the synthesis of ZrV2O7, a material known for its negative thermal expansion properties. We investigate the influence of solid-state and wet chemistry synthesis methods on the purity and homogeneity of ZrV2O7 samples. Our findings indicate that different synthesis methods significantly impact the material's characteristics. The solid-state reaction provided high-purity material through extended milling time and repeated calcination cycles, while the sol-gel reaction enabled a “near-atomic” level of mixing and, therefore, homogenous phase-pure ZrV2O7. We confirmed purity via X-ray diffraction and Raman spectroscopy, highlighting differences between phase-pure and multiphase ceramics. These analytical techniques allowed us to distinguish subtle differences in the structure of the material. Based on ab initio simulated phonon data, we were able to interpret the Raman spectra and visualise Raman active atom vibrations. We show that phase purity enables the unbiased characterisation of material properties such as negative thermal expansion. KW - NTE KW - Sol-gel KW - Solid-state KW - Ab-initio KW - XRD KW - Raman PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613643 DO - https://doi.org/10.26434/chemrxiv-2024-d4sj9 SN - 2573-2293 VL - 2024 SP - 1 EP - 60 PB - American Chemical Society CY - Washington, D.C. AN - OPUS4-61364 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Miliūtė, Aistė A1 - Bustamante, Joana A1 - Karafiludis, Stephanos A1 - Zöllner, Moritz A1 - Eddah, Mustapha A1 - Emmerling, Franziska A1 - Mieller, Björn A1 - George, Janine A1 - Stawski, Tomasz M. T1 - Synthesis and phase purity of the negative thermal expansion material ZrV2O7 N2 - Synthesis of pure, homogeneous, and reproducible materials is key for the comprehensive understanding, design, and tailoring of material properties. In this study, we focus on the synthesis of ZrV2O7, a material known for its negative thermal expansion properties. We investigate the influence of solid-state and wet chemistry synthesis methods on the purity and homogeneity of ZrV2O7 samples. Our findings indicate that different synthesis methods significantly impact the material's characteristics. The solid-state reaction provided high-purity material through extended milling time and repeated calcination cycles, while the sol-gel reaction enabled a “near-atomic” level of mixing and, therefore, homogenous phase-pure ZrV2O7. We confirmed purity via X-ray diffraction and Raman spectroscopy, highlighting differences between phase-pure and multiphase ceramics. These analytical techniques allowed us to distinguish subtle differences in the structure of the material. Based on ab initio simulated phonon data, we were able to interpret the Raman spectra and visualise Raman active atom vibrations. We show that phase purity enables the unbiased characterisation of material properties such as negative thermal expansion. KW - NTE KW - Sol-gel KW - Solid-state KW - Ab-initio KW - XRD KW - Raman PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624013 DO - https://doi.org/10.1039/d4tc04095c SN - 2050-7534 SP - 1 EP - 13 PB - Royal Society of Chemistry (RSC) AN - OPUS4-62401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eddah, Mustapha A1 - Markötter, Henning A1 - Mieller, Björn A1 - Sintschuk, Michael A1 - Beckmann, Jörg A1 - Bruno, Giovanni T1 - Mitigation of DMM-induced stripe patterns in synchrotron X-ray radiography through dynamic tilting N2 - In synchrotron X-ray radiography, achieving high image resolution and an optimal signal-to-noise ratio (SNR) is crucial for the subsequent accurate image analysis. Traditional methods often struggle to balance these two parameters, especially in situ applications where rapid data acquisition is essential to capture specific dynamic processes. For quantitative image data analysis, using monochromatic X-rays is essential. A double multilayer monochromator (DMM) is successfully used for this aim at the BAMline, BESSY II (Helmholtz Zentrum Berlin, Germany). However, such DMMs are prone to producing an unstable horizontal stripe pattern. Such an unstable pattern renders proper signal normalization difficult and thereby causes a reduction of the SNR. We introduce a novel approach to enhance SNR while preserving resolution: dynamic tilting of the DMM. By adjusting the orientation of the DMM during the acquisition of radiographic projections, we optimize the X-ray imaging quality, thereby enhancing the SNR. The corresponding shift of the projection during this movement is corrected in post-processing. The latter correction allows a good resolution to be preserved. This dynamic tilting technique enables the homogenization of the beam profile and thereby effectively reduces noise while maintaining high resolution. We demonstrate that data captured using this proposed technique can be seamlessly integrated into the existing radiographic data workflow, as it does not need hardware modifications to classical X-ray imaging beamline setups. This facilitates further image analysis and processing using established methods. KW - Double multilayer monochromators KW - Synchrotron X-ray imaging KW - Signal normalization KW - BAMline KW - Dynamic tilting PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615049 DO - https://doi.org/10.1107/S1600577524008646 SN - 1600-5775 VL - 31 SP - 1551 EP - 1560 PB - International Union of Crystallography (IUCr) AN - OPUS4-61504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Thin-film capability of commercial LTCC N2 - Low-temperature co-fired ceramics (LTCC) are used to fabricate multilayer circuits which are robust in harsh environments. Thick-film technology is well established for the metallization of circuit boards and microsystems. For specific sensor applications, the combination of LTCC and thin-film technology is advantageous to reach higher structure resolutions. Due to the high roughness of as-fired LTCC surfaces compared with silicon-wafers, the deposition of low-defect- films with narrowly specified properties is challenging. The deposited thin-films are structured either by lift-off or by etching. The latter is less error-prone and thus preferred in industry provided the selected materials allow it. There is spare literature about thin films on commercial LTCC comparing different material systems or sintering techniques. For developing thin-film sensors on multilayer circuits it is crucial to identify thin-film-compatible commercial LTCC material as well as the crucial surface properties. In this work we evaluate the thin-film capability of different LTCC compositions and surface qualities. To evaluate the influence of the material composition on the thin film capability, 200 nm Ni-thin films were deposited on three different constrained-sintered LTCC (CT708, CT800 and DP951) by electron beam physical vapour deposition. The effect of surface quality was assessed by thin-film deposition on free-sintered, pressure-assisted sintered, and polished DP951. The thin-films were structured by covering corresponding sections with a UV-curable photo resin and subsequent etching of the uncovered surface, leaving behind the desired structure. The etched Ni-thin films showed high difference in failure rate and sheet resistance regarding the used LTCC-material. DP951 had the lowest sheet resistance and no failure, whereas CT800 had a high sheet resistance and a failure rate of 40 %. These results are correlated with surface roughness of the LTCC, scanning electron micrographs of the deposited thin-films, and the chemical resistance of the LTCC against commonly used etching media. Contrary to the expectations, no correlation between roughness and thin-film capability was found. The LTCC with high failure rate showed a strong chemical attack by the used etching medium. Additionally, the adhesion of thin-films on DP951 is better than on CT708 and CT800. T2 - XVIII EcerS Conference & Exhibition CY - Lyon, France DA - 02.07.2023 KW - Glass-ceramics KW - Etching KW - Resistance PY - 2023 AN - OPUS4-58019 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė T1 - Structural evolution of ZrV2O7: supercell persistence revealing local and global structure duality N2 - In the AM2O7 family of negative thermal expansion materials (NTE), evidence of supercell at room temperature was reported following the Völlenke et al. discovery of missed superlattice due to the apparent linearity of the M-O-M bond in GeP2O7. Korthuis et al. and Khosrovani et al. demonstrated it to be true for cubic ZrV2O7 as well. It was concluded that at room temperature, the structure consists of 27 'subcells' with bent M2O7 groups that appear to form a linear configuration due to refinement of averaged position. However, around 100 °C, the transition to the “parent” cell was reported, where the cell volume increases, and the M-O-M angles are constrained by the Pa-3 space group symmetry to be 180°. We followed structural changes in the ZrV2O7 at high temperatures to demonstrate partial disorder within the crystal, local and global structural duality and supercell persistence at high temperatures. Total scattering measurements and Pair Distribution Function (PDF) analysis revealed that the experimental pattern cannot be fitted with the “parent structure” model, and only the 3×3×3 supercell model can correspond to local and global structures throughout the full 25-700 °C temperature range. We also show how short and long-range order within the crystal changes when approaching the phase transition, which might indicate the existence of coherent structural domains that evolve between order and disorder with increasing temperature. We further hypothesize how this can be related to the negative thermal expansion mechanism and the interpretation of structure solutions presenting data from high-temperature X-ray absorption fine structure (XAFS) and Transmission Electron Microscopy (TEM) measurements. T2 - 5th International Symposium on Negative Thermal Expansion and Related Materials (ISNTE-5) CY - Porto, Portugal DA - 29.07.2025 KW - NTE KW - Ab initio KW - PDF KW - CSM PY - 2025 AN - OPUS4-63874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė T1 - Theoretical and experimental development of negative thermal expansion material ZrV2O7 N2 - Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material which stands out for its remarkable isotropic unit cell contraction over a broad temperature range (130°C < T < 800°C). This enables the fabrication of composites where the overall expansion coefficient can be tailored to a specific negative, positive, or neutral value. Consequently, such composite materials are attractive for many device applications because they can compensate for damage caused by thermal expansion. They are relevant to optical systems, electronic and biomedical applications. In this study, we implement ab-initio-based vibrational computations with partially treated anharmonicity (quasi-harmonic approximation (QHA), temperature-dependent effective harmonic potentials (TDEP)[5]) in combination with experimental methods to follow and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder, microstructure, and defects. In analytical techniques that can provide structural information such as pair distribution function analysis (PDF), X-ray diffraction (XRD), and Extended X-ray Absorption Fine Structure (EXAFS), molecules and atoms are fit geometrically without consideration of atom interactions. Therefore, in combination with these methods, we also consider potential energy surfaces and conclude what structures are likely to form energetically in the full NTE temperature range, in addition to fitting experimental data geometrically. We also optimise experimentally fitted structures to their lowest energy configurations and re-generate comparative data to observe what differences would be visible experimentally. T2 - XLVIII International Congress of Theoretical Chemists of Latin Expression CY - Cartagena de Indias, Colombia DA - 13.07.2025 KW - NTE KW - Ab initio KW - QHA KW - TDEP KW - anharmonicity PY - 2025 AN - OPUS4-63873 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė T1 - How experimental and computational methods allow us to design negative thermal expansion materials N2 - Combined experimental and computational methods allow comprehensive understanding, design, and tailoring of material properties. We focus on a well-known negative thermal expansion (NTE) material, zirconium vanadate (ZrV2O7), and address synthesis, characterisation and validation of results with computational simulations. Experimental and computational X-ray diffraction and Raman spectroscopy data highlighted differences between phase-pure and multiphase ceramics. These techniques allowed us to distinguish subtle differences in the structure of the material. Based on ab initio simulated phonon data, unaffected by impurities or instrumental errors, we could interpret the Raman spectra and visualise Raman active atom vibrations. These computational models allowed better insight and further experimental improvement while high-quality experimental data granted the validation and improvement of computational simulation strategy. T2 - Application of Neutrons and Synchrotron Radiation in Engineering Materials Science CY - Hamburg, Germany DA - 23.03.2025 KW - NTE KW - Sol-gel KW - Ab initio KW - Raman KW - XRD PY - 2025 AN - OPUS4-62832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Bestimmung der elektrischen Durchschlagfestigkeit keramischer Werkstoffe - Einfluss von Messverfahren und -umgebung N2 - Als elektrische Durchschlagfestigkeit bezeichnet man die elektrische Feldstärke, bei der es zur Entladung durch ein isolierendes Medium kommt. Im Falle von Festkörpern ist dies ein zerstörender Prozess. Bei der messtechnischen Bestimmung der Durchschlagfestigkeit haben neben den verwendeten Messgeräten auch die eingesetzten Elektroden, die Form des Prüfkörpers und das Isoliermedium, in dem die Prüfung stattfindet, einen signifikanten Einfluss auf die ermittelten Messwerte. Im Vortrag werden die Einflüsse erläutert und anhand von Messreihen aus der Literatur und der eigenen Forschung quantifiziert. Aufgrund der vorgestellten Effekte wird klar, dass es sich bei elektrischer Durchschlagfestigkeit nicht um absolute Materialkennwerte handelt, sondern vielmehr um systemabhängige Größen. T2 - 7. Sitzung des Fachausschusses 6 - Material- und Prozessdiagnostik der Deutschen Keramischen Gesellschaft (DKG) CY - Online meeting DA - 16.02.2023 KW - Keramik KW - Hochspannungsprüfung KW - Durchschlagfestigkeit PY - 2023 AN - OPUS4-57015 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Belli, R. A1 - Hurle, K. A1 - Schürrlein, J. A1 - Petschelt, A. A1 - Werbach, K. A1 - Peterlik, H. A1 - Rabe, Torsten A1 - Mieller, Björn A1 - Lohbauer, U. T1 - Relationships between fracture toughness, Y2O3 fraction and phase content in modern dental Yttria-doped zirconias N2 - 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%. KW - Ceramics KW - Dental KW - Zirconia KW - Fracture toughness KW - X-ray-diffraction KW - Power law PY - 2021 DO - https://doi.org/10.1016/j.jeurceramsoc.2021.08.003 VL - 41 IS - 15 SP - 7771 EP - 7782 PB - Elsevier Ltd. AN - OPUS4-53107 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kang, M. T1 - Influence of mica particle content in composites for high voltage applications produced by additive manufacturing and mold casting N2 - 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. T2 - MaterialsWeek 2021 CY - Online meeting DA - 07.09.2021 KW - HV-Insulation KW - Polymer-Ceramic-Composite KW - Additive manufacturing PY - 2021 AN - OPUS4-54368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Development of textured multilayer thermoelectric generators based on calcium cobaltite N2 - 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. T2 - Virtual Conference on Thermoelectrics 2021 (VCT) CY - Online meeting DA - 20.07.2021 KW - Thermoelectrics KW - Multilayertechnik KW - Screen printing PY - 2021 AN - OPUS4-52993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Commercial LTCC for thin film deposition N2 - Low-temperature co-fired ceramics (LTCC) are used to fabricate multilayer circuits which are robust in harsh environments. Thick-film technology is well established for the metallization of circuit boards and microsystems. For specific sensor applications, the combination of LTCC and thin-film technology is advantageous to reach higher structure resolutions. Due to the high roughness of as-fired LTCC surfaces compared with silicon-wafers, the deposition of low-defect- films with narrowly specified properties is challenging. There is spare literature about thin films on commercial LTCC comparing different material systems or sintering techniques. For developing thin film sensors on multilayer circuits it is crucial to identify thin-film-compatible commercial LTCC material as well as the crucial surface properties. In this work we evaluate the thin-film capability of different LTCC surfaces. The as-fired surfaces of free-sintered, constrained-sintered (sacrificial tape), and pressure-assisted sintered commercial LTCCs (DP951, CT708, CT800), as well as respective polished surfaces, were analyzed by tactile and optical roughness measurements and scanning electron microscopy. The thin-film capability of the LTCC surfaces was assessed by sheet resistance and temperature coefficient of resistance (TCR) of deposited Ni thin-film layers. Contrary to the expectations, no correlation between roughness and thin-film capability was found. Ni thin films on constrained sintered DP951 show the lowest sheet resistance and highest TCR within the experimental framework of the as-fired surfaces. The influence of surface morphology on the film properties is discussed. T2 - KERAMIK 2022 / 97. DKG-Jahrestagung CY - Online meeting DA - 7.3.2022 KW - Roughness KW - Hydrogen sensor KW - LTCC PY - 2022 AN - OPUS4-54436 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Herstellung und Charakterisierung keramischer Federn N2 - Aufgrund ihres spezifischen Eigenschaftsprofils sind keramische Federn attraktiv für Spezialanwendungen in Maschinenanlagen, Metrologie und Sensortechnik. Durch Hartbearbeitung keramischer Hohlzylinder können Spiralfedern mit rechteckigem Windungsquerschnitt präzise gefertigt werden. Dabei kann durch gezielte Auslegung der Federgeometrie die Federkonstante über mehrere Größenordnungen variiert werden. Der Vortrag gibt einen Überblick über den Herstellungsprozess, verschiedene Eigenschaften keramischer Federn und Anwendungsbeispiele. T2 - Industrieller Arbeitskreis Keramikbearbeitung CY - Online meeting DA - 08.04.2022 KW - Keramik KW - Hartbearbeitung KW - Federkonstante PY - 2022 AN - OPUS4-54623 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Influence of surface treatment on the strength of a dental zirconia for implants N2 - Roughening of zirconia dental implants is a common clinical practice to improve ingrowth behavior. It depends on the manufacturer of the implant at which stage of the manufacturing process and by which method the surface is roughened. Systematic studies on this topic are rarely found in the literature. Therefore, the influence of surface treatment on the strength of a dental zirconia was investigated as part of a research project on the development of ceramic implants. The material under test was a commercial zirconia consisting of a Y-TZP matrix and Ce-TZP inclusions in the sintered state. This material is characterized by a slightly higher fracture toughness and slightly reduced strength compared to typical 3Y-TZP. Sets of samples were sandblasted in the white-fired or sintered condition. The ball-on-three-ball-strength of these samples was measured and compared to the strength of as-fired samples and polished samples. The complete study was performed two times for validation of the results. It is found that the average strength of TZP ceramics differs by almost 500 MPa depending on the surface treatment. Conventionally sintered specimens with as-fired surface exhibit a strength of 880 MPa. Sandblasting in the white fired state reduces the strength to 690 MPa. Both polishing and sandblasting in the sintered condition result in an increase in strength to about 1180 MPa. Comparative microstructural investigations, roughness measurements and X-ray phase analyses were carried out to determine the causes of these huge differences in strength. These findings may challenge the practice of white body surface treatment and give reason for further investigations on other commercial dental TZP materials. T2 - 97th DKG Annual Meeting - CERAMICS 2022 CY - Online meeting DA - 07.03.2022 KW - Ceramics KW - Implants KW - Biaxial strength PY - 2022 AN - OPUS4-54453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stargardt, Patrick T1 - Analysis of reaction layers and cooling simulations of co-fired thermoelectric multilayers N2 - 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. T2 - Virtual Conference on Thermoelectrics CY - Online meeting DA - 20.07.2021 KW - Ceramic multilayer KW - Cooling simulations KW - Thermal stress KW - Thermoelectric PY - 2021 AN - OPUS4-52994 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Electric field distribution on ceramic samples during dielectric strength testing N2 - 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. T2 - CERAMICS 2021 / 96th DKG Annual Meeting CY - Online Meeting DA - 19.04.2021 KW - Dielectric breakdown KW - Dielectric strength KW - Electric field strength KW - Ceramics PY - 2021 AN - OPUS4-52512 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stargardt, Patrick T1 - Dielectric properties of plasma sprayed coatings for insulation application N2 - Thermal spraying provides a rapid method for additive deposition of various ceramics as electrical insulation in applications where polymers are not suitable. New applications in complex shaped additive manufactured metal parts are emerging for example in large scale electrical devices. Microstructural and dielectric evaluation of coatings is crucial to the employment of such free-form processes. The properties and microstructure of the plasma sprayed alumina coatings are compared with dense reference samples of the same powder produced by spark plasma sintering (SPS). To obtain dense bulk samples from the coarse alumina powder for spray coating, SPS is used. Samples are fabricated by atmospheric plasma spraying (APS) of commercially available alumina powder (d50 = 33 µm) on copper substrates and by SPS of the same powder. Microstructure and porosity were analyzed by optical microscopy and scanning electron microscopy (SEM). Phase compositions were determined by X-ray diffraction (XRD). Dielectric properties such as DC resistance, dielectric strength, dielectric loss, and relative permittivity were determined according to the standards. The microstructure and dielectric properties of the coating and bulk material are compared to assess whether the coating is suitable for use in electrical insulation application. T2 - Ceramics in Europe 2022 CY - Krakow, Poland DA - 10.07.2022 KW - Dielectric characterization KW - Atmospheric plasma spraying KW - Spark plasma sintering KW - Electrical insulation PY - 2022 AN - OPUS4-55328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Ontologies and data pipelines - a field report from the development of multilayer ferrite inductors N2 - Digitalization is a current and prominent cross-cutting topic in ceramics and materials science in general. Many research initiatives and levels of significance are associated with this term. The Initiative Platform MaterialDigital (PMD), for example, aims to create a material data space filled with semantically linked data. The concept envisages that semantic relationships between the data are described as ontologies and that processing of data takes place via automated data pipelines. Various research projects from all areas of materials science are working on the implementation of this concept based on specific use cases. In the project presented here, the use case is the development of multilayer ferrite inductors as passive microelectronic components. The inductors are fabricated by ceramic multilayer technology and co-firing of metallized tapes of NiCuZn ferrite and a dielectric base material. Investigations focus on the effects of fabrication technology on the permeability of the ferrite. A data pipeline is introduced that automatically processes the unstructured experimental data into structured, machine-readable and semantically linked data. The concrete implementation of the data pipeline and a domain ontology is presented using examples. Challenges and advantages are discussed. T2 - CERAMICS 2024 / 99th DKG Annual Meeting CY - Höhr-Grenzhausen, Germany DA - 09.09.2024 KW - Ontology KW - Ceramic multilayer KW - MaterialDigital PY - 2024 AN - OPUS4-61037 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stargardt, Patrick T1 - Comparison of design concepts for ceramic oxide thermoelectric multilayer generators N2 - Multilayer thermoelectric generators are a promising perspective to the conventional π-type generators. Ceramic multilayer technology is well established for production of microelectronics and piezo-stacks. Key features of ceramic multilayer technology are full-automation, cost-effectiveness, and the co-firing of all materials in one single step. This requires similar sintering temperatures of all used materials. The development of multilayer thermoelectric generators is a subject of current research due to the advantages of this technology. One of the challenges is the compatibility of the different materials with respect to the specific design. The presented study compares three different designs of multilayer generators based on a given set of material properties. Dualleg, unileg and transverse multilayer generators are compared to conventional π-type generators., the designs are evaluated regarding the expected maximum output power and power density using analytical calculations and FEM simulations. Additionally, the complexity of the production process and material requirements are assessed and design optimizations to simplify production are discussed. Besides the theoretical aspects, unileg multilayer generator prototypes were produced by tape-casting and pressure-assisted sintering. These prototypes are compared to other multilayer generators from literature regarding the power factors of the used material system and the power density. Improvements of the power output by design optimizations are discussed T2 - 18th European Conference on Thermoelectrics CY - Barcelona, Spain DA - 13.09.2022 KW - Thermoelectric oxides KW - Thermoelectric generator design PY - 2022 AN - OPUS4-55820 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Destructive and non-destructive 3D-characterization of inner metal structures in ceramic packages N2 - Ceramic multilayer packages provide successful solutions for manifold applications in telecommunication, microsystem, and sensor technology. In such packages, three-dimensional circuitry is generated by combination of structured and metallized ceramic layers by means of tape casting and multilayer technology. During development and for quality assurance in manufacturing, characterization of integrity, deformation, and positioning of the inner metal features is necessary. Visualization with high resolution and material contrast is needed. Robot-assisted 3D-materialography is a useful technique to characterize such multimaterial structures. In that, many sections of the specimen are polished and imaged automatically. A three-dimensional representation of the structure is created by digital combination of the image stack. A quasi non-destructive approach is to perform X-ray computer tomography (CT) with different beam energies. The energies are chosen to achieve a good imaging of either the metal features, or the ceramic matrix of the structure. The combination of the respective tomograms results in a high contrast representation of the entire structure. Both methods were tested to characterize Ag and Ag/Pd conductors in a ceramic multilayer package. The results were compared in terms of information content, effort, and applicability of the methods. T2 - 98th DKG Annual Meeting - CERAMICS 2023 CY - Jena, Germany DA - 27.03.2023 KW - Ceramics KW - Synchrotron CT KW - 3D materialography PY - 2023 AN - OPUS4-57268 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Chemical resistance of commercial LTCC against thin film etching media N2 - Low-temperature co-fired ceramics (LTCC) are used to fabricate robust multilayer circuits. Typically, thick-film technology is applied for metallization. For specific sensor applications, thin films are deposited directly on the as-fired LTCC-surface. These deposited thin films are structured either by lift-off or by etching. The latter is less error-prone and thus preferred in industry provided the selected materials allow it. 200 nm Ni-thin films were deposited on three different commercial constrained-sintered LTCC (CT708, CT800 and DP951) by electron beam physical vapour deposition. The thin-films were structured by covering corresponding sections with a UV-curable photo resisn and subsequent etching of the uncovered surface, leaving behind the desired structure. The etched Ni-thin film showed high difference in failure rate and sheet resistance regarding the used LTCC-material. DP951 had the lowest sheet resistance and no failure, whereas the CT800 had a failure rate of 40 %. The LTCC with high failure rate showed a strong chemical attack by the used etching medium. To address this phenomenon, the chemical resistance of the three different commercial LTCC (CT708, CT800 and DP951) against four different commonly used etching media (sulphuric acid, phosphoric acid, aqua regia, and hydrofluoric acid) is investigated. The dissolved ions are analyzed by ICP-OES to correlate the LTCC-composition and its chemical resistance. T2 - KERAMIK 2023 / 98. DKG-Jahrestagung CY - Jena, Germany DA - 27.03.2023 KW - Glass-ceramics KW - Hydrogen sensors KW - Acids PY - 2023 AN - OPUS4-57273 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Moos, R. A1 - Rabe, Torsten T1 - Lowering the sintering temperature of calcium manganate for thermoelectric applications N2 - This study combines three different approaches to lower the sintering temperature of Sm-doped CaMnO3 to save energy in production and facilitate co-firing with other low-firing oxides or metallization. The surface energy of the powder was increased by fine milling, sintering kinetics were enhanced by additives, and uniaxial pressure during sintering was applied. The shrinkage, density, microstructure, and thermoelectric properties were evaluated. Compared to micro-sized powder, the use of finely ground powder allows us to lower the sintering temperature by 150 K without reduction of the power factor. By screening the effect of various common additives on linear shrinkage of CaMnO3 after sintering at 1100 ○C for 2 h, CuO is identified as the most effective additive. Densification at sintering temperatures below 1000 ○C can be significantly increased by pressure-assisted sintering. The power factor at room temperature of CaMnO3 nano-powder sintered at 1250 ○C was 445 μW/(m K2). Sintering at 1100 ○C reduced the power factor to 130 μW/(m K2) for CaMnO3 nano-powder, while addition of 4 wt.% CuO to the same powder led to ∼290 μW/(m K2). The combination of fine milling, CuO addition, and pressureassisted sintering at 950 ○C resulted in a power factor of ∼130 μW/(m K2). These results show that nano-sized powder and CuO addition are successful and recommendable strategies to produce CaMnO3 with competitive properties at significantly reduced temperatures and dwell times. KW - Sintering additive KW - Liquid phase sintering KW - Pressure assisted sintering PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555467 DO - https://doi.org/10.1063/5.0098015 SN - 2158-3226 VL - 12 IS - 8 SP - 1 EP - 9 PB - American Institute of Physics (AIP) CY - New York, NY AN - OPUS4-55546 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Stargardt, Patrick A1 - Moos, Ralf A1 - Mieller, Björn T1 - Co‐Fired Multilayer Thermoelectric Generators Based on Textured Calcium Cobaltite N2 - Thermoelectric generators are very attractive devices for waste heat energy harvesting as they transform a temperature difference into electrical power. However, commercially available generators show poor power density and limited operation temperatures. Research focuses on high‐temperature materials and innovative generator designs. Finding the optimal design for a given material system is challenging. Here, a theoretical framework is provided that allows appropriate generator design selection based on the particular material properties. For high‐temperature thermoelectric oxides, it can be clearly deduced that unileg multilayer generators have the highest potential for effective energy harvesting. Based on these considerations, prototype unileg multilayer generators from the currently best thermoelectric oxide Ca3Co4O9 are manufactured for the first time by industrially established ceramic multilayer technology. These generators exhibit a power density of 2.2 mW/cm² at a temperature difference of 260 K, matching simulated values and confirming the suitability of the technology. Further design improvements increase the power density by a factor of 22 to facilitate practicable power output at temperature differences as low as 7 K. This work demonstrates that reasonable energy harvesting at elevated temperatures is possible with oxide materials and appropriate multilayer design. KW - Optical and Magnetic Materials KW - Electronic PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-596306 DO - https://doi.org/10.1002/aelm.202300636 SN - 2199-160X VL - 10 IS - 3 SP - 1 EP - 12 PB - Wiley VHC-Verlag AN - OPUS4-59630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Tailoring the spring constant of ceramic helical compression springs N2 - 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. T2 - 45th International Conference and Exhibition on Advanced Ceramics and Composites (ICACC 2021) CY - Online meeting DA - 08.02.2021 KW - Ceramics KW - Hard machining KW - Spring constant PY - 2021 AN - OPUS4-52136 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Synthesis and testing of beta aluminate sodium electrolyte (BASE) for sodium ion battery development N2 - Sodium beta aluminate, or beta aluminate solid electrolyte (BASE), is an established material for tubular electrolytes in NaNiCl2 and NaS batteries, and a promising candidate for planar electrolytes in safe all solid-state batteries. The synthesis of BASE with high ionic conductivity is still challenging due to process dependent formation of different phases in the sintered material. However, to drive forward the development of active materials for all solid-state sodium ion batteries, the fabrication of solid electrolyte specimens with reproducible performance is required. With respect to the various testing scenarios in the field, for example cell assembly for cycling, electrolyte parts are needed in various shapes, sizes, and thicknesses in the lab. Different ceramic shaping technologies can be applied to produce such geometries, including pressing combined with green or hard machining, or tape casting combined with punching. Typically, different shaping technologies require adapted pre-treatment of the powder which might affect the resulting properties and thus need to be investigated. In this contribution, starting from the raw materials mixture, aspects of milling, drying, aqueous slurry preparation for tape casting, and firing are discussed with respect to particle size distribution, stability, energy consumption and resulting material properties. Finally, the fabrication and cyclic testing of Na/electrolyte/Na coin cells is presented. T2 - XIXth Conference of the European Ceramic Society / SBS6 International Sodium Battery Symposium CY - Dresden, Germany DA - 01.09.2025 KW - Ceramics KW - Beta aluminate solid electrolyte KW - Sodium ion battery PY - 2025 AN - OPUS4-64054 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stargardt, Patrick T1 - Bulk vs thermal sprayed alumina for insulation applications: A comparison of electrical and dielectrical properties N2 - Additive manufacturing (AM) processes are opening new design possibilities for large scale electrical devices such as power generators. Conventional manufacturing methods use copper rods which are wrapped, vacuum impregnated, bend and welded. These processes are labor-intensive and time-consuming. The introduction of AM methods for manufacturing the copper conductor and electrical insulation can reduce the size of the generator head, the most complex part of the generator. In this study, the electrical and dielectrical properties of additively deposited ceramic layers are investigated and compared with the properties of conventionally fabricated bulk ceramics. The ceramic layers are thermally deposited by atmospheric plasma spraying of a commercially available alumina powder. Bulk ceramics are fabricated by dry pressing and sintering of the same powder. Microstructure and porosity were analyzed by scanning electron microscopy (SEM). Electrical and dielectrical properties such as DC resistance, dielectric strength, dielectric loss, and relative permittivity were determined according to the standards. The microstructures of sprayed and sintered alumina show significant differences with respect to grain form and porosity. The density of the bulk ceramic is lower than the density of the sprayed layer due to the coarse particle size (d50 = 33 μm). Therefore, data from dense samples of the same chemical composition but lower particle size alumina powder were used for comparison. T2 - Keramik 2022 CY - Online meeting DA - 07.03.2022 KW - High Voltage Insulation KW - Thermal Spray KW - Dielectric Spectroscopy KW - Atmospheric Plasma Spraying PY - 2022 AN - OPUS4-54446 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -