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Die Integration und Wiederverwendung von Wissen und Daten aus der Herstellung, Bearbeitung und Charakterisierung von Materialien wird im Zuge der digitalen Transformation in der Materialwissenschaft und Werkstofftechnologie in verschiedenen Projekten behandelt. Dabei liegt der Fokus auf der Interoperabilität von Daten und Anwendungen, die nach den FAIR-Prinzipien erstellt und veröffentlicht werden. Zur Umsetzung eines komplexen Datenmanagements und der Digitalisierung im Bereich der Materialwissenschaften gewinnen Ontologien zunehmend an Bedeutung. Sie ermöglichen sowohl menschenlesbare als auch maschinenverständliche und -interpretierbare Wissensrepräsentationen durch semantische Konzeptualisierungen.
Im Rahmen des Projektes Plattform MaterialDigital (PMD, materialdigital.de), welches in dieser Präsentation vorgestellt wird, werden Ontologien verschiedener Ebenen entwickelt (verbindende mid-level sowie Domänen-Ontologien). Die PMD-Kernontologie (PMD Core Ontology - PMDco) ist eine Ontologie der mittleren Ebene, die Verbindungen zwischen spezifischeren MSE-Anwendungsontologien und domänenneutralen Konzepten herstellt, die in bereits etablierten Ontologien höherer Ebenen (top-level Ontology) verwendet werden. Sie stellt somit einen umfassenden Satz von durch Konsensbildung in der Gemeinschaft (geteiltes Vokabular) entstanden Bausteinen grundlegender Konzepte aus der Materialwissenschaft und Werkstofftechnik (MSE) dar. In dieser Präsentation wird die PMDco adressiert.
Weiterhin wird eine auf die PMDco bezogene normenkonforme ontologische Repräsentation zur Speicherung und Weiterverarbeitung von Zugversuchsdaten – die Tensile Test Ontology (TTO) – präsentiert, die in enger Zusammenarbeit mit dem zugehörigen DIN-Standardisierungsgremium NA 062-01-42 AA erstellt wurde. Dies umfasst den Weg von der Entwicklung einer Ontologie nach Norm, der Konvertierung von Daten aus Standardtests in das interoperable RDF-Format bis hin zur Verbindung von Ontologie und Daten. Auf Grundlage der dabei entwickelten Struktur und Vorgehensweise können weitere Materialcharakterisierungsmethoden semantisch beschrieben werden, woraus sich in diesem Zusammenhang Kooperationsmöglichkeiten ergeben.
Morphological and chemical analysis of mesoporous mixed IrOx-TiOy thin films as electrode materials
(2024)
Porous films play an important role particularly in energy applications like photovoltaics, electrolysis or batteries. Thin film properties such as thickness, chemical composition, crystallinity of the framework, and porosity define the activity of the porous films. The accurate morpho-chemical characterisation of mesoporous thin films is a challenging analytical task which requires the consideration of new analytical approaches based on the combination of data of different methods able to address the structure and chemical composition at the nanoscale. In this contribution we characterise thin mesoporous iridium-titanium mixed oxide film properties by Electron Probe Microanalysis (EPMA) with Energy-Dispersive X-ray Spectroscopy (EDS) at an SEM applied in a dedicated “thin film analysis” approach (1). Thus, the film mass deposition, film thickness and the film density can be determined. Further, by dividing the measured film density to an assumed (theoretical) metal oxide framework (skeletal) density, the thin film porosity can be extracted, too.
In order to assess the homogeneity of the thin film properties like the chemical composition, Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) and Auger Electron Spectrometry are applied in the depth profiling mode, so that possible in-depth gradients are detected. Lateral inhomogeneities in the chemical composition and structure of the thin mesoporous films are also identified by applying the same methods in the line-scan or mapping mode, which can be further combined with in-depth sputtering for 3D information. The role of the spatial resolution of the analytical methods considered, which can go down well below 100 nm, will be highlighted.
Traceable morphological and chemical characterization of nanomaterials with respect to the various possible sizes, size distributions, shapes, and concentrations of real-world nanoparticles (NPs) is a challenging task. Particularly for the nonspherical, non-monodisperse nanoparticles – as typically for most of the commercial particles, including their strong tendency to agglomerate, there is a lack of standard operation procedures providing accurate nanoparticle characterisation.
In the framework of the pre-standardisation framework of VAMAS (Versailles Project on Advanced Materials and Standards, www.vamas.org) two interlaboratory comparison (ILC) studies are being carried out under the Technical Working Area (TWA) 34 “Nanoparticle Populations”:i) Project #15 addresses the analysis of the size and shape distribution of TiO2 bipyramidal NPs by traceable imaging methods such as TEM, SEM, STEM-in-SEM, AFM as well as with SAXS as an ensemble method. This ILC is thought as the next level development of the case studies exemplified in the published ISO standards ISO 21363 and ISO 19749. It was agreed to complete the first ILC with the NPs already prepared according to the same procedure on a TEM grid, and, at a later stage, to carry out second ILCs with the same NPs distributed to the participants as liquid suspensions together with protocols for the uniform NP deposition on suited substrates - as developed and optimized within the European project nPSize. Once having good deposition protocols available, the door for automated image analysis gets opened. Corresponding image analysis protocols and reporting templates have been distributed to the ILC participants, too.
ii) Project #16: two spherical SiO2 NP samples with bi-modal size distributions in two nominal relative number concentrations were prepared and distributed also as liquid suspensions accompanied by sample preparation, measurement, and image analysis protocols and reporting templates. Here, the NP concentration is the primary parameter to be measured. For the imaging methods it is targeted to
measure the relative nanoparticle concentrations (relative populations of the two modes).
The results of all the participating laboratories, in both ILCs, compiled in comparative representations will be shown and discussed for the first time. The reduction of the measurement uncertainties associated to the size, shape and number-concentration results induced by the significant improvement of the sample preparation on substrates (as single particles with a high-density coverage), combined with welldefined image analysis procedures will be highlighted.
The consideration of ageing mechanisms is with integration into the IAEA-requirements now obligatory for the design of transport packages. 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 are required. Therefore, these packages have been maintained during storage in a manner that all requirements specified in the IAEA-requirements and in the applicable certificates of approval have been fulfilled.
BAM is the competent authority in Germany for evaluating the thermal and mechanical design of packages for the transport of radioactive materials. In this context, BAM also evaluates the aging mechanisms and aging effects occurring during the long-term storage period of such transport packages. BAM has developed a guideline for the implementation of ageing assessment and of the measures for ageing management into the approval procedure based on IAEA-requirements.
The goal of the presented paper is to introduce this guideline and the general approach for ageing management requirements and to describe the application to a specific package design. The type and amount of the ageing management not only depend on the use of the packaging, but also on the accessibility of the components that are considered in the ageing assessment. The different operating phases of a packaging are considered for the ageing assessment, such as loading, interim storage or transport.
The implementation of measures for ageing management is divided into three levels – systemic measures, package design related measures and documentation. The systemic measures are attributed to the general management system and define the whole activities for organization of ageing management like structure, responsibilities, documentation, reports and evaluation. The package design related measures are defined in an ageing management plan. These measures shall ensure that the anticipated changes of the package design under consideration of ageing effects still complies with the design approval specification. Therefore, an ageing surveillance program and, if necessary, a gap analysis program shall be developed. The ageing management documentation ensures the continuous documentation of the compliance of a specific package to the approved package design, comprising mainly records resulting from operation and surveillance.
Use/distribution of cost-effective and biocompatible pieces of cellulose paper as passive optical chemosensors and readout by the camera system.
Modification of the paper surface using various chemically sensitive dyes (indicators) provides an optically detectable reaction and conclusions about the target substances and precise location.
In infrared thermography, the interaction of the heat flow with the internal geometry or inhomogeneities in a sample and their effect on the transient temperature distribution is used, e.g., to detect defects non-destructively. An equivalent way of describing this is the propagation of thermal waves inside the sample. Although thermography is suitable for a wide range of inhomogeneities and materials, the fundamental limitation is the diffuse nature of thermal waves and the need to measure their effect radiometrically at the sample surface only. The crucial difference between diffuse thermal waves and propagating waves, as they occur, e.g., in ultrasound, is the rapid degradation of spatial resolution with increasing defect depth. This degradation usually limits the applicability of thermography for finding small defects on and below the surface.
A promising approach to improve the spatial resolution and thus the detection sensitivity and reconstruction quality of the thermographic technique lies in the shaping of these diffuse thermal wave fields using structured laser thermography.
Some examples are:
• Narrow crack-like defects below the surface can be detected with high sensitivity by superimposing several interfering thermal wave fields,
• Defects very close to each other can be separated by multiple measurements with varying heating structures,
• Defects at different depths can be distinguished by an optimized temporal shaping of the thermal excitation function,
• Narrow cracks on the surface can be found by robotic scanning with focused laser spots.
We present the latest results of this technology obtained with high-power laser systems and modern numerical methods.
Thermographic NDT is based on the interaction of thermal waves with inhomogeneities. The propagation of thermal waves from the heat source to the inhomogeneity and to the detection surface according to the thermal diffusion equation leads to the fact that two closely spaced defects can be incorrectly detected as one defect in the measured thermogram. In order to break this spatial resolution limit (super resolution), the combination of spatially structured heating and numerical methods of compressed sensing can be used.
The improvement of the spatial resolution for defect detection then depends in the classical sense directly on the number of measurements. Current practical implementations of this super resolution detection still suffer from long measurement times, since not only the achievable resolution depends on performing multiple measurements, but due to the use of single spot laser sources or laser arrays with low pixel count, also the scanning process itself is quite slow. With the application of most recent high-power digital micromirror device (DMD) based laser projector technology this issue can now be overcome.
Our studies deal with the application of fully 2D-structured DMD-based excitation and subsequent super-resolution-based defect reconstruction. We analyze the influence of different testing parameters, like the number of measurements or the white content of the excitation pattern. Furthermore, we have dealt with the choice of parameters in the reconstruction that have an influence on the underlying minimization problem in terms of compressed sensing. Finally, the results of the super resolution reconstruction are compared with the results based on conventional thermographic testing methods.
Die zunehmende Bedeutung der luftgekoppelten Ultraschallprüfung (ACUT) in der zerstörungsfreien Prüfung (ZfP) unterstreicht die Notwendigkeit von standardisierten Abläufen und Methoden. Bei der ACUT bestehen grundlegende Unterschiede zur manuell durchgeführten Ultraschallprüfung mit Kontakttechnik oder zur automatisierten Tauchtechnik. Die Unterschiede bei der Bestimmung von Prüfkopfparametern für ACUT wurde von Herstellern, Forschungseinrichtungen und Anwendern bereits als wichtig erkannt, was sie veranlasst hat, im Rahmen des Unterausschusses Luftgekoppelte Ultraschallprüfung der DGZfP die Richtlinie US08 zur standardisierten Charakterisierung von luftgekoppelten Ultraschallwandlern zu erarbeiten. Darüber hinaus bestehen auch bei der Durchführung einer Messung grundlegende Unterschiede, die aktuell in einem Leitfaden zusammengetragen und definiert werden.
In diesem Beitrag wird ein Überblick über die geplanten Inhalte dieses Leitfadens gegeben. Insbesondere wird die Auswahl von Prüfparametern in Form von Frequenzen, Abständen und Positionierung sowie die Auswertung behandelt. Darüber hinaus werden die Ergebnisse eines Ringversuchs vorgestellt, welcher an einem eigens hierfür entwickelten und mit Defekten versehenem Prüfkörper, der sog. ACUT-Prüfplatte, durchgeführt wurde. In diesem Ringversuch werden unterschiedliche Messanordnungen, die mittels luftgekoppeltem Ultraschall möglich sind, anhand des erreichbaren Signal-Rausch-Verhältnisses sowie der messbaren Defektgröße quantifiziert. Zudem findet eine Abgrenzung zu weiteren gängigen Verfahren der ZfP statt. Anhand der hier vorgestellten Ergebnisse ist es möglich, die Anwendbarkeit des luftgekoppelten Ultraschalls unter Berücksichtigung unterschiedlicher Messanordnungen besser einzuschätzen.
Die größten Vorteile der luftgekoppelten Ultraschallprüfung sind: die berührungslose Prüfung und der Verzicht auf ein flüssiges Koppelmittel. Allerdings weisen die meisten luftgekoppelten Prüfszenarien ein sehr geringes Signal-zu-Rausch-Verhältnis (SNR) auf und die Pegel, die von luftgekoppelten Ultraschallwandlern realisiert werden, sind um mehrere Größenordnungen kleiner.
Da diese Herausforderung auch in anderen Disziplinen wie bspw. der Radartechnik existiert und dort ebenfalls eine entscheidende Rolle spielt, wurde die dort eingesetzte Pulskompression auf die physikalischen Gegebenheiten der luftgekoppelten Ultraschallprüfung angepasst und angewandt.
Dieser Beitrag präsentiert die Ergebnisse von zwei Versuchsaufbauten: 1) ein thermoakustischer Sender und ein optisches Mikrofon und 2) ein Paar Ferroelektret-Wandler als Sender und Empfänger. Aufgrund der physikalischen Randbedingungen wurden unipolare Kodierungen verwendet. Die Verwendung von unipolaren Kodes zur Modulation der Anregungssignale stellt dabei eine neue Methode dar, die so die Pulskompression für Ferroelektret- und thermoakustische Wandler ermöglichen soll. Die Anwendung der Pulskompression auf die Kombination aus thermoakustischem Sender und optischem Mikrofon konnte das Signal-zu-Rausch-Verhältnis um bis zu 15 dB und für die Ferroelektret-Wandler um bis zu 23 dB erhöhen.
In this paper, we investigate the influence of different heat source pulse shapes by Infrared impulse thermography (IRT) on the results of the thermal shock response spectrum (TSRS) methodology. TSRS is a new alternative approach for evaluating impulse thermography (IRT) data based on an analogy to Shock Response Spectrum (SRS) analysis (ISO 18431) for mechanical systems. It allows processing the entire recorded signal without truncating the saturated thermogram, as in pulse-phase thermography (PPT) or thermal signal reconstruction (TSR). For this purpose, we use a widespread halogen lamp as heat source as well as laser spot. The laser source enables not only to generate a precise shape of the pulse, but also to heat a specific area of the sample uniformly. This makes it possible to suppress influences of lateral fluxes due to uneven distribution of the excitation source on the surface of the specimen and leads to improved results. In order to quantitatively compare the results and to investigate the possible influence of the source shape on the TSRS, the Tanimoto criterion and the signal-to-noise ratio (SNR) were applied to the region of interest (ROI) of the carbon fiber reinforced polymer (CFRP) laminate with artificial defects as defect detectability criterion.
Mikroplastik Detektion mit Thermoanalytischen Methoden: Analytik, Referenzmaterial, Ringversuche
(2024)
Ich dem Vortrag geht es um die Vorstellung von thermoanalytischen Methoden für die Mikroplastik-Detektion. Verschiedene Kopplungsmöglichkeiten werden gezeigt und die Funktionsweise der TED-GC/MS wird erklärt. Im zweiten Teil werden Referenzmaterialien für die Mikroplastik-Analytik diskutiert. PET -Tabletten des PlasticTrace Projektes werden vorgestellt. Am Ende wird der VAMAS Ringversuch zur Mikroplastik-Detektion gezeigt.
Die additive Fertigung von Metallen hat inzwischen einen Reifegrad erreicht, der einen Einsatz in vielen Industriezweigen ermöglicht oder in greifbare Nähe rückt. Die Vorteile liegen vor allem in der Möglichkeit der Fertigung komplexer Bauteile, die sich konventionell nicht oder nur sehr aufwändig produzieren lassen, sowie in der Fertigung von hochindividualisierten Bauteilen in kleinen Stückzahlen. Allerdings ist der additive Fertigungsprozess hoch komplex und fehleranfällig. Um eine insbesondere für sicherheitsrelevante Bauteile notwendige Qualitätskontrolle zu gewährleisten, ist aktuell aufwändige nachgelagerte ZfP der einzelnen Bauteile notwendig. Alternativen könnten die In-situ-Prozessüberwachung und -prüfung bieten, die aktuell aber noch keinen ausreichenden Entwicklungsstand erreicht haben. Industrielle Fertigungsanlagen bieten keine oder nur geringe Flexibilität und Zugänglichkeit, um umfangreiche Untersuchungen auf diesem Gebiet zu ermöglichen. Daher haben wir an der BAM ein System für den Prozess des selektiven Laserschmelzens (PBF-LB/M) entwickelt, genannt SAMMIE. Es bietet eine komplett offene Systemarchitektur mit voller Kontrolle über den Prozess und flexiblem Zugang zur Baukammer, z.B. optisch sowohl direkt als auch koaxial zum Fertigungslaser. In diesem Beitrag stellen wir das System vor und zeigen erste experimentelle Ergebnisse der In-situ-Überwachung und -prüfung: Thermografische Schmelzbadüberwachung, optische Tomografie und In-situ-Laserthermografie. SAMMIE ermöglicht uns grundlegende Untersuchungen, die helfen werden, die In-situ-Prozessüberwachung und -prüfung weiterzuentwickeln, neue Erkenntnisse über die additive Fertigung zu gewinnen und die Sicherheit und Zuverlässigkeit des Prozesses zu verbessern.
For a deep process understanding of the laser powder bed fusion process (PBF-LB/M), recording of the occurring surface temperatures is of utmost interest and would help to pave the way for reliable process monitoring and quality assurance. A notable number of approaches for in-process monitoring of the PBF-LB/M process focus on the monitoring of thermal process signatures. However, due to the elaborate calibration effort and the lack of knowledge about the occurring spectral directional emissivity, only a few approaches attempt to measure real temperatures. In this study, to gain initial insights into occurring in the PBF-LB/M process, measurements on PBF-LB/M specimens and metal powder specimens were performed for higher temperatures up to T = 1290 °C by means of the emissivity measurement apparatus (EMMA) of the Center for Applied Energy Research (CAE, Wuerzburg, Germany). Also, measurements at ambient temperatures were performed with a suitable measurement setup. Two different materials—stainless steel 316L and aluminum AlSi10Mg—were examined. The investigated wavelength λ ranges from the visible range (λ-VIS = 0.40–0.75 µm) up to the infrared, λ = 20 µm. The influence of the following factors were investigated: azimuth angle φ, specimen temperature TS, surface texture as for PBF-LB/M surfaces with different scan angles α, and powder surfaces with different layer thicknesses t.
Several investigation groups have studied the flame-retardancy modes of action and properties of epoxy resins in the past; nevertheless, the selection of suitable flame retardants for epoxy resins remains challenging, and the transfer to fiber composites is difficult. The addition of flame retardants and glass fibers (GFs) to a polymeric system in a fire scenario changes the polymer's pyrolytic path and burning characteristics, reduces the heat released in the combustion, and suppresses the modes of action in the condensed and gas phase. In this study, the thermal analysis, flammability, fire behavior, residue analysis, fire stability, and quantification of modes of action of three different systems with three halogen-free flame retardants (melamine polyphosphate (MPP), ammonium polyphosphate (APP), and silane ammonium polyphosphate (SiAPP)) and three different types of GFs (unidirectional (UD), bidirectional (BD), and woven roving (WR)) will be compared with pure epoxy resin as a reference.
Distributed fiber optic sensing (DFOS) technique is a promising and robust non-destructive testing tool that can seamlessly acquire environmental conditions over large scales. Therefore, it has found extensive applications in structural health monitoring. Its appeal for monitoring underground facilities lies in the intrinsic properties of the optical fiber, such as immunity to magnetic interference, small size, chemical inertia, etc. This paper provides a concise overview of DFOS applications in underground facility monitoring. Following a brief introduction to the working principle of the DFOS technique, various examples are provided to demonstrate how distributed fiber sensors contribute to monitoring underground facilities. The paper presents unpublished field test results with an emphasis in the energy sector, including monitoring gas storage facilities, geothermal reservoir exploration, and ground movement detection. Furthermore, the paper identifies several directions for enhancing the DFOS system.
Im Rahmen des BMBF-Vorhabens SEE-2L wurde auf dem Testgelände Technische Sicherheit (BAM TTS) ein Großversuchsstand für das thermische Durchgehen von Lithium-Batterien auf Modul- und Batterieebene entwickelt und aufgebaut. Im Zuge des Projektes konnte eine erste Versuchsserie zu den Auswirkungen des thermischen Durchgehens von Batteriemodulen durchgeführt werden. Im Vortrag werden die wesentlichen Ergebnisse der Versuche vorgestellt.
Im Rahmen des Forschungsprojekts "Artificial Intelligence for Rail Inspection" (AIFRI) wird ein KI-Algorithmus entwickelt, um die Fehlererkennung und Bewertung bei der Auswertung von Schienenprüfungen mittels Ultraschall- und Wirbelstromprüfverfahren zu verbessern. Die Bandbreite möglicher Defekte und die Menge an Einflussgrößen auf die Schienenprüfung ist sehr groß, aber die Prüfdaten aus dem Feld bilden diese Bandbreite nicht balanciert ab und sind unzureichend gelabelt. Durch Simulationen werden große Mengen detailliert gelabelter Daten für relevante Schienenschädigungen und Artefakte bereitgestellt. Aus diesen Daten werden wiederum virtuellen Prüffahrten erstellt, die für das Training und die Validierung der KI genutzt werden können.
In unserem Vortrag stellen wir den Erstellungsprozess der Datensätze vor. Jeder Schritt von der Geometriedarstellung bis zur Datenverarbeitung wird erfasst. Der Fokus wird auf Simulationsergebnisse und deren Verarbeitung gelegt. Die Signalverarbeitung spielt in den Datensätzen eine große Rolle, dabei werden die Datensätze an die realen Daten angepasst. Für Wirbelstrom und Ultraschall werden diese Prozesse im Hinblick auf die Fehlertypen Head Checks und Bohrungsanrisse veranschaulicht. Ferner diskutieren wir die Simulation von Schweißnähten, die von beiden Prüfsystem detektiert werden können; und somit besondere Abstimmung bedürfen aber auch Synergieeffekte zwischen den Prüfsystem ermöglichen.
Für die Ablage der Datensätze verweisen wir auf das ebenfalls eingereichte Poster „Verwendung von DICONDE bei der Eisenbahn-Schienenprüfung“.
Das Projekt AIFRI wird im Rahmen der Innovationsinitiative mFUND unter dem Förderkennzeichen 19FS2014 durch das Bundesministerium für Digitales und Verkehr gefördert.
Revolutionizing our polymer industry for adaption to a sustainable carbon circular economy has become one of today’s most demanding challenges. Exploiting renewable resources to replace fossil-fuel—based plastics with biopolymers such as poly(lactic acid) (PLA) is inevitable while using waste streams as a raw material resource at least is promising. When it comes to using PLA as technical polymer, its high flammability must be addressed by flame retardants compatible with the thermoplastic processing of PLA and its compostability. This study proposes microalgae enriched with phosphorus from wastewater (P-Algae) as an elegant way towards a kind of sustainable organophosphorus flame retardant. The concept is demonstrated by investigating the processing, pyrolysis, flammability, and fire behavior of PLA/P-Algae, while varying the P-Algae content and comparing P-Algae with four alternative bio-fillers (phosphorylated lignin, biochar, thermally treated sewage sludge, and metal phytate) with different P-contents as meaningful benchmarks.
This presentation gives an overview of the recent achievements in simulating piping erosion during the installation process of suction bucket foundations for offshore wind turbines. The physical correctness of the code is validated, and the simulation code's performance on the LUMI supercomputer is presented. The simulation results are compared to experimental data.
Low Transformation Temperature (LTT)-Schweißzusätze stellen einen innovativen Ansatz zur Erhöhung der Ermüdungsfestigkeit geschweißter Konstruktionen dar. LTT-Schweißzusätze zeichnen sich durch eine martensitische Phasenumwandlung nahe der Raumtemperatur aus, welche Druckeigenspannungen in der Schweißnaht und der Wärmeeinflusszone (WEZ) generieren.
Dieser Vortrag fokussiert sich auf die gezielte Einbringung zusätzlicher LTT-Lagen an ermüdungskritischen Stellen von konventionell geschweißten Verbindungen. Dies ermöglicht eine ökonomische Anwendung, ohne dass die Schweißnahtintegrität zu stark beeinflusst wird. Die Auswirkungen zusätzlicher LTT-Lagen wurden anhand geschweißter Längssteifen aus hochfestem Stahl hinsichtlich der chemischen Zusammensetzung und der Eigenspannungen untersucht. Unter Variation der Schweißgeschwindigkeit und Abstand zur konventionellen Naht konnten 3 unterschiedliche Nahtausführungen des Chrom-Nickellegierten LTT-Zusatzes bewertet werden.
Die chemische Zusammensetzung wurde mittels OES-Analysen untersucht. Dabei stellte heraus, dass die Aufmischung in allen Varianten sehr ähnlich war trotz teils unterschiedlicher LTT-Volumina. Härtebestimmungen ergaben in allen 3 Varianten eine ähnliche Härte. Daraus lässt sich annehmen, dass die Martensitstarttemperatur bei allen Nahtvarianten ähnlich ist.
Röntgenografische Eigenspannungsmessungen belegen, dass die Eigenspannungen am versa-genskritischen Nahtübergang bei Einsatz von LTT-Schweißzusätzen deutlich abgesenkt werden. Während die konventionelle Schweißnaht Zugeigenspannungen von ca. 350 MPa aufweist, können an den LTT-Nähten teilweise Druckeigenspannungen von bis zu -150 MPa nachgewiesen werden. Je höher der Abstand zur konventionellen Naht und je größer das eingebrachte LTT-Volumen ist, umso stärker sind die Eigenspannungsreduzierungen am Nahtübergang. Da in allen 3 Varianten eine ähnliche Martensitstarttemperatur angenommen werden kann, ist somit die Geometrische Komponente der LTT-Zusatzlage ein entscheidender Faktor für die Eigenspannungsreduzierung.
In 2007 the license for the German Konrad repository for low and intermediate level radioactive waste was finally confirmed. Since then, the site is improved, prepared and equipped for the currently planned start of waste package emplacement in 2029. Bundesanstalt fuer Materialforschung und -pruefung is regularly contracted by the Bundesgesellschaft für Endlagerung as the responsible authority for waste product control, waste container design testing, and waste package acceptance. In this context BAM is mainly responsible for design testing of various container types including the evaluation of quality assurance measures for container manufacturing.
In addition to general requirements concerning container design, the casks have to withstand specific mechanical load scenarios. Drop tests from different heights under consideration of the most damaging drop orientation and a stacking test are two examples for necessary safety demonstrations.
If the containers are made from concrete the reinforcement has the function to absorb tensile forces the concrete is not able to withstand by its own. Because of manufacturing imperfections of cylindrical concrete containers manufactured already decades ago, the reinforcement cages are not always exactly, asymmetrically positioned when they were poured. This inspired BAM to perform various ABAQUS® finite-element (FE) simulations by using the example of a simplified cylindrical container design with generic dimensions. On the basis of the calculated tensile and compressive stress distributions suggestions are derived on how a cylindrical concrete container with an imperfectly placed reinforcement cage has to be oriented for a drop or stacking test to ensure the most damaging test scenario.
Dem AVK-Arbeitskreis Wasserstoff-Drucktanks werden ausgehend von Zielen und Aufgaben der BAM sowie der Fachkompetenz auf dem Gebiet der Sicherheit von Composite-Druckbehältern über die prüftechnische Ausstattung, die angewendeten und weiterentwickelten Prüf- und Untersuchungsmethoden sowie zu Beispielen von Forschungsvorhaben wie DELFIN, COLIBRI und SH2APED berichtet.
An Trinkwasserrohren aus ferritischem Stahl (1.4521) sind bei einigen größeren Bauvorhaben massive Korrosionsschäden aufgetreten. Die Leckagen treten ausschließlich durch Spaltkorrosion in Pressverbindungen auf, wo konstruktionsbedingt ein mit Wasser gefüllter Spalt zwischen der Rohr-Außenseite und dem Pressfitting gebildet wird. Im Vortrag werden die gewonnenen Erkenntnisse aus verschiedenen Schadensfällen der jüngeren Vergangenheit vorgestellt.
Acceptable limits for activity release from transport casks for high-level radioactive material specified in the IAEA regulations must be kept by the integrity of cask body and the cask sealing system. BAM as the German competent authority for mechanical, thermal and containment assessment of packages liable for approval verifies the activity release compliance with the regulatory limits. The specification of conservative package design leakage rates is one of the most important aspects in assessment.
Metal seals of the Helicoflex® Type are usually used to ensure the required package tightness for both, storage, and transport of the cask before and after storage. Due to the long-term use the seal behavior is influenced by temperature and time. The mechanical and thermal loadings associated with the routine, normal and accident conditions of transport specified in the regulations can have a significant effect on the leak tightness of the sealing system. Whereas the safety for application of new, non- aged Helicoflex® seals is verified sufficiently, there are still technical data gaps concerning the efficiency of aged Helicoflex® seals.
BAM performed experiments to learn more about the sealing efficiency of aged Helicoflex® seals with Aluminum and Silver outer jackets. The seals were compressed in test-flanges and for artificial ageing the complete flange systems were stored in an oven for several month at a high temperature. After this ageing procedure the flanges were opened completely, the seals were moved a little to vary the contact area, and the flanges were compressed again. During the compression and decompression tests after the aging, load-deformation characteristics of the seals, and leakage rates were measured.
With these tests a load situation was simulated, which can occur in the regulatory drop test of the cask: Under high impact loads the bolted lid can lift a little for a short moment, allowing a little movement of the seal, so that the contact area can change before compressing again.
Details about test conditions and first results will be presented in the poster.
This paper explores combining a gimbal-mounted tunable diode laser absorption spectroscopy (TDLAS) sensor and a video camera to create a virtual gas camera for methane leak detection. This provides a low-to-zero-cost extension of typical TDLAS gas tomography systems. A prototype setup mounted on a ground robot is evaluated. Results acquired using a simulated methane leak show the feasibility of the virtual gas camera, accurately detecting methane leaks by overlaying concentrations onto a visual image. While the acquisition time is significantly longer than for traditional gas cameras, potential enhancements are discussed. The study concludes that the virtual gas camera is feasible and useful, despite its longer acquisition time. It serves as a valuable software-only addition to typical TDLAS gas tomography systems, offering quickly-available on-site data augmentation for visual leak assessment at low-to-zero cost.
This paper outlines significant advancements in our previously developed aerial gas tomography system, now optimized to reconstruct 2D tomographic slices of gas plumes with enhanced precision in outdoor environments. The core of our system is an aerial robot equipped with a custom-built 3-axis aerial gimbal, a Tunable Diode Laser Absorption Spectroscopy (TDLAS) sensor for CH4 measurements, a laser rangefinder, and a wide-angle camera, combined with a state-of-the-art gas tomography algorithm. In real-world experiments, we sent the aerial robot along gate-shaped flight patterns over a semi-controlled environment with a static-like gas plume, providing a welldefined ground truth for system evaluation. The reconstructed cross-sectional 2D images closely matched the known ground truth concentration, confirming the system’s high accuracy and reliability. The demonstrated system’s capabilities open doors for potential applications in environmental monitoring and industrial safety, though further testing is planned to ascertain the system’s operational boundaries fully.
Gas Distribution Mapping (GDM) is essential in monitoring hazardous environments, where uneven sampling and spatial sparsity of data present significant challenges. Traditional methods for GDM often fall short in accuracy and expressiveness. Modern learning-based approaches employing Convolutional
Neural Networks (CNNs) require regular-sized input data, limiting their adaptability to irregular and sparse datasets typically encountered in GDM. This study addresses these shortcomings by showcasing Graph Neural Networks (GNNs) for learningbased GDM on irregular and spatially sparse sensor data. Our Radius-Based, Bi-Directionally connected GNN (RABI-GNN) was trained on a synthetic gas distribution dataset on which it outperforms our previous CNN-based model while overcoming its constraints. We demonstrate the flexibility of RABI-GNN by applying it to real-world data obtained in an industrial steel factory, highlighting promising opportunities for more accurate GDM models.
Packages for the transport of radioactive material are designed to en-dure severe accidents. Packages for the transportation of radioactive material must demonstrate that the package can withstand certain prescribed tests from the IAEA Regulations [1]. In addition to mechanical tests, a thermal test in form of a fire test must be carried out. As packages to be tested at BAM are signifi-cantly larger than previous package designs, BAM has expanded an existing fire test stand. A modular concept is chosen, which means that the arrangement of the burner nozzles can be adapted to the test specimen. The dimensions of the burner rings, the type, the orientation and the number of burner nozzles can be varied depending on the test specimen. In addition, various pumps can be used to set the corresponding mass flow. With the help of a calorimeter test, the fire test stand can be qualified for a specific size of packages regarding the boundary conditions of the IAEA Regulations [1]. Due to the typically wood filled impact limiters in German package designs, a fire test is necessary, as experiments have shown that possible openings that occurred during a mechanical test contributed to the igni-tion of the wood filled impact limiters within the prescribed 30 minutes of the IAEA Regulations [1]. From a series of experiments, two experiments are pre-sented to show the possibilities to obtain different temperatures and temperature rates in the test specimen. In addition to sensor data, the heat flux into the package is calculated to verify that the IAEA boundary conditions are satisfied. In addition to the temperature data, other data such as wind speed and wind direction are also recorded to explain subsequent effects in the measurement data in a comprehen-sible manner.
Following the new paradigm of materials development, design, and optimization, digitalization is the main goal in materials sciences and engineering (MSE) which imposes a huge challenge. In this respect, the quality assurance of processes and output data as well as the interoperability between applications following FAIR principles are to be ensured. For storage, processing, and querying of data in contextualized form, Semantic Web technologies (SWT) are used since they allow for machine-actionable and human-readable knowledge representations needed for data management, retrieval, and (re)use.
The project ‘platform MaterialDigital’ (PMD) aims to bring together and support interested parties from both industrial and academic sectors in a sustainable manner in solving digitalization tasks and implementing digital solutions. Therefore, the establishment of a virtual material data space and the systematization of the handling of hierarchical, process-dependent material data are focused. Core points to be dealt with are the development of agreements on data structures and interfaces implemented in distinct software tools and to offer users specific support in their projects. Furthermore, the platform contributes to a standardized description of data processing methods in materials research. In this respect, selected MSE methods are semantically represented on a prototypical basis which are supposed to serve as best practice examples with respect to knowledge representation and the creation of knowledge graphs used for material data.
Accordingly, this poster presentation illustrates demonstrators developed and deployed within the PMD project. Semantically anchored using the mid-level PMD Core Ontology (PMDco), they address data transformation leading to a novel data management which is based on semantic integrated data. The PMD data acquisition pipeline (DAP), which is fueled by traditional, diverse data formats, and a pipeline applying an electronic laboratory notebook (ELN) as data source are displayed. Additionally, the efficient combination of diverse datasets originating from different sources is demonstrated by the representation of a use case dealing with the well-known Orowan relation.
This contributions shows the first results of the ongoing interlaboratory comparisons under VAMAS/TWA 34 Nanoparticle populations related on the determination of pasrticle size distribution and relative concentration of nanoparticles and an example of an ILC running under VAMAS/TWA 41 Graphene and Related 2D Materials on the determination of the lateral diemsnions of graphene oxide flakes by Scanning Electron Microscopy. The link to related standardisation projects at ISO/TC Nanotechnologies are explained.
Advanced materials, such as nanomaterials, 2D materials, or thin films, play a crucial role in driving economic development and addressing major challenges in the coming years. These challenges include mitigating the impact of climate change, advancing lightweight engineering, enhancing catalysis, and improving medical applications.
To comprehend the performance of these materials and ensure their acceptance across various sectors as safe and sustainable for both humans and the environment, the availability of reference procedures, materials, and data is essential. One versatile tool for establishing such references and evaluating the proficiency of individual laboratories and their competencies is through (international) interlaboratory comparisons (ILC). Notably, initiatives like the Versailles Project on Advanced Materials and Standards (VAMAS) provide a platform for conducting ILCs.
This webinar will showcase various examples of interlaboratory comparisons, illustrating their impact on the development of reference products.
The presentation provides an overview of the current European initiatives to introduce the Digital Product Passport (DPP). Starting from the political background, reference is made to the implementation in various European directives. According to current considerations, explosives and pyrotechnics are not excluded from this. The introduction of the DPP system requires the development of a solid basis of relevant standards, which are now being developed. The aim of BAM's efforts will be to digitally align the classification processes with a view to these developments.
Germany had been transporting spent fuel to the reprocessing plant in Sellafield and La Hague for decades until around 2005. Resulting from the obligation to take back the vitrified high-level waste from reprocessing six CASTOR® HAW28M filled with 168 canisters with radioactive waste in vitrified form were transported from Sellafield to the interim storage facility Biblis in 2020. Rail wagons were used for the transport to the port in Barrow-in-Furness, where they were loaded into a dedicated seagoing vessel, certified as INF Class 3 according to the INF Code. This was the first time that vitrified high level waste with considerable heat load was transported under a German design approval certificate.
BAM was involved in the authority assessment of the conditions for the sea transport. For the first transport BAM required among others, assessment of temperature distribution during transport, logging of temperatures of cargo bays and graphical imaging of temperatures of the bay with the cask in order to ensure compliance with temperature specifications, e.g. maximal neutron absorber and gasket temperatures. Special interest was taken in the identification of possible events exceeding the specified temperatures considering the different philosophies of IMDG code and its supplement INF code regarding temperature control of hatches. Results show compliance with assumed conditions.
Electron Back Scatter Diffraction (EBSD) is a very versatile analytical technique allowing for the characterization of material structure. Historically, diffraction images (Kikuchi patterns) registered during EBSD analysis were solved using Hough/Radon transformation. The last decade brought several novel techniques of experimental pattern analysis, focusing entirely on image analysis routines such as pattern matching, or various variants of High-Resolution EBSD. However, all the above-mentioned techniques require prior knowledge of the material structure to perform orientation analysis. The recently presented algorithm employed in Crystallographic Analysis of Lattice Metric (CALM) software, effectively removes this limitation enabling a standard-less analytical approach in EBSD systems. At its core, the CALM technique couples accurate detection of the Kikuchi bands position, with a rigid construction of reciprocal lattice resulting from translational crystal symmetry. A unique characteristic of the methodology also gives an opportunity for application in the analysis of continuous lattice changes, for example tetragonality mapping. During mapping, however, the geometry of the gnomonic projection (represented by the projection center) is continuously altered decreasing overall algorithm efficiency. The work presents an analysis of the projection center in terms of precision and accuracy.
The presentation includes aspects of material design and characterization with a focus on lignin. Examples are the structural elucidation of lignosulfonates by means of two-dimensional chromatography, the mechanochemical degradation and functionalization of Kraft-Lignin with accompanying analytics. Future projects involving the incorporation of lignin into polymers will be presented.
The characterization of really unknown phases typically uses 70 to 150 reflectors for lattice metric calculation. The determination of the lattice parameters follows with 4% accuracy. Including a Z correction up to 1% can be reached. The precision of the lattice parameters ratios (a:b:c) is, however, better than 0.1%.
The talk summarizes challenges in microplastic analysis. It shows the preparation of microplastic reference materials as well as the testing on homogeneity and stability. The reference material is used in an international laboratory comparison to compare different detection methods used for microplastic analysis. The methods used were µ-IR (FTIR+LDIR) for number-based methods and TED-GC/MS and Py-GC/MS for mass-based methods. The ILC was done under the umbrella of VAMAS TWA 45. Results of the participants are presented.
Efficient flame retardancy is often achieved only when applying synergistic multicomponent systems. Flame retardants are combined or used together with adjuvants or synergists to enhance their efficiency, reduce the amount required, or reduce the costs; fibers and fillers contribute to fire properties crucially. Although the main flame-retardant modes of action are known, the detailed scientific understanding usually falls short, when it comes to complex synergistic multicomponent systems, the important tiny optimizations, or quantifying in terms of specific fire properties. This paper tries to illuminate the concept of synergistic flame retardants. The need for the multicomponent approach and the main phenomena are described. Thought-provoking impulses are delivered on how the understanding of multicomponent systems promotes the evidence-based development of future flame retardant polymeric materials. Multicomponent systems are discussed in their capacity as general powerful strategy for achieving and optimizing flame retardant polymeric materials.
This paper is based mainly on the overall conclusions and concrete results of several projects performed in the group of the author. Thanks to my (former) students and co-operation partners in these projects. Thanks for financing to DFG (Scha 730/8-1 Scha 730/8-2, Br 3376/1-1, Scha 730/19-1), AiF IGF (438 ZN, 17833N/2, 19078 N/2), and BMBF (03X0111C, 01DN16040).
Normung und Standardisierung in der zerstörungsfreien Prüfung finden auf nationaler, europäischer und internationaler Ebene statt. Die Übernahme von Leitungsfunktionen in diesen Gremien erzeugt die Möglichkeit der Steuerung von Themen und Inhalte der relevanten Normen. Das persönliche Engagement der Fachexpert*innen in den nationalen Gremien und den europäischen und internationalen Arbeitsgruppen ist ein zusätzlicher Faktor für die inhaltliche Korrektheit und die erwünschte inhaltliche Ausrichtung der Norm. Denn wer nicht normt wird genormt und muss letztlich Regeln verwenden, die andere entsprechend ihrer eigenen Interessen gestalten. Voraussetzung für die Teilnahme in europäischen und internationalen Normungsgremien ist die Mitwirkung in den entsprechenden DIN-Spiegelgremien, welche die europäischen (CEN) und internationalen (ISO) Aktivitäten spiegeln und die Fachexperten für die Mitarbeit autorisieren. Auf internationaler Ebene findet die Normungsarbeit in den technischen Komitees ISO/TC 135 “Non-destructive testing” und ISO/TC 44/SC 5 “Testing and inspection of welds” und ihren Arbeitsgruppen statt. Das europäische Pendant ist das CEN/TC 138 “Zerstörungsfreie Prüfverfahren” mit seinen Arbeitsgremien. Die DIN-Spiegelgremien sind für die deutsche Mitarbeit in diesen Gremien und die inhaltliche Bewertung der Norm-Entwürfe zuständig.
Motivated by the aim of developing an additive manufacturing (AM) technology easily integrated in the process chains of the ceramic industry, the LSD-print technology was conceived as a slurry-based variation of binder jetting (BJ).
BJ and other powder bed technologies (such as powder bed fusion) are amongst the most successful AM techniques, especially for metals and polymers, thanks to their high productivity and scalability. The possibility to use commercially available feedstocks (in the form of powders or granules) makes BJ also attractive for ceramic materials. The application of these techniques to most advanced ceramics has however been difficult so far, because of the limitations in depositing homogeneous layers with fine, typically poorly flowable powders.
In this context, the "layerwise slurry deposition" (LSD) was proposed at TU Clausthal (Germany) as a slurry-based deposition of ceramic layers by means of a doctor blade. Combined with layer-by-layer laser sintering of the material, the LSD process was originally demonstrated for the rapid prototyping of silicate ceramics. Due to the difficulties in controlling the microstructure and the defect formation in laser-sintered technical ceramics, the LSD process was later combined with inkjet printing in the LSD-print technology, which has been further developed at BAM (Germany) in the past decade.
The LSD-print technology combines the high speed of inkjet printing, typical of BJ, with the possibility of producing a variety of high-quality ceramics with properties comparable to those achieved by traditional processing. Due to the mechanical stability of the powder bed, the process can also be carried out with continuous layer deposition on a rotating platform, which further increases its productivity.
This presentation will delve into 10 years of research on the LSD-print of a wide variety of technical ceramics including alumina, silicon carbides and dental ceramics. The discussion highlights how a seemingly small process and feedstock modification (from powders to slurries) has great influence on the challenges and potential of this process, which are being addressed on its path to industrialization.
Multiphoton lithography (MPL), an emerging microfabrication technique, shows great potential in a variety of applications ranging from tissue engineering to soft micro-robotics. Fabricated micro-objects often are expected to undergo shape morphing or bending. Furthermore, ensuring precise property tuning becomes detrimental for the functionality of MPL microstructures. Herein, we present novel MPL materials based on interpenetrating networks (IPNs), which effectively combine the advantages of acrylate and epoxy thermoset systems. A library of 3D MPL IPN microstructures with high 3D structural stability and tailored thermal and micromechanical properties is achieved. MPL laser velocity and fabrication power can be used to tune the morphology and therefore properties of IPN. New IPN microstructures with materials Young's moduli of 4 to 6 MPa demonstrate susceptibility to deformation with high to fully elastic response. Such soft elastic materials hold immense promise within morphable microsystems, soft micro-robotics and cell engineering applications.
Powder bed technologies are amongst the most successful Additive Manufacturing (AM) techniques. The application of these techniques to most ceramics has been difficult so far, because of the challenges related to the deposition of homogeneous powder layers when using fine powders.
In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method enabling the use of powder bed AM technologies also for advanced ceramic materials. The layerwise slurry deposition consists of the layer-by-layer deposition of a ceramic slurry by means of a doctor blade, in which the slurry is deposited and dried to achieve a highly packed powder. Not only very fine, submicron powders can be processed with low organics, but also the dense powder bed provides excellent support to the parts built. The LSD technology can be combined with binder jetting to develop the so-called “LSD-print” process. LSD-print combines the high-speed printing of binder jetting with the possibility of producing a variety of high-quality ceramics with properties comparable to traditional processing.
The latest development of this technology shows that it is possible to print ceramic parts in a continuous process by depositing a layer onto a rotating platform, growing a powder bed following a spiral motion. The unique mechanical stability of the layers in LSD-print allows to grow a powder bed several centimeters thick without any lateral support. The continuous layer deposition allows to achieve a productivity more than 10X higher compared to the linear deposition, approaching a build volume of 1 liter/hour.
Since microplastics (MPs) can be found everywhere and are becoming a problem of high concern, it is necessary to understand their physico-chemical properties. To obtain reliable analytical data a set of validated methods for sampling, sample preparation, detection, and data evaluation are needed.
To meet these needs an interlaboratory comparison (ILC) with 84 participants worldwide has been organized under the international pre-standardisation platform VAMAS (www.vamas.org/twa45/) as Project 2 “Development of standardized methodologies for characterisation of microplastics with microscopy and spectroscopy methods” within the Technical Working Area TWA 45 “Micro and Nano Plastics in the Environment”. In this ILC thermo-analytical methods (Py-GC/MS and TED-GC/MS) and vibrational methods (µ-Raman and µ-FTIR) have been tested and compared by providing a set of microplastic representative test materials and measurement protocols developed at BAM. The defined measurands were: particle number concentration, particle size distribution (PSD), and polymer identity and mass content. To increase the statistical quality, 6 samples were shipped together with blank samples. Hence, the ILC provides information on precision and accuracy of the results obtained with different methods as well as strengths and limitations of the proposed protocols.
The development of standards that include simulation models is often based on heuristics that include experimental data that is used to calibrate and validate the simulation models. However, these data and the corresponding calibration procedures are usually not part of the publicly accessible documentation making it very difficult to identify gaps in the current standard or extend it to new innovative solutions. The poster shows an adapted procedure that integrates the complete process into a database and a workflow to be published alongside the standard.
Fully automated and decentralized fused filament fabrication of ceramics for remote applications
(2024)
Manufacturing of ceramic components 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 ceramic components with complex geometries. 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. This poster presents an innovative approach: 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 parts are printed onto thin sacrificial rafts, which are built using an interface material with the same binder as the ceramic 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 of the ceramic parts and easy removal of the finished parts. In conclusion, our integrated approach enables significant advancements in the fabrication of complex ceramic components in remote environments with increased efficiency and minimal human handling.
The Laser-Induced Slip Casting is an additive manufacturing technology specifically developed for ceramic materials using water-based ceramic slurries. The process takes place layer-by-layer in a similar fashion as top-down vat photopolymerization, selectively consolidating each layer by means of a laser energy source positioned on the top. Contrary to vat photopolymerization, in which the consolidation is achieved by selectively cross-linking a ceramic-filled resin, LIS uses water-based slurries with a low amount of organic additives (typically < 5 wt%) as feedstocks.
In LIS, a green body is formed by local evaporation of water which causes the suspension to collapse forming a cast, following a mechanism similar to slip casting. Only a small content of organic additives is needed to effectively disperse the ceramic particles and to increase the green strength.
The technology is very versatile and can be applied to all ceramic systems that can be dispersed in water. One of the main advantages is that even dark materials such as silicon carbide can be processed without issues related to light scattering and absorption.
The presentation will discuss strengths and limitations of LIS compared to other AM technologies and will highlight the latest results for alumina and for silicon carbide ceramics.
Blast injuries are among the most common injuries in military operations. Also, in civilian environments, more explosive threats are expected in the future due to emerging conflicts and threats. While the effect of fragments, which is classified as secondary blast injury, could be minimized by police and military personnel’s modern ballistic body protection systems, the effects of shock wave propagation in the body as part of the primary explosion trauma still remain a serious threat needing further research.
The detonation-physical processes of highly dynamic pressure changes within the human body, the reflection-related amplification of shock waves at organ-dermis interfaces, and the consequences of injury mechanisms have become more prominent in international research. Various approaches have been used to investigate these aspects. Animal experiments on free field test sites or shock tube setups combined with a subsequent biological evaluation and numerical simulations provided promising results and allowed the discussion of different biomechanical aspects. However, due to poor reproducibility and a lack of short-term dynamic material properties, most research approaches have significant limitations. Laboratory test setups do not represent real-scale high explosive detonation parameters with regards to pressure characteristics, impulse duration and blockage problems. Measured values are interpreted with partly outdated, selective and not validated limit values for overpressures from field tests with animals. This is due to the lack of a validated and comprehensive data set covering a variation of the crucial parameter. Injury mechanisms and their effects have not yet been sufficiently elucidated for the torso and extremities.
In order to contribute to the research efforts on the primary explosion effects, the German Federal Armed Forces established an interdisciplinary military medical research project in cooperation of the Bundeswehr Hospital Berlin and the German Federal Institute for Materials Research and Testing (BAM). The aim of the planned investigation is the development of a multidisciplinary method to investigate shock wave behavior in various generic tissue simulants under the most reproducible conditions possible with realistic loads in an experimental test series with short set-up times.
The presentation will start with an overview of ceramic additive manufacturing (AM) technologies and will discuss the potential of AM in the field of bioceramics.
The presentation will then focus on two possible use cases of binder jetting technologies.
In the first example, standard powder-based binder jetting is used to manufacture a porous implant design for large scale bone defects. The related challenges in the process chain will be discussed, from powder synthesis to sintering and characterization of the printed part.
In the second example, the LSD-print slurry-based binder jetting technology is presented as a possibility to adapt powder-bed AM to produce dense ceramic parts. The use case will focus on an application in the field of dental ceramics, specifically for the manufacturing of patient individualized single tooth restorations (veneers, crowns) with a high throughput process chain.
Der Bau von Gründungs- und Turmstrukturen für Windkraftanlagen erfordert den Einsatz moderner, nachhaltiger und ressourcenschonender hochfester Feinkornbaustähle. Durch den Schweißprozess verursachte Schweißnahtfehler sind nicht akzeptabel. Um diese zu beheben, ist das lokale thermische Fugenhobeln mit anschließendem Reparaturschweißen ein gängiges und wirtschaftliches Verfahren. Die hohe Schrumpfbehinderung um die ausgefugte Nut durch das umgebende Gefüge kann zu Rissbildung führen, wenn sich konstruktiv bedingte Spannungen und Eigenspannungen aus der Reparaturschweißung überlagern. Diese Gefahr wird durch die Verschlechterung der Mikrostruktur und der mechanischen Eigenschaften hochfester Stähle während des Schweißreparaturprozesses noch verstärkt.
Der Vortrag stellt die wesentlichen Inhalte sowie die wichtigsten Änderungen der TRGS 510 "Lagerung von Gefahrstoffen in ortsbeweglichen Behältern" vor.
Die TRGS 510 zeichnet sich durch ein gestuftes Maßnahmenkonzept in Abhängigkeit von der Art und Menge der gelagerten Gefahrstoffe aus. Folgende Maßnahmenstufen werden durch die TRGS 510 beschrieben:
1. Kleinmengen -> Allgemeine Maßnahmen
2. Überschreitung der Kleinmengen -> Lagerung im Lager
3. Überschreitung bestimmter Mengen für spezielle Gefahrstoffe -> Spezielle Maßnahmen
4. Verschiedene Gefahrstoffe und Lagerung im Lager erforderlich -> ggf. Getrenntlagerung und Separatlagerung
Following directly from the information presented at IFBIC 2023 on the research project 'Investigation of intracorporeal shock wave propagation using a simplified torso model and a shock wave generator', the latest results are presented below [1]. In order to contribute to the research efforts on the primary explosion effects, the aim of the investigation is the development of a multidisciplinary method to investigate shock wave behavior in various generic tissue simulants under the most reproducible conditions possible with realistic loads in an experimental series with short set-up times.
To achieve this, an autoclave with a volume of 0.065 m3 is used to generate reproducible pressure waves (Fig. 1). The autoclave will be referred to as Shockwave Generator (SWG). The pressure wave is produced by the detonation of a stoichiometric mixture of acetylene and oxygen under atmospheric conditions. The SWG-outlet is sealed by a rupture disc, which can be adjusted in thickness to vary the initial pressure. Additionally, modifying the composition of the acetylene-oxygen mixture can result in different load cases. The SWG requires approximately 30 minutes of set-up time between trials. The SWG was adjusted to match the characteristics of a real and typical explosive through free-field measurements. The experiments demonstrated that the pressure wave propagates in a hemispherical shape and has sufficient reproducibility.
To represent soft tissue, a basic model made of homogeneous ballistic gelatin is used in a geometrically simplified torso model (STM) (Fig. 2). The STM was enlarged to outer dimensions of 400 x 250 x 240 mm. Viscoelastic behavior of the ballistic gelatin can be assumed due to the collagen structure [2]. The density of the ballistic gelatin, and therefore the sound velocity, can be adjusted by changing the mixing ratio. Simplified simulants, such as hollow and solid material (bone simulant), were embedded in the STM. Additionally, the STM has been tested as a carrier material for biological substances, such as indicator species. The next step is to test the STM as a carrier material for larger organic tissue structures such as lungs or kidneys. The organic tissue samples will undergo histological examination to analyze their structural changes afterwards. The STM is equipped with embedded piezoelectric pressure sensors, an accelerometer and a temperature sensor. Visual documentation is captured using a high-speed camera. This measurement setup allows for the tracking of the coupled pressure wave and its behavior within the model and at the media transitions. Pressure values can be recorded after certain media changes, such as from soft tissue to a solid material (Figure 3).
The following is a review of the optimizations made to the entire experimental setup. The reproducibility of the SWG was increased. This was achieved by extending the evacuation process to the entire feed system of the SWG. Nitrogen residues in the SWG system can thus be avoided. As a result, the double peaks that occur at the first maximum can be avoided, as combustion runs more evenly without the nitrogen residues. In addition, partially varying peak overpressures can be avoided, as the acytelene-oxygen mixture is not too lean due to the elimination of the nitrogen residues. The workflow has been streamlined, resulting in an average set-up time of 25 minutes for the SWG. In the case of the STM, the manufacturing process in particular was optimized by examining and defining the manufacturing process based on scientific publications, which increases the reproducibility of the STM base bodies. As already mentioned in the previous paragraph, the STM was equipped with various additives in order to investigate the transition behavior of the pressure wave.
The following trail serves as an example: A comparison is made between the STM in the basic structure (Fig. 2 l.s.) and with an embedded solid material (bone plate) (Fig. 3 l.s.). An external overpressure of 100 kPa is generated by the SWG at a distance of 1 m, where the STM is placed. For the basic STM structure, the sensor distance is consistently 100 mm. The internal overpressure is visible in Fig. 2 r.s.. A typical ideal pressure curve can be seen. The characteristic points are easily distinguishable from the reflection peaks. In the STM with an embedded solid material, the sensor distance remains consistently at 66.6 mm
Per- and polyfluoroalkyl substances (PFAS) were classified as a group of highly concerning chemicals over the last decades. Because of the high persistence of PFAS, their previous use led to contamination of the environment and human population. Due to ongoing use and incomplete remediation or destruction methods, the PFAS background in the environment is growing continuously.
The presence of ultrashort PFAS (with ≤3 carbon atoms) in the environment is often overlooked despite their contributions to PFAS levels. These compounds may directly contaminate the environment and arise from degradation of polyfluorinated compounds as well as incomplete PFAS destruction in certain industrial processes. Nonetheless, few approaches for targeted analysis of ultrashort PFASs have been developed, except for trifluoroacetic acid (TFA). Beside liquid (LC-MS/MS), supercritical fluid (SFC-MS/MS), and ion chromatography (IC-MS)-based systems, gas chromatography coupled with mass spectrometry (GC-MS) is a promising method for detection and quantification of ultrashort PFAS.
The goal of this study was to develop a simple headspace GC-MS method for the quantification of ultrashort perfluorocarboxylic acids (PFCAs) and polyfluorinated alcohols (PFOHs) in water samples. In contrast to PFOHs, functionalization of PFCAs was required for quantification. This was done by esterification with methanol at 80 °C, which can be carried out directly in the headspace GC-MS system.
Moreover, several parameters were optimized to achieve a low limit of quantification (LOQ) for the analytes used: i) The ratio of the aqueous solution, methanol, and available gas phase within the analysis vessel, ii) the concentration of additional acid in esterification mixtures of PFCAs, iii) shaking frequency and iv) shaking time before analysis. After optimizing the procedure, we were able to quantify ultrashort PFCAs and PFOHs. Thus, our developed headspace GC-MS method has the potential to be used as an alternative target analysis for ultrashort-chain PFCAs and PFOHs in various water samples (groundwater, wastewater).
Since microplastics (MPs) can be found everywhere and are becoming a problem of high concern, it is necessary to understand their occurrence and fate in the environment. However, to obtain data of high quality is very challenging, since measurement operating procedures differ from laboratory to laboratory. Currently, there are no standardized methods to analyze microplastics. One promissing possibility to adress standardization of the methodology and operating procedures are interlaboratory comparisons (ILCs). In this contribution we report the first results of an ILC on microplastic detection methods organized under the pre-stantdardisation plattform of VAMAS (www.vamas.org/twa45/) as Project 2 “Development of standardized methodologies for characterisation of microplastics with microscopy and spectroscopy methods”, within the Technical Working Area TWA 45 “Micro and Nano Plastics in the Environment”. The ILC has gathered 84 participants all over the world representing all continents. BAM, as the project leader, produced a set of reference microplastic materials, which have been distributed to all the participants together with the measurement protocols and reporting data templates.
Microplastic and nanoplastic particles (MNP) are spread all over the world in various types, shapes and sizes making it very challenging to accurately analyse them. Each sampling procedure, sample preparation method and detection technique needs suitable reference materials to validate the method for accurate results. Furthermore, the effects of these MNPs should be evaluated by risk and hazard assessment with test particles close to reality. To better understand MNP behavior and aid in clarification of their interactions with organisms, we produced several MNP materials by top-down procedure and characterized their properties. Since surface properties mostly determine particles’ toxicity, the aim of the present study was to determine which functional groups are present on MNPs and how the surface can be affected by the production process and particle’s environment.
Preliminary results of an interlaboratory comparison on microplastics organised by plasticsfate
(2023)
Microplastics are everywhere in the environment, but analytics is challenging. Since harmonisation is missing as well es suitable reference materials, BAM did under th umbrella of VAMAS funded by the EU Horizon 2020 project PlasticsFate a ILC for microplastic detection methods. Methods adressed were IR, Raman, Py-GC/MS and TED-GC/MS. The talk gives a first presentation and evaluation on the results.
Monitoring of microplastics in food matrices is crucial to determinate the human exposure. By direct ingestion microplastics could be released in the food during the production, through packaging and by consumer’s use. The absence of standard methods to quantify and detect different size range and type of microplastics has led to difficult and time consuming procedural steps, poor accuracy and lack of comparability. In this work, matrix characterization and laboratory experiments were used to investigate the efficiency of sample preparation in milk powder. This information is crucial to compile a standard procedure for sample preparation and digestion of common milk powder to detect different particle sizes and types of polymers. Charaterisation is done by TGA and TOC measurements.
Die Probenpräparation ist ein wichtiger Schritt für die Qualität der Massenspektren in MALDI-TOF MS. Es werden Polymerproben, die lösungsmittelbasiert und lösungsmittelfrei präpariert worden sind, verglichen. Dabei werden die Intensitätsverhältnisse von ternären Mischungen von PEG-, PS- und PMMA-Polymeren beachtet.
MALDI TOF Massenspektrometrie wurde verwendet, um Kristallisationsprozesse in Polyestern (Polylactide, Polyglycolide) zu untersuchen. Dabei konnte gezeigt werden, dass Zyklen und Linearen simultan, aber in unterschiedlichen Kristalliten, kristallisieren. Die dabei ablaufenden Umesterungen (Transesterifizierungen) konnten mit der MALDI TOF Massenspektrometrie nachgewiesen werden. Damit wurde ein völlig neues Anwendungsgebiet dieser MS Methode demonstriert.
An Amorphous Lewis-acidic Zirconium Chlorofluoride as HF Shuttle: C-F Bond Activation and Formation
(2024)
In recent years, fluorine chemistry has gained increasing political attention. Owing to a growing shortage of fluorspar, a raw material used for producing fluorinated base chemicals, fluorospar has been named among the 30 critical raw materials in the EU.2 As such, it becomes increasingly important to recycle existing fluorinated compounds and make them available as sources of fluorine for reactions. Significant progress has been made in the field of C-F bond activation using heterogeneous catalysts such as aluminum chlorofluoride (ACF).3–5 However, the transfer of fluorine atoms from one molecule to another using heterogeneous catalysts has not yet been reported. In this study, we successfully synthesized amorphous zirconium chlorofluoride (ZCF), and we were able to establish a catalytic behavior of ZCF in C-F bond activation reactions. We present a heterogeneous catalyst that performs dehydrofluorination of a fluoroalkane and consecutive hydrofluorination of an alkyne at room temperature.
Owing to a growing shortage of fluorspar, a raw material used for producing fluorinated base chemicals, fluorspar has been named among the 30 critical raw materials in the EU. 1 However, the sustainable transfer of fluorine atoms from one molecule to another using heterogeneous catalysts has not yet been reported. Herein, we present the heterogeneous catalyst zirconium chloro fluoride (ZCF) that performs dehydrofluorination of a fluoroalkane and consecutive hydrofluorination of an alkyne at room temperature.
Microplastic reference material is required for validation and harmonization purposes. This includes the analysis of the pure polymer particles and the validation of the respective measurement methods. In addition, there is the harmonization of different laboratories. On the other hand, sample preparation methods must be validated and harmonized with regard to their recovery and subsequent analysis in the respective matrices. For this purpose, we produce reference material candidates in the form of tablets with different mass fractions and particle numbers of polyethelene terephthalate. In the presentation first measurement results by µ-Raman, µ-FTIR, pyrolysis-GC-MS and TED-GC/MS will be presented.
Bei der zerstörungsfreien Prüfung verlegter Eisenbahnschienen werden die Rohdaten derzeit in proprietären Datenformaten gespeichert und auf Datenträgern zwischen den Prüfzügen und den auswertenden Stellen versendet. Die proprietären Datenformate sind in der Regel nur den Herstellern der Prüfsysteme bekannt und deren Dokumentation nicht allgemein zugänglich.
Die „Standard Practice for Digital Imaging and Communication in Nondestructive Evaluation“ (DICONDE), basierend auf dem medizinischen Standard „Digital Imaging and Communication in Medicine“ (DICOM), ermöglicht es, sowohl Prüfdaten als auch Prüfergebnisse und Streckeninformationen in einem standardisierten Format zu speichern und zwischen verschiedenen Endpunkten zu übertragen.
Das Poster gibt zunächst einen kurzen Überblick über die hierarchische Struktur von DICONDE und zeigt dann, wie DICONDE bei der Prüfung verlegter Eisenbahnschienen verwendet werden kann. Die geometrischen Besonderheiten (mehrere Kilometer Länge pro Prüffahrt, kurviger Streckenverlauf) stellen dabei eine besondere Herausforderung dar. Im Rahmen des mFUND-geförderten Projektes „Arteficial Intelligence for Railway Inspection (AIFRI)“, Förderkennzeichen 19FS2014C, wurde ein Vorschlag für eine Erweiterung des DICONDE-Standards für die Schienenprüfung erarbeitet und bei der ASTM eingereicht.
Following the recommendation of the European Chemicals Agency, on 25 September 2023 the European Commission passed a comprehensive new regulation to reduce emissions of microplastics (MP) into the environment, which includes the sale and use of intentionally added MP.1,2 This also applies to the application of synthetic rubber granulate infill in artificial turf systems and will ultimately have an impact on recreational sports. In Germany, rubber granulate made of ethylene-propylene-diene-monomer rubber (EPDM) is currently predominantly used. So far, there is no sufficient database for estimating MP emissions from artificial turf pitches into the environment and thus their relevance as a source of MP pollution.3 This topic is controversially discussed due to the complexity of sampling and analytics. To close this research gap, this project has the goal to determine mass balances for the emissions of MP from artificial turf pitches to allow an estimation of the amount of MP released per artificial turf pitch and year.
Within this study, MP emissions of three artificial turf scenarios at different time states (unaged, artificially aged and real-time aged) are compared: the past (old turf: fossil based, synthetic infill), present (most commonly installed in Europe: fossil based, EPDM infill), and the future (turf with recycled gras fibres, no synthetic infill). To simulate the outdoor weathering during the lifespan of an artificial turf of approx. 15 years, brand-new artificial turf and EPDM rubber granulate were accelerated aged by means of UV weathering and mechanical stress. Potential MP emissions into surface and groundwater are simulated by lysimeter and shake experiments. MP mass contents are subsequently determined by Thermal Extraction Desorption Gas Chromatography/Mass Spectrometry. Using special microfilter crucibles allows the estimation of the particle sizes of the emitted MP, which is a fundamental requirement for an assessment of potential health hazards for humans.
Es wird eine Studie zur Charakterisierung eines anisotropen Stahls vorgestellt, bei der Ultraschalluntersuchungen mit Mikrostrukturanalysen verbunden werden. Das Material weist hohe Festigkeit und Korrosionsbeständigkeit auf, zugleich ist mit anisotropen Eigenschaften die mechanischen und betrieblichen Eigenschaften beeinflussen zu rechnen. Vorläufige Ergebnisse lassen vermuten, dass weitere Untersuchungen notwendig sind, um die Fähigkeiten und Grenzen des Materials genau zu bestimmen. Es wird ein systematischer Ansatz mit Array- Prüfköpfen, Time-of-Flight Diffraction (TOFD) Technik und mikrostrukturellen Untersuchungen angewendet, um die Wechselwirkung zwischen Anisotropie und Mikrostruktur des Stahls zu analysieren. Ultraschallprüfungen mit der TOFD-Technik und in Tauchtechnik liefern Einblicke in das anisotrope Verhalten des Werkstoffes, einschließlich entsprechenden Kornorientierung, Dämpfung und Schallgeschwindigkeitsvariation. Diese Messungen führen in Verbindung mit mikrostrukturellen Analysen zu einem tieferen Verständnis des Materialverhaltens. Unser Hauptziel ist es, ein Framework zu erstellen, welches die Ultraschallantwort anisotroper Materialien mit ihren mikroskopischen Struktureigenschaften verbindet. Die vorgestellte Methodik ermöglicht eine zerstörungsfreie und zügige Bewertung der Materialintegrität, was besonders bei der Anwendung von Hochleistungsmaterialien relevant ist. Durch diesen integrativen Ansatz werden verschiedener Charakterisierungsmethoden kombiniert, um ein umfassenderes Materialverständnis zu erreichen.
Die laserbasierte aktive thermografische Prüfung als berührungslose Methode der zerstörungsfreien Werkstoffprüfung (NDT) basiert auf der aktiven Erwärmung des Testobjekts (OuT) und Messung des resultierenden Temperaturanstiegs mit einer Infrarotkamera. Dadurch bedingt können systematische Abweichungen vom vorhergesagten Erwärmungsverhalten Aufschluss über dessen innere Struktur geben. Jedoch ist das Auflösungsvermögen für innenliegende Defekte durch die diffusive Natur der Wärmeleitung in Festkörpern begrenzt. Thermografische Super-Resolution (SR)-Methoden zielen darauf ab, diese Limitation durch die Kombination mehrerer Messungen mit jeweils unterschiedlicher strukturierter Erwärmung und mathematischer Optimierungsmethoden zu überwinden.
Zur Rekonstruktion innerer Defekte mithilfe thermografischer SR-Rekonstruktionsmethodik wird für die Gesamtheit mehrerer Messungen ein schlecht gestelltes und stark regularisiertes inverses mathematisches Problem gelöst, was in einer dünnbesetzten Karte der internen Defektstruktur des OuTs resultiert.
Der vorliegende Vortrag gibt einen Überblick über die geleisteten Arbeiten in diesem Gebiet im Rahmen der hier mit dem Wissenschaftspreis der DGZfP 2024 prämierten Arbeit.
The variability and heterogeneity in their structural composition is significant for nearly all synthetic and natural polymers. Beside molar mass also functionality type distribution, copolymer composition distribution and architectural features are responsible for changing the material properties.
A wide range of analytical techniques are available to get insight into these parameters. However, in most cases it is essential to combine different sophisticated techniques to get closer to actual structures and to avoid statistical averages.
Different liquid chromatographic separation modes and their coupling in a two-dimensional way (SEC, LCCC, HILIC, 2D-LC) in combination with suitable detection techniques (e.g. UV, RI, LS, IR, MALDI/ESI-MS) as well as techniques like BET, DCS, SEM/TEM were applied to make structural features visible.
A few aspects are discussed for structural different polylactides from various synthesis routes and their behavior in LC-MS.
Im Rahmen des Vortrags wurden die Ergebnisse und die Methodik zur Erhebung von Forschungsbedarfen und Fähigkeitslücken bei den Behörden und Organisationen mit Sicherheitsaufgaben, welche im Rahmen des Projektes InnoBOSK durchgeführt wurden, vorgestellt. Den Schwerpunkt bildete dabei die Umsetzung der Workshops gemeinsam mit den Einsatzkräften und die Umsetzung der problemorientierten Erhebungsmethodik.
This study explores the acceleration of material design in the concrete industry, focusing on improving carbonation resistance, a key factor in the durability of concrete structures. Traditional tests for carbonation resistance are lengthy, but with the construction industry aiming for sustainable production, finding a balance between carbonation resistance and CO2 footprint is crucial. Our research employs two innovative methods: 1. Applying the Sequential Learning App for Materials Discovery (SLAMD), an AI materials design framework, to an extensive dataset of real-world concrete compositions to selectively test materials that meet market demands: maximum durability, optimal eco-durability, and the best cost-durability trade-off. 2. Investigating 1H Nuclear Magnetic Resonance (NMR) relaxometry as a quick alternative for characterizing carbonation behavior, as it saves time compared to traditional tests and assesses the complete material's pore space. Specific NMR features are then integrated into the material design model, with the model's performance compared against traditional approaches. The results of our study are compelling, demonstrating that materials can be precisely tailored to meet specific requirements with minimal data points. This marks a significant stride in the concrete industry, indicating that NMR-based, low-fidelity surrogate characterizations, combined with a focused, data-driven design approach, can substantially accelerate the development of durable, sustainable concrete mixtures.
The presentations discusses a use case for the optimization of concrete structures where structural and material design are integrated in a computational workflow. The workflow is based on both physics-based and data-based models and experimental data is used to calibrate/train these models with a specific focus on the integration of ucertainties.
In recent years, many protocols in computational materials science have been automated and made available within software packages (primarily Python-based). This ranges from the automation of simple heuristics (oxidation states, coordination environments) to the automation of protocols, including multiple DFT and post-processing tools such as (an)harmonic phonon computations or bonding analysis. Such developments also shorten the time frames of projects after such developments have been made available and open new possibilities. For example, we can now easily make data-driven tests of well-known rules and heuristics or develop quantum chemistry-based materials descriptors for machine learning approaches. These tests and descriptors can have applications related to magnetic ground state predictions of materials relevant for spintronic applications or for predicting thermal properties relevant for thermal management in electronics. Combining high-throughput ab initio computations with fitting, fine-tuning machine learning models and predictions of such models within complex workflows is also possible and promises further acceleration in the field. In this talk, I will show our latest efforts to link automation with data-driven chemistry and materials science.
Im Rahmen eines vom Umweltbundesamt geförderten Forschungsprojekts wurde untersucht, ob die Abtrennung der Feinfraktion (0-2 mm) eine Verbesserung der umweltrelevanten Eigenschaften bewirkt und somit HMVA-1 erreicht werden kann. In Deutschland wird die Rostasche durch Nassentschlackungssysteme aus dem Feuerraum ausgetragen. Durch den Kontakt mit Wasser setzen direkt hydraulische Reaktionen ein, die eine vollständige Abtrennung der Feinfraktion unmöglich machen. Das wurde bereits in den 1990er Jahren erkannt und führte zur Entwicklung des ABB InRec Verfahrens mit Trockenentaschung als ersten Verfahrensschritt. Auch damals war das Ziel eine möglichst inerte Rostasche für die Verwertung zu erzeugen. In den letzten Jahren wurden in der Schweiz Trockenentaschungssystem installiert, hier vor allem um die Rückgewinnung von elementaren Metallen auch in der Feinfraktion zu verbessern. Welche Potenziale sich dabei erschließen lassen, wurde in einem anderen UBA-Projekt untersucht. Im Rahmen unserer Arbeiten wurde versuchsweise trockene Rostasche an einer Anlage in Süddeutschland genommen und im Labor untersucht. Im Vortrag werden die Ergebnisse zum Auslaugverhalten und zur Gefahreneigenschaft HP14 (Ökotoxizität) vorgestellt.
This study aims to represent an approach for transferring the materials testing datasets to the digital schema that meets the prerequisites of the semantic web. As a use case, the tensile stress relaxation testing method was evaluated and the testing datasets for several copper alloys were prepared. The tensile stress relaxation testing ontology (TSRTO) was modeled following the test standard requirements and by utilizing the appropriate upper-level ontologies. Eventually, mapping the testing datasets into the knowledge graph and converting the data-mapped graphs to the machine-readable Resource Description Framework (RDF) schema led to the preparation of the digital version of testing data which can be efficiently queried on the web.
The presentation gives an overview of BAM's activities on processing influences and application properties of MPEAs in the form of joined and machined high and medium entropy alloys (CoCrFeMnNi and CoCrNi). In the case of welding, the focus is on defect-free welded joints with sufficient mechanical properties. In the case of machining, the focus is on the possible influence on the surface quality of the materials through adequate milling parameters. In addition, the hydrogen absorption and diffusion properties as well as the electrochemical corrosion behavior are fundamentally examined.
Aktive thermografische Prüfung ist ein vielseitiges Instrument in der Familie der zerstörungsfreien Prüfverfahren. Der Einzug moderner Lasertechnologie hat hier bedeutende neue Anwendungsfelder eröffnet. In Kombination mit Industrierobotik können nun beispielsweise beliebig komplex geformte Bauteile großflächig vollautomatisiert auf Oberflächenrisse überprüft werden. Der hier vorliegende Vortrag gibt einen Überblick über die Grundlagen der Laserthermografie, zeigt unsere Anstrengungen am Fachbereich im Bereich der automatisierten thermografischen Detektion von Oberflächenrissen und gibt ein Ausblick über neue moderne Thermografieverfahren aus der Forschung.
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.
Volatile organic compounds (VOCs) emitted by furniture and building materials can cause health issues. For an improvement of indoor air quality low emitting materials should be used. Quality assurance and –control (QA/QC) measures require an emission reference material (ERM) with a predictable emission rate of VOCs. The idea is to use porous materials as ERM, which store the VOCs inside their pores and emit them constantly.
Ground Granulated Blast-Furnace Slag (GGBFS), a by-product of the iron-making process, has gained significant attention as a supplementary cementitious material and has become increasingly popular in recent years due to its remarkable properties. GGBFS can significantly reduce the environmental impact of cement production when it comes to building concrete structures. GGBFS can either be blended with ordinary Portland cement (OPC) (up to a 90% replacement), or it can be used in the production of alkali-activated materials (AAMs). However, a comprehensive understanding of the pore solution composition is necessary for understanding various aspects of cementitious materials and their durability, including corrosion behavior, passivation of steel, and resistance to deteriorative processes. In the present work, the pore solutions of seven different GGBFS-containing cements (alkali-activated slag, alkali-activated slag/fly ash blends, a hybrid alkaline cement, CEM III/C, and CEM III/B) were extracted and analysed by inductively coupled plasma-optical emission spectroscopy, ion chromatography, pH, redox potential, and conductivity measurements. For comparison, a Portland cement pore solution was analysed similarly. The Concentrations of reduced sulfur were noteworthy in all GGBFS-containing cements, particularly in alkali-activated cements, where concentrations were notably higher compared to standard cements. The redox potentials of the pore solutions were primarily dictated by the concentrations of reduced sulfur, although other factors may contribute. Additionally, sulfur species in the pore solutions had an impact on pH, electrical conductivity, and other properties pertinent to the corrosion of reinforcements.
Volatile organic compounds (VOCs) emitted by furniture and
building materials can cause health issues. For an
improvement of indoor air quality low emitting materials
should be used. Quality assurance and –control (QA/QC)
measures require an emission reference material (ERM) with a
predictable emission rate of VOCs. The idea is to use porous
materials as ERM, which store the VOCs inside their pores and
emit them constantly.
Die additive Fertigung mittels Schweißverfahren bietet große ökonomische Vorteile für eine ressourceneffiziente Bauteilherstellung. Offene Fragen bezüglich Homogenität, Anisotropie der Schweißgefüge und den damit verbundenen Bauteileigenschaften stehen einer wirtschaftlichen Verarbeitung oftmals im Wege. Finale Bauteilgeometrie und Oberflächengüte erfordern meist komplementäre subtraktive Fertigungsschritte. Werkstoffe für hochbelastbare Komponenten sind oftmals schwer spanbar. In einem Vorhaben der BAM und des ISAF wurde untersucht, wie die Modifikation der AM-Schweißzusätze und das ultraschallunterstützte Fräsen (US) die Zerspanungssituation verbessern. Der vorliegende Artikel stellt wesentliche Zusammenhänge zwischen Legierung, Gefüge und Zerspanung zweier schwer spanbarer Hochleistungslegierungen (FeNi und CoCr) dar. Großes Potenzial zeigte neben dem US die Modifikation mit Zr und Hf bei Zulegierung in das Schweißgut mittels Beschichtung von Massivdrähten bzw. Herstellung von Fülldrähten.
Es werden die Ergebnisse eines mehrjährigen Forschungsvorhabens der BAM in Zusammenarbeit mit Straßenbauverwaltungen der Länder und Industriebeteiligten zur betriebstechnischen Ausrüstung von Straßentunneln präsentiert. Schwerpunkte waren die Bestimmung der Korrosivität der Atmosphäre von 3 ausgewählten Straßentunneln, die Analyse korrosionsrelevanter Ablagerungen und von Klimadaten. Die Auswirkungen dieser Einflussgrößen auf die Dauerhaftigkeit von Konstruktionen aus nichtrostenden Stählen wurde ermittelt und in Abhängigkeit verschiedener Einflussparameter dargestellt. Die Ergebnisse der systematischen Untersuchungen an Prüfköpern decken sich mit Beobachtungen an realen Bauteilen. Spaltbehaftete Konstruktionen aus Werkstoffen der CRC III führen demnach in Zeiträumen zwischen 10 und 15 Jahren zu Korrosionserscheinungen, welche die technische Sicherheit beeinträchtigen können und die erwartete Dauerhaftigkeit nicht erfüllen. Die Folge sind zusätzliche Sperrungen und ein vorzeitig notwendiger Unterhaltsaufwand, die erhebliche Kosten verursachen. Im Ergebnis ist eine Überarbeitung des aktuellen Regelwerkes erforderlich, um die angestrebte Dauerhaftigkeit von 30 Jahren zu gewährleisten.
Isotope analysis plays a critical role in various disciplines, including environmental science, archaeology, and forensic investigations. Traditional methods such as mass spectrometry provide precise isotopic data but often require complex, costly setups and extensive sample preparation. As an alternative, optical spectrometry has emerged as a versatile and less invasive technique. This presentation explores the advancements and applications of optical spectrometry methods in isotope analysis, emphasizing their benefits and challenges.
Lithium (Li), Boron (B), Nitrogen (N), Magnesium (Mg), and Calcium (Ca) are pivotal elements across various spheres such as the hydrosphere, biosphere, and lithosphere, significantly impacting (bio-) geochemical and physiological processes. These elements exhibit stable isotopes with substantial roles in geological, environmental, and biological studies. The traditional method for measuring isotope amount ratios has been through mass spectrometry, which, despite its accuracy, comes with high operational costs, the need for skilled operators, and time-consuming sample preparation processes.
Combining optical spectroscopy with chemometrics introduces an innovative, cost-effective approach by the hand of high-resolution continuum source atomic and molecular absorption spectrometry (HR-CS-AAS and HR-CS-MAS) for the analysis of isotope ratios in Li, B, N, Mg, and Ca. By analyzing the atomic or molecular absorption spectrum of the in-situ generated cloud of atoms of diatomic molecules (e.g., Li, BH, NO, MgF, CaF) during the electronic transition from the fundamental state, this method allows for the rapid determination of isotope ratios directly from sample solutions without the need for complex sample preparation.
For each element, the respective atomic or molecule's absorption spectrum was deconvoluted into its isotopic components using partial least squares regression or machine learning algorithms. Robust calibration models were developed, calibrated with enriched isotope, and validated against certified reference materials. Spectral data underwent preprocessing to optimize the modeling to determine the optimal number of latent variables.
The findings showcase that this optical spectrometric method yields results that agree with those obtained via inductively coupled plasma mass spectrometry (ICP-MS), offering a promising, cost-effective, and rapid alternative for isotope analysis with precisions as low as ± 0.2‰. This approach is a significant advancement in analytical chemistry, providing a new way to study isotope variations in biological, environmental, and geological samples.
What does GD-OES reveal about the aging and manufacturing processes of lithium-ion batteries?
(2024)
Glow-Discharge Optical Emission Spectroscopy (GD-OES), a powerful analytical technique, sheds light on the two critical aspects of lithium-ion batteries (LIBs): manufacturing and aging 1, 2. We optimized cell production in manufacturing by adjusting parameters, including cathode doping, electrolyte concentration, and pressing force. GD-OES provided in-depth elemental composition and homogeneity analysis, which is crucial for identifying optimal manufacturing conditions. These findings were validated by electrochemical impedance spectroscopy, confirming the quality of the manufactured batteries.
Shifting the focus to aging, we use GD-OES for fluorine depth profiling, a key element in understanding polymer and electrolyte degradation. However, fluorine presents analytical challenges. We addressed this by substituting argon with a neon:argon mixture, which significantly enhanced fluorine detection sensitivity. This advancement not only improves accuracy but also holds the potential to guide sustainable and cost-efficient manufacturing strategies.
Through its versatility, GD-OES has proven to be a powerful tool for not only optimizing LIB manufacturing processes but also gaining deeper insights into their aging mechanisms. This research extends beyond academic interest, offering tangible benefits for the industry by translating into improved battery quality, extended lifespan, and overall performance.
-Über 80 Mio. Schwellen im deutschen Schienennetz verbaut
-Lebensdauer einer Schwelle beträgt ca. 20 bis 50 Jahre
-Über 2 Mio. Schwellen werden jährlich ausgetauscht, obwohl die Mehrzahl noch intakt ist
-Zustandsbewertung mittels ZfP kann Ausschuss verringern
-Schadhafte Schwellen könnten mittels ZfP frühzeitig im Gleis erkannt werden, um Gefahren und Unfälle abzuwenden
The properties of laser radiation result in a wide range of applications, making laser technologies indispensable in areas such as industry, science and medicine. The possible areas of application for thermography in this context are just as diverse. Thermography is used in laser applications when permanent monitoring and control of thermal development is necessary. Among others, this is the case in additive manufacturing, laser-based measuring devices and non-destructive testing. Furthermore, thermography is ideally suited as a testing method when it comes to ensuring the quality of the laser itself. In this talk it is outlined, how lasers can be used as a heat source in active thermographic testing. Furthermore, two special variants (spatial & temporal structured heating) are described, for which lasers are highly suitable.
Im Rahmen der von der BAM und anderen Partnern ins Leben gerufenen Initiative „Digitale Qualitätsinfrastruktur“ liegt der Fokus u.a. auf der Entwicklung von neuen Zertifizierungsworkflows. Dabei ist eine besondere Bedeutung dem Zusammenführen von Operational Technology (OT) und Informationstechnik (IT) beizumessen. Zur Datenintegration aus der Sensor-Feldebene einer Versuchs-wasserstofftankstelle wurde eine solche Infrastruktur zunächst in einer Laborumgebung aufgebaut.
The ongoing geo-political conflicts and the increasing need for the implementation of measures to improve the energetic system sustainability are increasing the importance of tanks for storing cryogenic fluids in the energy industry. The most common example of cryogenic tank applications is the transport of natural gas and hydrogen in their liquid form (LNG and LH2 respectively) for which, considering the same transport volume cryogenic storage ensures significantly higher transport capacities with respect storage based solely on overpressure.
A common feature of all cryogenic transported fluids is that their condition must be maintained minimizing heat leaks from the environment as much as possible. This is achieved by the implementation of thermal super Insulations (TSI) systems based on e. g. rock wool, perlites, microspheres, multilayer insulations (MLI), and vacuum which have proven to be effective in applications. However, due to the relatively short period of use in some applications, the small number of documented incidents, and the still few investigations carried out in the field, the exploitation of such systems in the cryogenic fluids transport sector still suffers from insufficient knowledge about the course and consequences of incidents. Accidents involving collisions, fires, and their combination are quite common in the transportation sector and may generate extraordinary loads on the tank and its insulation system, eventually leading to tank failure.
The present study focuses on the behavior of TSI systems in tanks when it is exposed to an external heat source representative of a hydrocarbon fire scenario. This may cause an increase of the heat flux into a tank by several orders of magnitude with respect to normal design conditions, thus inducing severe and in the TSI, causing the rapid release of flammable gas and even resulting in a Boiling Liquide Expanding Vapour Explosion (BLEVE).
To study such scenarios a test rig was developed at BAM that allows testing of TSI at industrial conditions and enables subsequent analysis of TSI samples. This test rig considers the typical double-walled design of tanks for cryogenic fluids with vacuum and an additional insulating material in the interspace. Adjustable electrical heating elements simulate the fire on one side of the double wall. This process allows the implementation of repeatable heat loads of up to 100 kW/m². The other side of the double wall is represented by a fluid-supported heat exchanger, which allows the simulation of cold or cryogenic conditions in the test rig, and to determine the heat flux transmitted through the double wall. Thus, the test rig allows thermal loading and performance analysis of TSI samples at the same time.
In the presentation, the results of diverse tested TSI systems will be presented and discussed. As a result of this study, the list of advantages and disadvantages for the choice of tested TSI expands. Within the test, all samples degraded as a consequence of a hydrocarbon fire-orientated thermal load. Strong differences in the behavior of the tested TSI systems over temperature, location, and time were observed. Additionally, the tested MLI insulations were significantly more resistant to their base materials. These results are relevant for the design, the definition of national and international regulations, the Risk assessment, and the development of safety concepts for cryogenic tanks.
To combat climate change the share of renewable energy production must increase drastically. Offshore energy production – offshore wind and power-to-X – are crucial to achieving climate targets. However, the impact of these offshore constructions – wind turbines and production platforms – on the marine environment remains unclear in many aspects. Potential sources of chemical emissions are corrosion protection systems, remobilization of contaminants from old sediments during construction, the brine of desalination plants and increased shipping for maintenance and transportation. In order to minimize the environmental impact of renewable energies, close monitoring is essential. The goal of this project is the development of a monitoring concept for an offshore power-to-X production platform.
Maritime exposure poses particular challenges for corrosion
protection in plant construction. In addition to the right choice
of materials, special design features that can have an impact
on corrosion resistance must also be taken into account to
ensure long-lasting corrosion protection. In practice, structural
crevice arrangements are unavoidable, and therefore the
crevice corrosion resistances of stainless steels are of
particular importance. These and other influences are being
investigated in this joint project.
While alkali-activated binders offer certain advantages over traditional Portland cement binders, particu¬larly in terms of resistance against chemical attacks and potentially environmental footprint, their degra¬dation mechanisms remain incompletely understood at present, specifically carbonation. Thus, this study investigates the impact of natural and accelerated carbonation (1% and 4% CO2) on three different compositions of alkali-activated concretes: 100% calcined clay (C100) binder, 100% ground blast furnace slag (S100) binder, and a 40% calcined clay and 60% blast furnace slag blend (C40S60). C100 concretes exhibit faster carbonation kinetics, with five times greater natural carbonation depths than S100. This difference diminishes under accelerated carbonation, showing a 1.5 times difference for 1% CO2 and complete carbonation for 4% CO2 at 90 days. The results thus confirm that accelerated carbonation testing of low-Ca alkali-activated concretes yields results that are not representative of natural carbonation. The C40S60 sample demonstrates a carbonation profile similar to a CEM I concrete, i.e., a high carbonation resistance. Microstructure analysis indicates the formation of three polymorphs of calcium carbonate for S100 (calcite, vaterite, and aragonite), with a higher CO2 concentration favouring aragonite over vaterite. C100 exhibits no calcium carbonates; instead, sodium carbonates form, including trona for 4% CO2 and natrite for both accelerated tests. C40S60 shows calcium and sodium carbonates, although to a lesser extent, containing predominantly calcite and minor signals of natrite. Suitable compositions, like C40S60, prove as effective during natural or accelerated carbonation tests as conventional Portland cement concrete.
3D concrete printing is an innovative new construction technology offering the potential to enable an efficient production of individual structures with less consumption of resources. The technology will mainly shape the future construction philosophy, automate the build process and help reaching the climate goals in civil engineering. From the design of a structure to the printed component, many individual steps based on different software are required which must be repeated for each new or changed structure. First, the geometry of the structure is created in a CAD program. Second, the print path is defined in a slicer software creating the machine code for the printer (G-Code). Finally, the structure can be printed. Furthermore, a numerical model of the printed structure is necessary for process optimization and control. In that way the number of test prints can be reduced, costs can be saved, and the component behavior can be predicted. For those purposes, an automated workflow allowing to run all steps or individual steps without interacting with each individual software program is required. Furthermore, changes in parameters or the exchange of parts (using a different design or different printer) must be possible in a simple manner. In the presented work, such an automated workflow based on the example of a parametrized wall element for extrusion-based concrete printing is developed. The investigated wall structure is parametrized using the global geometry parameters: height, width, thickness, radius, kind of infill structure (honey-comb, zig-zag) and number of repeated infills. All above mentioned steps are implemented via python interfaces using pydoit as workflow tool. General interfaces with prescribed input and output files are defined allowing adaptations for different software and tools. The described workflow is tested by performing a test series investigating the influence of the in-fill structure on the mechanical properties of the test walls.
Sicherheitstechnische Untersuchungen von Wasserstoff Freistrahlflammen bei Hochdruck im Realmaßstab
(2024)
Wasserstoff als Energieträger gewinnt zunehmend an Bedeutung. Die Untersuchung von Störfallauswirkungen mit Wasserstoff rückt somit stärker in den Fokus. Da Wasserstoff meist unter Druck gelagert und transportiert wird, ist ein zu betrachtendes Szenario die Freisetzung aus einer Leckage mit anschließender Zündung. Die daraus resultierende Freistrahlflamme (Jet Flame) muss hinsichtlich der in die Umgebung emittierten Wärmestrahlung charakterisiert werden. In der Literatur existieren bereits verschiedene Modelle, welche jedoch vermehrt auf Daten aus Kohlenwasserstoffflammen mit geringem Impuls basieren. Zur Überprüfung dieser Modelle wird im Zuge des BAM internen H2 Jet Flame Projektes die sicherheitstechnische Untersuchung von impulsbehafteten Wasserstoff Freistrahlflammen vorgenommen. Hierfür finden Versuche im Realmaßstab auf dem Testgelände Technische Sicherheit der BAM (BAM-TTS) statt. Gegenstand der Untersuchungen ist die Beurteilung der Auswirkungen von realistischen Freisetzungsszenarien hinsichtlich der Flammengeometrie und der freigesetzten Wärmestrahlung. Dabei werden Parameter wie Freisetzungswinkel, Leckagedurchmesser (z.Zt. 1 mm bis 30 mm), Druck (z.Zt. bis max. 250 bar) und Massenstrom (bis max. 0,5 kg/s) variiert. Zusätzlich können auch Einflüsse wie Art der Zündung, Zündort sowie Zündung mit zeitlichem Verzug untersucht werden. Gewonnene Erkenntnisse werden mit den Ergebnissen bereits vorhandener Modelle verglichen und diese im Bedarfsfall weiterentwickelt. Insbesondere wird der Fokus auf die Modellierung der freigesetzten Wärmestrahlung von Wasserstoffflammen gelegt. Herausforderung dabei stellt die IR-Vermessung und Modellierung von Sichtmodellen der Flammen dar. Die Visualisierung der Flammengeometrie wird mit Hilfe mehrerer Infrarot Kamerasystemen (aus mindestens zwei Blickwinkeln) vorgenommen.
Bisherige Messungen, die in der Literatur zu finden sind, basieren meist auf instationären Auströmbedingungen. Der hier verwendete Versuchsaufbau ermöglicht ein stationäres Ausströmen für mehrere Minuten und somit eine direkte Vergleichbarkeit mit den existierenden (stationären) Modellen.
Weiterhin ist der Versuchsstand umrüstbar für Vergleichsmessungen mit Kohlenwasserstoffen (Methan etc.) sowie Mischungen aus Wasserstoff und Kohlenwasserstoffen.