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Standardised methods need validation. The main validation parameters like trueness, repeatability and intermediate precision and reproducibility are presented. Furthermore, different methods for the validation are disussed: (certified) reference materials, representative testing materials and interlaboratory comparisons. At last, the need of proficiency testing is stressed.
Small-area XPS analysis is one of the most popular and powerful methods for analysing the surface of features in the micro-range. When measuring microstructures, the ques-tion arises whether the measuring point is really located at the point intended to be ana-lysed. Information in a measured spectrum might originate within the field of view (FoV) on the surface of the sample, from outside the FoV, or even from inherent contamination. To ensure that small structures can be measured correctly regardless of user and instru-ment, certain instrument and sample settings must be known and selected correctly: beam and aperture size as well as the aperture settings and the approximate dimensions of the structure to be analysed. This is the only way to ensure that the information in the spectrum originates only from the FoV on the analysed structure.
To test the performance of the XPS instruments, a dedicated test material was developed that consists of a gold surface on which 8 circles and 8 squares of chrome are incorpo-rated using a masking process, so that the Au substrate and the Cr structure surfaces are in the same surface plane. In order to be able to test as many as possible instruments from different manufacturers, the structures have been designed with a size ranging from 300 µm down to 7 µm. The layout of the test material has been optimised in regard of the handling. The structures are arranged along lines instead of a circumference, marking arrows around the smaller structures (≤50 µm) are added, and the lithography mask is optimised regarding edge and diffraction effects. Furthermore, the manufacturing process was changed from electron-beam deposition to mask lithography due to costs reasons. The structures on the test material were measured with a metrological SEM to determine their accurate dimensions and check the repeatability of the manufacturing process. XPS investigations with a Kratos AXIS Ultra DLD and an ULVAC-Phi Quantes demonstrates the suitability of this new test material for measuring the analysed area.
Bei Geräten und Maschinen zur bestimmungsgemäßen Verwendung in explosionsgefährdeten Bereichen gemäß 2014/34/EU muss in der europäischen Union eine Zündgefahrenbewertung durchgeführt werden. Dabei müssen unter anderem die Gefahren von nichtelektrischen Zündquellen betrachtet werden, zu denen auch die mechanischen Schlagvorgänge gehören.
Bei mechanischen Schlagvorgängen kommt es infolge des Zusammenstoßes zweier Werkstücke bzw. Bauteile zu einer Umwandlung der kinetischen Energie. Dabei erhöht sich die Temperatur der Werkstoffe an der Kontaktstelle und es kommt unter Umständen zu einem Abtrennvorgang kleiner Partikel erhöhter Temperatur. Sowohl die heißen Kontaktstellen (Zündquelle "heiße Oberflächen") als auch die abgetrennten Partikel (Zündquelle "mechanisch erzeugte Funken") können eine wirksame Zündquelle für ein explosionsfähiges Gasgemisch darstellen.
Zur Festlegung von Grenzwerten wurden in der Norm DIN EN ISO 80079-36:2016 die Gasgemische anhand ihrer Explosionsgruppe klassifiziert und zu jeder Gruppe die maximale Energie des Schlagvorgangs festgelegt, unter derer die Entstehung einer wirksamen Zündquelle als unwahrscheinlich angenommen werden kann.
Weitere Festlegungen von Grenzwerten für die kinetische Schlagenergie und geeignete Werkstoffpaarungen finden sich u.a. in der DIN EN 1755 (ex-geschützte Flurförderzeuge) und in der DIN EN 14986 (ex-geschützte Ventilatoren).
The main properties and main methods which are needed for the physico-chemical characterisation of graphene related 2D materials are discussed. As expample for standardization, protocols for the measurement of the chemical composition with XPS are discussed. The results of an interlaboratory comparisons led to new recommendations for the reliable measurments protocols.
Fire-induced spalling of normal strength concrete with different types of blended Portland cement
(2024)
The cement industry is looking to reduce its overall CO2 footprint. Greener manufacturing can be achieved by the introduction of more clinker-reduced cements. Concrete exposed to fire tends to show explosive spalling caused by thermomechanical and thermohydraulic processes. It is therefore essential to determine how concretes with clinker-reduced cements behave under fire exposure, especially for concretes containing calcined clays, as these are expected to be the supplementary cementitious material of the future. In this paper, normal strength concretes with four different cements (CEM I, CEM II/A-LL, CEM III/A and CEM II/B-Q) were examined for their fire-induced spalling behaviour. In addition, a mix with PP fibres was investigated for each concrete. The experiments were conducted on ring-restrained cylindrical specimens exposed to the hydrocarbon fire curve. The results showed that the cement type influences spalling behaviour. Samples with CEM I spalled the least, followed by CEM II/A-LL and CEM III/A. Finally, samples with CEM II/B-Q showed the most severe damage. It was found that the spalling behaviour of different concretes correlates with the moisture content before exposure to fire, meaning that higher moisture content leads to higher spalling susceptibility. The use of 2 kg/m³ PP fibres completely inhibited spalling regardless of the cement type used and therefore remains a successful avoidance strategy.
Graphene and related 2D materials (GR2Ms) are now entering an exciting phase of commercialization and use in products. Graphene nanoplatelets (GNPs) can be obtained in rather large quantities, but the properties of these industrially produced powders can vary depending on the production method, and even from batch to batch. Understanding and optimizing the surface chemistry of GNPs, modified through chemical functionalization processes is crucial, because it affects their dispersibility in solvents and matrices for the purpose of embedding them into real-world products. Therefore, reliable and repeatable measurements of the surface chemistry of functionalized GNPs are an important issue for suppliers as well as users of these materials. To address these concerns, international documentary ISO standards for measurement methodologies are under development which incorporate protocols that are becoming widely accepted in the community.
Recently, it was shown that pelletizing led to lower average O/C atomic ratios than those measured for powders [1]. In another study, the influence of the morphology on the degree of functionalization was shown [2]. As expected, a higher degree of functionalization was detected for smaller GNPs. The functionalization was located at the outermost surfaces of the GNPs by comparing experiments using photoelectron with soft (Al Kα, 1.486 keV) and hard X-rays (Cr Kα, 5.405 keV). Therefore, it is important for those using GNPs to understand both the physical and chemical properties of these particles, when considering their use in different applications.
The next step for reliable characterization protocols was the realization of an interlaboratory comparison under the auspices of VAMAS (Versailles Project on Advanced Materials and Standards) with 22 participating laboratories from all over the world. Samples of oxygen-, nitrogen-, and fluorine- functionalized GNPs were provided to the participants along with a measurement protocol. Participants were asked to prepare the samples as powders on a tape, powders in a sample holder recess, or as pellets. The lower measured O/C ratio reported for pelletized samples [1] was confirmed. The lowest scattering of the results was observed for the powders measured in the recess (Fig. 1). Furthermore, an influence of the humidity on the results was observed.
Interlaboratory comparisons (ILCs) are an important tool for the validation of characterisation methods, and, herwith, a prerequisite for standardisation. The "Versailles Project on Advanced Materials and Standards" offers a framework for performing such ILCs: (i) TiO2 nanoparticles using ToF-SIMS, and (ii) the chemical composition of functionalized graphene using XPS. The results of both ILCs underline the importance of sample preparation for the measured results.
Wir stellen unseren Ansatz und unsere Methodik zur Simulation von Piping-Erosion vor, welche während des Installationsprozesses von Suction Bucket Fundamenten für Offshore-Windkraftanlagen auftreten kann und ein kritisches Versagen des Installationsprozesses darstellt. Wir zeigen die Ergebnisse mehrere Simulationen und analysieren die hydrodynamischen und Kontaktkräfte, die auf das granulare Medium wirken, sowie die Druckdifferenz der flüssigen Phase. Solche Simulationen können zum besseren Verständnis von Piping-Erosion und letztendlich zu dessen Verhinderung beitragen.
Transportierbarkeit von Transport- und Lagerbehältern für radioaktive Stoffe, welche nach eine längerfristigen trockenen Zwischenlagerung
transportiert werden müssen. Überblick über die aktuellen Regelwerke und Richtlinien sowie die Zeitpläne für das Finden eines Endlagers für hochradioaktive Stoffe und die damit verbundene verlängerte Zwischenlagerung. Des Weiteren werden das für die verlängerte Zwischenlagerung notwendige Alterungsmanagement und die noch erforderlichen Forschungstätigkeiten vorgestellt.
Transportierbarkeit von Transport- und Lagerbehältern für radioaktive Stoffe, welche nach eine längerfristigen trockenen Zwischenlagerung
transportiert werden müssen. Überblick über die aktuellen Regelwerke und Richtlinien sowie die Zeitpläne für das Finden eines Endlagers für hochradioaktive Stoffe und die damit verbundene verlängerte Zwischenlagerung. Des Weiteren werden das für die verlängerte Zwischenlagerung notwendige Alterungsmanagement und die noch erforderlichen Forschungstätigkeiten vorgestellt.
Optical measurements of scattering luminescent materials dispersed in liquid and solid matrices and luminescent powders play an important role in fundamental research and industry. Typical examples are luminescent nano- and microparticles and phosphors of different composition in different matrices or incorporated into ceramics with applications in energy conversion, solid-state lighting, medical diagnostics, and security barcoding. The key parameter for the performance of these materials is the photoluminescence quantum yield QY, i.e., the number of emitted photons per number of absorbed photons. QY of transparent luminophore solutions can be determined relatively to a fluorescence quantum yield standard of known QY. Such standards are meanwhile available as certified reference materials.[1] The determination of QY of scattering liquid and solid samples like dispersions of luminescent nanoparticles, solid phosphors, and optoceramics requires, however, absolute measurements with an integrating sphere setup. Although the importance of reliable absolute QY measurements has been recognized, no interlaboratory comparisons (ILCs) on measurement uncertainties and the identification of typical sources of uncertainty have been yet reported. Also, no scattering reference materials with known QY are available.
We present here the results of a first ILC of 3 laboratories from academia and industry performed to identify and quantify sources of uncertainty of absolute QY measurements of scattering samples. Thereby, two types of commercial stand-alone integrating sphere setups with different illumination and detection geometries were utilized for measuring QY of transparent and scattering dye solutions and solid phosphors. As representative and industrially relevant solid and scattering samples, YAG:Ce optoceramics of varying surface roughness were chosen, applied, e.g., as converter materials for blue light emitting diodes. Special emphasis was dedicated to the influence of the measurement geometry, the optical properties of the blank, utilized to determine the number of photons of the incident excitation light absorbed by the sample, and the sample-specific surface roughness. While matching QY values could be obtained for transparent dye solutions and scattering dispersions, here using a blank with scattering properties closely matching those of the sample, QY measurements of optoceramic samples with different blanks revealed substantial differences, with the blank's optical
properties accounting for measurement uncertainties of more than 20 %. Based upon the ILC results, we recommend non-absorbing blank materials with a high reflectivity (>95 %) such as a 2 mm-thick PTFE target placed on the sample holder which reveals a near-Lambertian light scattering behavior, yielding a homogeneous light distribution within the integrating sphere.
Ausgehend von den Grundlagen der Korrosion stellt der Vortrag die Möglichkeiten des Korrosionsschutzes mit Zink vor. Dabei wird sowohl auf den kathodische Korrosionsschutz mit aktiven Zink-Anoden, als auch auf den Korrosionsschutz durch Deckschichtbildung an Zink und Zinküberzügen eingegangen. Veränderte Umweltbedingungen in Europa in den letzten Jahrzehnten, ermöglichen mit Schichtdicken um 80 µm einen Korrosionsschutz von über 100 Jahren, wenn konstruktive Randbedingungen beachtet werden.
Characterization and quantification of functional groups and coatings on nanoobjects an overview
(2024)
Characterization of Nanoparticles – Questions to Ask, Functional Nanoparticles (NPs) – Organic, Inorganic, and Hybrid Nanoparticles Nanomaterial Characterization Standardization – Addressing Remaining Gaps Surface FGs Particle Surface Chemistry - Why is it Important? Particle Surface Chemistry - A Key Driver for Performance, Applications, and Safety Aspects Method Development for Quantifying FGs and Ligands on Particle Surfaces FG Quantification – Method Choice & Criteria Relevant for Data Interpretation Quantifying the Amount of Total and Accessible FGs on Aminated Silica Nanoparticles (SiO2-NH2) Comparing the Total and Accessible –NH2 Content on Aminated Silica NPs of Different Size Characterization of Nanoparticles Standardization Standardized Measurements of Surface FGs on Nanoparticles EMP Project SMURFnano EMP Project SMURFnano Work Packages & Goals Certified Reference Materials from BAM
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 ([1], [2]), 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 10 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.
For industrial applications dealing with hydrogen, the definition of safety distances and the assessment of possible hazards emanating from releases is mandatory. Since hydrogen is usually stored and transported under pressure, one scenario to be considered is the momentum driven release of hydrogen from a leakage with subsequent ignition. In this scenario, the emitted heat radiation from the resulting jet flame to the surroundings has to be determined to define adequate safety distances. For hydrocarbon flames, different jet flame models are available to assess the hazards resulting from an ignited jet release. Since hydrogen flames differ from hydrocarbon flames in their combustion behavior, it has to be checked if these models are also applicable for hydrogen. To evaluate the accuracy of these models for hydrogen jet flames, tests at real-scale are carried out at the BAM Test Site for Technical Safety (BAM-TTS). Herein, the flame geometry and the heat radiation at defined locations in the surroundings are recorded for varying release parameters such as leakage diameter (currently up to 30 mm), release pressure (currently up to max. 250 bar) and mass flow (up to max. 0.5 kg/s). The challenge here is the characterization of the flame geometry in an open environment and its impact on the thermal radiation. Existing heat radiation data from the literature are mostly based on unsteady outflow conditions. For a better comparability with the steady state jet flame models, the experiments presented here are focused on ensuring a constant mass flow over the release duration to obtain a (quasi) stationary jet flame. In addition, stationary outflow tests with hydrocarbons (methane) were also carried out, which are intended to serve as reference tests for checking flame models based on hydrocarbon data.
Cryogenic liquefied gases, such as liquid hydrogen (LH2) and liquefied natural gas (LNG), are becoming more popular as eco-friendly energy sources. However, using these gases more often increases the risk of accidents, making it important to conduct thorough risk assessments. The storage systems for these gases rely on thermal superinsulation (TSI), which can fail under extreme heat, especially during fires. Therefore, it is essential to study how and why TSI fails. This research (part of PhD topic) aims to examine insulation performance, thereby improving the overall safety of cryogenic storage systems.
An overview with the basics of size and shape measurement of particles and 2D structures according to established methodologies (and popular imaging processing software packages) with imaging techniques is given. Main descriptors are explained based on practical cases are determined interactively at the flipchart.
To reduce carbon dioxide emissions, energy carries such as hydrogen consider to be a solution. Consumption of hydrogen as a fuel meets several restrictions such as its low volumetric energy density in gas phase. To tackle this problem, storage as well as transportation in liquid phase is recommended. To be able to handle this component in liquid phase, an efficient thermal insulation e.g., MLI insulation is required. Some studies have been revealed vulnerability of this type of insulation against high heat flux, for instance a fire accident. Some investigations have been depicted the importance of consideration of the MLI thermal degradation in terms of its reflective layer. However, limited number of studies have been focused on the thermal degradation of spacer material and its effect on the overall heat flux.
In this study, through systematic experimental measurements, the effect of thermal loads on glass fleece, glass paper as well as polyester spacers are investigated. The results are reported in various temperature and heat flux profiles. Interpreting the temperature profiles revealed as the number of spacers in the medium increases, the peak temperature detectable by the temperature sensor on the measurement plate decreases. Moreover, the contribution of each individual spacer in all cases regarding the experimental temperature range is assessed to be around 8%. This value may increase to around 50% for glass paper and polyester spacers, and to around 25% for glass fleece spacers as the number of spacer layers increases up to six layers.
To utilize the outcomes of the experiment later and integrate the results into numerical and CFD simulations, a model is proposed for the mentioned experimental temperature range up to 300°C to predict a heat flux attenuation factor. The model proposes a fitting factor that can reproduce the least square fitted line to the experimental data.
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.
Following parts of the research project as proceeded at University of Birminngham are presented: Translocation, Experiments, Synthesis of DNA Structures, Antibody, Biomarker, Binding. Following works have been carried out at BAM: High Resolution Electron Microscopy, Dedicated Sample Preparation, Surface Analysis Methods.
In the course of decarbonizing the energy industry, cryogenic energy carriers as liquefied hydrogen (LH2) and liquefied natural gas (LNG) are seen as having great potential. In technical applications, the challenge is to keep these energy carriers cold for a long time. This is achieved in the road transport sector and also stationary applications by thermal super insulations (TSI) which based on double-walled tanks with vacuum and multilayer insulation (MLI) in the interspace. This study focuses on the behaviour of widely used combustible MLI in a fire scenario, at vacuum and atmospheric pressure conditions. The former corresponds to the typical design condition and the latter to the condition after an outer hull rapture of a tank. Furthermore, two fire scenarios were taken into account: a standard-oriented approach and a hydrocarbon fire-oriented approach. For the study, a test rig was applied that allows testing of TSI at industrial conditions and subsequent analysis of TSI samples. The test rig allows thermal loading and performance analysis of TSI samples at the same time. Comparing the tests, the samples degraded differently. However, no sudden failure of the entire MLI was observed in any test. These results are relevant for the evaluation of incidents with tanks for the storage of cryogenic fluids and can thus contribute to the improvement of TSI and the development of emergency measures for the protection of persons and infrastructures.
Analyzing materials composed of multiple elements with spectroscopic techniques such as X-ray Photoelectron Spectroscopy (XPS), Auger-Electron Spectroscopy (AES) or Electron Probe Microanalysis (EPMA), can be challenging due to spectral overlap. Moreover, each analytical method introduces its own set of challenges, e.g., the strong secondary fluorescence effect for neighbor elements in EPMA, thus, making the accurate elemental quantification in such materials difficult. When the material is available as thin film, additional constraints are inherently present. To provide a reference material for these analytical challenges high entropy alloys (HEAs) are excellent candidates. Currently, there is no thin film reference available containing more than 2 elements.
Unlike traditional alloys, which typically consist of one or two main elements and smaller amounts of secondary elements, HEAs are characterized by the presence of multiple principal elements in almost equal proportions. This unique composition results in a high degree of disorder at the atomic level, leading to exceptional mechanical, physical, and often unexpected properties. HEAs have garnered significant attention in materials science and engineering due to their potential applications in a wide range of industries, from aerospace and automotive to electronics and renewable energy.
For the preparation of a dedicated thin film reference material, we have chosen to prepare HEAs by magnetron sputtering, since it is not associated with elemental segregation that may occur due to the high configurational entropy of HEAs, which promotes atomic rearrangements. Our goal was to prepare films with a homogeneous thickness and defined chemical composition to be analyzed by various methods dedicated to surface analysis.
The material, consisting of titanium, chromium, manganese, iron, and nickel was deposited as film on silicon substrates - to our knowledge the first HEA thin film of this type reported in literature. A set of different thickness of the films was chosen, on the one hand to facilitate the analysis with different techniques, and on the other side to evaluate the limitations of the respective methods. The films morphology was characterized as prepared by SEM followed by the analysis of their 2D compositional homogeneity by EDX, XRF, ToF-SIMS and XPS. in-depth chemical composition was evaluated by ToF-SIMS and AES. The outcomes of analyzing the initial batches of films will be presented.
Laser Powder Bed Fusion (PBF-LB/M) is a layer wise metal additive manufacturing (AM) technology, which enables significant advancements of component design, leading to potential efficiency and performance improvements. However, the thermal cycles inherent to the process comprising large localized thermal gradients and repeated melting and solidification cycles leads to the generation of high magnitude residual stresses. These residual stresses can be detrimental both during manufacturing of components and in subsequent application. Therefore, a deep understanding of the influence of process parameters on the residual stresses are crucial for efficient manufacturing and safe application. The experimental characterization of these residual stresses is therefore crucial and can provide a reliable baseline for simulations of both the process and applications.
Diffraction-based methods for residual stress analysis using penetrating neutrons and high energy X-rays enable non-destructive spatially resolved characterization of both surface and bulk residual stresses. However, the unique microstructural features inherent to the process can challenge some of our assumptions when using these methods. These challenges include the determination of a stress-free reference, the use of correct elastic constants (both SCEC and DEC) and the influence of surface roughness, texture, and porosity on residual stresses.
This presentation will detail recent insights and recommendations for the characterization of residual stresses in a range of PBF-LB/M metallic alloys (Fe, Ni, Al and Ti)
Graphene has been commercialized for over a decade. It is usually used in the form of suspensions or inks. In this study, we analyze the starting material for commercial functionalized graphene (FG) solutions and inks as well as their starting material (FG powders) using X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM), energy-dispersive X-Ray spectroscopy (EDX), time of flight secondary ion mass spectrometry (ToF-SIMS) and Auger electron spectroscopy (AES). Graphene was functionalized with fluorine, oxygen, ammonia, and carboxylic acid.
Our results suggest a significant effect of water and commercial resins on the presence as well as the morphological behavior of graphene and associated functionalized group. For example, XPS analysis shows some significant differences between the solutions and the starting materials (powders). These changes can be explained by the location of the functionalization at the outer most surface as indicated by Chemello et al.
The determination of residual stress in additively manufactured materials is a challenge, even after decades from the establishment of the basics of residual stress analysis. This is due to the peculiar microstructure of such materials. In fact, researchers have discovered that conventional methods for the determination of RS in materials do not properly work for AM materials. In this tutorial, the basics of RS analysis will be explained, together with the basics of AM manufacturing techniques. The microstructure of the peculiar materials (AM) dealt with here will be elucidated. Successively, the necessary modifications to the conventional approaches to RS analysis will be explained and case studies will be displayed, for the attendant to touch with hands the peculiarities of the approaches. Finally, a few experimental and theoretical tips will be given on dos and don’ts for a correct determination of RS in AM materials.
Graphene has been commercialized for over a decade. It is usually used in the form of suspensions or inks. In this study, we analyze the starting material for commercial functionalized graphene (FG) solutions and inks as well as their starting material (FG powders) using X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM), energy-dispersive X-Ray spectroscopy (EDX), time of flight secondary ion mass spectrometry (ToF-SIMS) and Auger electron spectroscopy (AES). Graphene was functionalized with fluorine, oxygen, ammonia, and carboxylic acid.
Our results suggest a significant effect of water and commercial resins on the presence as well as the morphological behavior of graphene and associated functionalized group. For example, XPS analysis shows some significant differences between the solutions and the starting materials (powders). These changes can be explained by the location of the functionalization at the outer most surface as indicated by Chemello et al.
Ensuring the purity of air and water is essential for the overall well-being of life on earth and the sustainability of the planet's diverse ecosystems. To achieve the goal of zero pollution, as outlined in the 2020 European Green Deal by the European Commission,[1] significant efforts are in progress. A key aspect of this commitment involves advancing more efficient and economically viable methods for treating wastewater. This includes the systematic monitoring of harmful pollutants such as heavy metals, microplastics, pesticides, and pharmaceuticals.
One example is the presence of the anti-inflammatory drug diclofenac in water systems, primarily originating from its use as a gel or lotion for joint pain treatment. Diclofenac contamination in surface waters has been detected at approximately 10 μg L-1 (0.03 μM)[2] which is not solely due to widespread usage but also because of the drug's resistance to microbial degradation. Conventional wastewater treatment plants (WWTPs), which rely on biodegradation, sludge sorption, ozone oxidation, and powdered activated carbon treatment, struggle to efficiently remove diclofenac from wastewater.[3],[4] For instance, to enable WWTPs to efficiently monitor and optimize their processes, it would be advantageous to develop on-site detection and extraction methods for persistent pharmaceutical residues in aqueous samples.
In this work, a sol-gel process was used to prepare Nile blue-doped silica nanoparticles (dSiO2-NPs) with a diameter of ca. 30 nm that were further functionalized to enable reversible-addition-fragmentation chain-transfer (RAFT) polymerization. To achieve fluorescence detection, a fluorescent monomer was used as a probe for diclofenac in ethyl acetate, generating stable complexes through hydrogen bond formation. The diclofenac/fluorescent monomer complexes were imprinted into thin molecularly imprinted polymer (MIP) shells on the surface of the dSiO2-NPs. Thus, the MIP binding behaviour could be easily evaluated by fluorescence titrations to monitor the spectral changes upon addition of the analyte. Doping the core substrate with Nile blue generates effective dual fluorescent signal transduction. This approach does not solely depend on a single fluorescence emission band in response to analyte recognition. Instead, it enables the fluorescent core to function as an internal reference, minimizing analyte-independent factors such as background fluorescence, instrumental fluctuation, and operational parameters.[5] Rebinding studies showed that the MIP particles have excellent selectivity towards the imprinted template and good discrimination against the competitor ibuprofen, with a discrimination factor of 2.5. Additionally, the limit of detection was determined to be 0.6 μM. Thus, with further optimization of the MIP, there is potential for the development of a MIP-based biphasic extract-&-detect fluorescence assay for simple, sensitive and specific sensing of diclofenac in aqueous samples down to the required concentrations of 0.03 μM.
Electron microscopy applied in different operating modes, e.g., SEM, TEM or STEM-in-SEM, is the gold standard method to investigate the exact size and shape of individual nanoparticles. However, when fine nanoparticles with a non-monodisperse size distribution and non-spherical shapes are analysed, achieving an accurate result is challenging. Deviations in size measurements of more than 10% may occur. Understanding of the contrasts and sensitivities characteristic to the individual operating modes of an electron microscope is key in interpreting and evaluating quantitatively the measurement uncertainties needed for an eventual certification of specific nanoparticles via traceable results. Further, beyond the pure measurement, the other components in the analysis workflow with significant impact on the overall measurement uncertainties are the sample preparation and the image segmentation. In the present study the same areas of selected iron oxide fine nanoparticles (<25 nm) as reference nanomaterial (candidate) prepared on substrate for electron microscopy imaging are analysed correlatively with SEM, STEM-in-SEM and TEM with respect to their size and shape distribution. Individual significant measurement uncertainties are discussed, e.g., the sensitivity of secondary electron detectors of InLens-type to the surface morphology, particularly to the presence of an ultrathin organic coating or signal saturation effects on the particle edges, to electron beam exposure, to surface contamination, or the selection of the threshold for image segmentation. Another goal of this study is to establish a basis of analysis conditions which shall guarantee accurate results when both manual and particularly (semi-)automated segmentation approaches are applied. Advantages as well as limitations of the use of different electron microscopy operating modes, applied individually and correlatively, are highlighted.
The EU member states have set out ambitious long-term goals for deploying offshore wind energy. The installed offshore wind capacity is set to increase from 14.6 GW in 2021 to around 320 GW in 2050. This signifies the role of offshore wind energy as a major contributor to reaching the EU’s climate and energy goals. To ensure that the defined targets are met, a significant number of new wind farms has to be installed and existing wind farms reaching the end of their planned life need to be reused efficiently. Some of the relevant reuse alternatives are lifetime extension, repowering based on the existing support structures and repowering with new turbines.
As a basis of the decision-making regarding the reuse of existing offshore wind farm, the expected utility of each relevant option should be determined based on the associated expected rewards, costs and risks. The optimal concept maximizes the utility of the decision-maker and fulfills the existing constraints and requirements. To facilitate such a quantitative decision-making, models and methods have to be developed. In particular, models are required that enable predictions of (a) the condition and performance of the turbines and support structures and (b) the renumeration, costs and consequences of adverse events. These predictions have to consider (a) the governing uncertainties, (b) the available information from the planning, construction, installation and operating phase, (b) potential repair, retrofitting and strengthening schemes and (c) possible monitoring, inspection and maintenance regimes for the future operating phase.
Over the past years, several models, methods and tools have been developed at the Bundesanstalt für Materialforschung und -prüfung (BAM) to support the structural integrity management of offshore wind turbine substructures. These include:
(a) a prototype for reliability-based, system-wide, adaptive planning of inspections of welded steel structures in offshore wind farms,
(b) a method for monitoring and risk-informed optimization of inspection and maintenance strategies for jacket structures subject to fatigue, and
(c) a probabilistic cost model of inspection and maintenance of welded steel structures in offshore wind farms.
This contribution provides an overview on these works and discusses how they can be adapted and extended to support the decision-making regarding lifetime extensions and repowering of offshore wind farms.
Due to the advantages of Laser Powder Bed Fusion (PBF-LB), i.e., design freedom and the possibility to manufacture parts with filigree structures, and the considerable amount of knowledge available for 316L in its conventional variant, the mechanical behavior, and related microstructure-property relationships of PBF-LB/316L are increasingly subject of research. However, many aspects regarding the - application-relevant - mechanical behavior at high temperatures are not yet fully understood. Here, we present the results of an experimental study on the LCF behavior of PBF-LB/316L featuring a low defect population, which makes this study more microstructure-focused than most of the studies in the literature. The LCF tests were performed between room temperature (RT) and 600 °C. The mechanical response is characterized by strain-life curves, and hysteresis and cyclic deformation curves. The damage and deformation mechanisms are studied with X-ray computed tomography, and optical and electron microscopy. The PBF-LB/M/316L was heat treated at 450 °C for 4 h, and a hot‑rolled (HR) 316L variant with a fully recrystallized equiaxed microstructure was tested as a reference. Besides, selected investigations were performed after a subsequent heat treatment at 900 °C for 1 h. The PBF-LB/316L exhibits higher cyclic stresses than HR/316L for most of the fatigue life, especially at room temperature. At the smallest strain amplitudes, the fatigue lives of PBF-LB/M/316L are markedly shorter than in HR/316L. The main damage mechanisms are multiple cracking at slip bands (RT) and intergranular cracking (600 °C). Neither the melt pool boundaries nor the gas porosity have a significant influence on the LCF damage mechanism. The cyclic stress-strain deformation behavior of PBF-LB/M/316L features an initial hardening followed by a continuous softening. The additional heat treatment at 900 °C for 1 h led to decreased cyclic stresses, and a longer fatigue life.
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.
The strength of age-hardenable aluminum alloys is based on the controlled formation of nm-sized precipitates, which represent obstacles to dislocation movement. Transmission electron microscopy (TEM) is generally used to identify precipitate types and orientations and to determine their size. This geometric quantification (e.g., length, diameter) is often performed by manual image analysis, which is very time consuming and sometimes poses reproducibility problems. The present work aims at the digital representation of this characterization method by proposing an automatable digital approach. Based on DF-TEM images of different precipitation states of alloy EN AW-2618A, a modularizable digital workflow is described for the quantitative analysis of precipitate dimensions. The integration of this workflow into a data pipeline concept is also presented. The semantic structuring of data allows data to be shared and reused for other applications and purposes, which enables interoperability.
The determination of residual stress in additively manufactured materials is a challenge, even after decades from the establishment of the basics of residual stress analysis. This is due to the peculiar microstructure of such materials. In fact, researchers have discovered that conventional methods for the determination of RS in materials do not properly work for AM materials. In this tutorial, the basics of RS analysis will be explained, together with the basics of AM manufacturing techniques. The microstructure of the peculiar materials (AM) dealt with here will be elucidated. Successively, the necessary modifications to the conventional approaches to RS analysis will be explained and case studies will be displayed, for the attendant to touch with hands the peculiarities of the approaches. Finally, a few experimental and theoretical tips will be given on dos and don’ts for a correct determination of RS in AM materials.
The experimental determination of residual stress becomes more complicated with increasing complexity of the structures investigated. Unlike the conventional and most of the additive manufacturing (AM) fabrication techniques, laser powder bed fusion (PBF-LB) allows the production of complex structures without any additional manufacturing step. However, due to the extremely localized melting and solidification, internal stress-induced deformation and cracks are often observed. In the best case, significant residual stress is retained in the final structures as a footprint of the internal stress during manufacturing.
Here we report solutions to the most prevalent challenges when dealing with the diffraction-based determination of residual stress in AM structures, in particular the choice of the correct diffraction elastic constants. We show that for Nickel-based alloys, the diffraction elastic constants of AM material significantly deviate from their conventional counterparts. Furthermore, measurement strategies to overcome the hurdles appearing when applying diffraction-based techniques to complex-shaped lattice structures are presented: a) proper sample alignment within the beam, b) the proper determination of the residual stress field in a representative part of the structure (i.e., with an engineering meaning). Beyond the principal stress magnitude, the principal direcions of residual stress are discussed for different geometries and scan strategies, as they are relevent for failure criteria.
We show that the RS in the lattice struts can be considered to be uniaxial and to follow the orientation of the strut, while the RS in the lattice knots is more hydrostatic. Additionally, we show that strain measurements in at least seven independent directions are necessary for the correct estimation of the principal stress directions. The measurement directions should be chosen according to the sample geometry and to an informed choice on the possible strain field (i.e., reflecting the scan strategy).
We finally show that if the most prominent direction is not measured, the error in the calculated stress magnitude increases in such a manner that no reliable assessment of RS state can be made.
The influence of test temperature and frequency on the fatigue life of the alloy EN AW-2618A (2618A) was characterized. The overaged condition (T61 followed by 1000 h/230 °C) was investigated in load-controlled tests with a stress ratio of R = -1 and two test frequencies (0.2 Hz, 20 Hz) at room temperature and at 230°C, respectively. An increase in the test temperature reduces fatigue life, whereby this effect is more pronounced at lower stress amplitudes. Decreasing the test frequency in tests at high temperatures further reduces the service life.
The determination of residual stress in additively manufactured materials is a challenge, even after decades from the establishment of the basics of residual stress analysis. This is due to the peculiar microstructure of such materials. In fact, researchers have discovered that conventional methods for the determination of RS in materials do not properly work for AM materials. In this tutorial, the basics of RS analysis will be explained, together with the basics of AM manufacturing techniques. The microstructure of the peculiar materials (AM) dealt with here will be elucidated. Successively, the necessary modifications to the conventional approaches to RS analysis will be explained and case studies will be displayed, for the attendant to touch with hands the peculiarities of the approaches. Finally, a few experimental and theoretical tips will be given on dos and don’ts for a correct determination of RS in AM materials.
A damaging action of HNO3-55% only occurs in combination with its decomposition into nitrous gases, which can be caused by UV radiation. In a laboratory test, transparent HDPE jerrycans have been exposed to both UV radiation and 55 wt-% nitric acid solution at (41 ± 2)°C, for up to 20 days. For comparison, UV radiant exposure (21 days) and nitric acid exposure (up to 6 weeks) were performed separately, at nearly equal temperatures. The respective damages are compared with FTIR spectroscopy in ATR and HT-gel permeation chromatography (GPC) on a molecular level and with hydraulic internal pressure testing as a component test. For the used jerrycans, relevant oxidation can only be found after the combined exposure. The gradual increase in oxidative damage shows the good reproducibility of the lab exposure. The decomposition of nitric acid into nitrous gases by UV radiation – as well as the jerrycan oxidation – is also observed at lower HNO3 concentration (28 wt- %). Similar results are obtained after outdoor tests. Again, the damage occurs only after combined exposure, in contrast to the exposures to UV only and to HNO3 only, which were conducted in parallel. Outdoor exposures are most readily accepted as they represent possible end-use conditions. However, the reproducibility of these exposures is poor due to the large temporal variations in weather. There are also several safety risks, which is why the number of replicates remains limited. Since the outdoor and lab exposure tests show the same qualitative results, it is appropriate to conduct systematic studies in the laboratory. After 6 days of lab exposure, the oxidation damage is rated as critical, which corresponds to about 1/10 year in Central Europe, according to the UV radiant exposure. It should be noted that this amount can also occur in two sunny weeks.
A common engineering practice is to optimize the geometry of a structure by an iterative process, in which an objective function is minimized by systematically choosing the value of design variables and computing the value of the objective function many times.
However, regarding multiscale problems, this direct numerical approach is not feasible for a number of reasons.
The model has to take into account both the structural and unit cell (UC) scale, because the objective function to be minimized is a global quantity, while the parameters are related to the shape or material parameters of the UC.
In the absence of a clear separation of scales, the direct resolution of both scales in the numerical model leads to a significant increase in computational cost, which makes it impossible to repeatedly evaluate the model during the optimization process.
The main goal of this contribution is to overcome the aforementioned limitations and develop a new efficient computational framework for the optimal design of lattice structures.
To this end, parametric MOR is combined with DD methods.
The change in geometry of each UC within the lattice is modelled by introducing a transformation that maps the reference to the physical domain.
In offline simulations, suitable localized approximation spaces, that account for the change in geometry of the UC and its neighbours, are constructed using the concept of oversampling and random sampling.
These are then integrated into a dual DD framework to derive a robust and scalable solver, i.e. a fast-to-evaluate reduced order model (ROM).
The ROM is validated on the example of optimizing a concrete arc or pre-stressed multi beam structure minimizing its mass.
Optical glasses and glass ceramics are present in many devices often used in our daily routine, such as the mobile phones and tablets. Since the 1960´s with the development of glass lasers, and more recently, within the search for efficient W-LEDs, sensors and solar converters, this class of materials has experienced extreme research progress. In order to tailor a material for such applications, it is very important to understand and characterize optical properties such as refractive index, transmission window, absorption and emission cross sections, quantum yields, etc. These properties can often be tuned by appropriate compositional choice and post-synthesis processing. In this lecture we will discuss the optical properties of glasses and glass ceramics, relevant to that end.
Non-Destructive Testing (NDT) of type 4 composite pressure vessels can be seen as key to better understanding the behaviour of the composite structure and the impact of the manufacturing process on its quality. In this presentation, NDT methods used in the “Trustworthy Hydrogen” project are introduced. A brief discussion of the observed phenomena is provided.
Society is currently confronted with two global challenges, climate change and sustainable development. This reality reverberates amongst the leading nations of the world and is articulated as a priority by the United Nations through the Framework Convention on Climate Change and its seventeen Sustainable Development Goals. In 2016, under the Paris Accord, Mission Innovation, MI, emerged as a global response to climate change and developed eight innovation challenges to mitigate its effect, including Clean Energy Materials, IC6. This innovation challenge focused its efforts on accelerating the development and deployment of clean energy materials by more than a factor of ten through Materials Acceleration Platforms, MAPs – autonomous, self-driving materials laboratories and renewed itself under the current mandate as Materials for Energy, M4E.
Self-driving labs deploy artificial intelligence, robotic automation and high-performance simulation and modeling in a closed loop system of material synthesis and characterization. An international ecosystem for accelerated materials discovery has been established and finds applications in many enabling materials technologies, including nanomaterials. The importance of nanomaterials to catalysis for hydrogen production and carbon dioxide conversion as well as energy storage in batteries is well known. In this work, the international efforts under Materials for Energy will be elaborated including the development of MINERVA - MAP for Intelligent Nanomaterial synthesis Enabled by Robotics for Versatile Applications. MINERVA was specifically built to include the specialized equipment required for the synthesis, characterization and closed-loop optimization of various nano- and advanced materials, ranging from simple inorganic (silica, metal, metal oxide) or polymeric nanoparticles to more complex core-shell architectures and materials with well-defined porosity or surface chemistry. Currently, we are investigating materials for applications in antimicrobial and antibiofouling surface coatings, sensor materials, as well as the reproducible synthesis of reference materials with this platform.
Material Acceleration Platforms (MAPs) represent a transformative approach to the development of resilient and sustainable technology value chains. These platforms can identify candidate chemistries and structures via simulations, and database searches and leverage machine learning-based rapid screening to accelerate the discovery and deployment of novel materials, thereby addressing critical challenges in modern technology sectors.
Incorporating high-fidelity advanced characterization in the early phases of material development is crucial for early de-risking. Advanced characterization techniques, such as X-ray diffraction, advanced electrochemical and spectroscopic techniques provide comprehensive insights into the structural, chemical, and physical properties of materials. Long-term testing further contributes to the de-risking process by evaluating the durability and stability of materials under various environmental and operational conditions. Early identification of potential degradation mechanisms enables the refinement of material compositions and processing methods, ultimately leading to the development of more resilient materials.
Early upscaling attempts are integral to assessing the feasibility of material leads generated through machine learning-based rapid screening to evaluate the scalability of synthesis and processing techniques. This step is critical for identifying potential challenges in manufacturing, such as issues related to reproducibility, yield, and cost-effectiveness. Process design has to be a major part of the MAP-based material design to cope with the increasing share of secondary raw materials in supply chains.
This presentation will briefly summarize possible strategies to address these issues and provide deep-dives on best practices. As the demand for advanced materials continues to grow, MAPs will play an increasingly vital role in driving technological advancements and addressing global challenges.
Übersicht über den Aktuellen Stand der Durchführungsmaßnahmen der EU zur Ökodesign-Richtlinie sowie der delegierten Rechtsakte zum EU Energielabel. Der Fokus liegt auf die Änderungen bzgl. gesetzlicher Anforderungen, die Überwachung durch die Vollzugsbehörden und mögliche diesbezügliche Informationsquellen.
Übersicht über die Umsetzung des EU Green New Deal, des Circular Economy Action Plan sowie der Sustainable Product Initiative. Ebenfalls erfolgt eine Zusammenfassung der Auswirkungen der Änderungen im EU-Produktrecht auf die Revision des geltenden Rechts und das Zusammenspiel zwischen Rechtssetzung und Normung.
Überblick über den Paradigmenwechsel der EU-Rechtsetzung zu Produkten, sowie die Erweiterung des Geltungsbereiches auf Zirkularitätsaspekte (Circular Economy). Der Überblick wird anhand des Beispieles Produktlebensdauer erklärt und die Vorteile eines Zusammenspiels zwischen der Legislative und Normungsarbeit erörtert.