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Quality-by-design and current good practices for the production of test and reference materials for micro- and nano-plastic research
No full textUnderstanding the environmental and human health impacts of micro- and nanoplastic pollutants is currently a high priority, stimulating intensive methodological research work in the areas of sampling, sample preparation and detection as well as intensive monitoring and testing. It is challenging to identify and quantify microplastics in complex organic matrices and concepts for nanoplastic detection are still in their infancy. All analytical techniques employed in studying micro- and nanoplastics require suitable reference materials for validation measurements, with requirements as diverse as the analytical tools used, ranging from different polymer types, size distributions and shapes of the material to the concentrations employed in different experimental set ups (ng to g amounts). The aim of this manuscript is to outline current good practices for small-scale laboratory production and characterization of suitable test and reference materials. The focus is placed on top-downfragmentation methods as well as bottom-up precipitation methods. Examples using polyethylene, polypropylene, polystyrene and polyethylene terephthalate with size distribution classes of mainly 10–1000, 1–10 and <1 μm particles will be provided. Experiences and suggestions on how to produce well-characterized micro- and nano-plastics for internal research needs will ensure that studies using the materials have robust and informative outcomes
Continuous layer deposition for the Additive Manufacturing of ceramics by Layerwise Slurry Deposition
No full textPowder bed technologies are among the most successful additive manufacturing (AM) techniques. The application of these techniques to most ceramics has been difficult due to the challenges associated with the deposition of homogeneous powder layers when using fine powders.
In this context, layerwise slurry deposition (LSD) has been developed as a deposition method that enables the use of powder bed AM technologies for advanced ceramic materials. In layerwise slurry deposition, a ceramic slurry is deposited in layers using a doctor blade and dried to produce a highly compacted powder. Not only can very fine submicron powders with low organic content be processed, but the dense powder bed also provides excellent support for the manufactured parts.
The latest development of this technology shows that it is possible to print ceramic parts in a continuous process by depositing a layer on a rotating platform on which a powder bed grows in a spiral motion. The unique mechanical stability of the layers in LSD printing makes it possible to build up a powder bed several centimeters thick without lateral support. Continuous layer deposition achieves more than 10 times the productivity of linear deposition, approaching a build volume of 1 liter per hour
Pulverbasierte additive Fertigung unter reduzierten Schwerkraftbedingungen
No full text2014 wurden die ersten additiv gefertigten Bauteile in der Internationalen Raumstation (ISS) hergestellt. Die Ära des 3D Drucks im Weltraum startete bereits 2010 mit einem NASA Projekt. Made in Space Inc. entwickelte im Auftrag der NASA einen 3D Drucker auf Basis der Fused Deposition Modeling (FDM) Technologie. Seit 2016 gibt es in der ISS eine Additive Manufacturing Facility und seitdem wurden mittels FDM mehr als hundert Teile aus Kunststoff 3D gedruckt. Die ESA arbeitet gleichfalls an der Entwicklung eines FDM-3D Druckers für die Schwerelosigkeit, z.B. im ESA Projekt „IMPERIAL“, „MELT 3D printer“. Metallische Bauteile mit guten mechanischen Eigenschaften und guter Genauigkeit können kommerziell mittels des Laserstrahlschmelzens (Laser Powder Bed Fusion LPBF) dargestellt werden. Diese Technologie kann allerdings im Weltraum nur unter der Voraussetzung angewendet werden, dass das Pulvermaterial in der Schwerelosigkeit manipuliert und in Form einer dünnen Schicht stabilisiert werden kann. Standard LBM-Anlagen sind deshalb für einen Betrieb in Schwerelosigkeit nicht geeignet, was z.B. auch von Made in Space Inc. in der Vergangenheit beleuchtet wurde. Die pulverbasierte additive Fertigung unter Schwerelosigkeit erfordert die Entwicklung völlig neuartiger Technologien zum Schichtauftrag.
Methoden:
Mit Hilfe der „Gasflussunterstützten Pulverdeposition“ wurden im Rahmen des Projekts unter reduzierter Schwerkraft systematische Parameterstudien zum LPBF-Prozess durchgeführt. Das Projekt knüpfte an erfolgreiche Vorarbeiten zur Gasflussunterstützten Pulverdeposition unter µg Bedingungen aus vier DLR Parabelflugkampagnen (30., 31., 33. und 34.) an.
Ergebnisse:
In den Parabelflugkampagnen 76 der ESA und 38 des DLR wurde eine neue Einheit in Wabenform für den Schichtauftrag von Pulver getestet. Es konnte gezeigt werden, dass diese Einheit, die auch als Pulverreservoir funktionierte und mittels eines Aktuators in Schwingungen versetzt wurde, einen reproduzierbaren Schichtauftrag mit geringem Pulververlust unter Schwerelosigkeit ermöglicht. Um die Qualität der aufgetragenen Schicht überwachen zu können, wurde ein Linienscanner beschafft und in die Anlage integriert. Mit diesem kann ein 3D Profil der Schichten im laufenden Prozess erstellt werden, was eine Qualitätskontrolle jeder einzelnen Schicht im Prozess erlaubt. Neben Edelstahl (316L) wurde das Schmelzverhalten von Regolith direkt im Pulverbett unter Bedingungen reduzierter Schwerkraft ebenfalls untersucht. Ein Modell zum Verständnis der Einflussgrößen Gravitation, Schmelzbadgröße, Partikelgröße und Zusammensetzung des Regolith wurde entwickelt.
Schlussfolgerungen:
Die Entwicklung einer leistungsfähigen Rakeleinheit für den Schichtauftrag unter Schwerelosigkeit ist Voraussetzung für die Generierung defektfreier Bauteile in der pulverbasierten additiven Fertigung in Schwerelosigkeit. Der Übergang zum Werkstoff Regolith hat die Thematik der Verwendung von lokalen Rohstoffen (ISRU), z.B. Mondstaub auf dem Mond, in Kombination mit dem Ziel einer hohen Produktivität beim Aufbau großer Strukturen hervorgebracht. Hierbei ist das Thema einer handhabbaren Schmelzpoolgröße im Laserschmelzprozess unter variierender Schwerkraft in den Fokus gerückt und wird derzeit noch beforscht
The Effect of Pore Functionality in Multicomponent Covalent Organic Frameworks on Stable Long‐Term Photocatalytic H<sub>2</sub> Production
No full textAbstractIn nature, organic molecules play a vital role in light harvesting and photosynthesis. However, regarding artificial water splitting, the research focus is primarily on inorganic semiconductors. Although organic photocatalysts have high structural variability, they tend to exhibit lower quantum efficiencies for water splitting than their inorganic counterparts. Multicomponent reactions (MCRs) offer an attractive route to introduce different functional units into covalent organic frameworks (COFs) and enable semiconducting properties and high chemical stability, creating promising materials for long‐term photocatalytic applications, such as H2 production. Herein, five highly crystalline donor‐acceptor based, 4‐substituted quinoline‐linked MCR‐COFs are presented that are prepared via the three‐component Povarov reaction. The pore functionality is varied by applying different vinyl derivatives (e.g., styrene, 2‐vinyl pyridine, 4‐vinylpyridine, 4‐vinyl imidazole, 2,3,4,5,6‐pentafluorostyrene), which has a strong influence on the obtained photocatalytic activity. Especially an imidazole‐functionalized COF displays promising photocatalytic performance due to its high surface area, crystallinity, and wettability. These properties enable it to maintain its photocatalytic activity even in a membrane support. Furthermore, such MCR‐COFs display dramatically enhanced (photo)chemical stability even after long‐term solar light irradiation and exhibit a high and steady H2 evolution for at least 15 days
Experiences with the implementation of ageing management for packages for transport of radioactive materials in Germany
No full textThe consideration of ageing mechanisms is now obligatory for the design of transport packages with integration of the para 613A into IAEA SSR-6 (Rev. 1). In addition, para 809(f) of SSR-6 (Rev. 1) requires for packages intended to be used for shipment after storage the consideration of the effects of ageing mechanisms during storage in safety analyses and the implementation of corresponding instructions for operation and maintenance. Para 503(e) requires that these packages have been maintained during storage in a manner that all requirements specified in SSR-6 (Rev.1) and in the applicable certificates of approval have been fulfilled.
The evaluation of ageing mechanisms and their effects including monitoring are part of BAM’s authority assessment tasks related to the mechanical and thermal package design and quality assurance aspects. BAM has compiled the guideline BAM-GGR 023 for the implementation of ageing assessment and related measures into the approval procedure.
The implementation of ageing management measures is obligatory in case of extension/renewal of package design approval certificates. BAM has evaluated package designs which are used only for transport as well as package designs for long term interim storage. The assessment of ageing mechanisms associated with the identification of ageing effects on components is the main part of the ageing management plan (AMP). Different approaches regarding AMP structure are introduced. Experiences and approaches about the evaluation of components for the expected package operating time are shown. We are focusing the evaluations of proofs for not accessible and not replaceable components. Operational experiences for these package designs are available and should be considered in the ageing evaluation. Corresponding measures for package monitoring are to be derived based on these results. The measures for monitoring shall be fixed in the Ageing Surveillance Program (ASP) to maintain a specification conform package for the transport on public routes. We show exemplary how results from ageing evaluation during the approval procedure are transferred into the ASP
Performance Assessment of Methane and Carbon Dioxide Sensors for D rone Based Environmental Gas Monitoring
No full textThis study evaluates the performance of methane (CH₄) and carbon dioxide (CO₂) sensors mounted on an unmanned aerial vehicle (UAV) for gas detection in open-field environments. Sensors were tested simultaneously during UAV flights over artificial gas sources, with wind data collected from two anemometers to understand plume dynamics. Field-deployed CH₄ sensors provided validation for the UAV-based measurements. The results demonstrate the sensors' effectiveness in gas detection
Synthesis and testing of beta aluminate sodium electrolyte (BASE) for sodium ion battery development
No full textSodium 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
Characterization of Beta-Alumina Solid Electrolyte by Coin Cell Testing
No full textAll solid-state batteries (ASSBs) are the subject of widespread research, one reason being their predicted increased safety [1]. Variants of beta-alumina solid electrolyte (BASE), a promising solid electrolyte for sodium ion batteries, exhibit ion conductivities up to 5 mS/cm at room temperature, which motivates targeted research and testing [2]. Dedicated measurement cells for conductivity measurements and cycling of ASSBs are available, providing even pressure and temperature control. However, these are often costly and thus unsuitable for long-term studies with many cells. In contrast, coin cells are a practical and scalable approach for such ASSB studies, despite poor pressure control and other influencing factors that may affect the reproducibility of results [3].
This study investigates the extent to which reliable measurement data can be obtained from symmetrical Na/BASE/Na coin cells. Therefore, several testing procedures and different cell architectures are considered. The experiments are supported by an electrical equivalent circuit model. The modeling approach and both measured and numerically simulated data are presented. The coin cell results are compared to data acquired using a designated ASSB setup (CompreCell and CompreFrame by RHD)
The Influence of Hydrogen Loading and Prestressing on the Sensitivity of Prestressing Steel to Stress Corrosion Cracking
No full textThis talk addresses the issue of hydrogen-induced stress corrosion cracking (HiSCC) in prestressing steels. The susceptibility to HiSCC is evaluated using free corrosion tests according to ISO 15630-3, which is problematic as it produces unreliable results. However, a new test method shows promising reproducible results and reveals that Cr-alloyed quenched and tempered (Q&T) steels are as sensitive to HiSCC as unalloyed Q&T steels
Large scale impact tests with reinforced concrete plates for impact safety
No full textAs part of a nuclear safety research project, large-scale impact tests were conducted on reinforced concrete slabs to investigate the structural integrity of containment structures under aircraft crash scenarios. The aim was to experimentally validate numerical models for both hard and soft impact conditions. Using a drop tower, concrete slabs were subjected to controlled impacts with a 404 kg impactor dropped from a height of 9.5 meters. The tests included force measurements, photogrammetric evaluations, and 3D scans to analyze deformations and damage. A total of six impact experiments were performed (2x hard impact, 2x combined hard/soft impact). The results provide a robust basis for advancing safety assessments of nuclear facilities