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Paper des Monats
- ja (32)
The development of a robust hydrogen infrastructure poses challenges to materials exposed to high pressurized hydrogen environments. Polymeric materials, which are expected to perform as seals, gaskets, O-rings, hoses among other applications face high risk of damage due to rapid gas decompression (RGD) which might cause operational safety issues. In this study, we intend to assess the effects of a high pressurized hydrogen environment on carbon black filled (CB) elastomers. The materials were exposed to 100 MPa hydrogen atmosphere at room temperature and at 85°C. Ex-situ characterization was performed during the first 30 minutes after decompression and repeated two days after the exposure when total gas desorption has taken place. The physical and mechanical characteristics of the materials were determined by means of density and volume change, hardness and tensile tests, and dynamic mechanical analysis.
Intermittent microplasticity via dislocation avalanches indicates scale-invariance, which is a paradigm shift away from traditional bulk deformation. Recently, we have developed an experimental method to trace the spatiotemporal dynamics of correlated dislocation activity (dislocation avalanches) in microcrystals (Phys. Rev. Mat. 2 (2018) 120601; Phys. Rev. Mat. 3 (2019) 080601). Here we exploit the temperature sensitive deformation of bcc metals. A marked change of the slip-size distribution is observed in the studied microcrystals, with increasingly small event-sizes dominating with decreasing temperature. This shows how a reduction in thermal energy increasingly suppresses the length-scale of dislocation avalanches, indicating how long-range correlations become gradually limited to the scale of the lattice. Our results further show that the stress-strain response is composed of strain-increments that are either thermally activated or essentially athermal. Temperature-dependent small-scale testing in combination with state-of-the-art discrete dislocation dynamics (DDD) simulations of Nb microcrystals are used to reveal these insights.
Quenching a metallic liquid sufficiently fast can give rise to an amorphous solid, typically referred to as a metallic glass. This out-of-equilibrium material has a long suite of remarkable mechanical and physical properties but suffers from property deterioration via structural relaxation. As a function of time, relaxation may indeed constitute significant threads to safe applications. Consequently, relaxation of glasses has a long history across different amorphous materials and typical characterization methods promote a picture of gradually evolving and smooth relaxation, as for example obtained from mechanical spectroscopy. However, the true structural dynamics and underlying mechanisms remain far from understood and have hampered a physically informed atomic-scale picture of transport and physical aging of glasses.
Here we exploit the ability to track atomic-scale dynamics with x-ray photon correlation spectroscopy (XPCS) and resolve an unprecedented spectrum of short- and long-term relaxation time scales in metallic glasses. Conducted across temperatures and under the application of stress, the results reveal anything else than smooth aging and gradual energy minimization. In fact, temporal fluctuations persist throughout isothermal conditions over several hundred thousand of seconds, demonstrating heterogeneous dynamics at the atomic scale. In concert with microsecond molecular dynamic simulations, we identify possible mechanisms of correlated atomic-scale dynamics that can underly the temporal fluctuations and structural decorrelations. Despite temporally heterogeneous, the Kohlrausch-Williams-Watts functions is well suited to capture the average intermediate relaxation time regime, but at very long time scales an asymptotic power-law emerges. This indicates anomalous diffusion and gives overall strong evidence for temporal fractional diffusion in metallic glasses. We discuss these results in terms of the structural fast and slow relaxation modes as well as a true microstructure in metallic glasses.
Inspired by the ability to track atomic-scale dynamics with x-ray photon correlation spectroscopy (XPCS)1 and recent results of long-term atomistic simulations on material transport2, we reveal here an unprecedented spectrum of short- and long-term relaxation dynamics. Tracked along a 300 000 s long isotherm at 0.98Tg, a Zr-based bulk metallic glass exhibits temporal fluctuations that persist throughout the entire isotherm, demonstrating a continuous heterogeneous dynamics at the probed length scale. In concert with microsecond molecular dynamic simulations, we identify intermittent cluster dynamics as the origin for temporal signatures in the corresponding intensity cross-correlations. Despite temporally heterogeneous aging, the Kohlrausch-Williams-Watts functions is well suited to capture the average intermediate relaxation time regime, but at very long time scales an asymptotic power-law better describes the data. This indicates anomalous diffusion and gives overall strong evidence for temporal fractional diffusion in metallic glasses. We discuss these results in terms of the underlying structural fast and slow relaxation modes and their manifestation in the temporal form of the structural decorrelations.
Metallic glasses (MGs) are disordered solids that exhibit a range of outstanding mechanical, thermomechanical, and functional properties. Whilst being a promising class of structural materials, well-defined and exploitable structure-property relationships are still lacking. This offsets them strongly from the crystalline counterparts, for which length-scale based property determination has been key for decades.
In recent years, both atomistic simulations and experiments have nurtured the view of heterogeneities that manifest themselves either as a structural partitioning into well-relaxed percolated network components and more frustrated domains in atomistic simulations, or as spatially-resolved property fluctuations revealed with atomic force microscopy. These signatures depend sensitively on the processing history and likely reflect emerging medium-range order fluctuations at the scale of 1-10 nanometers.
Here we demonstrate and discuss the emergence of spatially resolved property fluctuations at length scales that are one to two orders of magnitude larger. Such long-range decorrelation length scales are hard to reconcile in a monolithic glass but may offer the perspective of experimentally easy-to-access length-scale based structure-property relationships. Whilst long-range property fluctuations can be seen in both the plastic and elastic response, we focus here on high-throughput elastic nanoindentation mapping across the surface of a Zr-based model glass. After a deconvolution of surface topography and curvature effects, the spatially-resolved elastic response reveals an elastic microstructure with a correlation length of ca. 150-170 nm. Analytical scanning-transmission electron microscopy (STEM) is used to link the elastic property fluctuations to the chemistry and structure of the MG. In concert, nano-elastic mapping and STEM suggests that structural variations in the glass are responsible for the unexpectedly large length scales. We discuss these findings in terms of the materials processing history and the perspective of exploiting nanoindentation-based spatial mapping to uncover structural length scales in atomically disordered solids.
Compatibility of welded austenitic stainless steel (316L) tube for green hydrogen applications
(2024)
The increase in the energy demand and the need to comply to net zero carbon regulations, as per the Paris 2015 climate agreement by 2050, has necessitated the urgency to consider hydrogen as alternative energy carrier. Moreover, hydrogen interaction with metals tend to cause degradation of the mechanical properties in terms of the ductility of the materials. More concern is on the weldment and repair of tubes or pipelines of hydrogen transportation and storage systems. In this study, the heat inducted weld tubes of the cold drawn and annealed austenitic stainless steel (316L) were investigated by slow strain rate test. To achieve the most realistic component-related testing, hollow tube specimens have been fabricated from 1/2-inch Swagelok pipes filled with internal gaseous hydrogen or inert air for reference. The hydrogen concentration measurement is undertaken before and after the autoclave high-pressure pre-charging of the specimens using carrier gas hot extraction. SEM analysis was used to carry out fractographic analysis to determine the crack initiation sites, crack size and was compared for the base material and heat affected zone influence in the gaseous hydrogen. The effect of hydrogen on the material compatibility of the welded austenitic stainless steel is assessed and compared to none-welded tubes tested in defined testing parameters that contribute to Hydrogen Assisted Cracking. A better understanding on the impact of weldment on the structural integrity for stainless steel is elucidated for green hydrogen application.
A hybrid deterministic-probabilistic framework is presented that combines in-situ measurements and numerical analysis to predict the characteristic size of corrosion pits over extended periods of exposure to seawater. A probabilistic model, informed by corrosion current density and temperature data, applies a sampling method to a range of overpotential values to reflect the surface deterioration in terms of pitting. The model is calibrated and validated with pit size data obtained from corroded coupons. Results reveal a positively skewed truncated lognormal distribution of pit depths which implies a higher prevalence of smaller pit depths, corroborated both experimentally and numerically.
Welded steel structures used in the offshore wind industry are exposed to harsh marine environments, which can result in corrosion-induced fatigue damage. Of particular concern is the heat affected zone (HAZ) of welded joints, a region known for its altered microstructure and mechanical properties, which can significantly influence the initiation and propagation of fatigue cracks. This study investigates the short and long fatigue crack growth rates, and the effect of seawater exposure, for the HAZ in S355 steel weldments. Single-edge notch bend (SENB) specimens are used, with a shallow notch in the HAZ. A series of specimens is immersed in synthetic seawater that is continuously circulated at a controlled temperature to assess the synergistic effects of corrosion and fatigue. The experimental method integrates a novel application of front face strain compliance for monitoring short cracks, alongside an extended back-face strain compliance approach for monitoring long crack propagation. It is concluded that the short fatigue crack growth rate of the HAZ is 2.7 to 3.5 times higher in seawater as compared to air. As the crack propagates and enters into the long crack regime, the ratio decreases to 2.2 times at the transition point of the two-stage crack growth curve and further decreases to 1.5 times when the notch advances towards fracture. The findings indicate that the fatigue crack growth rates documented in standards tend to be on the conservative side. This study significantly enriches the fatigue crack growth data available in literature, which will contribute to a more accurate lifetime assessment offshore wind turbine structures.
Early detection of fatigue cracks and accurate measurements of the crack growth play an important role in the maintenance and repair strategies of steel and composite structures exposed to cyclic loads during their service life. Commonly used non-destructive techniques such as strain gauges, clip gauges, ultrasound, etc. used for detection and monitoring of fatigue damage are contact-based and perform local measurements. In addition, complex full-field techniques are commonly investigated, such as digital image correlation (DIC) and infrared thermography (IRT). In this work, a specific implementation of IRT, called lock-in IRT, is implemented for fatigue damage detection. This technique evaluates the thermal stress response of test specimens, specifically focusing or “locking-in” on the frequency of applied cyclic loads. Three different test scenarios are presented.
First, a section of a wind turbine rotor blade made of a glass fibre reinforced plastic (GFRP) shell structure under cyclic load was examined with Lock-In IRT along with DIC. The primary advantage of Lock-In IRT in this test setup was that it required no sample preparation, as compared to the painting and speckle pattern required for DIC. In the frequency domain, specifically the frequency of applied cyclic load, it was possible to extract local directional inhomogeneous loading within the shell structure due to progressive damage, confirmed with the deformation obtained from DIC results.
Second, thick welded specimens made of structural steel S355 were subjected to multiple NDT methods such as strain gauges, crack luminescence penetration (developed specifically at BAM), ultrasound, and IRT, with the aim of investigating the ability of each technique to detect fatigue damage initiation as early as possible in the total fatigue life of the specimen. Amongst the range of implemented techniques, Lock-In IRT provided the first indication of fatigue crack initiation at the weld toe of the specimens. This was validated with the other techniques as well as fractography.
Third, steel S355 specimens used to manufacture offshore wind turbine monopiles were tested. The specimens were extracted from a plate that was submerged in a marine environment, resulting in a corroded surface with corrosion pits. These specimens were subjected to cyclic tensile loads without removing the corrosion pits. The fatigue tests were monitored using IRT in a special full-field capturing setup that enables both sides of the specimen to be examined with one IRT camera. This allowed the entire pitted surface to be monitored for fatigue damage initiation at the same time. With the implementation of Lock In IRT, the surface stress distribution could be captured (the stress concentration at the pits), and fatigue crack initiation could be detected and linked with specific corrosion pits.
Passive infrared thermography as an inspection tool for operational wind turbine rotor blades
(2024)
The growing wind energy infrastructure presents a significant challenge in the maintenance and operation of wind turbines (WT) and their intricate components. An important aspect of WT maintenance is the inspection of wind turbine rotor blades (WTB) to ensure the overall health and safety of the turbine. This inspection process involves both visual and mechanical examinations of the blades to identify any indicators of damage or wear that could compromise their performance and, consequently, the structural integrity of the entire WT system. The complexity of WTBs is compounded by their ever-expanding dimensions, exceeding 100 meters in length for 16 MW WT systems, and their multi-material composition. Within this context, passive infrared thermography emerges as a potential alternative to conventional contact- or proximity-based inspection methods. Unlike active thermography, passive thermography uses solar radiation and ambient temperature variation for thermal contrast, eliminating the need for traditional heat lamps, flash, or laser-based techniques.
A novel inspection method has been developed to semi-autonomously assess wind turbine blades (WTBs) while the wind turbine (WT) is operational, from ground level. This approach leverages optimal thermal contrast, which depends on prevailing weather conditions during field measurements, enabling the visualization of both external and internal features of the WTBs through post-processing techniques. In this study, thermal data obtained through passive thermography is compared with contemporaneous visual imagery to definitively classify observed features in thermal images as either surface or sub-surface features. This analysis, coupled with corresponding weather conditions, provides valuable insights into the capabilities and limitations of the inspection technique. Additionally, finite-element-based (FE) thermal simulations of a WTB section are employed to parametrically assess the influence of weather conditions, beyond those observed during field measurements, based on a validated model.
In addition, the thermal images also consist of thermal signatures of leading-edge turbulence due to possible leading-edge erosion in WTBs. These are primarily vortices, and their shape and size depend on the morphology of the damage as well as the rotational speed of the WTBs. The inspections are accompanied by automatic data evaluation of the thermal signatures. To improve the precision of erosion damage identification, a fully convolutional network (FCN) is employed, trained, and tested using over 1000 annotated thermographic blade images. Additionally, the study introduces strategies for grouping smaller damage indications and simplification rules based on realistic thermal imaging resolutions. As leading-edge erosion could potentially lead to annual energy production (AEP) losses, this technique could prove to be a powerful tool in establishing the presence of damage and the resulting AEP loss.
Arai, Marylyn Setsuko ; Kim, Hyunho ; Pascavis, Madeleine ; Cha, Baekdong ; Brambilla, Gabriel ; Cho, Young Kwan ; Park, Jinho ; Vilela, Raquel R. C. ; de Camargo, Andrea S. S. ; Castro, Cesar M. ; Lee, Hakho
Development of efficient portable sensors for accurately detecting biomarkers is crucial for early disease diagnosis, yet remains a significant challenge. To address this need, we introduce the enhanced luminescence lateral-flow assay, which leverages highly luminescent upconverting nanoparticles (UCNPs) alongside a portable reader and a smartphone app. The sensor’s efficiency and versatility were shown for kidney health monitoring as a proof of concept. We engineered Er3+- and Tm3+-doped UCNPs coated with multiple layers, including an undoped
inert matrix shell, a mesoporous silica shell, and an outer layer of
gold (UCNP@mSiO2@Au). These coatings synergistically enhance emission by over 40-fold and facilitate biomolecule conjugation, rendering UCNP@mSiO2@Au easy to use and suitable for a broad range of bioapplications. Employing these optimized nanoparticles in lateral-flow assays, we successfully detected two acute kidney injury-related biomarkers-kidney injury molecule-1 (KIM-1) and neutrophil gelatinase-associated lipocalin (NGAL)-in urine samples. Using our sensor platform, KIM-1 and NGAL can be accurately detected and quantified
within the range of 0.1 to 20 ng/mL, boasting impressively low limits of detection at 0.28 and 0.23 ng/mL, respectively. Validating our approach, we analyzed clinical urine samples, achieving biomarker concentrations that closely correlated with results obtained via ELISA. Importantly, our system enables biomarker quantification in less than 15 min, underscoring the performance of our novel UCNP-based approach and its potential as reliable, rapid, and user-friendly diagnostics.
Parameter studies are a common step in selecting process parameters for powder bed fusion of metals with laser beam (PBF-LB/M). Density cubes manufactured with varied process parameters exhibit distinguishable surface structures visible to the human eye. Industrial visual in-situ monitoring systems for PBF-LB/M currently have limited resolution and are incapable of reliably capturing differences in the surface structures. For this work, a 65 MPixel high resolution monochrome camera is integrated in an industrial PBF-LB/M machine together with a high intensity led bar. Post-exposure images are taken to analyze differences in light reflection on the specimen’s surface. The grey level co-occurrence matrix is used to quantify the in-situ measured visual surface structure of nickel-based super alloy IN939 density cubes. The properties of the grey level co-occurrence matrix correlate to the energy input and resulting porosity of specimens. Low energy samples with lack of fusion flaws show an increased contrast in the grey level co-occurrence matrix compared to specimens with an optimal energy input. The potential of high-resolution images as reference data in in-situ process monitoring in PBF-LB/M is discussed.
Grimault de Freitas, Tomás ; de Araujo Abilio, André ; Konert, Florian ; Nietzke, Jonathan ; Krzysch, Zephanja ; Böllinghaus, Thomas ; Sobol, Oded
The hydrogen economy is one of the most important solutions to achieve climate neutrality in Europe. It involves the production, storage, transport and use of large quantities of hydrogen in existing and new infrastructures. Components along this supply chain, such as pipelines and storage tanks, are made of various metallic materials, with steel being the most common construction material. The rapid introduction of hydrogen therefore brings with it major challenges, in particular the need for comprehensive qualification of components and materials to ensure the sustainable and safe use of hydrogen technologies. This article provides an overview of the state of the art in the testing of materials and components as well as corresponding future trends and developments for a successful transition to a hydrogen economy.
Antimicrobial resistance (AMR) is a global health problem. It is well known that antibiotics can drive evolutionary processes that underlie antimicrobial resistance (AMR) evolution and spread in clinical and environmental settings. In contrast, less is known about the effects of antimicrobial substances that are used as biocides (i.e. disinfectants and preservatives) on AMR evolution and spread. Biocides are present in various settings, interacting with diverse microbial communities. Therefore, it is crucial to evaluate their role in the evolution and dissemination of antimicrobial resistance. Biocides occur in a wide range of concentrations in various environmental settings. By examining how the various concentrations affect selection mechanisms, we gain insights into potential developments related to antimicrobial resistance. The aim of this PhD thesis is to investigate the effects of biocides on processes underlying resistance evolution. Specifically, the work focused on key mechanisms for resistance spread, resistance evolution, and the effect of selection pressures on evolved resistance mechanisms. The thesis is structured around three major objectives: (i) to determine the effect of biocides on the evolution of resistance by affecting the rate of occurrence of de novo mutations, (ii) to determine the effect of biocides on the spread of resistance genes by modifying the rate of horizontal gene transfer (HGT) processes, and (iii) to investigate the selective drivers of the emergence of antimicrobial resistance in adaptive laboratory evolution (ALE) experiments. De-novo mutations are spontaneous mutations that occur at a certain rate in microorganisms. The effect of biocides at subinhibitory environmentally relevant concentrations on the mutation rate in Acinetobacer baylyi, Bacillus subtilis and Escherichia coli was assessed with the fluctuation assay. The results showed that biocides affected mutation rates in a species and substance dependent matter. The bisbiguanide chlorhexidine digluconate, the quaternary ammonium compound didecyldimethylammonium chloride, the metal copper, the pyrethroid-insecticide permethrin, and the azole-fungicide propiconazole increase mutation rates in E. coli, whereas no increases were identified for B. subtilis and A. baylyi. Horizontal gene transfer refers to diverse mechanisms that mediate the transfer of mobile genetic elements between microorganisms. This work focused on conjugation and transformation. Conjugation is a process whereby a conjugative plasmid is transferred from a donor cell to a recipient cell. Transformation is a process whereby exogenous donor DNA is taken up into a recipient cell and integrated into the recipient’s’ genome. The effects of subinhibitory environmentally relevant biocide concentrations on the conjugation rate of E. coli and the transformation rate of the naturally competent organisms A. baylyi in were assessed. The results showed that benzalkonium chloride (BAC), chlorhexidine and permethrin increased conjugation in E. coli, while none of the biocides increased transformation rates in A. baylyi. To further understand the molecular mechanisms underlying the effects on mutation and conjugation rates, I investigated the induction of the RpoS-mediated general stress and the RecA-linked SOS response upon biocide exposure. The results show a link between the general stress and the SOS response with increased rates of mutation and conjugation, but not for all biocides. One major approach to study the evolutionary response of bacteria to antimicrobials are ALE experiments with growth at subinhibitory concentrations linked to serial subculturing over many generations. Such experiments have been used to study resistance evolution to antibiotics and biocides. However, previous work showed that adaptation to biocide stress may be mediated by different evolutionary drivers. Here, I investigated the contributions of evolution for increased survival as opposed to improved growth in ALE experiments with E. coli exposed to subinhibitory BAC concentrations. Two distinct evolutionary treatments selecting for survival only or survival and growth led to specific evolutionary adaptations apparent in the phenotypes and genotypes of the evolved populations. Populations growing in the presence of BAC evolved increased fitness in the presence of BAC associated with higher resistance to BAC and cross-resistance to antibiotics, while this was not the case for populations evolving for increased survival only. Genotypic characterization by whole genome sequencing of the evolved populations revealed parallelism in mutated genes among replicate populations and distinct differences across treatments. Treatments selecting for survival and growth showed mutations in stress response related genes (hslO and tufA), while selection for survival led to mutations in genes for metabolic regulation (cyaA) and cellular structure (flagella fliJ). In summary, this thesis shows that biocides affect AMR evolution and emphasizes the importance of understanding of how biocides impact the molecular and evolutionary process that underlie AMR evolution.
The application of an external magnetic field has been found to significantly mitigate the porosity ratio in laser beam welded joints of AlMg3 aluminum alloy. To investigate the suppression mechanism, a 3D transient multi-physics coupled numerical model of laser beam welding (LBW), including laser propagation, laser-material interaction, and magnetohydrodynamic effects, has been developed to calculate the keyhole dynamics and weld pool behaviors during the welding process. The induced time-averaged Lorenz force is directed downward. Under the effects of the external magnetic field, the fluid flow pattern and the weld pool profile are both affected. The keyhole geometry reconstruction algorithm is proposed to calculate the keyhole diameter and its fluctuation, which is used to evaluate the keyhole stability. The results indicate that the oscillating magnetic field does not affect keyhole stability obviously in the LBW of aluminum alloy. Moreover, an electromagnetic expulsive force is induced on the bubble because of the time-averaged downward Lorentz force. This electromagnetic expulsive force can accelerate the bubble escape speed considerably. An analytical model is developed for investigating the bubble escape window, which shows that the bubble escape window is expanded by 45% under the effect of the external magnetic field. The calculated results based on the developed model agree well with the experimental results.
Advanced light weight applications like aircrafts and wind turbine blades are made of fibre reinforced plastics (FRP) with continuous fibre reinforcement and must withstand a high thermo-mechanical cyclic loading. The quality of the fibre matrix interface has a high impact on the fatigue life and was continuously improved over the years since the 50th. The fatigue life of glass fibre reinforced plastics (GFRP) used in aircraft industry is 10 to 100 times higher compared to glass fibre non crimp fabrics used for wind turbine blades.
To assure a constant and reliable high quality and strength of reinforcement fibres, synthetic fibre production is state of the art (CF, GF). There is a need for recycling GFRP and CFRP waste due to the upcoming use. Pyrolysis and solvolysis are more expensive than the mechanical route however enable a more sustainable recycling. Natural fibres and recycled synthetic fibres have a high scatter in quality and strength. Hence it is a challenge to optimize the production / recycling processes to get a reliable quality for any demanding (second life) application.
Chemical routes for using renewables resources and recycling, is going to be a good approach especially for polymer-matrix systems to get 100% quality (back) compared to the state of the art.
Finally, a proper design, life-time extension and repair is preferable to recycling to keep the carbon footprint as low as possible.
The Modified Varestraint Transvarestraint test is a local variant of the globally used Varestraint test. With these tests, measuring solidification cracking susceptibility as a function of welding parameters is possible. A wide range of welding parameters for four high-strength steel filler wires, including three solid wires and one-flux cored metal wire, were tested. All wires do show a very low solidification cracking susceptibility, regardless of the paramaters. On a low level, it could be shown that solidification cracking susceptibility increases with heat input and welding speed.
Testing of highly restraint high-strength fillet welds with regards to solidification cracking susceptibility. The Controlled Thermal Severity test was used to apply a high amount of strain to solidifying welds. Test welds were cut and observed under an optical light microscope. A clear positive correlation between restraint intensity and measured crack sizes, as well as heat input and measured crack sized could be observed.
Since the original report in 2004 by Novoselov and Geim, Graphene gained incredible attention due to its fascinating properties. In the past 20 years, the synthesis and functionalization of graphene has evolved significantly[3]. Different synthesis techniques were developed which led to other graphenerelated materials such as graphene oxide (GO) or elemental-doped graphene. Further chemical functionalization can enhance but also alter or reduce specific properties of the graphene. To reveal the nature of these materials a proper physico‑chemical characterization with different analytical techniques is crucial.
Single-layer GO flakes kindly provided by Graphenea (Spain) were prepared for systematic image analysis. These flakes were disposed on an alignment-marked SiO2 substrate and correlatively imaged by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Raman spectroscopy. The high lateral resolution and/ or extreme surface sensitivity of the mentioned
techniques is necessary to explore monolayers. The ToF-SIMS images match well with the SEM and AFM images and provide information about the chemistry. With 2D Raman spectroscopy it is possible to differentiate between the number of stacked single-layer flakes. This is visualized in a 3D image (Figure b). Well-defined GO flakes could be used as a reference material for imaging of graphene-like structures but also of other types of 2D materials.
In addition to these monolayer GO flakes, commercial graphene-containing inks (Haydale) with a more complex morphology were also correlatively imaged. ToF-SIMS and SEM images were merged to identify the origin of different chemical fragments. The findings correlate closely with the expectation that the specific functionalizations (with fluorine and nitrogen as marker elements) are present only on the graphene flakes as presumed from the SEM images. Energy-dispersive X-ray spectroscopy (EDX) supports these results, yet with a much lower sensitivity compared to ToF-SIMS.
Since the original report in 2004 by Novoselov and Geim, Graphene gained incredible attention due to its fascinating properties. In the past 20 years, the synthesis and functionalization of graphene has evolved significantly[3]. Different synthesis techniques were developed which led to other graphenerelated materials such as graphene oxide (GO) or elemental-doped graphene. Further chemical functionalization can enhance but also alter or reduce specific properties of the graphene. To reveal the nature of these materials a proper physico‑chemical characterization with different analytical techniques is crucial.
Single-layer GO flakes kindly provided by Graphenea (Spain) were prepared for systematic image analysis. These flakes were disposed on an alignment-marked SiO2 substrate and correlatively imaged by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Raman spectroscopy. The high lateral resolution and/ or extreme surface sensitivity of the mentioned
techniques is necessary to explore monolayers. The ToF-SIMS images match well with the SEM and AFM images and provide information about the chemistry. With 2D Raman spectroscopy it is possible to differentiate between the number of stacked single-layer flakes. This is visualized in a 3D image (Figure b). Well-defined GO flakes could be used as a reference material for imaging of graphene-like structures but also of other types of 2D materials.
In addition to these monolayer GO flakes, commercial graphene-containing inks (Haydale) with a more complex morphology were also correlatively imaged. ToF-SIMS and SEM images were merged to identify the origin of different chemical fragments. The findings correlate closely with the expectation that the specific functionalizations (with fluorine and nitrogen as marker elements) are present only on the graphene flakes as presumed from the SEM images. Energy-dispersive X-ray spectroscopy (EDX) supports these results, yet with a much lower sensitivity compared to ToF-SIMS.
Pirskawetz, Stephan ; Bösche, Thomas ; Carstens, Ole ; Hille, Falk ; Holst, Ralph ; Käding, Max ; Kaplan, Felix ; Löhr, Manuel ; Richter, Walter ; Saloga, Katrin ; Schmidt, Sebastian ; Sodeikat, Christian ; Thenikl, Thomas
Dieses Dokument beschreibt das Verfahren Schallemissionsanalyse zur Detektion von Spanndrahtbrüchen in Spannbetonbrücken im Rahmen einer kontinuierlichen Überwachung. Die Überwachung mit Schallemission liefert eine Aussage über die Anzahl von Spanndrahtbrüchen innerhalb des Überwachungszeitraumes und innerhalb der Reichweite der installierten Sensoren. Mit dem Verfahren können die Spanndrahtbrüche lokalisiert werden. Auf Basis einer weitgehend automatisierten Datenanalyse stehen Informationen über Drahtbrüche kurzfristig nach dem Ereignis zur Verfügung.
Der Anwendungsbereich des Dokuments umfasst Brücken- und Ingenieurbauwerke mit Spanndrähten mit sofortigem oder nachträglichem Verbund. Spannsysteme ohne Verbund fallen nicht in den Anwendungsbereich. Die beschriebenen Verfahren können auf Spannsysteme ohne Verbund übertragen werden. Mit dem Verfahren Schallemissionsanalyse ist es nicht möglich, Spanndrahtbrüche zu finden, die vor dem Beginn der Überwachung entstanden sind.
Das Dokument richtet sich an Baulastträger, Anbieter und Betreiber von Monitoringsystemen auf Basis der Schallemissionsanalyse sowie Ingenieurbüros, welche die Ergebnisse der Überwachung bewerten und Maßnahmen daraus ableiten. Es gibt Hinweise zur Planung, Ausschreibung, Installation und zum Betrieb von Monitoringsystemen zur Detektion von Spanndrahtbrüchen mit Schallemission sowie zur Überprüfung der Funktion installierter Systeme. Zur Funktionskontrolle werden Signale mit der Referenzquelle am Bauwerk ausgelöst. Diese Signale sind zu detektieren, innerhalb der vorgegebenen Genauigkeit zu
lokalisieren und die vorgegebene Alarmkette muss angestoßen werden.
Contemporary steels creep-resistant steels like the 13CrMoV9-10 are used as thick plates e.g., for applications in hydrocrackers. The large plate thickness requires high efficiency welding processes like submerged arc welding (SAW) and a mandatory post weld heat treatment (PWHT). The PWHT-parameters stem from a combination of empirical knowledge and traditional experiments on free shrinking (FS) welds. In that connection, the formation of so-called stress-relief cracking (SRC) must be anticipated. The SRC susceptibility of a welded component is a complex combination and interaction of com-ponent specific, thermal, and metallurgical factors. Many of which have to date not been conclusively researched. For example, it is well known that SRCs develop during PWHT due to formation and growth of carbides on prior austenite grain boundaries, resulting in a significant hardness increase (secondary hardening) and toughness decrease. This leads to a high SRC susceptibility of the coarse grain heat-affected zone (CGHAZ) of the last weld bead during PWHT. This is intensified in case of high residual stresses from the component-specific, structurally induced stiffness. In combination with multi-layer welding this leads to a multiaxial stress distribution. Nonetheless, the combined effect of PWHT and high-residual stresses on the SRC formation is merely unknown. For that reason, this study presents the effect of different heating rates in conjunction with a certain component stiffness. For that reason, SAW joints of 13CrMoV9-10 steel were investigated under FS and defined external restraint condition.
Based on the initial call in March 2024, an update time-frame is introduced on the working plan for a comprehensive review paper series on joining and welding technologies for the manufacturing of components and parts used in sustainable energy generation, conversion, and transport with focus on hydrogen and wind energy.
As energy carrier of the future, green hydrogen can make a decisive contribution to a sustainable energy supply. In Europe concrete plans for a hydrogen pipeline grid already exist, as the so called “European Hydrogen backbone”. As building a completely new pipeline grid is economically not justifiable, a dual-way strategy of repurposing natural gas (NG) pipelines and newly built pipelines is intended. Long distance pipeline grids require regular maintenance and repairs. In that conection, for natural gas (NG) pipelines in-service welding is state of the art. Concepts such as hot-tapping (drilling into pressurized pipelines) and “stoppling” (sealing off pipeline sections after installing bypasses or pressure relieves) allow the repair of damaged pipeline sections or the installation of new branches without shutting the pipeline down. The EIGA 121/14 guideline already pointed out in 2014 that “a hydrogen hot-tap shall not be considered a routine procedure”. This shows that the determination of the transferability of these repair concepts to hydrogen pipelines is of utmost importance. Due to the degrading effects of hydrogen on mechanical proper-ties, commonly referred to as “hydrogen embrittlement” it is necessary to understand and investigate the occurring effects. In the special case of repair welding on in-service hydrogen pipelines an increased hydro-gen uptake due to a large heat input and microstructural changes in the material needs to be considered. For this reason, this paper gives an overview on existing weld repair concepts and its risks and limitations in terms of hydrogen absorption and possible embrittlement effects when transferred to hydrogen pipelines. The complexity lies in a large variety of materials (low alloyed steels), pipeline diameters and corresponding welded joints. The material compatibility of materials in used (repurposed NG-pipelines) and new condition must be investigated. Particularly for repurposed/used pipelines the effect of a pre-matured/corroded inner surface and sometimes insufficient documentation of the material “history” needs to be considered. An overview on ongoing and completed R&D-projects with respect to repair concepts for hydrogen pipelines and hydrogen effects on pipeline materials is given.
Long-term dry interim storage may adversely affect the mechanical properties of spent fuel rods, possibly resulting in a reduced resilience during handling or transport after storage. The cladding is the first barrier for the spent fuel pellets. An established method for characterising the cladding material is the ring compression test (RCT), in which a small, cylindrical sample of the cladding tube is subjected to a compressive load. Radial hydrides may precipitate in zirconium-based alloys (Zircaloy) under pre-storage drying and during slow cooling, which result in embrittlement of the cladding material and eventually a possible sudden failure of cladding integrity under additional mechanical loads. The focus of the presented research is on the development of appropriate nu-merical methods for predicting the mechanical behaviour and identification of limiting conditions to prevent brittle fracture of Zircaloy claddings. A modelling approach based on cohesive zones is ex-plained which is able to reproduce the propagation of cracks initiated at radial hydrides in the zir-conium matrix. The developed methods are applied to defueled samples of cladding alloy ZIRLO®, which were subjected to a thermo-mechanical treatment to reorient existing circumferential hy-drides to radial hydrides. A selected sample showing sudden load drops during a quasi-static ring compression test is analysed by means of fracture mechanics for illustrative purposes. Based on the developed fracture mechanics approach, not only the deformation behaviour but also the fail-ure behaviour of irradiated as well as unirradiated Zircaloy claddings with radial hydrides under RCT loading conditions can be adequately described.
Long-term dry interim storage may adversely affect the mechanical properties of spent fuel rods, possibly resulting in a reduced resilience during handling or transport after storage. The cladding is the first barrier for the spent fuel pellets. An established method for characterising the cladding material is the ring compression test (RCT), in which a small, cylindrical sample of the cladding tube is subjected to a compressive load. Radial hydrides may precipitate in zirconium-based alloys (Zircaloy) under pre-storage drying and during slow cooling, which result in embrittlement of the cladding material and eventually a possible sudden failure of cladding integrity under additional mechanical loads. The focus of the presented research is on the development of appropriate nu-merical methods for predicting the mechanical behaviour and identification of limiting conditions to prevent brittle fracture of Zircaloy claddings. A modelling approach based on cohesive zones is ex-plained which is able to reproduce the propagation of cracks initiated at radial hydrides in the zir-conium matrix. The developed methods are applied to defueled samples of cladding alloy ZIRLO®, which were subjected to a thermo-mechanical treatment to reorient existing circumferential hy-drides to radial hydrides. A selected sample showing sudden load drops during a quasi-static ring compression test is analysed by means of fracture mechanics for illustrative purposes. Based on the developed fracture mechanics approach, not only the deformation behaviour but also the fail-ure behaviour of irradiated as well as unirradiated Zircaloy claddings with radial hydrides under RCT loading conditions can be adequately described.
The European Joint Programme on Radioactive Waste Management (EURAD) is working on Spent Fuel Characterization (SFC) in its work package (WP) 8. Inspired by the EURAD activities, the International Atomic Energy Agency (IAEA) established an international Coordinated Research Project (CRP) on SFC. The EURAD WP SFC participants are collaborating as a team on the IAEA CRP on SFC. The EURAD WP SFC project consists of four tasks. Task 3 investigates the behaviour of nuclear fuel and cladding after discharge. The aim of these activities is to understand and describe the evolution of the cladding-pellet system and its ageing under conditions of extended interim storage, transportation and emplacement in a final disposal system. At the Third Research Coordination Meeting on Spent Fuel Characterization, BAM as contributor to Task 3 reported on the activities and status of its research work.
Anisotropy investigation of a single crystal superalloy using laser-spot infrared thermography
(2024)
Thermal property investigation of anisotropic materials such as single crystal superalloys are still in interest of practical and fundamental reasons but remains challenging using conventional testing methods. In this study, a single crystal superalloy is tested using laser-spot thermography, and its thermal anisotropy is investigated. Determining anisotropic thermal conductivity at microscopic scales is challenging, as it appears isotropic at the macroscopic scale. Infrared thermography is one of the best-known techniques for measuring material heat transfer properties and facilitating visualization of temperature distribution through the specimen. The proposed study uses the active thermography method of laser-spot infrared thermography, in which a laser spot is focused onto the sample surface and the thermal response is captured from the surface of the specimen with an infrared camera. A detailed analysis of temperature gradients and heat diffusion patterns aids in the measurement of thermal conductivity values along the sample's different crystallographic directions. The directional bonding characteristics and inherent crystallographic structure of the alloy account for the in-plane thermal conductivities calculated from experimental thermal measurements. The laser-spot thermography method has proven to be an effective tool for mapping the material's thermal conductivity anisotropy with high sensitivity and high spatial and temporal resolution. The investigation into the anisotropy of the material provides an insight into heat flow in the structure and helps in optimizing the design and overall performance of the material system.
The BAMline at the synchrotron X-ray source BESSY II (Berlin, Germany) is supporting researchers especially in materials science [1]. As a non-destructive characterization method, synchrotron X-ray imaging, especially tomography (SXCT) with hard X-Rays, plays an important role in structural 3D characterization. The imaging capabilities allow for in-situ and operando experiments. In this presentation the equipment, data handling pipeline as well as various examples from material science are presented.
In series-connected lithium-ion cells are susceptible to an electrical safety hazard called over-discharge. Here the behavior of copper dissolution and deposition during over-discharge is presented, which leads to irreversible loss of capacity and internal short circuits. The concentration of dissolved and deposited copper is quantified. Also, a non-uniform distribution pattern of copper deposition on the cathode is shown.
The second example deals with an Al alloy 7017 customized for a 3d-printing process by means of laser-based powder bed fusion (PBF-LB) technique. These advanced alloys have a significantly higher modulus of elasticity than conventional Al alloys, making them attractive for applications requiring high stiffness. SXCT during In-situ tensile tests confirmed that fracture initiation strongly depends on defects created during printing. However, the cracks are deflected from decohesion around inclusions/precipitates embedded in the Al matrix, increasing ductility.
Low temperature cofired ceramic (LTCC) multilayer housings offer 3D-circuits for a wide range of applications in telecommunications, microsystems and sensor technology. Such housings are produced by combining structured and metallized ceramic layers using tape-casting and multilayer technology. The characterization of the integrity, deformation, defects, and positioning of the internal metal features was carried out using in-situ SXCT at up to 950°C.
A high-precision nail penetration tool was developed to characterize the mechanically induced thermal runaway (TR) of lithium-ion battery (LIB) cells in a dynamic temperature range down to -190 °C. To investigate safety-specific low-temperature transport conditions, the damaged cells were tomographically imaged during thawing.
Planning an academic career is a bit like enjoying a box of chocolate – you never know what you are going to get next. In this talk, I will begin with sharing how luck, difficult decisions, fate, and family constraints affected my career path across continents, universities, the private sector, and to becoming a director at a national laboratory. This journey was certainly not planned and highlights how opportunities and compromises together allow you to make much more out of your engineering degree than you ever have dreamed of.
After this unusual journey as a materials scientist, I am transitioning to the technical part of my talk, where we will discuss transport in metallic glasses. This out-of-equilibrium material has a long suite of remarkable mechanical and physical properties but suffers from property deterioration via physical aging. As a function of time, relaxation may indeed constitute significant threads to safe applications, such as a complete loss of toughness.
In the search for a physical understanding of aging, we exploit here the ability to track atomic-scale dynamics with coherent x-ray scattering. Conducted across temperatures and under the application of stress, the results reveal unexpected transport. In concert with microsecond molecular dynamic simulations, we identify possible mechanisms of atomic-scale dynamics that underly physical aging of metallic glasses. We find that classical Kohlrausch-Williams-Watts behavior is only suited for the short relaxation-time regime, whereas anomalous diffusion emerges at practically relevant times. We discuss these results in terms of the structural relaxation modes and propose a picture of a true microstructure in metallic glasses.
Plastic deformation in crystals is mediated by the motion of line defects known as dislocations. For decades, dislocation activity has been treated as a homogeneous, smooth continuous process that relies on well-average quantities. However, it is now recognized that plasticity can be determined by long-range correlated and intermittent collective dislocation activity, known as avalanches. These abrupt plastic fluctuations often exhibit pure power-law scaling or truncated power-law scaling, which indicates at least some degree of scale-free dislocation behavior. Intriguingly, such statistical signatures can persist across scales exceeding those of the material’s microstructure, raising the question of what relationship there may be between structure and long-range correlated dislocation activity that underlie power-law scaling.
In this talk, we address this question by highlighting examples in which a transition from scale-free to scale-dependent plastic deformation is observed either due to changing external testing conditions (stress-state or temperature) or by tuning the microstructure. In particular, we will focus on the details of the temperature-driven change, that demonstrates how scale-free intermittent flow in body-centered cubic Nb is progressively quenched out with decreasing temperature. The plastic response of Nb is shown to be bimodal across the studied temperature regime, with conventional thermally-activated smooth plastic flow coexisting with sporadic bursts controlled by athermal screw dislocation activity, thereby violating the classical notion of temperature-dependent screw dislocation motion at low temperatures. An abrupt increase of the athermal avalanche component is identified at the critical temperature of the material. We combine the experimental observations with 3D dislocation dynamics simulations, identify a possible origin to athermal screw activity, and discuss the co-existence scale-free and scale-dependent plasticity.
Bonds and local atomic environments are crucial descriptors of material properties. They have been used to create design rules and heuristics and as features in machine learning of materials properties. Implementations and algorithms (e.g., ChemEnv and LobsterEnv) for identifying local atomic environments based on geometrical characteristics and quantum-chemical bonding analysis are nowadays available. Fully automatic workflows and analysis tools have been developed to use quantum-chemical bonding analysis on a large scale. The lecture will demonstrate how our tools, that assess local atomic environments and perform automatic bonding analysis, help to develop new machine learning models and a new intuitive understanding of materials. Furthermore, the general trend toward automation in computational materials science and some of our recent contributions will be discussed.
One contribution of materials science to energy efficiency is the continuous development of novel high-performance structural materials that push the strength-ductility envelope. A prominent example are modern advanced high-strength steels (AHSSs), which have enabled considerable weight reductions in the automotive sector, thereby enabling greenhouse emission reductions. To protect such advanced alloys from property degradation via corrosion, zinc (Zn) coatings are often applied through galvanization. Whilst protective, a Zn-coating comes with problems – the AHSS substrate becomes susceptible for liquid-metal embrittlement (LME) than can be the origin of significant mechanical property degradation when liquified Zn infiltrates into the steel substrate. Being for from understood, we focus here on non-cracked environments to capture the early stages of LME. This approach revealed the nucleation and growth of nano-scale intermetallic phases inside uncracked GBs (Materials Today Advances 13, 100196, 2022), highlighting the complex multi-phase microstructure developing before cracking occurs. To shed further light on the early stages of LME in AHSSs, we also consider the microstructural evolution of interrupted welds. We discuss our findings in the context of the time-resolved substructure evolution right beneath the interface between the AHSS and the Zn-based coating and track how Zn progressively infiltrates the substrate along phase and grain boundaries. The experimental results are further corroborated with thermodynamic simulations.
The investigation of the long-term performance of sealing systems employed in containers for radioactive waste and spent nuclear fuel is one research focus area for division 3.4 “Safety of Storage Containers” at the Bundesanstalt für Materialforschung und -prüfung. Metallic seals are in use in interim storage casks for used fuel and high active waste. Their change in performance over time is of high importance for maintaining safe enclosure. Therefore, investigations on these systems were started at BAM to get a general understanding of the relevant processes. Our investigations comprise investigations on different parameters which influence the seal performance and the main part is focussed on the time and temperature dependent behaviour.
In this contribution an update on the performed tests and their respective results will be given in respect to the overview presented in 2020.
The understanding of the long-term behaviour of the sealing systems and the performance evaluation during interim storage and subsequent transportation are our goals.
Technik, Teamwork und Wirksamkeit - Ein Berufsleben als Ingenieur für die technische Sicherheit
(2024)
Der Vortrag beleuchtet verschiedene Aspekte einer ingenieurtechnischen Tätigkeit zur Gewährleistung der technischen Sicherheit. Er gibt Einblicke in die unterschiedlichen Herausforderungen und die Komplexität der Aufgabenstellungen. An Beispielen wird dargestellt, wie die Ergebnisse der Tätigkeit für die Gesellschaft wirksam werden.
Pimienta, Pierre ; McNamee, Robert ; Hager, Izabela ; Mróz, Katarzyna ; Boström, Lars ; Mohaine, Siyimane ; Huang, Shan-Shan ; Mindeguia, Jean-Christophe ; Robert, Fabienne ; Davie, Colin ; Felicetti, Roberto ; Miah, Md Jihad ; Lion, Maxime ; Lo Monte, Francesco ; Ozawa, Mitsuo ; Rickard, Ieuan ; Sideris, Kosmas ; Alonso, Maria Cruz ; Millard, Alain ; Jumppanen, Ulla-Maija ; Bodnarova, Lenka ; Bosnjak, Josipa ; Dal Pont, Stefano ; Dao, Vinh ; Dauti, Dorjan ; Dehn, Frank ; Hela, Rudolf ; Hozjan, Tomaz ; Juknat, Michael ; Kirnbauer, Johannes ; Kolsek, Jerneja ; Korzen, Manfred ; Lakhani, Hitesh ; Maluk, Cristian ; Meftah, Fekri ; Moreau, Bérénice ; Pesavento, Francesco ; Pham, Duc Toan ; Pistol, Klaus ; Correia Rodrigues, Joao Paulo ; Roosefid, Mohsen ; Schneider, Martin ; Sharma, Umesh Kumar ; Stelzner, Ludwig ; Weber, Benedikt ; Weise, Frank
The recommendation is based on the coauthors’ work organized by the RILEM TC 256-SPF ‘‘Spalling of concrete due to fire: testing and modelling’’. The Committee has defined two types of screening tests for characterization of concrete propensity to fire spalling: Material screening tests and Product screening tests. Definitions of both types of tests are given in the paper. The following recommendations apply to Material screening tests. The material screening tests described in these recommendations are a set of minimum requirements to test concrete spalling propensity (for example, the minimal specimen size). This document covers the aspects of concrete characterization, specimen geometries, storage conditions, test methods and measured parameters.
The amount of absorbed energy in the keyhole as well as its distribution is essential to model the laser beam welding process. The recoil pressure is a key determining factor for the macroscopic flow of the molten metal in the weld pool during high-power laser beam welding. Consequently, a realistic implementation of the laser radiation on the weld metal is crucial to obtain accurate simulation results.
The following developments on the laser-material interaction are discussed for the numerical simulation of the laser beam welding process. The first implemented improvements relate to locating the exact reflection points in the ray tracing method in the determination algorithm for the intersection of the reflected rays and the keyhole surface. A second correction refers to the numerical treatment of the Gaussian distribution of the laser beam, whose beam width is defined by a decay of the laser intensity by a factor of 1/e2 thus ignoring around 14 % of the total laser beam energy. In a third step, the laser radiation distribution in vertical direction was approximated according to the beam caustics. Finally, a virtual mesh refinement was adopted in the ray tracing routine. The obtained numerical results were validated with experimental measurements.
Since we are facing more extreme weathers, the occurrence
of wildfire has also increased accordingly. The EU project
TREEADS aims to adopt a holistic forest fire management
and an adaptive, collaborative governance approach based
on the deployment of a new systemic and technological
framework covering all three interconnected fire
management stages: prevention & preparedness, detection &
response, and restoration & adaptation.
As part of the task in the so-called German pilot, numerical
simulations are performed to investigate the influencing
factors for vegetation fires with fire dynamics simulator
(FDS). The characteristics of vegetation are strongly related
to the local weather and ecosystem. The investigation of the
fire behavior of vegetation must be based on the local
vegetation in Germany. Thus, the flame propagation of typical
vegetation in Germany (pine needles, oak leaves, European
beech leaves etc.) was investigated in small scale and medium
scale experiments. These results are used as validation case
studies for the further simulations.
Der Arbeitsschwerpunkt „Sauerstoff“ des Fachbereichs 2.1 ist v.a. durch seine wissenschaftlich-technischen Tätigkeiten und seine Einnahmen aus Dienstleistungsvorgängen geprägt und bekannt. Die Durchführung standardisierter und nichtstandardisierter Prüfungen zur Untersuchung der Eignung nichtmetallischer Materialien sowie die Prüfung auf Ausbrennsicherheit von Armaturen und Anlagenteilen für den Einsatz in Sauerstoff stellen einen Großteil der Tätigkeiten und Arbeiten dar. Weit weniger bekannt sind die Forschungsaktivitäten des Arbeitsschwerpunkts, von denen drei Beispiele in diesem Vortrag kurz vorgestellt werden:
Die in Normen für Druckstoßprüfungen festgelegte Sauerstofftemperatur beträgt bei den nichtmetallischen Materialien 60 °C, bei den Armaturen aber 65 °C. Seit mehr als zwei Jahren werden nunmehr systematische Untersuchungen durchgeführt, ob dieser Temperaturunterschied zu signifikanten Unterschieden bei den Prüfergebnissen der nichtmetallischen Materialien führt. Ziel ist es, einerseits den Prüfaufwand zu optimieren und andererseits die entsprechenden Normen zu harmonisieren.
Es ist bekannt, dass Bearbeitungsverfahren, Probenvorbereitung und Vorkonditionierung einen Einfluss auf die Eignung nichtmetallischer Materialien für den Einsatz in Sauerstoff haben können. Anhand einer Charge eines Referenzmaterials werden diese möglichen Einflussfaktoren in Kooperation mit industriellen Partnern systematisch untersucht. Ziel hierbei ist es, unterschiedliche Prüfergebnisse einer Materialcharge zu erklären, die kritischsten Prüfbedingungen herauszufinden und Möglichkeiten der Übertragbarkeit von Prüfergebnissen auszuloten.
Wasserstoff gilt als zukunftsweisender Energieträger, der bei der Elektrolyse von Wasser anfallende Sauerstoff soll dabei ebenfalls genutzt werden. Die Anforderungen an die eingesetzten Materialien (Kombination aus niedrigem Druck, hohem Wasserdampfanteil im Sauerstoff und hoher Temperatur) führen dazu, dass bestehende und bewährte Prüfeinrichtungen modifiziert werden müssen. Im Rahmen BAM-interner Forschungsvorhaben und mit Unterstützung industrieller Partner wurde damit begonnen, die Zündtemperaturbestimmung sowie die Untersuchung des Alterungsverhaltens nichtmetallischer Materialien in Wasserdampf-gesättigtem Sauerstoff zu untersuchen
We introduce the REINCARNATE project, funded by the European Union's Horizon Europe program, to boost circularity by merging digital innovations with practical applications and a focus on material reuse. The heart of REINCARNATE is the Circular Potential Information Model (CP-IM), a digital platform designed to assess and enhance the recyclability of construction materials, construction products, and buildings. The CP-IM integrates advanced technologies such as digital twins, AI, and robotics to revolutionize the handling of construction waste, turning it into valuable resources and cutting the environmental footprint of the sector. Among its features are digital tracing, material durability predictions, and CO2 reduction materials design. These are showcased in eleven European demonstration projects, highlighting the practical benefits of these technologies in reducing construction waste and CO2 emissions by up to 80% and 70% respectively. REINCARNATE aims to marry innovation with real-world application, providing the construction industry with strategies for sustainable and circular practices.
Das EU-finanzierte Projekt REINCARNATE, im Rahmen des Horizont Europa Programms, setzt neue Maßstäbe in der Kreislaufwirtschaft des Bauwesens durch den Einsatz fortschrittlicher Bauwerksdiagnose-Tools. Diese Werkzeuge, insbesondere die Zerstörungsfreie Prüfung (ZfP), spielen eine zentrale Rolle bei der Förderung der Zirkularität in der Baubranche. Die ZfP ermöglicht es, die Qualität und Eignung von Baumaterialien präzise zu bestimmen, ohne diese zu beschädigen. Dies ist entscheidend für die Wiederverwendung und das Recycling von Baustoffen und trägt wesentlich zur Reduzierung des Bauabfalls bei. Durch die Integration dieser Technologie in die Planungs- und Entwurfsphase können Architekten und Ingenieure aktiv einen nachhaltigeren Bauprozess fördern. REINCARNATE verbindet diese Diagnosemethoden mit digitalen Innovationen wie der Technologie des digitalen Zwillings und KI-gesteuerten Lösungen. Diese Kombination ermöglicht eine noch genauere und effizientere Bewertung und Nutzung von Baustoffen, was die Wiederverwendbarkeit und das Recycling verbessert. Im Rahmen des Projekts werden elf Demonstrationsprojekte in ganz Europa umgesetzt, die die praktische Anwendung dieser Technologien zeigen. Diese Projekte demonstrieren, wie ZfP und digitale Werkzeuge zusammenwirken, um Materialien, die traditionell als Abfall angesehen werden, in wertvolle Ressourcen umzuwandeln. Das Ziel von REINCARNATE ist eine 80-prozentige Verringerung der Bauabfälle und eine 70-prozentige Reduzierung des CO2-Fußabdrucks. Mit diesem Beitrag demonstrieren wir eine klare, umsetzbare Anleitung für die Bauindustrie, wie Innovationen in die Praxis umgesetzt werden können. Wir präsentieren greifbare Strategien zur Implementierung nachhaltiger, zirkulärer Praktiken im Bauwesen und markiert einen Wendepunkt in Richtung einer nachhaltigeren Bauindustrie.
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.
The following contribution presents the analyses of additively manufactured (AM) 316L using hollow specimens at 200 bar hydrogen and a strain rate of 1E-5 s-1. The work includes a comparison of three types of hollow specimens: mechanically extracted from fully additively manufactured cylinders, near-net-shape additively manufactured specimens, i.e. as printed, and specimens made of conventional 316L. AM specimens were manufactured via powder bed fusion with laser beam of metals (PBF-LB/M). For the near-net-shape specimens the inner hole remained without any mechanical processing. The inner holes of the cylindric specimens were manufactured by drilling with subsequent honing.
The susceptibility to hydrogen embrittlement was found to be strongly dependent on the surface being in contact with hydrogen. While specimens with a clean surface had a relative reduction of area (RRA) of around 78 %, those with an as-printed surface showed a significantly larger RRA of around 90 %. One possible reason for this are oxide layers formed due to small amounts of oxygen during the AM-process.
Further research is required to determine if the lower effect on the mechanical properties is permanently for as printed parts or e.g. time dependent. Additionally, further work with variation in the nominal strain rate is required.
Validated and standardized methods in microplastic analysis are indispensable for robust monitoring and regulation. Alongside also reference materials are urgently needed. An interlaboratory comparison (ILC) offers a powerful tool to address both these challenges. The present study aimed to compare the precision and accuracy of various methods for the detection and quantification of microplastic in a water-soluble matrix. Additionally, it evaluated the suitability of the test materials (containing environmentally relevant plastic polymers) to serve as reference materials for the microplastic analysis.
In this ILC several most used thermo-analytical and spectroscopic methods have been addressed: Pyrolysis-Gas Chromatography Mass Spectrometry (Py-GC/MS), Thermal Extraction-Desorption Gas Chromatography Mass Spectrometry (TED-GC/MS), micro-Fourier Transform Infrared Spectroscopy (µ-FTIR), and micro-Raman Spectroscopy and Laser Direct Infrared Spectroscopy (LDIR). Microplastic powders of polyethylene (PE) and polyethylene terephthalate (PET) were used to assess suitability of the test materials (microplastic tablets) for method validation and use in the ILCs. The participants were guided with a SOP how to dissolve the test samples and, depending on their selected method, either quantify the number of particles (by the spectroscopic methods) or determine the mass fraction of microplastic particles per sample (by the thermo-analytical methods).
This article presents two case studies for a full-probabilistic assessment of existing concrete bridges combined with the use of the finite element method for the evaluation of the internal forces. Since the structures already exist, additional information about material parameters and loading conditions can be collected. With a sensitivity analysis, the contribution of each parameter to the total uncertainty is examined and the relevance of their actual value and variation is shown. The first case study is a single-span reinforced concrete frame bridge on the German highway A92 constructed in the year 1985. With a span of around 5 m, but a width of 27 m and a skewness of 70 gon, the bridge is modelled as a three-dimensional finite element model. The second case study is a two-span reinforced concrete frame bridge from 1986 with span lengths of about 7,50 m each. The superstructure is a 45 cm thick slab and the base plate has a thickness of 80 cm. The assessment is performed based on the semi-probabilistic safety concept according to the codes first and secondly with a full-probabilistic calculation. In this article the selection of parameters for the relevant input data are presented and discussed. The results of the sensitivity analysis are used for the setup of measurements to acquire important data for the modelling in the critical limit states.
In reliability assessment of existing bridges, collected information about the structure can be utilized to modify partial safety factors and to refine characteristic values individually. In this way, uncertainties covered in initial calculation models and arising from assumptions can be reduced as well as biases identified and corrected. This allows for more realistic assessments and more appropriate decisions on actions to be taken. However, the on-site observation of information is generally associated with certain costs. For this reason, an efficient data-supported reassessment requires that only the individually relevant testing tasks are solved. Additional sensitivity analyses can further be used to specify the requirements on certain inspections, such as the testing result quality to be achieved, in order to avoid too imprecise or too expensive measurements on-site. In this contribution, the methodology for the demand-actuated definition of measurement objectives is demonstrated using the example of non-destructive concrete testing methods and findings from reassessments of two prestressed concrete bridges. Each case study includes the semi-probabilistic identification of structural weak points in ultimate and serviceability limit states, a comparison with respective probabilistic sensitivity analyses, and the subsequent derivation of parameters that are a) measurable and b) highly relevant in the individual reliability analyses.
AbstractIm zweiten Teil dieses Beitrags werden die Grenzzustandsfunktionen für die Nachweise im Grenzzustand der Tragfähigkeit für Biegung mit Normalkraft, Querkraft mit Querkraftbewehrung und Torsion vorgestellt. Die Eingangsgrößen der mechanischen Widerstandsmodelle werden durch zahlreiche Abbildungen illustriert. Auf Grundlage der probabilistischen Modelle aus dem ersten Teil dieses Aufsatzes und der mechanischen Modelle aus diesem zweiten Teil werden die probabilistischen Nachweise geführt. Die Ergebnisse aus der Zuverlässigkeitsanalyse werden mit den semiprobabilistischen Berechnungsergebnissen verglichen. Mittels Parameterstudien wird gezeigt, welche Eingangsgrößen im Standsicherheitsnachweis die größten Einflüsse auf die Bauwerkszuverlässigkeit haben. Die Messung dieser Parameter ist entsprechend besonders nützlich. Auf dieser Basis wird abschließend gezeigt, welche Chancen sich aus der Durchführung von zerstörungsfreien Bauwerksprüfungen für die Nachrechnung ergeben.
The constantly increasing demand for renewable energy sources lead to the necessity of transporting large amounts of hydrogen. Since pipelines enable a cost-effective way for the distribution of gaseous hydrogen, the interaction of hydrogen and the pipeline materials must be carefully investigated as hydrogen can cause a degradation of the mechanical properties under certain conditions. Especially welds, which are assumed to be more susceptible to the degradation enhanced by hydrogen, are of great interest. The aim of this study is to investigate the effect of gaseous hydrogen on the mechanical properties of an X65 pipeline, and the longitudinal submerged arc welding (SAW) welded joint. The tests are conducted using the hollow specimen technique on two types of specimens: one extracted from the base material (BM) and the other extracted as a cross-weld (CW) specimen consisting of base material and weld seam. The specimens are charged in-situ under a pressure of 60 bar and tested using slow strain rate (SSR) tensile tests with a nominal strain rate of 10-5 s-1. The performed tests showed a decrease of the reduction of area (RA) from 72% in inert atmosphere to 52% in hydrogen atmosphere for the CW-specimen and a decrease from 73% in inert atmosphere to 51% for the BM. Metallographic analyses showed the crack initiation between fine grain heat affected zone (FGHAZ) and BM for the specimens tested in hydrogen atmosphere as well as for the reference specimens. This leads to the conclusion that the location of the crack initiation does not change due to the presence of gaseous hydrogen.
AbstractDer Erhalt der bestehenden Verkehrsinfrastruktur ist eine große Herausforderung, da die Bauwerke fortwährend altern, die Verkehrsbeanspruchung zunehmend steigt und deren umfassender Ersatz mit Blick auf begrenzte Budgets und Ressourcen nicht möglich ist. An Bestandsbauten können tatsächliche Materialkennwerte, Geometrien oder Einwirkungen objektspezifisch erfasst werden. Die Nachrechnung von Bestandsbrücken erfolgt in Deutschland gemäß Nachrechnungsrichtlinie nach Stufen 1 und 2 mit dem semiprobabilistischen Teilsicherheitskonzept. Nur im Ausnahmefall wird eine messbasierte Bewertung oder eine wissenschaftliche Betrachtung gemäß Stufen 3 und 4 durchgeführt. Die Einbeziehung zusätzlicher Informationen aus der Zustandserfassung bietet jedoch viele Vorteile für eine realitätsnahe Bewertung. In probabilistischen Berechnungsmethoden können solche Kenntnisse direkt in der Berechnung berücksichtigt werden. Ziel dieses zweiteiligen Beitrags ist die Vorstellung der Potenziale und Vorteile bei der direkten Berücksichtigung der Ergebnisse von zerstörungsfreien Prüfverfahren bei der Zustandsbewertung von Brückenbauwerken. Das Konzept wird an einer Spannbetonbrücke vorgestellt. Der erste Teil befasst sich mit den Möglichkeiten zur Überführung der Eingangswerte der üblichen semiprobabilistischen Berechnung in stochastische Modelle. Ausgehend von der semiprobabilistischen Nachrechnung nach derzeitigem Regelwerk wird die probabilistische Modellierung aller relevanten Basisvariablen für die Grenzzustände der Tragfähigkeit Biegung, Querkraft und Torsion ausgeführt.
Nichtelektrischer Explosionsschutz - Grundlagen und Maßnahmen zum nichtelektrischen Explosionsschutz
(2024)
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).
Moisture testing and mapping
(2024)
Most building materials are porous and hydrophilic. Thus, for condition assessment and damage detection a determination of the material moisture is required. In this lecture, a short overview is given regarding moisture transport in porous media in the hygroscopic range. Then, several non-destructive measurement techniques are introduced. Here, the focus lies on their practical application and limitations.
In the approval process of dangerous goods packagings, drop tests onto a flat, essentially unyielding surface are used to assess resistance against mechanical damage. International adopted regulations like ADR and RID define filling good dependent drop heights and filling degrees whilst the user needs to define the maximum gross mass to be tested and approved. Maximum packaging gross mass is defined conservatively and not reached in practice. To meet the defined gross mass in testing, using additives is permitted. However, in some cases, additives are not desirable due to packaging design or filling substance properties. This leads to deviations from the initial gross mass definition. Hence, a certain drop height adjustment is necessary to achieve the required impact loading. Laboratories frequently adjust drop height assuming a perfectly elastic collision which is inaccurate. Appropriate adjustment is not trivial due to energy conversion processes, e.g., plastic deformation. In this work, a test stand is developed for measuring the change in kinetic energy of different packaging designs and filling substances in regulative drop tests. The experimental results are used to validate finite-element (FE) models so that packaging properties can be varied in simulated drop test scenarios. The findings intend to describe the appropriate drop height adjustment of the respective packaging with same design but deviating gross mass to produce comparable mechanical response. The results are highly beneficial for testing laboratories, approval issuing authorities and packaging institutes confronted with the problem of testing packages with gross masses other than those to be approved.
Hybrid additive manufacturing is becoming increasingly important in the field of additive manufacturing. Hybrid approaches combine at least two different manufacturing processes. The focus of this work is the build-up of geometries onto conventionally manufactured parts using laser-based powder bed fusion of metals (PBF-LB/M). The hybrid build-up requires a precise position detection system inside the PBF-LB/M machines to determine the exact position of the existing component. For this purpose, high-resolution camera systems can be utilized. However, the use of a camera system is associated with several challenges. The captured images are subject to various distortions of the optical path. Due to these distortions, it is not possible to use the images for measurements and, therefore, it is not possible to calculate the positions of objects. In this study a homography matrix is calculated to correct keystone distortion in the images. Different calibration patterns have been tested for the calculation of the homography matrix. The influence of the number of calibration points on the precision of position detection of objects is determined. Furthermore, the influence of an additional camera calibration by using ChArUco boards is evaluated. The result is a camera calibration workflow with associated calibration pattern for a precise position detection of parts inside PBF-LB/M machines allowing a hybrid build-up with minimum physical offset between base component and build-up.
Das Laserstrahl-Lichtbogen-Hybridschweißverfahren kombiniert Laserstrahl- und Lichtbogenschweißverfahren in einem gemeinsamen Schmelzbad. Das Verfahren wurde Ende der 70er Jahre entwickelt, um die Synergieeffekte der Schweißprozesse effektiv zu nutzen. Durch die hohe Strahlungsintensität des Laserstrahls werden hohe Einschweißtiefen erreicht. Es ist möglich, die Anzahl der Schweißlagen zu reduzieren und somit die thermische Belastung des Grundwerkstoffes zu senken, da der Wärmeeintrag verringert wird. Die Überbrückung von Spalten und Kantenversatz kann durch die Zufuhr eines geschmolzenen Zusatzdrahtes durch das MSG-Verfahren erreicht werden. Der Zusatzdraht kann zudem das metallurgische Gefüge positiv beeinflussen. Daher ist das Laser-Hybridschweißverfahren ideal für das einlagige Schweißen von Dickblechen und wird bereits erfolgreich in der Schiffbauindustrie zum Schweißen von Blechen mit einer Dicke von bis zu 15 mm verwendet. Obwohl Hochleistungslaser heutzutage bereits im Multi-Kilowatt-Bereich verfügbar sind, sind sie für den industriellen Einsatz nur auf Stahlbleche mit einer Dicke von max. 15 mm geeignet. Hohe Abkühlgeschwindigkeiten, gravitationsbedingtes Austropfen beim einlagigen Schweißen von Dickblechen, Prozessinstabilitäten bei höheren Laserleistungen und Schweißnahtimperfektionen wie Rissbildung sind einige Faktoren, die den Einsatz von Laser-Hybridschweißtechnologien aktuell begrenzen. Ohne eine Badstütze ist eine Verringerung der Schweißgeschwindigkeit und somit der Abkühlgeschwindigkeit aufgrund unzulässiger Wurzelüberhöhungen oder gravitationsbedingtem Austropfen nicht möglich. Bei herkömmlichen Badstützen ist es allerdings erforderlich, dass sie mechanisch befestigt und die Wurzel entfernt oder nachbearbeitet werden muss. In dieser Arbeit wird als Alternative das innovative Konzept der elektromagnetischen Schweißbadsicherung vorgestellt und die Fähigkeiten dieses Verfahrens erläutert.
Auf dem Weg zum einlagigen Schweißen von dickwandigen Bauteilen – Prozesse, Potenziale, Beispiele
(2024)
Bislang kommt das Laserstrahlschweißen bzw. Laserhybridschweißen hauptsächlich bei Dickblechen mit einer Wandstärke von bis zu 15 mm zum Einsatz. Für Anwendungen über 20 mm war dieses Verfahren aufgrund einiger Herausforderungen bisher nur bedingt realisierbar. Die von der Ausgründung WeldNova GmbH der Bundesanstalt für Materialforschung und -prüfung (BAM) entwickelte Schweißbadsicherung ermöglicht nun ein einlagiges Schweißen von bis zu 40 mm Wandstärken mit einer Laserleistung von bis zu 20 kW.
Aschen und Schlacken aus der thermischen Abfallbehandlung stellen mit rund 25% Massenanteil die größte Reststofffraktion dar. In Deutschland fallen pro Jahr rund 6 Millionen Tonnen an. Während sich die Verwertung der metallischen Anteile problemlos gestaltet, werden an die mineralische Fraktion Anforderungen bezüglich der möglichen Freisetzung von Schwermetallen sowie Chlorid und Sulfat gestellt. In der Ersatzbaustoffverordnung sind für Aschen und Schlacken aus der Abfallverbrennung zwei Materialklassen mit unterschiedlich hohen Anforderungen an die Umweltverträglichkeit definiert. Im Rahmen eines Forschungsprojekts wurde untersucht, ob mit Abtrennung der Feinfraktion von 0–2mm die höhere Materialklasse HMVA-1 erreicht werden kann. Im Ergebnis wurde eine Verbesserung des Auslaugverhaltens erzielt, doch nicht in dem Maß, dass eine Qualität nach HMVA-1 erreicht wird. Rostaschen halten aber die Anforderungen zur Deponierung auf einer DK I-Deponie sowie die Anforderungen zur Verwertung gemäß HMVA-2 sicher ein.
Hybrid additive manufacturing is becoming increasingly important in the field of additive manufacturing. Hybrid approaches combine at least two different manufacturing processes. The focus of this work is the build-up of geometries onto conventionally manufactured parts using Powder Bed Fusion with Laser Beam of Metals (PBF-LB/M). The hybrid build-up requires a precise position detection system inside the PBF-LB/M machines to determine the exact position of the existing component. For this purpose, high-resolution camera systems can be utilized. However, the use of a camera system is associated with several challenges. The captured images are subject to various distortions of the optical path. Due to these distortions, it is not possible to use the images for measurements and, therefore, it is not possible to calculate the positions of objects. In this study a homography matrix is calculated to correct keystone distortion in the images. Different calibration patterns have been tested for the calculation of the homography matrix. The influence of the number of calibration points on the precision of position detection of objects is determined. Furthermore, the influence of an additional camera calibration by using ChArUco boards is evaluated. The result is a camera calibration workflow with associated calibration pattern for a precise position detection of parts inside PBF-LB/M machines allowing a hybrid build-up with minimum physical offset between base component and build-up.
Soybean oil takes around half of the vegetable oil resources in the world, increasing in importance constantly. Besides, soy oil plants have experienced numerous accidents due to the coexistence of soy flour and hexane (as a solvent) in the extraction process, thus creating a hazardous environment. This study aims to find the maximum pressure, the maximum rate of pressure rise, and the minimum ignition energy of soy flour−hexane mixtures through specific experiments by varying the concentration of fuels in air and ignition mechanism (chemical igniters or exploding wires). The results have shown that soy flour alone is hard to ignite, whereas adding hexane even in small amounts increases the hazard and the severity of the explosions considerably. Eventually, the substitution of hexane with a greener and safer extraction agent should be of utmost focus.
Stable metal isotopes receive increasing attention as medical biomarkers due to their potential to detect changes of the metal metabolism related to disease. Potential mechanisms causing isotope fractionation include biological processes that involve redox- or bond-forming reactions and interaction of metals during transmembrane import and export. In order to advance our understanding of the underlying processes responsible for isotope fractionation between normal and diseased cells, we need in situ, spatially resolved methods. Despite its frequent use, laser ablation - multi-collector - inductively coupled plasma mass spectrometry (LA-MC-ICPMS) analysis of biological material is severely limited by the scarcity of matrix-matched standards. Such matrix-matched standards are necessary to correct for instrumental sources of isotope fractionation such as particle size distribution, ablation physics and differential ionization.
Copper stable isotopes have proven to be a particularly powerful tool to identify differences in isotope composition between tumors and healthy tissue suggesting application in cancer diagnosis [1, 2]. To further our knowledge of Cu isotope fractionation processes induced by diseases we have developed gelatin-based bracketing standards allowing to correct instrumentally induced isotope fractionation during LA-MC-ICPMS analysis. Since gelatin properties resemble properties of protein-rich cellular material, they mimic biological matrices and their ablation behaviour. Hence, gelatin standards are spiked with known amounts of Cu stable isotopes of a known Cu isotope composition and used as matrix-matched bracketing standard. A Ni reference solution was aspirated to the plasma to allow for mass bias correction and laser energy densities were below the glass ablation threshold. The method achieved reproducibilities of better than 0.10‰ (2SD) for inorganic reference materials and reproducibilities of better than 0.17‰ (2SD) for biological reference materials. The developed routine is tested on biomedical samples and the in situ Cu isotope data will be presented.
The stress–strain behavior of certain ceramics, such as aluminum titanate (AT, Al2TiO5), has features that are unusual for brittle material. In particular, a substantial nonlinearity under uniaxial tension, and load–unload hysteresis caused by the increase of the incremental stiffness at the beginning of unloading. These features are observed experimentally and attributed to microcracking. In this study, we investigate the mechanical response of an AT material at room and high temperature. Microstructure and microcracking are analyzed by means of electron microscopy, and both synchrotron micro computed tomography (µCT) and refraction radiography (SXRR). Synchrotron refraction radiography is combined with in-situ heating at high-temperatures (up to 1400°C) to be able to monitor the relative closure of microcracks as a function of increasing/decreasing temperatures.
Diller, Johannes ; Siebert, Ludwig ; Winkler, Michael ; Siebert, Dorina ; Blankenhagen, Jakob ; Wenzler, David ; Radlbeck, Christina ; Mensinger, Martin
AbstractThis research aims to detect and analyze critical internal and surface defects in metal components manufactured by powder bed fusion of metals using a laser beam (PBF‐LB/M). The aim is to assess their impact on the fatigue behavior. Therefore, a combination of methods, including image processing of micro‐computed tomography (CT) scans, fatigue testing, and machine learning, was applied. A workflow was established to contribute to the nondestructive assessment of component quality and mechanical properties. Additionally, this study illustrates the application of machine learning to address a classification problem, specifically the categorization of pores into gas pores and lack of fusion pores. Although it was shown that internal defects exhibited a reduced impact on fatigue behavior compared with surface defects, it was noted that surface defects exert a higher influence on fatigue behavior. A machine learning algorithm was developed to predict the fatigue life using surface defect features as input parameters.
In der automatisierten Ultraschallprüfung von Komponenten mit komplexen Oberflächengeometrien werden zur Führung des Prüfkopfes zunehmend 6-Achsen-Roboter erprobt. Diese stellen die notwendige Automatisierbarkeit und Flexibilität bereit, um die lokal senkrechte Einschallung sicherzustellen. Durch den Einsatz von linearen Arrays und bildgebenden Verfahren können die Bilder oder die daraus extrahierten Merkmale zu einer Rekonstruktion in 3D zusammengesetzt werden. Die Anforderungen an die Prüfbahnen für die bildgebende Array-Ultraschallprüfung gehen dabei über konventionellen Bahnplanungsprogramme hinaus. Es wird ein Prozess vorgestellt, der Roboterbahnen auf der Grundlage des 3D-Modells von Körpern mit doppelt gekrümmter Oberfläche unter Berücksichtigung der Prüfparameter erzeugt. Hierbei wird zum einen die senkrechte Prüfkopfstellung und zum anderen eine optimale Abdeckung der Oberfläche realisiert. Dabei wird die lokale Oberflächengeometrie beachtet, da diese das Reflexionsverhalten beeinflusst und sich daher auf die optimale Verteilung und Orientierung der Prüfpositionen auswirkt. Damit einhergehend erfolgt eine Ablösung von konventionellen Konzepten, die auf linearen Prüfbahnen basieren, welches spannende neue Prüfstrategien eröffnet.
Durch das alkalische Porenwassermilieu ist Stahl im Beton vor Korrosion geschützt. Unter ungünstigen Umgebungsbedingungen (Karbonatisierung, Chlorideintrag) kann die passive Deckschicht auf der Stahloberfläche zerstört werden. Im weiteren Verlauf können sich korrosionsbedingte Folgeschäden, wie Risse und Abplatzungen am Bauwerk ergeben. Um notwendige Sanierungsmaßnahmen sind frühzeitige und weitgehend zerstörungsfrei ermittelte Informationen über das aktuelle Korrosionsverhalten der Stahlbewehrung von großer Bedeutung. Die Potentialfeldmessung ist ein etabliertes und weit verbreitetes Verfahren zur Beurteilung des Korrosionszustandes der Bewehrung in Stahlbetonbauwerken. Mit Hilfe dieses Verfahrens können Bereiche aktiv korrodierender Bewehrung zerstörungsfrei lokalisiert werden. In der Regel kommt diese Messmethode bei der Detektion chloridinduzierter Korrosion zum Einsatz. Wie und unter welchen Randbedingungen dieses Messverfahren zielführend eingesetzt werden kann, ist im Merkblatt B 03 der dgzfp erörtert.
Electrochemical potential mapping is a recognized technique for the localization of corroding reinforcing steels. Areas of corroding reinforcement steel can be located in a non-destructive manner by means of this procedure. Half‐cell potential measurements are used in order to detect chloride‐induced corrosion. However, it is not recommended in order to assess the risk of carbonation‐induced corrosion. For this purpose, determining the carbonation depth and the concrete cover appears more appropriate. The content of this specification exclusively refers to the application of mobile, local variable reference electrodes, which are only placed on the concrete surface while measuring. The technique distinguishes itself thereby from the range of corrosion monitoring systems with stationary installed reference electrodes and sensor systems, respectively, whereby it is possible to continuously track measurements within the area of the installed electrodes. However, these methods are not dealt with in this specification.
The stress–strain behavior of certain ceramics, such as aluminum titanate (AT, Al2TiO5), has features that are unusual for brittle material. In particular, a substantial nonlinearity under uniaxial tension, and load–unload hysteresis caused by the increase of the incremental stiffness at the beginning of unloading. These features are observed experimentally and attributed to microcracking. In this study, we investigate the mechanical response of an AT material at room and high temperature. Microstructure and microcracking are analyzed by means of electron microscopy, and both synchrotron micro computed tomography (µCT) and refraction radiography (SXRR). Synchrotron refraction radiography is combined with in-situ heating at high-temperatures (up to 1400°C) to be able to monitor the relative closure of microcracks as a function of increasing/decreasing temperatures.
Non-specific Gd-based contrast agents (GBCAs) have long been routinely used in clinical magnetic resonance imaging (MRI). However, the interaction of such contrast agents with tissue components is not yet fully understood.
Alongside cells, the extracellular matrix (ECM) is an important component of mammalian tissue. It is a three-dimensional network of macromolecules that provides structural and biochemical support to the surrounding cells. Many diseases, including inflammation, fibrosis, and tumour invasion, are associated with characteristic ECM changes. The ECM consists of structural proteins (e.g., collagen, elastin) and proteoglycans, which are composed of glycosaminoglycans (GAGs) covalently linked to a protein core. GAGs are long, linear polysaccharides consisting of repeated disaccharide units widely varying in molecular mass, disaccharide structure, and sulfation degree. Characteristic of GAGs is their ability to form complexes with cations such as lanthanides. Thus, GAGs could be a potential binding partner for GBCA molecules as a whole or for dechelated Gd.
Currently, there are still many unanswered questions about the interaction of contrast agents with ECM components. This study therefore investigated the uptake and distribution of different GBCAs in spheroids that mimic biological tissue and have different ECM expressions.
Chinese hamster ovary (CHO) cells and GAG-depleted CRL-2242 cells were used to prepare spheroids. These were then incubated for several minutes with gadolinium chloride and various linear and macrocyclic GBCAs. Cryosections of the spheroids were used for imaging measurements with a low-dispersion laser ablation system coupled to an inductively coupled plasma time-of-flight mass spectrometer (LA/ICP-ToF-MS). Gelatine doped with multi-element solutions was used for matrix-matched quantification of Gd and other relevant elements such as Cu, Fe and Zn.
Although all spheroids were incubated with identical Gd concentrations, significant differences in the amount of Gd taken up were observed. Gadolinium chloride is absorbed more strongly than the contrast agents and accumulates mainly in the outer regions of the spheroids. In contrast, after incubation with the linear and macrocyclic contrast agents, Gd is detected in the interior of both types of spheroids.
DIN 4871
(2024)
Laboratory sources offer a unique advantage compared to synchrotron sources, largely in terms of freedom of operation. This freedom from user obligations, technology and software stacks and legacy decisions make the laboratory a very flexible place to develop and explore new ideas. The unparalleled availability furthermore allows for iterative improvement of instrumentation, sample environments and measurement methodologies to maximise the quality of the data obtained.
This talk will highlight the use of the laboratory as an agile test-bed and development space, by giving examples of some complete and incomplete investigations undertaken in our laboratory over the last years. Furthermore, it will introduce the concept of holistic experimentation, where the laboratory provides broad-ranging support for materials science investigations. This means that we assist in the experimental preparation, perform the measurements, correction and analysis, and follow-up with assistance in interpretation of our analyses in light of the results from other techniques applied to the investigation.
A chemical engineer by training, Brian drifted towards physics and now focuses on a broad spectrum of activities with the aim to improve scientific reproducibility. This includes studies on holistically improving data quality, data collection efficiency and traceability, as well as concomitant laboratory automation for the preparation of consistent, well-documented sample series. The need for pragmatism led to an inexpensive, flexible laboratory automation platform that can be implemented in a modest amount of time. This talk presents that effort.
Additive manufacturing is one of the most promising techniques for industrial production and maintenance, but the specifics of the layered structure must be considered. The Direct Energy Deposition-Arc process enables relatively high deposition rates, which is favourable for larger components. For this study, specimens with different orientations were prepared from one AISI316 steel block – parallel and orthogonal to the deposition plane. Quasistatic tensile loading tests were carried out, monitored by an infrared camera. The obtained surface temperature maps revealed structural differences between both orientations. The consideration of surface temperature transients yields more details about the behaviour of the material under tensile loading than the conventional stress-strain-curve. These preliminary investigations were supplemented by thermographic fatigue trials. Although the anisotropy was also observed during fatigue loading the fatigue behaviour in general was the same, at least for both inspected specimens. The presented results demonstrate the abilities and the potential of thermographic techniques for tensile tests.
ACCORDs is an Horizon Europe project working in the development of an imaging-based characterization framework (ACCORDs framework) for the holistic correlative assessment of Graphene Family Materials (GFMs) as a representative of 2D nanomaterials (NMs) to assess and predict 2D NMs health and environmental risks. The ACCORDs framework will operationalise safe and sustainable by design (SSbD) strategies proposed in past or ongoing H2020 projects or within OECD by correlating low-, medium-, and high-resolution physico-chemical-biological imaging-based methods with non-imaging methods in a tiered approach. ACCORDs will deliver the ACCORDs framework and user guidance, new imaging-based characterisation methods, reference in vitro tests, new reference 2D NMs for different matrices, a new minimum information reporting guideline for FAIR data sharing and reuse of images as well as an atlas with reference images for diagnostics of compromised safety of GFMs/GFM products. The new guidelines and standard proposals will be submitted to standardisation bodies to allow creation of regulatory ready products. The novelty of ACCORDs is in translating the principles of medical imaging-based diagnostics to 2D material hazard diagnostics. ACCORDs will accelerate industrial sectors in the area of aviation, marine construction, drone production, flexible electronics, photovoltaics, photocatalytics and print inks-based sensors. The value ACCORDs proposes to the graphene industry are practical, easy, imaging-based tools for GFM quality monitoring next to the production line with a possibility to be correlated with advanced highresolution imaging characterization methods in case hazard i.e. deviation from controls (benchmark values) are diagnosed. The ACCORDs framework and tools will contribute to the European Green Deal by addressing the topic: “Graphene: Europe in the lead” and to a new European strategy on standardization, released on 2nd February, 2022.
Obwohl der Leichtbau mit carbonfaserverstärkten Kunststoffen (CFK) einen wichtigen Beitrag zum Klimaschutz und zur Ressourceneffizienz liefert, stellt der wachsende Abfallstrom von aktuell 62 kt/a eine große Herausforderung dar. Weil die Produktion von Carbonfasern (CF) überwiegend auf fossilen Rohstoffen basiert und sehr energieintensiv ist, werden nachhaltige Recyclinglösungen dringend benötigt. Hier wird ein Überblick über aktuelle Recyclingprozesse gegeben und deren Limitierungen diskutiert. Darüber hinaus wird eine Möglichkeit zur sicheren chemischen Nutzung von CF-haltigen Reststoffen aufgezeigt, die nicht zur Wiederverwertung geeignet sind. Das Projekt CF Pyro untersucht deren Einsatz als Sekundärrohstoff in der Pyrometallurgie und setzt besondere Schwerpunkte bei der Reaktivität von CF, der Prozessstabilität und der Vermeidung von Emissionen gesundheitsschädlicher WHO-Fasern. Abschließend wird eine, auf den experimentellen Ergebnissen und im Dialog mit Expertinnen und Experten aus Wirtschaft, Wissenschaft und Politik entwickelten, Technologiebewertung vorgestellt.
Im Rahmen des Projektes MRO2.0, das sich mit der digitalen Transformation des Servicezyklus von modernen Gasturbinenschaufeln beschäftigt, wurde gezeigt, wie sich automatisiert und flächendeckend die (Rest-)Wanddicke an variabel gekrümmten Prüfgeometrien bestimmen lässt. Es wurde ein Roboterarm verwendet, der ein lineares Ultraschallarray in Tauchtechnik führt und Prüfdaten aufnimmt, die mit einer adaptierten TFM (Total Focusing Method) zu Rekonstruktionen der Außen- und Innenoberfläche verarbeitet werden. In der aktuellen zweiten Projektphase wird die Methode für Werkstoffe erweitert, die anisotrope akustische Eigenschaften aufweisen. In diesem Beitrag wird eine Methode vorgestellt, wie sich die Kristallausrichtung bzw. die richtungsabhängige Schallgeschwindigkeit mittels eines linearen Ultraschallarrays bestimmen lässt. Für den Sendefall eines Randelements in Kontakttechnik können dabei Wellen identifiziert werden, die sich parallel zur Prüfkopfapertur im Prüfobjekt ausbreiten und mit der richtungsabhängigen Schallgeschwindigkeit skalieren. Die ermittelte Schallgeschwindigkeitsverteilung kann dann verwendet werden, um die lokale Wanddickenbestimmung für die Anisotropie zu adaptieren.
Obwohl der Leichtbau mit carbonfaserverstärkten Kunststoffen (CFK) einen wichtigen Beitrag zum Klimaschutz und zur Ressourceneffizienz liefert, stellt der wachsende Abfallstrom von aktuell 62 kt/a eine große Herausforderung dar. Weil die Produktion von Carbonfasern (CF) überwiegend auf fossilen Rohstoffen basiert und sehr energieintensiv ist, werden nachhaltige Recyclinglösungen dringend benötigt. Hier geben wir einen Überblick über aktuelle Recyclingprozesse und diskutieren deren Limitierungen. Darüber hinaus zeigen wir eine Möglichkeit zur sicheren chemischen Nutzung von CF-haltigen Reststoffen auf, die nicht zur Wiederverwertung geeignet sind. Das Projekt CF Pyro untersucht deren Einsatz als Sekundärrohstoff in der Pyrometallurgie und setzt besondere Schwerpunkte bei der Reaktivität von CF, der Prozessstabilität und der Vermeidung von Emissionen gesundheitsschädlicher WHO-Fasern. Nach der Präsentation der Projektergebnisse erfolgte in der Diskussion mit Expertinnen und Experten aus Wirtschaft, Wissenschaft und Politik eine Technologiebewertung für die Nutzung von CF in pyrometallurgischen Prozessen.
Ultrasonic testing (UT) of objects with complex geometries often requires the use of a robotic arm to position the probe perpendicular to the local surface. Using immersion makes it possible to test these objects with standard ultrasonic linear array probes. Here, the probe positions and orientations provided by the robot are used for merging the locally acquired image data into a 3D-reconstruction. The quality of this reconstruction is highly dependent on the alignment of the tool center point (TCP) of the physical probe with the TCP used in the digital model. For common industrial tools, the TCP is usually acquired using geometric features of the tools. However, for ultrasonic arrays in immersion, there is a water standoff between the probe and the test object, therefore the TCP is in free space in front of the array and cannot be acquired with the common method. To overcome this challenge, we propose a method that allows the robotic ultrasonic system to automatically self-adjust the positioning of the UT probe using a test block made of steel with defined geometric features as a target for referencing. For each of the six degrees of freedom, a scan and adjustment routine are established using the data acquired by the UT probe to update the TCP’s position and orientation in the robot control. Given a coarse pre-definition of the TCP and the known target test block, no human interaction is required while the system determines the optimum tool position and orientation. Part of this work will be used to improve and extend standards for robotic ultrasonic test systems, e.g. ISO 24647.
A new hydrogen-based test rig is being developed for a feasibility study on the use of hydrogen as an energy source for thermal testing in accordance with the IAEA SSR-6 guidelines for transport packages containing radioactive materials.
The test rig will be capable of combusting hydrogen for a wide range of different burner geometries, mass flows and if necessary hydrogen blends. As this type of fire test according to the IAEA boundary conditions (SSR-6 & SSG-26) does not yet exist, a large number of preliminary investigations, safety assessments and calculations must be carried out in order to develop a viable concept for hydrogen fires.
A new hydrogen-based test rig is being developed for a feasibility study on the use of hydrogen as an energy source for thermal testing in accordance with the IAEA SSR-6 guidelines for transport packages containing radioactive materials.
The test rig will be capable of combusting hydrogen for a wide range of different burner geometries, mass flows and if necessary hydrogen blends. As this type of fire test according to the IAEA boundary conditions (SSR-6 & SSG-26) does not yet exist, a large number of preliminary investigations, safety assessments and calculations must be carried out in order to develop a viable concept for hydrogen fires.
Referenzmaterialien sind entscheidend für die Qualitätssicherung von Laboratorien. Diese nutzen Referenzmaterialien unter anderem zur Validierung von Messverfahren und zur Kalibrierung von Geräten. Dabei ist zu beachten, dass zertifizierte Merkmalswerte stets eine gewisse Unsicherheit aufweisen. Die Ermittlung dieser Unsicherheitsbeiträge ist Gegenstand des Artikels. Des Weiteren wird ein Vorgehen beschrieben, wie die Unsicherheit von Messverfahren mit Hilfe eines Referenzmaterials bestimmt werden kann.
Modern laser systems have proven to be versatile heat sources for active thermographic testing applications. Compared to more traditional light sources, e.g. flash or halogen lamps, their output power can be easily modulated at high rates, allowing a wide variety of complex excitations to be realized. Although their total optical output power can be theoretically scaled to arbitrary values, the maximum output power is practically limited by many factors: the maximum power that the sample under test can absorb without altering the lighted surface itself, the trade-off between power density and inspected area, the cost of the laser system, etc. Furthermore, when working with spatial modulator systems, the output power could be limited to avoid provoking any damages on such devices. Nevertheless, to guarantee sufficient heating even for highly thermally conductive materials and/or deeply buried defects, the heating times can be extended, e.g., either by using step heating, long pulse thermography, or by lock-in thermography with a continuously modulated heating. However, for all these approaches, the ranging capabilities of the thermographic defect detection are reduced due to the limited frequency content of the excitation.
To tackle this problem, i.e. to increase the excitation energy while preserving its frequency content, new approaches have been developed in the last two decades, among which the use of coded excitations combined with pulse-compression, and the use of multiple lock-in analysis or of a frequency modulated excitation signal. The challenges of such temporally structured heating techniques are manifold, for example, the DC component inherent in optical heating must be taken into account. In general, a wider frequency bandwidth or greater variability of the frequency components also means greater complexity for signal generation and data processing. In this paper, temporal structured excitation schemes with different degrees of complexity are compared on a high power laser system.
Guaranteeing safety and security of citizens requires a significant effort and innovative tools from national and international agencies and governments, especially when it comes to the field of explosives detection. The need to detect Improvised Explosive Devices (IEDs) and Home-made Explosives (HMEs) at a point of suspicion, has grown rapidly due to the ease with which the precursors can be obtained and the reagents synthesised. The limited availability of immunoanalytical tools for HME detection presents an opportunity for the development of new devices, which enable a rapid detection and recognise the target analyte with high specificity and sensitivity. In this work, we introduce an optical biosensor for highly specific and sensitive HME detection. The immunoassay system is placed in a hydrogel environment permeable to the analyte and transparent to light interrogating the fluorescently labelled antibodies. The readout of the immunoanalytical system is realized with Supercritical Angle Fluorescence (SAF), an advanced microscopy technique. To accomplish this, we made use of recent, commercial high resolution (< 22 µm) Liquid Crystal Display 3D printers to fabricate a parabolic optical element with high refractive index (RI>1.5) and transmission values (>90%) from photo-resin. Aiming at a new generation of sensors, which not only can meet the requirements of trace detection, but can also be used for substance identification, the combination of immunoanalytical recognition with SAF detection offers a modularity and versatility that is principally well suitable for the measurements of target analytes at trace levels.
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 global plastic industry relies on fossil-based materials, presenting environmental challenges. A sustainable polymer namely poly(limonene carbonate) (PLimC), made of limonene and CO2 as two monomers from non-food sources, shows advances in various applications where additives such as flame retardants (FRs) are crucial to comply with fire safety measures.
The variety of FRs is wide, and therefore the approach involved conducting a comparative study of four different halogen-free flame retardant systems that are conventionally used in polycarbonates and polyolefins to understand which FR enhances the flame resistance of PLimC most effectively. The primary task of the project is to conduct experimental evaluations to analyze the thermal properties, flammability, and fire behavior of each system. This data will offer valuable insights towards the advancement of safer and more sustainable materials.
Skłodowska, Anna Maria ; Lay, Vera ; Baensch, Franziska ; Niederleithinger, Ernst ; Kühne, Hans-Carsten
To safely dispose of nuclear waste in underground facilities, engineered barrier systems are needed to seal shafts and galleries. The material used in these barriers must be adapted to the host rock parameters. Shrinking and cracking must be avoided to provide a barrier with almost zero permeability. For repositories in salt rock environments, several types of salt concrete (SC) are possible construction materials.
Within the project SealWasteSafe, we compared the behavior of an innovative alkali-activated material (AAM) with standard SC in their hydration and hardening phase. To monitor the microstructural changes within the two materials SC and AAM, acoustic emission (AE) signals have been recorded for up to ~250 days on 340-liter-cubic specimens.
The phenomenon of AE is defined as the emission of elastic waves in materials due to the release of localized internal energy. Such energy release can be caused by the nucleation of micro-fracture, e.g., in concrete while curing or when exposed to load. The occurrence of AE events gives first rough indications of microstructural changes and potentially occurring cracking and thus, provides insights for structural health monitoring (SHM).
The results show, that for the first 28 days after casting, less AE activity was detected in the AAM compared to SC. After 61 days, in the AAM material, the number of AE events exceeded those observed in the SC. However, the majority of the AE detected and located in AAM was related to surface effects, and not to microstructural changes or occurring cracks within the bulk volume. Additionally, the source location analysis indicated, that despite lower activity in SC, we observed some clustering of the events. In contrast, in AAM, the activity inside the specimen is randomly distributed over the whole volume. The monitoring results help to estimate the material’s sealing properties which are crucial to assess their applicability as sealing material for engineered barriers.
The crucial part of nuclear waste storage is the construction of sealing structures made of reliable, well-understood, and safe materials. Within the SealWasteSafe project, we compared the performance of an innovative alkali-activated material (AAM) and standard salt concrete (SC), as potential materials for sealing structures for nuclear waste repositories. Two 340-liter-cubic specimens were studied for up to ~250 days by a multisensory monitoring setup. Specifically, the long-term acoustic emission monitoring aimed to analyze the development of microstructural changes within materials.
The monitoring analysis showed fewer acoustic emission events in AAM compared to SC in the first 61 days. After approximately two months of monitoring, the number of AE events in AAM significantly exceeded the number of events in SC. The analysis showed, however, that the increased AE activity was mainly caused by surface effects of the AAM material and not by the formation of cracks within the material.
This contribution presents the use of acoustic emission analysis, both in the time and frequency domains, for monitoring and characterization of materials with potential use as engineering barriers for nuclear waste repositories.
Clute, C. ; Balasooriya, Winoj ; Cano Murillo, Natalia ; Theiler, Géraldine ; Kaiser, A. ; Fasching, M. ; Schwarz, Th. ; Hausberger, A. ; Pinter, G. ; Schloegl, S.
Effects of NBR formulations on properties for high-pressure gas systems were tested. Functionalized silica enhances typical properties to a comparable range like CB. The balance of additives results in suitable RGD performance. Silica filled NBR shows lower H2 uptake compared to non-plasticized CB filled NBR. Morphology of CB filled NBR is less affected by H2 than silica filled grades.
Infraleichtbeton zeichnet sich durch eine äußerst geringe Trockenrohdichte von maximal 800 kg/m³ aus, bei gleichzeitig ausreichender Festigkeit. Daraus resultieren geringe Wärme- und Schallleitfähigkeiten. Dies ermöglicht den Einsatz als Sichtbeton in Wandelementen ohne die Notwendigkeit einer zusätzlichen Dämmschicht.
Vielversprechend erscheint der Einsatz von Leichtgranulaten in Infraleichtbeton, um seinen ökologischen Fußabdruck zu reduzieren und somit ein energieeffizientes und zugleich nachhaltiges Bauen zu ermöglichen. Die Leichtgranulate werden in einem thermo-chemischen Prozess aus gemischtem Mauerwerkbruch hergestellt. Ihre Verwendung bietet neben der Alternative zu herkömmlichen leichten Gesteinskörnungen auch die Möglichkeit, Abfallprodukte sinnvoll zu nutzen. In diesem Artikel werden die Leichtgranulate vorgestellt, ihre Anwendung in Infraleichtbeton geprüft und mit konventionellem Blähton verglichen.
Skłodowska, Anna Maria ; Lay, Vera ; Baensch, Franziska ; Niederleithinger, Ernst ; Kühne, Hans-Carsten
One of the major tasks in nuclear waste management is to design safe and reliable sealing structures for radioactive waste repositories. Particularly for salt as a host rock, engineered barrier systems for underground waste disposal must be constructed of well-understood (cementitious) materials that will sustain environmental conditions and ensure high durability.
Within the SealWasteSafe project, we studied two materials with a potential for sealing structures for nuclear waste repositories: an innovative alkali-activated material (AAM) and standard salt concrete (SC). To analyze the development of microstructural changes within the materials, we monitored microseismicity (aka acoustic emission monitoring) occurring during the hardening and setting period in two 340-liter-cubic specimens for up to ~250 days.
The monitoring results showed, that in the first 61 days, fewer events occurred in AAM compared to SC. After this time the number of events in AAM sharply increased and significantly exceeded those observed in SC. However, the source localization analysis revealed that the increase of microseismicity in AAM material was not related to the formation of macro-cracks within the material but was mainly caused by the surface effects. Accompanying analysis of the test specimens with additional methods (such as e.g., X-ray CT) proved that no macro-cracks were observed inside the AAM specimen. Further analysis in the time and frequency domains helped to characterize the tested materials and to estimate their potential to be used for engineered barriers in nuclear waste repositories.
Overall, our study shows the potential of microseismicity monitoring for feasibility studies and quality assurance in a broad range of applications, also in structural health monitoring.
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.
Revealing surface functionalities of micro- and nanoplastic particles’ surface by means of XPS
(2024)
Over the last 20 years, many researchers, politicians, and citizens themselves have become increasingly aware of the growing plastic problem of our time. Inadequate recycling concepts, collection points, and careless dumping of plastic products in the environment lead to an accumulation of plastic. External weather influences can cause these to degrade and fractionate, so that today microplastics (1-1000 µm, ISO/TR 21960:2020) [1] of different polymer materials can be detected in all parts of the world.
The precautionary principle applies to microplastics. The particles can break down further to form nanoplastics (<1 µm, ISO/TR 21960:2020) [1]. Whether microplastics or nanoplastics pose a toxicological hazard is being investigated in a variety of ways. Valid results are still pending, however, investigations into the frequency, transport, possible sinks and entry paths must be taken into account. This is why monitoring of microplastics is already required in the revision of the Drinking Water Framework Directive [2]. The same is still pending in the final version of the revision of the Waste Water Framework Directive this year, but is expected.
Nanoplastics are particularly under discussion for having a toxic effect on humans and animals, as these particles are small enough to be absorbed by cells. For targeted toxicological studies, it is important to have test and reference materials that resemble the particles found in the environment. To mimic environmental samples, these materials should also have an irregular shape and show aging at the surface, which can be detected with XPS or SEM/EDS.
BAM in collaboration with the EMPIR project "PlasticTrace" works on a reference material candidate of nano-sized polypropylene (nano-PP) [3]. The nano-PP vials were tested for homogeneity with PTA and further characterized with bulk and surface-sensitive techniques. An SEM image and a corresponding XPS spectrum are presented in Figure 1. Raman measurements as well as XPS indicate an aged surface.
Wasserstoff stellt einen potenziellen Energieträger für den großskaligen Import von Energie nach Europa dar. Von seinen verschiedenen Speicherformen eignet sich hierfür insbesondere verflüssigter Wasserstoff, mit dem sich auf gleichem Volumen deutlich mehr Energie speichern lässt als bei der druckbasierten Speicherung. Verflüssigter Wasserstoff wird bei minus 253°C gespeichert und muss für dessen Transport lange bei dieser niedrigen Temperatur gehalten werden. Dies stellt besondere Herausforderungen an die thermische Isolation von Tanks. Der Erforschung nachhaltiger, kosten- und energieeffizienter sowie sicherer thermischen Isolationen wird im NICOLHy Projekt, unter Leitung der BAM, nachgegangen.
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.
Ni-Fe oxide nanoparticles have gained a lot of interest because of their high activity in the oxygen evolution reaction (OER) which is crucial for water splitting. [1] Although there have been great efforts in the last years, the understanding of the synergistic effect between Fe and Ni is still under discussion.
Therefore, we prepared different Ni-Fe oxide nanoparticles with different compositions from pure iron oxide to pure nickel oxide adapting a known procedure. [2,3] Size and morphology of the nanoparticles depend on the composition which was shown with Transmission Electron Microscopy (TEM). The compositions of the nanoparticles were measured with a comparative approach using X-ray Photoelectron Spectroscopy (XPS), Hard X-ray Photoelectron Spectroscopy (HAXPES), and Energy Dispersive X-Ray Spectroscopy (EDS) coupled with the TEM providing detailed chemical information of the nanoparticles in different sample regions. EDS reveals that the different sample regions are dominated by one of the components, Fe or Ni, but a slight mixing between the components can be found (see Figure 1), which was confirmed with X-ray Diffraction (XRD). XPS indicates the enrichment of Fe at the sample surface, while HAXPES and EDS data agree on the stoichiometry of the bulk. High-resolution XPS and HAXPES exhibit some differences in the valence states of Fe and Ni, whereas Ni seems to be easier to reduce than Fe. Further investigations combining these different techniques and additionally Secondary Ion Mass Spectrometry (ToF-SIMS) are ongoing by using in situ approaches and coupling cyclic voltammetry to the analytical techniques.