TY - CONF A1 - Schröder, Jakob T1 - Neutron Diffraction Based Residual Stress Analysis of Additively Manufactured Alloys N2 - Additive manufacturing methods such as laser powder bed fusion offer an enormous flexibility in the efficient design of parts. In this process, a laser locally melts feedstock powder to build up a part layer-by-layer. It is this localized processing manner imposing large temperature gradients, resulting in the formation of internal stress and characteristic microstructures. Produced parts inherently contain high levels of residual stress accompanied by columnar grain growth and crystallographic texture. On a smaller scale, the microstructure is characterized by competitive cell-like solidification with micro segregation and dislocation entanglement. In this context, it is crucial to understand the interplay between microstructure, texture, and residual stress to take full advantage of the freedom in design. In fact, X-ray and neutron diffraction are considered as the benchmark for the non-destructive characterization of surface and bulk residual stress. The latter, characterized by a high penetration power in most engineering alloys, allows the use of diffraction angle close to 90°, enabling the employment of a nearly cubic gauge volume. However, the complex hierarchical microstructures produced by additive manufacturing present significant challenges towards the reliable characterization of residual stress by neutron diffraction. Since residual stress is not the direct quantity being measured, the peak shift imposed by the residual stress present in a material must be converted into a macroscopic stress. First, an appropriate lattice plane must be selected that is easily accessible (i.e., high multiplicity) and insensitive to micro strain accumulation. Second, a stress-free reference must be known to calculate a lattice strain, which can be difficult to define for the heterogeneous microstructures produced by additive manufacturing. Third, an appropriate set of diffraction elastic constants that relate the lattice strain to the macroscopic stress must be known. In this presentation, advancements in the field of residual stress analysis using neutron diffraction are presented on the example of the Ni-based superalloy Inconel 718. The effect of the complex microstructure on the determination of residual stress by neutron diffraction is presented. It is shown, how to deal with the determination of the stress-free reference. It is also shown that the selection of an appropriate set of diffraction elastic constants depends on the microstructure. Finally, the role of the crystallographic texture in the determination of the residual stress is shown. T2 - Deutsche Neutronenstreutagung CY - Aachen, Germany DA - 16.09.2024 KW - Additive Manufacturing KW - Neutron Diffraction KW - Electron Backscatter Diffraction KW - Laser Powder Bed Fusion PY - 2024 AN - OPUS4-61476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ulbricht, Alexander T1 - Formation of Creep Damage of 316L Produced by Laser Powder Bed Fusion N2 - The damage mechanisms of metallic components produced by process laser powder bed fusion differ significantly from those typically observed in conventionally manufactured variants of the same alloy. This is due to the unique microstructures of additively manufactured materials. Herein, the focus is on the study of the evolution of creep damage in stainless steel 316L specimens produced by laser powder bed fusion. X-ray computed tomography is used to unravel the influence of the process-specific microstructure from the influence of the initial void distribution on creep damage mechanisms. The void distribution of two specimens tested at 600 °C and 650 °C is analyzed before a creep test, after an interruption, and after fracture. The results indicate that the formation of damage is not connected to the initial void distribution. Instead, damage accumulation at grain boundaries resulting from intergranular cracking is observed. T2 - 4th Symposium on Materials and Additive Manufacturing - Additive 2024 CY - Berlin, Germany DA - 12.06.2024 KW - AISI 316L KW - Additive Manufacturing KW - Computed Tomography KW - Creep KW - Laser Powder Bed Fusion KW - Microstructure KW - PBF-LB/M/316L PY - 2024 AN - OPUS4-60295 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schröder, Jakob T1 - Diffraction and Single-Crystal Elastic Constants of Laser Powder Bed Fused Inconel 718 N2 - Laser powder bed fusion (PBF-LB/M) of metallic alloys is a layer-wise additive manufacturing process that provides significant scope for more efficient designs of components, benefiting performance and weight, leading to efficiency improvements for various sectors of industry. However, to benefit from these design freedoms, knowledge of the high produced induced residual stress and mechanical property anisotropy associated with the unique microstructures is critical. X-ray and neutron diffraction are considered the benchmark for non-destructive characterization of surface and bulk internal residual stress. The latter, characterized by the high penetration power in most engineering alloys, allows for the use of a diffraction angle close to 90° enabling a near cubic sampling volume to be specified. However, the complex microstructures of columnar growth with inherent crystallographic texture typically produced during PBF-LB/M of metallics present significant challenges to the assumptions typically required for time efficient determination of residual stress. These challenges include the selection of an appropriate set of diffraction elastic constants and a representative lattice plane suitable for residual stress analysis. In this contribution, the selection of a suitable lattice plane family for residual stress analysis is explored. Furthermore, the determination of an appropriate set of diffraction and single-crystal elastic constants depending on the underlying microstructure is addressed. In-situ loading experiments have been performed at the Swiss Spallation Neutron Source with the main scope to study the deformation behaviour of laser powder bed fused Inconel 718. Cylindrical tensile bars have been subjected to an increasing mechanical load. At pre-defined steps, neutron diffraction data has been collected. After reaching the yield limit, unloads have been performed to study the accumulation of intergranular strain among various lattice plane families. T2 - 11th European Conference on Residual Stresses CY - Prag, Czech Republic DA - 03.06.2024 KW - Additive Manufacturing KW - Laser Powder Bed fusion KW - Diffraction Elastic Constants KW - Microstructure KW - Electron Backscatter Diffraction PY - 2024 AN - OPUS4-60289 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schröder, Jakob T1 - Diffraction and Single-Crystal Elastic Constants of Laser Powder Bed Fused Inconel 718 N2 - In this presentation, the results of the determination of the diffraction and single-crystal elastic constants of laser powder bed fused Inconel 718 are presented. The analysis is based on high-energy synchrotron diffraction experiments performed at the Deutsches Elektronen-Synchrotron. It is shown that the characteristic microstructure of laser powder bed fused Inconel 718 impacts the elastic anisotropy and therefore the diffraction and single-crystal elastic constants. Finally, the consequences on the diffraction-based residual stress determination of laser powder bed fused Inconel 718 are discussed. T2 - AWT-Fachausschuss 13 "Eigenspannungen" CY - Wolfsburg, Germany DA - 19.03.2024 KW - Additive Manufacturing KW - Laser Powder Bed fusion KW - Diffraction KW - In-Situ Testing KW - Diffraction Elastic Constants PY - 2024 AN - OPUS4-59900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schröder, Jakob T1 - Influence of Microstructure on the Diffraction-Based Residual Stress Determination in Laser Powder Bed Fused Inconel 718 N2 - Additive manufacturing processes such as laser powder bed fusion (PBF-LB) offer the ability to produce parts in a single manufacturing step. On the one hand, this manufacturing technique offers immense geometric freedom in part design due to its layer-by-layer manufacturing strategy. On the other hand, the localized melting and solidification impose the presence of large temperature gradients in the process. From a microstructural perspective, this inevitably results in micro-segregation and a columnar grain structure, often paired with a significant crystallographic texture. Even worse, these large temperature gradients can lead to internal stress-induced deformation or cracking during processing. At the very least, residual stress is retained in the final structures as a footprint of this internal stress. In this context, diffraction-based methods allow the non-destructive characterization of the residual stress field in a non-destructive fashion. However, the accuracy of these methods is directly related to the microstructural characteristics of the material of interest. First, diffraction-based methods access microscopic lattice strains. To relate these lattice strains to a macroscopic stress, so-called diffraction elastic constants must be known. The deformation behavior is directly linked to the microstructure. Therefore, the diffraction elastic constants also depend on the microstructure. Second, the presence of crystallographic texture should be considered in the residual stress determination, as variations in crystal orientations contribute differently to the diffraction signal. Here we present the influence of the microstructure on the determination of residual stress by diffraction-based methods in as-built PBF-LB Inconel 718 parts. We obtained different microstructures by employing two different scanning strategies. In particular, different crystallographic textures were obtained by changing the relative angle of the scan vectors to the geometric axes of the part. The texture-based characterization of the residual stress field was carried out by surface, sub-surface, and bulk residual stress measurements. It was found that the residual stress determination significantly depends on the microstructure for strong crystallographic textures. T2 - Material Science and Engineering Congress CY - Darmstadt, Germany DA - 24.09.2024 KW - Additive Manufacturing KW - Electron Backscatter Diffraction KW - Microstructure KW - Residual Stress KW - X-ray Diffraction PY - 2024 AN - OPUS4-61475 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 wellknown 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 - SALSA Make and Measure 2024 CY - Berlin, Germany DA - 11.09.2024 KW - NTE KW - Sol-gel KW - Ab initio KW - Raman KW - XRD PY - 2024 AN - OPUS4-61358 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Miliūtė, Aistė T1 - Synthesis and phase purity of the negative thermal expansion material ZrV2O7 N2 - This repository contains computational and experimental data for the manuscript titled “Synthesis and phase purity of the negative thermal expansion material ZrV2O7”. KW - NTE KW - Sol-gel KW - Solid-state KW - Ab-initio KW - XRD KW - Raman PY - 2024 DO - https://doi.org/10.5281/zenodo.12688634 PB - Zenodo CY - Geneva AN - OPUS4-61360 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beygi Nasrabadi, Hossein A1 - Skrotzki, Birgit T1 - Ontology-Oriented Modeling of the Vickers Hardness Knowledge Graph N2 - This research deals with the development of the Vickers hardness knowledge graph, mapping the example dataset in them, and exporting the data-mapped knowledge graph as a machine-readable Resource Description Framework (RDF). Modeling the knowledge graph according to the standardized test procedure and using the appropriate upper-level ontologies were taken into consideration to develop the highly standardized, incorporable, and industrial applicable models. Furthermore, the Ontopanel approach was utilized for mapping the real experimental data in the developed knowledge graphs and the resulting RDF files were successfully evaluated through the SPARQL queries. KW - Data Mapping KW - FAIR Data KW - Ontology KW - Knowledge Graph KW - Vickers Hardness PY - 2024 DO - https://doi.org/10.4028/p-k8Gj2L VL - 149 SP - 33 EP - 38 PB - Trans Tech Publications Ltd CY - Switzerland AN - OPUS4-59981 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bayerlein, Bernd T1 - Adapting FAIR Practices in Materials Science: Digital Representation of Material-Specific Characterization Methods N2 - Age-hardenable aluminum alloys undergo precise heat treatments to yield nanometer-sized precipitates that increase their strength and durability by hindering the dislocation mobility. Tensile tests provide mechanical properties, while microstructure evaluation relies on transmission electron microscopy (TEM), specifically the use of dark-field TEM images for precise dimensional analysis of the precipitates. However, this manual process is time consuming, skill dependent, and prone to errors and reproducibility issues. Our primary goal is to digitally represent these processes while adhering to FAIR principles. Ontologies play a critical role in facilitating semantic annotation of (meta)data and form the basis for advanced data management. Publishing raw data, digital workflows, and ontologies ensures reproducibility. This work introduces innovative solutions to traditional bottlenecks and offers new perspectives on digitalization challenges in materials science. We support advanced data management by leveraging knowledge graphs and foster collaborative and open data ecosystems that potentially revolutionize materials research and discovery. T2 - TMS - Specialty Congress 2024 CY - Cleveland, Ohio, US DA - 16.06.2024 KW - FAIR KW - Research Data Management KW - Semantic Interoperability KW - Ontologies KW - Materials and Processes Data Reusability PY - 2024 AN - OPUS4-60375 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Skrotzki, Birgit T1 - Fatigue Crack Growth of Heat Resistant Austenitic Cast Iron under Isothermal and Anisothermal Conditions N2 - The heat-resistant cast iron EN-GJSA-XNiSiCr35-5-2 (Ni-Resist D-5S) was investigated for its fatigue crack growth behavior at room and high temperatures. Force-controlled tests were carried out at constant temperatures (20 °C, 500 °C, 700 °C) without and with hold time and different load ratios. The crack growth behavior was also characterized under TMF loading (Tmin = 400 °C, Tmax = 700 °C) by applying IP and OP conditions and different load ratios. Three different techniques were combined to monitor crack growth: potential drop, thermography, and compliance method. The effect of the different loading conditions on the fatigue crack growth behavior will be presented and discussed. T2 - TMF Workshop 2024 CY - Berlin, Germany DA - 25.04.2024 KW - Fatigue crack growth KW - Thermomechanical fatigue KW - Austenitic cast iron KW - Ni-Resist PY - 2024 AN - OPUS4-59964 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bhadeliya, Ashok T1 - High temperature fatigue crack growth in nickel-based alloys joined by brazing and additive manufacturing N2 - Gas turbine components, made of nickel-based alloys, undergo material damage due to high temperatures and mechanical stresses. These components need periodic replacement to avoid efficiency loss and failure. Repair of these parts is more cost-effective than replacement. State-of-the-art repair technologies, including different additive manufacturing (AM) and brazing processes, are considered for efficient restoration. Materials properties mismatches and/or internal defects in repaired parts may expedite crack initiation and propagation, reducing fatigue life. To understand the crack growth behavior in joining zones and predict the remaining life of repaired components, fatigue crack growth (FCG) tests were conducted on specimens of nickel-based alloys joined via brazing, pre-sintered preforms and AM. The FCG experimental technique was successfully adapted for joined specimens and results indicate that the investigated braze material provides a lower resistance to crack growth. In AM-sandwich specimens, the crack growth rates are significantly reduced at the interface of AM and cast material. T2 - TMS 2024 Annual Meeting & Exhibition CY - Orlando, Florida, USA DA - 03.03.2024 KW - Fatigue crack growth KW - Joined nickel-based alloys PY - 2024 AN - OPUS4-59854 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bhadeliya, Ashok T1 - High temperature fatigue crack growth in nickel-based alloys joined by brazing and additive manufacturing N2 - Nickel-based alloys have been widely used for gas turbine blades owing to their excellent mechanical properties and corrosion resistance at high temperatures. The operating temperatures of modern gas turbines have been increased in pursuit of increased thermal efficiency. Turbine blades are exposed to these high temperatures combined with mechanical stresses, resulting in material damage through creep, fatigue, and other mechanisms. These turbine blades must be regularly inspected and replaced as needed, to prevent the loss of efficiency, breakdown, and catastrophic failure. Repair of the damaged turbine blades is often a more practical and cost-effective option than replacement, as replacement is associated with high costs and loss of material resources. To this end, state-of-the-art repair technologies including different additive manufacturing and brazing processes are considered to ensure efficient repair and optimum properties of repaired components. In any repaired part, materials property-mismatches and/or inner defects may facilitate the crack initiation and propagation and thus reduce the number of load cycles to failure. Therefore, a fundamental understanding of the fatigue crack growth and fracture mechanisms in joining zones is required to enable the prediction of the remaining life of repaired components and to further improve and adapt the repair technologies. Fatigue crack growth experiments have been conducted on SEN (Single Edge Notch) specimens joined via brazing, and pre-sintered Preform (PSP) and multi-materials (casted/printed) specimens layered via additive manufacturing (AM). The experiments were performed at 950 °C and various stress ratios. The crack growth was measured using DCPD (Direct Current Potential Drop) method. The stress intensity factors for joined SEN specimens were calculated using the finite element method and then used to derive the fatigue crack growth curves. Metallographic and fractographic analyses were conducted to get insight into the fracture mechanism. Results show that the experimental technique for fatigue crack growth was successfully adapted and applied for testing joined specimens. Furthermore, the initial tests indicate that the investigated braze filler material provides a lower resistance to crack growth, and bonding defects cause a crack to deviate to the interface of the base material and joining zone. In AM-sandwich specimens, the crack growth rates are significantly reduced when the crack reaches the interface of printed material and casted material. The obtained crack growth data can be used to calibrate a crack growth model, which will further be utilized to predict the remaining life of repaired components. T2 - Fatigue 2024 Conference CY - Cambridge, UK DA - 19.06.2024 KW - Fatigue crack growth KW - Joined nickel-based alloys PY - 2024 AN - OPUS4-60893 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis T1 - Creep Behavior of Stainless Steel 316L Manufactured by Laser Powder Bed Fusion N2 - Metal additive manufacturing (Metal AM) continues to gain momentum. Many companies explore the manufacturing of innovative products, including components for safety critical applications. Despite the intensive research of recent years, a fundamental understanding of the process‑structure‑property relationships remains challenging due to, i.a., the inherently complex and highly hierarchical microstructures arising from the wide range of build process parameter variability. This contribution presents the resu lts of an experimental study on the creep behavior of an austenitic 316L stainless steel produced by laser powder bed fusion (PBF LB/M/316L) with an emphasis on understanding the effects of microstructure on creep mechanisms. Hot tensile tests and constant force creep tests at 600 °C and 650 °C, X ray computed tomography, as well as optical and electron microscopy were performed. The produced PBF LB/M/316L exhibits a low void population 0.01 %) resulting from the manufacturing parameters used and which a llowed us to understand the effects of other microstructural aspects on creep behavior, e.g., grain morphology and dislocation substructure. A hot‑rolled variant of 316L hwas also tested as a reference. The produced PBF LB/M/316L possesses shorter primary and secondary creep stages and times to rupture and smaller creep stress exponents than the hot‑rolled variant. Overall, the creep damage is more extensive in the PBF LB/M/316L and is characterized as predominantly intergranular. It is considered that the damage behavior is mainly impacted by the formation of precipitates at the grain boundaries combined with their unfavorable orientation. The dislocation substructure and local elemental segregation appear to have a decisive impact on the overall creep behavior. T2 - 16th International Conference on Creep and Fracture of Engineering Materials and Structures CY - Bangalore, India DA - 28.07.2024 KW - AGIL KW - 316L KW - Additive Manufacturing KW - Creep KW - Microstructure evolution PY - 2024 AN - OPUS4-60839 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Camin, B. T1 - Grenzflächenanalyse diffusionsgeschweißter Werkstoffpaarungen Nickel/ Nickelbasis-Superlegierung CMSX-4 N2 - Der Kirkendall-Effekt tritt bei aneinandergrenzenden Metallpaarungen auf, die höheren Temperaturen ausgesetzt sind. Es findet als Funktion von der Temperatur, der Zeit und der Konzentration die Diffusion von Atomen und Leerstellen über die Phasengrenze hinweg statt. Für die Untersuchung des Kirkendall-Effekts wurde mittels Diffusionsschweißens eine Werkstoffpaarung bestehend aus reinem Nickel (Ni) und der Nickelbasis-Superlegierung CMSX-4 hergestellt. Das Gefüge des reinen Nickels ist polykristallin und von CMSX-4 einkristallin. Da der Kirkendall-Effekt neben den oben genannten Parametern zudem von der Kristallorientierung abhängig ist, wurden zwei verschiedene Kristallorientierungen, die [111]- und [001]-Richtungen, gewählt. Aus 3D µ-tomografischen Untersuchungen ist bekannt, dass heiß-isostatisches Pressen (HIP) eine Verringerung der Porosität in CMSX-4 bewirkt, die durch die Erstarrung des Einkristalls bei der Herstellung entsteht [1]. Daher wurden bei den Diffusionsschweißungen Werkstoffpaarungen von reinem Nickel mit drei CMSX-4-Varianten -mit einer γ/γ‘-Mikrostrukturkombiniert: Ni/ CMSX-4 [111], Ni/ CMSX-4 [001] und Ni/ CMSX-4 [001]-HIPed. Die bei der Diffusionsschweißung entstehenden Grenzschichten wurden mittels Stereo-, Licht- und Rasterelektronenmikroskopie sowie EDX-Analysen untersucht. Bei allen Diffusionsschweißungen entstand eine feste Verbindung zwischen den Werkstoffpaarungen. Wie bereits aus [2] bekannt, bildet sich bei allen Proben auf der Rein-Nickelseite der Grenzfläche ein Porensaum aus, während sich auf der CMSX-4-Seite ein γ‘-freie Zone bildet (Abbildung 1). Sowohl die jeweilige Porosität als auch Porengröße des Porensaums der drei Werkstoffpaarungen ist verschieden. Dieses gilt ebenso für die durchschnittliche Schichtdicke der γ‘-freie Zone. Die geringste durchschnittliche Schichtdicke mit 1,45 µm weist die Paarung Ni/ CMSX-4 [001]-HIPed (Abbildung 1b) auf, wobei die Dicke über den Probenquerschnitt konstant ist. Dagegen schwanken die Schichtdicken der γ‘-freie Zonen bei Ni/ CMSX� 4 [111] (Abbildung 1c) zwischen 1,82 – 4,1 µm und Ni/ CMSX-4 [001] (Abbildung 1a) zwischen 1,36 - 4,55 µm. EDX-Messungen (Linescans) von der CMSX-4-Seite über die γ‘-freie Zone bis in den Nickelwerkstoff zeigen den qualitativen Verlauf der Elementkonzentrationen von Nickel und Aluminium (Abbildung 2). Bei allen Werkstoffpaarungen nimmt die Konzentration des Elements Nickel kontinuierlich zu. Während in der Werkstoffpaarung Ni/CMSX-4 [111] der Konzentrationszunahme symmetrisch über die Grenzfläche verläuft, weist Nickel bei den Werkstoffpaarungen Ni/CMSX-4 mit [001]-Orientierung keinen symmetrischer Konzentrationsverlauf auf. Daraus lässt sich schließen, dass hier die Diffusion von Nickel über die Grenzfläche in die γ‘-freie Zone in Abhängigkeit von der Kristallorientierung unterschiedlich stattfindet. Entgegengesetzt diffundiert das Element Aluminium von der CMSX-4-Seite zur Nickelseite, wie sich aus dem ebenfalls unsymmetrischen Elementverlauf schließen lässt. Bemerkenswert ist hier ein Knick, der sich nach einem Steilabfall einem Plateau anschließt, wie im vergrößerten Ausschnitt in Abbildung 2 mit einem roten Pfeil markiert ist. Dieser Verlauf ist von der Kristallorientierung unabhängig und ist auf die bessere Diffusivität von Al im Vergleich zu Ni zurückzuführen. T2 - Materialographie 2024 CY - Berlin, Germany DA - 18.09.2024 KW - Diffusionsschweißen KW - Grenzfläche KW - Nickelbasis-Superlegierung KW - Kirkendall-Effekt PY - 2024 AN - OPUS4-61095 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stargardt, Patrick A1 - Bresch, Sophie A1 - Falkenberg, Rainer A1 - Mieller, Björn T1 - Effect of Reaction Layers on Internal Stresses in Co‐Fired Multilayers of Calcium Manganate and Calcium Cobaltite N2 - A widespread recovery of waste heat requires a cost‐effective production of thermoelectric generators. Thermoelectric oxides are predestined for use at high temperatures. For manufacturing reasons, a multilayer generator design will be easily scalable and cost‐effective. To evaluate the potential of ceramic multilayer technology for that purpose, a multilayer of the promising thermoelectric oxides calcium cobaltite (Ca3Co4O9), calcium manganate (CMO, CaMnO3), and glass–ceramic insulation layers is fabricated. Cracks and reaction layers at the interfaces are observed in the microstructure. The compositions of these reaction layers are identified by energy‐dispersive X‐ray spectroscopy and X‐ray diffraction. Mechanical and thermal properties of all layers are compiled from literature or determined by purposeful sample preparation and testing. Based on this data set, the internal stresses in the multilayer after co‐firing are calculated numerically. It is shown that tensile stresses in the range of 50 MPa occur in the CMO layers. The reaction layers have only a minor influence on the level of these residual stresses. Herein, it is proven that the material system is basically suitable for multilayer generator production, but that the co‐firing process and the layer structure must be adapted to improve densification and reduce the tensile stresses in the CMO. KW - Ceramic multilayers KW - Co-firings KW - Internal stresses PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601626 DO - https://doi.org/10.1002/pssa.202300956 SP - 1 EP - 9 PB - Wiley VHC-Verlag AN - OPUS4-60162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zocca, Andrea A1 - Günster, Jens T1 - Towards a debinding-free additive manufacturing of ceramics: A development perspective of water-based LSD and LIS technologies N2 - Ceramic additive manufacturing (AM) requires a complex process chain with various post-processing steps that require expensive machines and special expertise. The key to further market penetration is AM that makes it possible to integrate into an already established ceramic process chain. Most successful AM technologies for ceramics are, however, based on processes that initially have been developed for polymeric materials. For ceramics AM, polymers or precursors are loaded with ceramic particles. This strategy facilitates the entry into AM, however the introduction of organic additives into the ceramic process chain represents a considerable technological challenge to ultimately obtain a ceramic component after additive shaping. In the present communication, two technologies based on ceramic suspensions will be introduced, the “layerwise slurry deposition” (LSD) and “laser induced slip casting” (LIS) technology. Both technologies take advantage of the high packing densities reached by conventional slip casting and moreover enable the processing of fines, even nanoparticles. KW - Additive Manufacturing KW - Ceramic KW - Water-based KW - Debinding KW - Slurry PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-605531 DO - https://doi.org/10.1016/j.oceram.2024.100632 SN - 2666-5395 VL - 19 SP - 1 EP - 13 PB - Elsevier B.V. AN - OPUS4-60553 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoffmann, Moritz A1 - Stawarczyk, Bogna A1 - Günster, Jens A1 - Zocca, Andrea T1 - Influence of additives and binder on the physical properties of dental silicate glass-ceramic feedstock for additive manufacturing N2 - Objectives The aim of the study was to investigate the impact of organic additives (binder, plasticizer, and the cross-linking ink) in the formulation of water-based feedstocks on the properties of a dental feldspathic glass-ceramic material developed for the slurry-based additive manufacturing technology “LSD-print.” Material and methods Three water-based feldspathic feedstocks were produced to study the effects of polyvinyl alcohol (AC1) and poly (sodium 4-styrenesulfonate) (AC2) as binder systems. A feedstock without organic additives was tested as the control group (CG). Disc-shaped (n = 15) and bar (n = 7) specimens were slip-cast and characterized in the green and fired states. In the green state, density and flexural strength were measured. In the fired state, density, shrinkage, flexural strength (FS), Weibull modulus, fracture toughness (KIC), Martens parameters, and microstructure were analyzed. Disc-shaped and bar specimens were also cut from commercially available CAD/CAM blocks and used as a target reference (TR) for the fired state. Results In the green state, CG showed the highest bulk density but the lowest FS, while the highest FS in the green state was achieved with the addition of a cross-linking ink. After firing, no significant differences in density and a similar microstructure were observed for all slip-cast groups, indicating that almost complete densification could be achieved. The CAD/CAM specimens showed the highest mean FS, Weibull modulus, and KIC, with significant differences between some of the slip-cast groups. Significance These results suggest that the investigated feedstocks are promising candidates for the slurry-based additive manufacturing of restorations meeting the class 1a requirements according to DIN EN ISO 6871:2019–01. KW - Firing KW - 3D-printing KW - Silicate glass-ceramics KW - Debinding PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600516 DO - https://doi.org/10.1016/j.jmbbm.2024.106563 SN - 1751-6161 VL - 155 SP - 1 EP - 12 PB - Elsevier B.V. AN - OPUS4-60051 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sänger, Johanna A1 - König, N.F. A1 - De Marzi, A. A1 - Zocca, Andrea A1 - Franchin, G. A1 - Bermejo, R. A1 - Colombo, P. A1 - Günster, Jens T1 - Linear volumetric additive manufacturing of zirconia from a transparent photopolymerizable ceramic slurry via Xolography N2 - Advanced ceramics printed with photon-based additive manufacturing deals with anisotropic mechanical properties from the layer-by-layer manufacturing. Motivated by the success in using highly filled transparent slurries containing nanoparticles for powder-based two-photon-polymerization (2PP) for advanced ceramic printing, this works approach is the transfer to Xolography, a volumetric additive manufacturing technology based on linear two-photon excitation and without recoating steps. This paper reports the results of a preliminary investigation optimizing the photocurable slurry to the requirements of Xolography in terms of transparency, over a significantly larger mean free path, compared to 2PP. A feedstock filled with 70 % weight fraction of ceramic particles (∼30 vol%) exhibiting an exceptionally high degree of transparency in the relevant wavelength range of 400–800 nm was prepared from 5 nm zirconia nanoparticles. The high transparency of the photocurable slurry is attributed to the near-monomodal particle size distribution of the zirconia nanoparticles used. KW - Additive manufacturing KW - Xolography KW - Ceramic PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608908 DO - https://doi.org/10.1016/j.oceram.2024.100655 SN - 2666-5395 VL - 19 SP - 1 EP - 9 PB - Elsevier BV AN - OPUS4-60890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Günster, Jens T1 - Ceramic Processing with Light N2 - In order to be able to manipulate ceramic powder compacts and ceramic suspensions (slurries) in their volume with light, a minimum transparency of the materials is required. Compared to polymers and metals, ceramic materials are characterized by the fact that they have a wide electronic band gap and therefore a wide optical window of transparency. The optical window generally ranges from less than 0.3 µm to 5 µm wavelength. Therefore, to focus light into the volume of a ceramic powder compact, its light scattering properties need to be tailored. In this study, we present the physical background and material development strategies for the application of two-photon polymerization (2PP), Xolography and selective volumetric sintering for the additive manufacturing of structures in the volume of ceramic slips and green compacts. T2 - CMCEE 14 CY - Budapest, Hungary DA - 18.08.2024 KW - Ceramic KW - Additive manufacturing KW - Light PY - 2024 AN - OPUS4-60892 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sänger, Johanna A1 - Riechers, Birte A1 - Pauw, Brian Richard A1 - Günster, Jens T1 - Transparent feedstocks for photon-based additve manufacturing technologies for powder processing of ceramics N2 - Photon-based additive manufacturing technologies such as SLA, DLP, LCM, moreover volumetric two-photon-polymerization, Xolography and holographic technologies promise the highest accuracy and dimensional freedom. But to transfer the light through the feedstock it needs sufficient transparency at the used light wavelength. Ceramic particles used for powder processing routes act as scattering sites and therefore hinder the light transmission, unless… The particle size and particle size distribution are chosen small and narrow enough. Particles which are smaller than roughly 1/10th of the light wavelength, mostly nanoparticles around 5nm size, decrease scattering vastly. This turns resins even with homogeneously distributed ceramic weight fraction of up to 80% transparent again. Feedstocks could be prepared for the highly accurate two-photon-polymerization gaining the smallest yttria stabilized zirconia structures with a resolution of 500nm and unique mechanical properties. The same feedstocks could be applied to DLP and LCM as layer-by-layer AM-technologies for bigger parts. Hybridizing both technologies lead to ceramic parts with microscopic accuracy at macroscopic dimensions. The feedstock was even applied to the volumetric Xolography with the highest transparency requirement so far and to versatile and flexible holographic AM. Highly filled nano-particle containing transparent ceramic feedstocks open the way for technical ceramics in high precision manufacturing where the performance and durability and accessibility are increased and created by the unique ceramic properties such as mechanical strength, chemical and thermal resistance and biocompatibility T2 - 14th International Conference on Ceramic Materials and Components for Energy and Environmental Systems CY - Budapest, Hungary DA - 18.08.2024 KW - Transparent KW - Ceramic KW - Additive manufacturing PY - 2024 AN - OPUS4-60891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -