TY - JOUR A1 - Gumenyuk, Andrey A1 - Bakir, Nasim A1 - Rethmeier, Michael T1 - Two-colour thermography for measurement of temperature distribution in laser beam welding N2 - Solidification cracking is a frequently observed phenomenon in laser beam welding of austenitic stainless steels and other metallic alloys. Characterisation of cracking susceptibility requires knowledge of the precise and spatially resolved temperature distribution near the solidification front in the welding process. Thermography is a standard tool that provides a qualitative estimate of the 2D temperature field. The general disadvantage of this method is its dependence on the emission characteristics of the measured object. For welding applications, these can vary significantly in the temperature range above and below the melting temperature. For this purpose, we have developed a thermography-based measurement technique using a SWIR camera system in combination with two narrow bandpass filters that use the principle of two-wavelength pyrometry to estimate absolute temperature values. This technique was used to determine the temperature distributions and gradients near the solidification front of laser-welded austenitic steel. The results were validated by other measurements. KW - Laser beam welding KW - Two-colour thermography KW - Solidification cracking PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612070 DO - https://doi.org/10.1016/j.procir.2024.08.155 VL - 124 SP - 468 EP - 471 PB - Elsevier BV AN - OPUS4-61207 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yang, Keke A1 - El-Sari, Bassel A1 - Olfert, Viktoria A1 - Wang, Zhuoqun A1 - Biegler, Max A1 - Rethmeier, Michael A1 - Meschut, Gerson T1 - Expulsion prevention in resistance spot welding of dissimilar joints with ultra-high strength steel: An analysis of the mechanism and effect of preheating current N2 - The widespread adoption of ultra-high strength steels, due to their high bulk resistivity, intensifies expulsion issues in resistance spot welding (RSW), deteriorating both the spot weld and surface quality. This study presents a novel approach to prevent expulsion by employing a preheating current. Through characteristic analysis of joint formation under critical welding current, the importance of plastic material encapsulation around the weld nugget (plastic shell) at high temperatures in preventing expulsion is highlighted. To evaluate the effect of preheating on the plastic shell and understand its mechanism in expulsion prevention, a two-dimensional welding simulation model for dissimilar ultra-high strength steel joints was established. The results showed that optimal preheating enhances the thickness of the plastic shell, improving its ability to encapsulate the weld nugget during the primary welding phase, thereby diminishing expulsion risks. Experimental validation confirmed that by employing the optimal preheating current, the maximum nugget diameter was enhanced to 9.42 mm, marking an increase of 13.4 % and extending the weldable current range by 27.5 %. Under quasi-static cross-tensile loading, joints with preheating demonstrated a 7.9 % enhancement in maximum load-bearing capacity compared to joints without preheating, showing a reproducible and complete pull-out failure mode within the heat-affected zone. This study offers a prevention method based on underlying mechanisms, providing a new perspective for future research on welding parameter optimization with the aim of expulsion prevention. KW - Resistance spot welding KW - Finite element modelling KW - Preheating KW - Weldable current range KW - Ultra-high strength steel PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621719 DO - https://doi.org/10.1016/j.jmapro.2024.06.034 VL - 124 SP - 489 EP - 502 PB - Elsevier Ltd. AN - OPUS4-62171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Uhlmann, Eckart A1 - Polte, Julian A1 - Fasselt, Janek Maria A1 - Müller, Vinzenz A1 - Klötzer-Freese, Christian A1 - Kleba-Ehrhardt, Rafael A1 - Biegler, Max A1 - Rethmeier, Michael T1 - A Comparative Evaluation of Powder Characteristics of Recycled Material from Bronze Grinding Chips for Additive Manufacturing N2 - In the manufacturing process of ship propellers, large quantities of grinding chips are generated. These grinding chips result from the finishing of the blade surfaces after the primary casting process of the propeller. The aim of this study was to investigate and compare different preparation processes used to produce chip powders with sufficient powder quality for the additive manufacturing process of directed energy deposition. The preparation of the samples was performed through different sieving, milling and re-melting processes. For the characterization of the prepared samples, powder analysis according to relevant industry standards was carried out. It was found that the re-melting processes result in superior powder quality for additive manufacturing in terms of particle size, morphology, and flowability. For some characteristics, the powder exhibits even better properties than those of commercial powders. Furthermore, the powder properties of the milled samples demonstrate a promising potential for u KW - Grinding chips KW - Comminution KW - Aluminium bronze KW - Additive manufacturing KW - Recycling KW - Sustainability PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621696 DO - https://doi.org/10.3390/ma17143396 VL - 17 IS - 14 SP - 1 EP - 15 PB - MDPI AG AN - OPUS4-62169 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Raute, Julius A1 - Beret, Alexander A1 - Biegler, Max A1 - Rethmeier, Michael T1 - Life cycle assessment in additive manufacturing of copper alloys—comparison between laser and electron beam N2 - Additive manufacturing is becoming increasingly important for industrial production. In this context, directed energy deposition processes are in demand to achieve high deposition rates. In addition to the well-known laser-based processes, the electron beam has also reached industrial market maturity. The wire electron beam additive manufacturing offers advantages in the processing of copper materials, for example. In the literature, the higher energy efficiency and the resulting improvement in the carbon footprint of the electron beam are highlighted. However, there is a lack of practical studies with measurement data to quantify the potential of the technology. In this work, a comparative life cycle assessment between wire electron beam additive manufacturing (DED-EB) and laser powder additive manufacturing (DED-LB) is carried out. This involves determining the resources for manufacturing, producing a test component using both processes, and measuring the entire energy consumption. The environmental impact is then estimated using the factors global warming potential (GWP100), photochemical ozone creation potential (POCP), acidification potential (AP), and eutrophication potential (EP). It can be seen that wire electron beam additive manufacturing is characterized by a significantly lower energy requirement. In addition, the use of wire ensures greater resource efficiency, which leads to overall better life cycle assessment results. KW - Life cycle assessment (LCA) KW - Additive manufacturing KW - Directed energy deposition KW - Wire electron beam additive manufacturing KW - Copper alloys PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621705 DO - https://doi.org/10.1007/s40194-024-01856-9 SP - 3169 EP - 3176 PB - Springer Science and Business Media LLC AN - OPUS4-62170 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Marquardt, R. A1 - Biegler, M. A1 - Rethmeier, Michael T1 - Functionally graded material for improved wear resistance manufactured by directed energy deposition N2 - Protecting components against wear and corrosion is a common way to improve their lifetime. This can be achieved by coating them with a hardfacing material. Common coatings consist of materials such as tungsten carbide or cobalt-chromium alloys, also known as Stellite. Hardfacing materials can be deposited by welding methods like plasma welding or laser cladding. The discrete change of the base material to the hardfacing layer can lead to cracks and chipping. Studies showed a reduced risk of cracking when a functionally graded material is used to create a smooth transition between the base and the hardfacing. Gradings from austenitic steel to cobalt-chromium alloys are already known in the literature. However, there is no knowledge about austenitic- ferritic duplex steels as base material. Therefore, this study aims to demonstrate the feasibility of a functionally graded material from duplex steel to cobalt-chromium alloy with a new approach. By using powder-based directed energy deposition, a graded material with smooth material transition is manufactured additively. Cracking and porosity are examined through metallography. Microhardness measurements as well as the analysis of the chemical composition by energy dispersive X-ray spectroscopy and X-ray fluorescence are used to validate the build-up strategy. KW - Additive manufacturing KW - Functionally graded material KW - Functionally graded additive manufacturing KW - Directed energy deposition KW - Laser metal deposition PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621683 DO - https://doi.org/10.1007/s40964-024-00879-4 SP - 1 EP - 6 PB - Springer Science and Business Media LLC AN - OPUS4-62168 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yang, Fan A1 - Meng, Xiangmeng A1 - Putra, Stephen Nugraha A1 - Bachmann, Marcel A1 - Rethmeier, Michael T1 - Assessment of keyhole stability in laser beam welding with external magnetic field using numerical simulation N2 - The challenge of understanding the physical mechanisms behind porosity reduction by a magnetic field during laser beam welding (LBW) is partly due to the difficulty in quantitatively evaluating keyhole stability. The commonly used index, such as keyhole depth, is typically one-dimensional, which is insufficient to capture the dynamic and three-dimensional fluctuations of the keyhole. In this paper, by utilizing a 3D multiphysical model of LBW with magnetic field, a novel keyhole geometry reconstruction algorithm has been developed to describe the keyhole profile and its fluctuation in a statistical manner to evaluate keyhole stability quantitatively. An equivalent diameter is proposed in this algorithm to reduce the irregularity of the keyhole geometry. The calculation results indicate that the time-averaged keyhole shape over 300 ms in the LBWof steel is conical, regardless of the application of an external magnetic field, which provides a more representative shape. Meanwhile, it is observed from the statistical aspect that the keyhole diameter becomes smaller, except the top part, under the influence of the magnetic field. The standard deviation of the equivalent diameter can be used as a physical variable to assess the keyhole stability quantitatively. The application of an external magnetic field can produce a noticeable reduction of the standard deviation of the equivalent diameter, namely, stabilizing the keyhole during LBW of steel. However, the different contribution from the keyhole stability affected by a magnetic field in suppressing porosity is different with materials. T2 - International Congress of Applications of Lasers & Electro-Optics 2024 CY - Los Angeles, CA, USA DA - 04.11.2024 KW - Deep penetration laser beam welding KW - Numerical simulation KW - Keyhole shape KW - Keyhole stability KW - Magnetic field PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-614984 DO - https://doi.org/10.2351/7.0001528 VL - 36 IS - 4 SP - 1 EP - 7 PB - AIP Publishing CY - Melville, NY AN - OPUS4-61498 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meng, Xiangmeng A1 - Putra, Stephen Nugraha A1 - Bachmann, Marcel A1 - Rethmeier, Michael T1 - Parametric study of the laser energy absorption in high-power laser beam welding N2 - Laser energy absorption on the keyhole wall is decisive for the thermodynamic behavior and the resultant weld properties in the high-power laser beam welding process. However, its highly transient nature on a microsecond scale makes the quantitative analysis challenging. In this paper, the influence of the relevant welding parameters on laser energy absorption is studied statistically by utilizing multiphysical modeling, in which the three-dimensional transient keyhole dynamics and thermo-fluid flow are calculated. A dynamic mesh adaption technique and a localized level-set-based ray-tracing method are employed to improve the model accuracy further. The results show that the focus position has a remarkable effect on the time-averaged laser absorption, and in contrast, the laser energy distribution regime is only slightly influenced by the welding speed in the studied parameter range (1.5–3.0 m/min). The absorption ratio of the laser energy on the keyhole front wall decreases with increasing welding speed and increases with upward-moving focus positions. The comparison between the calculated results and the experimental measurements ensures the validity of the proposed model. T2 - International Congress of Applications of Lasers & Electro-Optics 2024 CY - Los Angeles, CA, USA DA - 03.11.2024 KW - Laser beam welding KW - Laser energy absorption KW - Weld pool KW - Parametric study KW - Multiphysics modeling PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-616070 DO - https://doi.org/10.2351/7.0001537 SN - 1042-346X VL - 36 IS - 3 SP - 1 EP - 6 PB - AIP Publishing AN - OPUS4-61607 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Putra, Stephen Nugraha A1 - Meng, Xiangmeng A1 - Yang, Fan A1 - Bachmann, Marcel A1 - Rethmeier, Michael T1 - Numerical study on the temperature characteristic of material absorptivity and its significance in high-power laser beam welding N2 - The absorptivity of metallic materials plays an important role in high-power laser beam welding. It affects the amount of absorbed laser power leading to the heating and melting of the surfaces to be joined and is highly dependent on the temperature. Nonetheless, this key characteristic is often ignored in numerical simulations and an empirical parameter determined by trial-and-error approaches is rather implemented to calibrate the results. In the present work, the temperature dependence of laser absorption is included in a three-dimensional multiphase numerical model considering the coupled fluid flow and heat transfer. The calculated laser absorption is determined by the temperature-dependent material properties, laser characteristics, and incident angle of the laser beam. It is found that the temperature dependence of the laser absorption is crucial for accurately determining the keyhole and weld pool geometries, which is validated by experimental measurements using 304 austenitic steel. T2 - 13th CIRP Conference on Photonic Technologies [LANE 2024] CY - Fürth, Germany DA - 15.09.2024 KW - Laser beam welding KW - Temperature dependent absorption KW - Weld pool KW - Keyhole dynamics KW - Numerical modelling PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-616146 DO - https://doi.org/10.1016/j.procir.2024.08.179 VL - 124 SP - 585 EP - 589 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-61614 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yang, Fan A1 - Meng, Xiangmeng A1 - Putra, Stephen Nugraha A1 - Bachmann, Marcel A1 - Rethmeier, Michael T1 - Numerical studies of magnetohydrodynamic technology in suppressing process porosity during laser beam welding N2 - The magnetohydrodynamic (MHD) technology is employed to mitigate the porosity problem during partial penetration laser beam welding (LBW) of 10 mm thick aluminum alloy. The effectiveness and universal applicability of the MHD technology in reducing porosity during the LBW process are confirmed by a reduction in the porosity ratio of more than 89%. A transient 3D multi-physical model coupled with the MHD effect has been developed to investigate the suppression mechanism of process porosity. Due to the influence of Lorentz force, there is an obvious change in the weld pool length. This change widens the escaping channel of bubbles escaping from the weld pool. The application of an oscillating magnetic field changes the fluid flow pattern noticeably, whose influence on the formation of porosity defects is highly complicated and nonlinear. T2 - CIRP Conference on Photonic Technologies [LANE 2024] CY - Fürth, Germany DA - 15.09.2024 KW - Laser beam welding KW - Aluminum alloy KW - Process Porosity KW - Porosity suppression KW - Magnetohydrodynamic technology PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-616053 DO - https://doi.org/10.1016/j.procir.2024.08.175 VL - 124 SP - 565 EP - 569 PB - Elsevier B.V. AN - OPUS4-61605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Seitz, Georg A1 - Bantle, Patrick A1 - Biegler, Max A1 - Elsner, Beatrix A. M. A1 - Rethmeier, Michael T1 - An Inherent Strain Method Using Progressive Element Activation for Fast Distortion Calculation in Directed Energy Deposition N2 - The finite element analysis (FEA) simulation of directed energy deposition (DED) processes offers many potential cost savings during the build job optimization process, through, e.g., distortion predictions. However, the biggest challenge is the long calculation time, frequently exceeding the actual build time. One way of simplifying the simulation with the aim of reducing the calculation times is the inherent strain method. While this method is already used commercially in the simulation of powder bed-based processes and conventional welding technologies, its use in DED is still the subject of research. In this work, an inverse determination of an inherent strain is carried out on a 20-layer-high, single-track-wide wall, common theories are reviewed, and an approach based on thermal strain is introduced. As a result, the calculation time could be reduced by 83% and the accuracy remained at 92%. KW - Inherent strain method KW - Simulation KW - Finite element analysis KW - Directed energy deposition KW - Additive manufacturing PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-622595 DO - https://doi.org/10.3390/met14121338 SN - 2075-4701 VL - 14 IS - 12 SP - 1 EP - 12 PB - MDPI AN - OPUS4-62259 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yang, Keke A1 - Sowada, Matthias A1 - Olfert, Viktoria A1 - Seitz, Georg A1 - Schreiber, Vincent A1 - Heitmann, Marcel A1 - Hein, David A1 - Biegler, Max A1 - Jüttner, Sven A1 - Rethmeier, Michael A1 - Meschut, Gerson T1 - Influence of liquid metal embrittlement on the failure behavior of dissimilar spot welds with advanced high-strength steel: A component study N2 - This study investigates the effects of liquid metal embrittlement (LME) cracks on the mechanical performance of resistance spot-welded joints in zinc-coated advanced high-strength steel (AHSS) at the component level. To this end, a novel component-level test specimen featuring a hat and L-shaped profile was developed to identify critical failure points under three-point bending loads. Load-bearing capacity tests were subsequently conducted under both quasi-static and impact loading conditions, specifically targeting LME cracks with an average depth reaching 63.6% of the sheet thickness. By monitoring the surface strain of spot welds affected by LME cracks, the study visualizes stress concentration effects at the crack tips and traces the propagation of these cracks into the base material, which ultimately leads to material tearing and joint failure. The findings reveal that the effect of LME cracks in reducing load-bearing capacity is more pronounced under impact loading than under quasi-static loading, highlighting a previously underexplored aspect of LME behavior under impact loading. Specifically, the peak load decreased by 3.9% and 10.8%, while energy absorption declined by 52.2% and 78.3% under quasistatic and impact loading, respectively. KW - Liquid metal embrittlement KW - Resistance spot welding KW - Impact loading KW - Crack propagation KW - Advanced high-strength steel PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621727 DO - https://doi.org/10.1016/j.jmrt.2024.11.166 VL - 33 SP - 8321 EP - 8328 PB - Elsevier B.V. AN - OPUS4-62172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lemke, Josefine A1 - Höfemann, Matthias A1 - Biegler, Max A1 - Rethmeier, Michael T1 - Process strategies for optimizing the cooling behaviour of laser-welded Tailor Welded Blanks made of advanced high strength steels (AHSS) N2 - AHSS with 1000 MPa tensile strength show promising properties for the use in Tailor Welded Blanks (TWBs) to locally strengthen car body parts. Challenges in laser beam welding of the sheets are hardness-drops and -peaks in the heat-affected zone (HAZ) and weld, which cause risks during cold-forming. This happens due to rapid cooling caused by laser welding. A numerical approach aiming for slower cooling rates in the weld region is presented in this article. Laser welded sheets served as reference for setting up a process simulation. Models for pre-heating and a coaxial setup with power split were set up. A correlation between cooling-rate and hardness in the joining zone was established and applied to the modelled strategy. Splitting the power led to a slightly narrower weld seam and experimental pre-heating of the sheets to 600 °C could lower total seam hardening. It achieved a homogenization of the fusion zone. KW - AHSS KW - Laser welding KW - Tailor Welded Blanks KW - Hardness KW - FEM KW - HAZ PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-622324 DO - https://doi.org/10.1016/j.procir.2024.08.176 VL - 124 SP - 570 EP - 573 PB - Elsevier B.V. AN - OPUS4-62232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Castanon-Jano, Laura A1 - Palomera-Obregon, Paula A1 - Lázaro, Mariano A1 - Blanco-Fernandez, Elena A1 - Blasón Gonzalez, Sergio T1 - Enhancing sustainability in polymer 3D printing via fusion filament fabrication through integration of by-products in powder form: Mechanical and thermal characterization N2 - FFF (fused filament fabrication) is a type of 3D printing that utilizes filament for part creation. This study proposes using by-products or waste to replace part of the plastic in FFF filament, reducing environmental impact. The aim is to maintain a simple manufacturing process involving extrusion on a single-screw desktop machine followed by printing. The plastic matrix comprises polylactic acid (PLA) and polyethylene glycol (PETG), with added powdered by-products: seashells, car glass and mill scale (metal). Additives will be incorporated at 10% and 20% by weight, with two grain sizes: up to 0.09 mm and up to 0.018 mm. Mechanical tests (tensile, flexural and hardness) and thermal characterization tests will be conducted. Findings suggest adding 10%w powder of any variety to PETG increases tensile strength up to 48%, with metal powder (mill scale) showing the highest enhancement, even at 20%w, resulting in a 41% increase. Conversely, adding powder to PLA worsens mechanical properties without stiffening the material; instead, the elastic modulus decreases. Metal grain size has minimal impact, with grain sizes lower than 0.09 mm optimal for PLA. Thermal conductivity in polymers blended with powder additives is lower than in virgin polymers, likely due to air void formation, supported by density and microscopic evaluations. This research underscores the potential of utilizing waste materials with a simple FFF filament production to enhance sustainability in 3D printing practices. KW - 3D printing KW - FFF KW - PLA KW - PETg KW - Metal powder KW - Glass powder KW - Seashells powder KW - Tension KW - Bending KW - Thermal properties KW - Sustainability KW - Plastic consumption PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635027 DO - https://doi.org/10.1007/s00170-024-13635-3 SN - 0268-3768 VL - 133 IS - 3-4 SP - 1251 EP - 1269 PB - Springer CY - London AN - OPUS4-63502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Monavari, Mahshid A1 - Sohrabi, Razieh A1 - Motasadizadeh, Hamidreza A1 - Monavari, Mehran A1 - Fatahi, Yousef A1 - Ejarestaghi, Negin Mousavi A1 - Fuentes-Chandia, Miguel A1 - Leal-Egaña, Aldo A1 - Akrami, Mohammad A1 - Homaeigohar, Shahin T1 - Levofloxacin loaded poly (ethylene oxide)-chitosan/quercetin loaded poly (D,L-lactide-co-glycolide) core-shell electrospun nanofibers for burn wound healing N2 - This study developed a new burn wound dressing based on core-shell nanofibers that co-deliver antibiotic and antioxidant drugs. For this purpose, poly(ethylene oxide) (PEO)-chitosan (CS)/poly(D,L-lactide-co-glycolide) (PLGA) core-shell nanofibers were fabricated through co-axial electrospinning technique. Antibiotic levofloxacin (LEV) and antioxidant quercetin (QS) were incorporated into the core and shell parts of PEO-CS/PLGA nanofibers, respectively. The drugs could bond to the polymer chains through hydrogen bonding, leading to their steady release for 168 h. An in vitro drug release study showed a burst effect followed by sustained release of LEV and QS from the nanofibers due to the Fickian diffusion. The NIH 3T3 fibroblast cell viability of the drug loaded core-shell nanofibers was comparable to that in the control (tissue culture polystyrene) implying biocompatibility of the nanofibers and their cell supportive role. However, there was no significant difference in cell viability between the drug loaded and drug free core-shell nanofibers. According to in vivo experiments, PEO-CS-LEV/PLGA-QS core-shell nanofibers could accelerate the healing process of a burn wound compared to a sterile gauze. Thanks to the synergistic therapeutic effect of LEV and QS, a significantly higher wound closure rate was recorded for the drug loaded core-shell nanofibrous dressing than the drug free nanofibers and control. Conclusively, PEO-CS-LEV/PLGA-QS core-shell nanofibers were shown to be a promising wound healing material that could drive the healing cascade through local co-delivery of LEV and QS to burn wounds. KW - Core-shell nanofiber KW - Co-axial electrospinning KW - Drug delivery KW - Burn wound KW - Wound healing PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635115 DO - https://doi.org/10.3389/fbioe.2024.1352717 SN - 2296-4185 VL - 12 SP - 1 EP - 14 PB - Frontiers Media CY - Lausanne AN - OPUS4-63511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Erxleben, Kjell A1 - Richter, Tim A1 - Schröpfer, Dirk A1 - Mente, Tobias A1 - Michael, Thomas T1 - Local mechanical properties of dissimilar metal TIG welded joints of CoCrFeMnNi high entropy alloy and AISI 304 austenitic steel N2 - Multiple principal element alloys encompass the well-known high entropy alloys (HEA). The alloy system represents a new class of materials consisting of at least three alloying elements, each containing 5 to 35 at.%. Thus, this alloying concept differs fundamentally from conventional materials such as steel or nickel alloys. For this purpose, the alloying elements are specifically selected, the microstructures are adjusted in a single-phase and, in some cases, multi-phase manner. In particular, conflicting goals, such as the trade-off between strength and ductility in conventional steels, are overcome. However, in the last 20 years, the focus has been on material synthesis. With the increase in available material quantities, the focus is now on processing issues such as joining and welding processes. The weldability of HEAs has received very little attention so far. The experience with dissimilar metal welds is completely lacking but is essential for the application of these materials in combination with conventional materials. The present study presents comprehensive experimental results on the weldability of an equimolar CoCrFeMnNi-HEA in cold-rolled and heat-treated condition, which was joined by tungsten inert gas welding to an austenitic steel AISI 304. The mechanical properties of the dissimilar metal welds were characterized by cross-weld tensile samples, whereas the local deformation in the weld of the different welding zones was measured by digital image correlation. In accordance with the respective initial HEA condition (cold-rolled vs. heat-treated), the local strain behavior was divergent and influenced the global mechanical properties of both DMW types. Nonetheless, the experiments provided proof in principle of the weldability for dissimilar joints of the CoCrFeMnNi-HEA welded to conventional materials like austenitic stainless steels ensuring a corresponding capability for mechanical loading. This allows further considerations on the application of these innovative materials. KW - TIG welding KW - High-entropy alloys KW - Mechanical properties KW - Dissimilar metal weld PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595775 DO - https://doi.org/10.1007/s40194-024-01718-4 SN - 0043-2288 SP - 1 EP - 11 PB - Springer Science and Business Media LLC AN - OPUS4-59577 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Salari, Farid A1 - Zocca, Andrea A1 - Bosetti, Paolo A1 - Hlaváček, Petr A1 - Italiano, Antonino A1 - Gobbin, Filippo A1 - Colombo, Paolo A1 - Kühne, Hans-Carsten A1 - Sglavo, Vincenzo M. T1 - Powder-bed 3D printing by selective activation of magnesium phosphate cement: Determining significant processing parameters and their effect on mechanical strength N2 - The present work addresses powder bed binder jetting additive manufacturing by selective magnesium phosphate cement activation. Despite the potential of this technology to aid the digitalization of the construction industry, the effect of processing parameters on the mechanical performance of printed materials has not yet been studied to generate a guideline for the further development of the technology. Statistical methodologies were used to screen the effect of four printing process parameters (printing speed, layer thickness, raster angle, and build direction on flexural and compressive strength). As the exploited technology works with constant fluid pressure, the physical interpretation of the effect of each factor can be considered taking into account the interactions between the binder materials in the powder bed. Analysis of variance (ANOVA) indicated that printing speed and layer thickness significantly affect mechanical performances. Furthermore, the layout of samples for the printing process is preferable to be parallel the printhead movement. An anisotropic behavior was observed, and the samples subjected to compressive forces parallel to the layer plane possessed lower strength values. This effect can be interpreted as a result of a weak area of low density in between layers, leading to a pronounced delamination under compression. Even though the strength of the printed material is not suitable for a structural concrete, it can be marginally improved by design of experiment and optimized for non-structural applications, such as for porous artificial stone. Design of experiment coupled with ANOVA methods can be used in the future to support the development of novel material mixtures, thus expanding the fields of application of this novel additive manufacturing technology. KW - Concrete 3D-printing KW - Particle-bed binder jetting KW - Design of experiment PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601654 DO - https://doi.org/10.1016/j.oceram.2024.100609 VL - 18 SP - 1 EP - 11 PB - Elsevier B.V. AN - OPUS4-60165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bernardy, Christopher A1 - Habib, Abdel Karim A1 - Kluge, Martin A1 - Schalau, Bernd A1 - Schulze, Marcel A1 - Kant, Hanjo A1 - Orchini, Alessandro ED - Di Benedetto, Almerinda ED - Portarapillo, Maria T1 - Investigation of the thermal radiation from hydrogen jet flames N2 - For industrial applications dealing with hydrogen, the definition of safety distances and the assessment of possible hazards emanating from releases is mandatory. Since hydrogen is usually stored and transported under pressure, one scenario to be considered is the momentum driven release of hydrogen from a leakage with subsequent ignition. In this scenario, the emitted heat radiation from the resulting jet flame to the surroundings has to be determined to define adequate safety distances. For hydrocarbon flames, different jet flame models are available to assess the hazards resulting from an ignited jet release. Since hydrogen flames differ from hydrocarbon flames in their combustion behavior, it has to be checked if these models are also applicable for hydrogen. To evaluate the accuracy of these models for hydrogen jet flames, tests at real-scale are carried out at the BAM Test Site for Technical Safety (BAM-TTS). Herein, the flame geometry and the heat radiation at defined locations in the surroundings are recorded for varying release parameters such as leakage diameter (currently up to 30 mm), release pressure (currently up to max. 250 bar) and mass flow (up to max. 0.5 kg/s). The challenge here is the characterization of the flame geometry in an open environment and its impact on the thermal radiation. Existing heat radiation data from the literature are mostly based on unsteady outflow conditions. For a better comparability with the steady state jet flame models, the experiments presented here are focused on ensuring a constant mass flow over the release duration to obtain a (quasi) stationary jet flame. In addition, stationary outflow tests with hydrocarbons (methane) were also carried out, which are intended to serve as reference tests for checking flame models based on hydrocarbon data. T2 - 15th International Symposium on Hazards, Prevention and Mitigation of Industrial Explosions (ISHPMIE) CY - Neaples, Italy DA - 10.06.2024 KW - Hydrogen KW - Release KW - Jet flame KW - Thermal radiation PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-605107 DO - https://doi.org/10.5281/zenodo.12515710 VL - 2024 SP - 1322 EP - 1333 PB - Zenodo CY - Geneva AN - OPUS4-60510 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Balscheit, Hagen A1 - Geißler, Peter A1 - Cuéllar, Pablo A1 - Basedau, Frank A1 - Baeßler, Matthias T1 - Large-scale field tests on plastic pile tip failure upon monopile installation N2 - Large-diameter monopiles are the most common foundation structures for offshore wind turbines. One relevant failure mode during installation is plastic failure of the pile tip which may increase progressively during further driving (pile tip buckling; extrusion buckling). This paper presents the details and results of a large-scale field-test campaign with dynamic pile installation for the validation and calibration of different numerical approaches concerning pile-tip buckling phenomena. The phenomenology of observed pile-tip failures is here described in detail and a first quantitative approach is evaluated based on the field-test data. As the number of new projects continues to grow and the necessity to construct wind farms in challenging terrain increases, such field data-sets will become increasingly relevant. KW - Monopile KW - Offshore Windenergy KW - Pfahlfußbeulen KW - Pile Tip Buckling KW - Reference Tests PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611651 DO - https://doi.org/10.1016/j.oceaneng.2024.119322 VL - 313 SP - 1 EP - 14 PB - Elsevier B.V. AN - OPUS4-61165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohr, Gunther A1 - Chaudry, Mohsin Ali A1 - Scheuschner, Nils A1 - Blasón Gonzalez, Sergio A1 - Madia, Mauro A1 - Hilgenberg, Kai T1 - Thermal history transfer from complex components to representative test specimens in laser powder bed fusion N2 - Additively manufactured components are characterized by heterogeneous mechanical properties due to variations of the microstructure, flaws and residual stresses resulting from the inhomogeneous fabrication process. The large number of influencing factors poses a further challenge in understanding the correlation between material properties, process parameters and component geometry. Therefore, the qualification of components based on witness specimens produced within the same job is questionable. This work aims to present a new strategy for the characterization of PBF-LB/M components based on representative specimens. The key assumption is the feasibility of a transfer of the thermal history from a component to a specimen. It is assumed that similar material properties are determined for components and specimens produced adopting a similar thermal history. After the definition of a region of interest in the component, a combination of thermal analyses by means of finite elements and in-situ experimental determination of the thermal history through infrared thermography is used to produce test coupons with a similar thermal history. The effectiveness of the procedure is demonstrated on a pressure vessel for applications in the chemical industry. KW - Additive manufacturing KW - Heat accumulation KW - Thermal history KW - In situ monitoring KW - Process simulation KW - Representative specimens PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-602651 DO - https://doi.org/10.1007/s40964-024-00689-8 SN - 2363-9512 SN - 2363-9520 SP - 1 EP - 16 PB - Springer CY - Cham, Switzerland AN - OPUS4-60265 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nourinejhad Zarghani, S. A1 - Monavari, Mehran A1 - Nourinejhad Zarghani, A. A1 - Nouri, S. A1 - Ehlers, J. A1 - Hamacher, J. A1 - Bandte, M. A1 - Büttner, C. T1 - Quantifying plant viruses: Evolution from bioassay to infectivity dilution curves along the model of tobamoviruses N2 - This review describes the development of the bioassay as a means of quantifying plant viruses, with particular attention to tobamovirus. It delves into various models used to establish a correlation between virus particle concentration and the number of induced local lesions (the infectivity dilution curve), including the Poisson, Furumoto and Mickey, Kleczkowski, Growth curve, and modified Poisson models. The parameters of each model are described, and their application or performance in the context of the tobacco mosaic virus is explored. This overview highlights the enduring value of the infectivity dilution curve in tobamovirus quantification, providing valuable insights for researchers or practitioners of bioassays and theoreticians of modeling. KW - Local lesion KW - qRT-PCR KW - Nicotiana KW - ToBRFV KW - TMV KW - CGMMV KW - Disinfection KW - Modeling PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630142 DO - https://doi.org/10.3390/v16030440 SN - 1999-4915 VL - 16 IS - 3 SP - 1 EP - 14 PB - MDPI CY - Basel AN - OPUS4-63014 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oster, Simon A1 - Scheuschner, Nils A1 - Chand, Keerthana A1 - Altenburg, Simon T1 - Local porosity prediction in metal powder bed fusion using in-situ thermography: A comparative study of machine learning techniques N2 - The formation of flaws such as internal porosity in parts produced by Metal-based Powder Bed Fusion with Laser Beam (PBF-LB/M) significantly hinders its broader industrial application, as porosity can potentially lead to part failure. Addressing this issue, this study explores the efficacy of in-situ thermography, particularly short-wave infrared thermography, for detecting and predicting porosity during manufacturing. This technique is capable of monitoring the part’s thermal history which is closely connected to the flaw formation process. Recent advancements in Machine Learning (ML) have been increasingly leveraged for porosity prediction in PBF-LB/M. However, previous research primarily focused on global rather than localized porosity prediction which simplified the complex prediction task. Thereby, the opportunity to correlate the predicted flaw position with expected part strain to judge the severity of the flaw for part performance is neglected. This study aims to bridge this gap by studying the potential of SWIR thermography for predicting local porosity levels using regression models. The models are trained on data from two identical HAYNES®282® specimens. We compare the effectiveness of feature-based and raw data-based models in predicting different porosity types and examine the importance of input data in porosity prediction. We show that models trained on SWIR thermogram data can identify systematic trends in local flaw formation. This is demonstrated for forced flaw formation using process parameter shifts and, moreover, for randomly formed flaws in the specimen bulk. Furthermore, we identify features of high importance for the prediction of lack-of-fusion and keyhole porosity from SWIR monitoring data. KW - PBF-LB/M KW - In situ monitoring KW - Thermography KW - Additive Manufacturing KW - Process monitoring KW - Porosity prediction KW - Machine Learning KW - Feature extraction PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621798 DO - https://doi.org/10.1016/j.addma.2024.104502 SN - 2214-7810 VL - 95 SP - 1 EP - 17 PB - Elsevier B.V. AN - OPUS4-62179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kromm, Arne A1 - Thomas, Maximilian A1 - Kannengießer, Thomas A1 - Gibmeier, Jens T1 - On the interpretation of Varestraint and Transvarestraint hot cracking test results N2 - The Varestraint test and its variant Transvarestraint are one of the most widely used techniques for evaluating a material solidification cracking sensitivity during welding. The result of such tests is a crack length which is proportional to the material’s cracking susceptibility. Nevertheless, the welding and load parameters can unintentionally influence the crack length, which in some cases can distort the material evaluation. An approach is described as to how these effects can be assessed with the aid of a digital crack analysis. The crack lengths are compared position-dependently with their possible propagation due to the weld pool movement during continuous loading. The index derived from this can be used by the operator to evaluate his test parameters. In addition, a comparison of the results of different Varestraint setups is made possible. Alongside experimental results, a numerical sensitivity analysis is presented on how individual welding and loading parameters can affect the crack lengths. KW - Varestraint test KW - Solidification cracking KW - Weldability PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595089 DO - https://doi.org/10.1007/s40194-024-01706-8 SN - 0043-2288 SP - 1 EP - 13 PB - Springer Science and Business Media LLC AN - OPUS4-59508 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Griesche, Axel A1 - Nietzke, Jonathan A1 - Kannengießer, Thomas T1 - In situ measurement of hydrogen concentration in steel using laser‑induced breakdown spectroscopy (LIBS) N2 - The ISO 3690 standard “Determination of hydrogen content in arc weld metal” requires a thermal activation of the diffusible hydrogen in a piece of weld metal for the subsequent ex situ concentration measurement by carrier gas hot extraction CGHE or thermal desorption spectroscopy (TCD). Laser-induced breakdown spectroscopy (LIBS) offers a time and spatially resolved, almost non-destructive, in situ measurement of hydrogen at surfaces without sample preparation. We measured hydrogen in steels, which were charged either electrochemically or by high-pressure hydrogen gas, and compared the results. Further, the feasibility of quantitative hydrogen line scan measurements with LIBS was demonstrated by measuring hydrogen at water jet cut surfaces. The hydrogen concentrations measured with the help of LIBS were compared with CGHE measurements. It was observed that hydrogen can be reliably measured with LIBS for concentrations larger than 2 wt.-ppm. The maximum hydrogen concentration achieved using electrochemical charging was 85.1 ppm. The results show that LIBS is a promising technique for time- and spatially resolved measurements of hydrogen in steels. T2 - IIW Annual Assembly 2023 CY - Singapore KW - LIBS KW - Hydrogen measurement KW - Welding KW - Stainless steel KW - Diffusible hydrogen PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593664 DO - https://doi.org/10.1007/s40194-023-01677-2 SP - 1 EP - 9 PB - Springer AN - OPUS4-59366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wandtke, Karsten ED - Becker, Amadeus ED - Schröpfer, Dirk ED - Kromm, Arne ED - Kannengießer, Thomas ED - Scharf-Wildenhain, R. ED - Hälsig, A. ED - Hensel, J. T1 - Residual Stress Evolution during Slot Milling for Repair Welding and Wire Arc Additive Manufacturing of High-Strength Steel Components N2 - High-strength steels offer potential for weight optimization due to reduced wall thicknesses in modern constructions. Additive manufacturing processes such as Wire Arc Additive Manufacturing (WAAM) enable the resource-efficient production of structures. In the case of defects occurring in weld seams orWAAM components due to unstable process conditions, the economical solution is local gouging or machining and repair welding. It is important to understand the effects of machining steps on the multiaxial stress state in conjunction with the design-related shrinkage restraints. Research into how welding and slot milling of welds andWAAM structures affects residual stresses is still lacking. For this reason, component-related investigations with high-strength steels with yield strengths ≥790 MPa are carried out in our research. In-situ digital image correlation (DIC) and ex-situ X-ray diffraction (XRD) were used to analyze the stresses and strains induced on specimens during and after milling. The systematic analyses revealed a significant interaction of the stiffness and microstructure of the specimens with the initial residual stresses induced by welding. Subsequent repair welds can result in significantly higher residual stresses. KW - High strength steels KW - Additive manufacturing KW - Residual stress KW - Repair welding KW - Ditigtal image correlation PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593515 DO - https://doi.org/10.3390/met14010082 VL - 14 IS - 1 SP - 1 EP - 11 PB - MDPI CY - Basel AN - OPUS4-59351 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröpfer, Dirk A1 - Witte, Julien A1 - Kromm, Arne A1 - Kannengießer, Thomas T1 - Stresses in repair welding of high-strength steels—part 1: restraint and cold cracking risk N2 - AbstractThe sustainable and resource-efficient production of wind energy plants requires the use of modern high-strength fine-grain structural steels. This applies to both foundation and erection structures, like mobile or ship cranes. During the assembly of steel structures, unacceptable defects can occasionally be found in the weld area. In most cases, the economical solution would be local thermal gouging of the affected areas and re-welding. Due to the high shrinkage restraint of the joint groove in the overall structure, the superposition of global and local welding-induced stresses may lead to crack formation and component failure, particularly in interaction with the degradation of the microstructure and mechanical properties of high-strength steels during the repair process. However, manufacturers hardly have any information about these issues and there is a lack of recommendations and guidelines to take these safety-relevant aspects into account in adequate repair concepts. The aim of this research is to derive recommendations for repair concepts appropriate to the stresses and materials involved providing a basis for standards and guidelines to avoid cold cracking, damage and expensive reworking especially for high-strength steels. Part 1 of this study involves systematic investigations of influences of shrinkage restraint during repair welding of two high-strength steels S500MLO for offshore application and S960QL for mobile crane structures. The quantification of the shrinkage restraint of repair weld joints was achieved by means of experimental and numerical restraint intensity analysis. In welding experiments with self-restrained slot specimens, restraint intensity and introduction of hydrogen via the welding arc using anti spatter spray were varied systematically to analyse the effect on welding result, residual stresses and cold cracking. It could be shown that increasing restraint intensities result in significantly higher transverse residual stress levels. In the case of hydrogen introduction S500MLO showed no cold cracking independent of the restraint conditions. However, S960QL was found to be considerably cold cracking sensitive if hydrogen is introduced. With increasing restraint intensity length and number of cold cracks increases significantly. Part 2 [1] of this study is focussed on microstructure and residual stresses due to gouging and stress optimization via adequate heat control parameters in repair welding. KW - Metals and Alloys KW - Mechanical Engineering KW - Mechanics of Materials PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595212 DO - https://doi.org/10.1007/s40194-024-01691-y SN - 0043-2288 SP - 1 EP - 13 PB - Springer Science and Business Media LLC AN - OPUS4-59521 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröder, Nina A1 - Rhode, Michael A1 - Kannengießer, Thomas T1 - Influence of microalloying on precipitation behavior and notch impact toughness of welded high‑strength structural steels N2 - Microalloying elements such as Nb and Ti are essential to increase the strength of quenched and tempered high-strength low alloy (HSLA) structural steels with nominal yield strength ≥ 690 MPa and their welded joints. Standards such as EN 10025–6 only specify limits or ranges for chemical composition, which leads to variations in specific compositions between steel manufacturers. These standards do not address the mechanical properties of the material, and even small variations in alloy content can significantly affect these properties. This makes it difficult to predict the weldability and integrity of welded joints, with potential problems such as softening or excessive hardening of the heat-affected zone (HAZ). To understand these metallurgical effects, previous studies have investigated different microalloying routes with varying Ti and Nb contents using test alloys. The high-strength quenched and tempered fine-grained structural steel S690QL is the basic grade regarding chemical composition and heat treatment. To evaluate weldability, three-layer welds were made using high-performance MAG welding. HAZ formation was investigated, and critical microstructural areas were identified, focusing on phase transformations during cooling and metallurgical precipitation behavior. Isothermal thermodynamic calculations for different precipitations were also carried out. Mechanical properties, especially Charpy notch impact toughness, were evaluated to understand the influence of different microalloys on the microstructure of the HAZ and mechanical properties. KW - High-strength structural steel KW - Gas metal arc welding KW - HAZ-softening KW - Notch impact toughness KW - Microalloying influences KW - Thermodynamic simulation PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608548 DO - https://doi.org/10.1007/s40194-024-01827-0 SN - 0043-2288 SP - 1 EP - 13 PB - Springer AN - OPUS4-60854 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Gornushkin, Igor B. A1 - Griesche, Axel A1 - Kannengießer, Thomas A1 - Treutler, Kai A1 - Wesling, Volker T1 - In situ chemical analysis of duplex stainless steel weld by laser induced breakdown spectroscopy N2 - The high corrosion resistance and good mechanical properties of duplex stainless steel (DSS) are due to its special chemical composition, which is a balanced phase ratio of ferrite (α) and austenite (γ). Many industrial applications require the integration of DSS components. For this, Gas tungsten arc welding (GTAW) is an excellent choice, as it allows an automated operation with high reproducibility. However, when the weld pool solidifies, critical ratios of α- and γ- phases can occur, which lead to solidification cracking, increased susceptibility to corrosion, and a decrease in ductility and critical strength. Previous studies have shown that these defects can be caused by the accumulation of manganese and chromium in the heat affected zone (HAZ), requiring ongoing monitoring of this accumulation. A suitable method for such monitoring is laser-induced breakdown spectroscopy (LIBS), which can be used in two operating modes: calibration using standard reference samples and calibration-free. Unlike conventional quantitative LIBS measurements, which require reference samples to generate a calibration curve, calibration-free LIBS (CF-LIBS) allows chemical compositions to be determined solely from the emission spectrum of the plasma. Numerous publications show that CF-LIBS is a fast and efficient analytical method for the quantitative analysis of metal samples. In this work, CF-LIBS is applied to spectra obtained during GTAW DSS welding and the result is compared with those obtained by PLS analysis. A good correlation was found between both types of analysis, demonstrating the suitability of the CF-LIBS method for this application. The CF-LIBS method has a significant advantage over conventional LIBS due to the rapid in situ measurement of concentrations of major alloying elements without calibration procedure. This, combined with fast feedback and appropriate adjustment of welding parameters, helps prevent welding defects. KW - Duplex stainless steels KW - In situ measurement KW - LIBS KW - GMAW PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597940 DO - https://doi.org/10.1016/j.sab.2024.106899 SN - 0584-8547 VL - 214 SP - 1 EP - 7 PB - Elsevier B.V. AN - OPUS4-59794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Westin, Elin Marianne A1 - Griesche, Axel A1 - Kromm, Arne A1 - Kannengießer, Thomas A1 - Treutler, Kai A1 - Wesling, Volker A1 - Wessman, Sten T1 - Assessing ferrite content in duplex stainless weld metal: WRC ‘92 predictions vs. practical measurements N2 - AbstractThe weldability of stainless steels is largely controlled by the chemical composition, and alloys with ferritic or ferritic-austenitic solidification show the highest resistance to hot cracking. As the resulting phase balance also affects the final properties, it may be beneficial to both foresee and measure the weld metal ferrite content. The WRC ‘92 constitution diagram is currently the most accurate prediction tool available, but it does not take the cooling rate into consideration and the precision may be less accurate for stainless steels with high ferrite numbers (FNs). This study aims to assess the reliability of the WRC ‘92 diagram for weld metals with FN  50. The chemical composition was altered through gas tungsten arc welding (GTAW) of UNS S32205 with ER347 filler wire that had been coated using physical vapor deposition (PVD) with either niobium (Nb), copper (Cu), nickel (Ni), manganese (Mn), carbon (C), or silicon (Si). The actual ferrite content was evaluated using image analysis, FeriteScope and X-ray diffraction (XRD). While predictions from the WRC ‘92 diagram were deemed acceptable for Ni, Si, and Mn, notable deviations were observed for Nb, Cu, and C. The FeriteScope exhibited a consistent trend with image analysis, albeit with slightly higher FN values, wider scatter, and the conversion factor from FN to vol% is open for discussion. The lowest accuracy and largest spread were obtained using non-contact XRD, rendering it unsuitable for ferrite measurements of welds. These findings underscore the need for improved prediction tools and appropriate measurement methods for assessing ferrite content in duplex weld metals. KW - Duplex stainless steel KW - Welding KW - Phase balance KW - Microscopy KW - Microstructure PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618777 DO - https://doi.org/10.1007/s40194-024-01878-3 SN - 1878-6669 VL - 69 IS - 1 SP - 31 EP - 45 PB - Springer CY - Berlin AN - OPUS4-61877 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Westin, Elin Marianne A1 - Griesche, Axel A1 - Kromm, Arne A1 - Kannengießer, Thomas A1 - Treutler, Kai A1 - Wesling, Volker A1 - Wessman, Sten T1 - Assessing ferrite content in duplex stainless weld metal: WRC ‘92 predictions vs. practical measurements N2 - AbstractThe weldability of stainless steels is largely controlled by the chemical composition, and alloys with ferritic or ferritic-austenitic solidification show the highest resistance to hot cracking. As the resulting phase balance also affects the final properties, it may be beneficial to both foresee and measure the weld metal ferrite content. The WRC ‘92 constitution diagram is currently the most accurate prediction tool available, but it does not take the cooling rate into consideration and the precision may be less accurate for stainless steels with high ferrite numbers (FNs). This study aims to assess the reliability of the WRC ‘92 diagram for weld metals with FN  50. The chemical composition was altered through gas tungsten arc welding (GTAW) of UNS S32205 with ER347 filler wire that had been coated using physical vapor deposition (PVD) with either niobium (Nb), copper (Cu), nickel (Ni), manganese (Mn), carbon (C), or silicon (Si). The actual ferrite content was evaluated using image analysis, FeriteScope and X-ray diffraction (XRD). While predictions from the WRC ‘92 diagram were deemed acceptable for Ni, Si, and Mn, notable deviations were observed for Nb, Cu, and C. The FeriteScope exhibited a consistent trend with image analysis, albeit with slightly higher FN values, wider scatter, and the conversion factor from FN to vol% is open for discussion. The lowest accuracy and largest spread were obtained using non-contact XRD, rendering it unsuitable for ferrite measurements of welds. These findings underscore the need for improved prediction tools and appropriate measurement methods for assessing ferrite content in duplex weld metals. KW - Duplex stainless steel KW - Phase fraction prediction KW - WRC diagram PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623682 DO - https://doi.org/10.1007/s40194-024-01878-3 VL - 69 SP - 31 EP - 45 PB - Springer Science and Business Media LLC AN - OPUS4-62368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Giese, Marcel A1 - Gräbner, Maraike A1 - Schröpfer, Dirk A1 - Treutler, Kai A1 - Lorenz, Svenja A1 - Kannengießer, Thomas A1 - Wesling, Volker T1 - Alloy modification and ultrasonic-assisted milling of wear-resistant alloys with defined surfaces N2 - The reduction of CO2 emissions is closely linked to the development of highly efficient and economical steel components in plant and process engineering. To withstand the high combined corrosive, tribological, thermal, and mechanical stresses, wear-resistant coatings tailored to the application and steel grade are used. In addition to the increasing demand to substitute conventional cobalt alloys with nickel alloys, there is also a growing need for defined or functional surfaces of high integrity. Due to high tool wear, milling operations required to produce the complex geometries of the components are often not economically feasible for SMEs. By means of alloy modification of the filler metals for nickel-based plasma build-up welded wear-resistant coatings and by the use of innovative ultrasonic-assisted milling processes more favourable machinability shall be achieved without reducing the wear protection potential. In this paper, the influence of the microstructure and precipitation morphology adjusted by means of alloy modification on the machinability is investigated. This is done based on a wear protection alloy NiCrMoSiFeB (trade name: Colmonoy 56 PTA) typically used for screw machines, which substitutes conventional CoCr alloys (Stellite). Metallurgical investigations and in-situ measurements of occurring process forces and temperatures at the tool cutting edge during milling as well as subsequent investigations of tool wear and surface integrity allow a detailed analysis and correlation between microstructural properties and machinability. For the cast samples, a clear change in the microstructure and hardness can be seen through the addition of Al, Ti, or Nb. These differences lead to an improvement in the machining process for Nb. Al and Ti cause long-needled or star-shaped precipitations and hardness increases, which lead to higher cutting forces and increased tool wear. KW - Cladding KW - Wear resistant alloys KW - Alloy modification KW - Post-processing KW - Ultrasonic assisted milling KW - Renewable energy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-622918 DO - https://doi.org/10.1007/s40194-024-01786-6 SN - 1878-6669 VL - 68 SP - 2567 EP - 2575 PB - Springer Science and Business Media LLC CY - Berlin ; Heidelberg AN - OPUS4-62291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rabin, Ira A1 - Gordon, Nehemia A1 - Calvillo, Nelson T1 - Coloured Ruling Lines in a Fourteenth-Century Ashkenazi Torah Scroll N2 - Rabbinic halakhah required that Torah scrolls be written with relief ruling, horizontal and vertical lines scored into the writing surface. Coloured ruling with plummet or ink would make a Torah scroll invalid for liturgical use. Ruling lines on some leather fragments of early Oriental Torah scrolls give the impression of being produced with plummet or ink but may be the result of dust in the furrows of relief ruling. Erfurt 9, a fourteenth-century Ashkenazi Torah scroll, has coloured ruling, which is partial secondary re-ruling, on 13 of the 34 surviving sheets, perhaps added when the original relief ruling was difficult to see. The coloured ruling in Erfurt 9 is brown, giving it the visual appearance of iron-gall ink. However, XRF tests showed that the only meaningful metallic component in the coloured ruling was lead (Pb). Lead plummet ruling tends to have a greyish appearance. Black specks under near infrared light are consistent with minium, a lead-based red ink that can turn brown when it degrades. Partial secondary re-ruling added with minium to the original relief ruling comes as a surprise as it would have rendered Erfurt 9 unfit for liturgical use. KW - Hebrew Manuscripts KW - Ruling Lines KW - Coloured Ink PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-628531 DO - https://doi.org/10.25592/uhhfdm.17169 SN - 2410-0951 VL - 10 SP - 9 EP - 32 AN - OPUS4-62853 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wätzold, Florian A1 - Popiela, Bartosz A1 - Mayer, Jonas T1 - Methodology for AI-Based Search Strategy of Scientific Papers: Exemplary Search for Hybrid and Battery Electric Vehicles in the Semantic Scholar Database N2 - The rapid development of artificial intelligence (AI) has significantly enhanced productivity, particularly in repetitive tasks. In the scientific domain, literature review stands out as a key area where AI-based tools can be effectively applied. This study presents a methodology for developing a search strategy for systematic reviews using AI tools. The Semantic Scholar database served as the foundation for the search process. The methodology was tested by searching for scientific papers related to batteries and hydrogen vehicles with the aim of enabling an evaluation for their potential applications. An extensive list of vehicles and their operational environments based on international standards and literature reviews was defined and used as the main input for the exemplary search. The AI-supported search yielded approximately 60,000 results, which were subjected to an initial relevance assessment. For the relevant papers, a neighbourhood analysis based on citation and reference networks was conducted. The final selection of papers, covering the period from 2013 to 2023, included 713 papers assessed after the initial review. An extensive discussion of the results is provided, including their categorisation based on search terms, publication years, and cluster analysis of powertrains, as well as operational environments of the vehicles involved. This case study illustrates the effectiveness of the proposed methodology and serves as a starting point for future research. The results demonstrate the potential of AI-based tools to enhance productivity when searching for scientific papers. KW - Search strategy KW - Methodology KW - Artificial intelligence KW - Literature review KW - Battery electric vehicles KW - Hydrogen-powered vehicles PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-622012 DO - https://doi.org/10.3390/publications12040049 VL - 12 IS - 4 SP - 1 EP - 16 PB - MDPI CY - Basel, Switzerland AN - OPUS4-62201 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roveda, Ilaria A1 - Serrano-Munoz, Itziar A1 - Haubrich, Jan A1 - Requena, Guillermo A1 - Madia, Mauro T1 - Investigation on the fatigue strength of AlSi10Mg fabricated by PBF-LB/M and subjected to low temperature heat treatments N2 - This work provides an investigation of the influence of low temperature heat treatments on the fatigue behavior of a PBF-LB AlSi10Mg alloy. Fatigue specimens are produced in form of round bars on a build platform preheated at 200 ◦C. The specimens have been tested in three different conditions: as-built, and after heat treatments at 265 ◦C for 1 h and 300 ◦C for 2 h. Prior to the fatigue testing, the defect distribution is analyzed by means of micro computed tomography. Subsequently, the peak over threshold method is successfully applied to provide a prediction of the size of killer defect. The defect population was of gas porosity type. No clear improvement of the fatigue performance is observed after the heat treatments. The fatigue strength predicted using fracture mechanics-based approaches is in good agreement with the experimental data. Among the studied approaches, short crack models provided the most conservative predictions. KW - PBF-LB/M AlSi10Mg KW - Fatigue strength KW - Defects KW - Kitagawa-Takahashi Diagram KW - Short Crack Models PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-607071 DO - https://doi.org/10.1016/j.matdes.2024.113170 SN - 0264-1275 VL - 244 SP - 1 EP - 12 PB - Elsevier Ltd. AN - OPUS4-60707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lozano-Martín, D. A1 - Pazoki, F. A1 - Kipphardt, Heinrich A1 - Khanipour, P. A1 - Tuma, Dirk A1 - Horillo, A. A1 - Chamorro, C. R. T1 - Thermodynamic (p, ρ, T) characterization of a reference high-calorific natural gas mixture when hydrogen is added up to 20 % (mol/mol) N2 - The injection of hydrogen into the natural-gas grid is an alternative during the process of a gradual decarbonization of the heat and power supply. When dealing with hydrogen-enriched natural gas mixtures, the performance of the reference equations of state habitually used for natural gas should be validated by using high-precision experimental thermophysical data from multicomponent reference mixtures prepared with the lowest possible uncertainty in composition. In this work, we present experimental density data for an 11-compound high-calorific (hydrogen-free) natural gas mixture and for two derived hydrogen-enriched natural gas mixtures prepared by adding (10 and 20) mol-% of hydrogen to the original standard natural gas mixture. The three mixtures were prepared gravimetrically according to ISO 6142–1 for maximum precision in their composition and thus qualify for reference materials. A single-sinker densimeter was used to determine the density of the mixtures from (250–350) K and up to 20 MPa. The experimental density results of this work have been compared to the densities calculated by three different reference equations of state for natural gas related mixtures: the AGA8-DC92 EoS, the GERG-2008 EoS, and an improved version of the GERG-2008 EoS. While relative deviations of the experimental density data for the hydrogen-free natural gas mixture are always within the claimed uncertainty of the three considered equations of state, larger deviations can be observed for the hydrogen-enriched natural gas mixtures from any of the three equations of state, especially for the lowest temperature and the highest pressures. KW - Hydrogen-enriched natural gas KW - Single-sinker densimeter KW - High-pressure density KW - Equations of state PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-604742 DO - https://doi.org/10.1016/j.ijhydene.2024.05.028 SN - 0360-3199 VL - 70 SP - 118 EP - 135 PB - Elsevier BV CY - Amsterdam AN - OPUS4-60474 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghata, Anupama A1 - Bernges, Tim A1 - Maus, Oliver A1 - Wankmiller, Björn A1 - Naik, Aakash A1 - Bustamante, Joana A1 - Gaultois, Michael W. A1 - Delaire, Olivier A1 - Hansen, Michael Ryan A1 - George, Janine A1 - Zeier, Wolfgang G. T1 - Exploring the Thermal and Ionic Transport of Cu+ Conducting Argyrodite Cu7PSe6 N2 - AbstractUnderstanding the origin of low thermal conductivities in ionic conductors is essential for improving their thermoelectric efficiency, although accompanying high ionic conduction may present challenges for maintaining thermoelectric device integrity. This study investigates the thermal and ionic transport in Cu7PSe6, aiming to elucidate their fundamental origins and correlation with the structural and dynamic properties. Through a comprehensive approach including various characterization techniques and computational analyses, it is demonstrated that the low thermal conductivity in Cu7PSe6 arises from structural complexity, variations in bond strengths, and high lattice anharmonicity, leading to pronounced diffuson transport of heat and fast ionic conduction. It is found that upon increasing the temperature, the ionic conductivity increases significantly in Cu7PSe6, whereas the thermal conductivity remains nearly constant, revealing no direct correlation between ionic and thermal transport. This absence of direct influence suggests innovative design strategies in thermoelectric applications to enhance stability by diminishing ionic conduction, while maintaining low thermal conductivity, thereby linking the domains of solid‐state ionics and thermoelectrics. Thus, this study attempts to clarify the fundamental principles governing thermal and ionic transport in Cu+‐superionic conductors, similar to recent findings in Ag+ argyrodites. KW - Thermoelectrics KW - Phonons KW - Chemically Complex Materials KW - DFT KW - Bonding Analysis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608866 DO - https://doi.org/10.1002/aenm.202402039 SP - 1 EP - 9 PB - Wiley AN - OPUS4-60886 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Naik, Aakash A1 - Ueltzen, Katharina A1 - Ertural, Christina A1 - Jackson, Adam J. A1 - George, Janine T1 - LobsterPy: A package to automatically analyze LOBSTERruns N2 - The LOBSTER (Deringer et al., 2011;Maintz et al., 2013 ,2016 ;Nelson et al., 2020 ) software aids in extracting quantum-chemical bonding information from materials by projecting the plane-wave based wave functions from density functional theory (DFT) onto an atomic orbital basis. LobsterEnv, a module implemented in pymatgen (Ong et al., 2013) by some of the authors of this package, facilitates the use of quantum-chemical bonding information obtained from LOBSTER calculations to identify neighbors and coordination environments. LobsterPy is a Python package that offers a set of convenient tools to further analyze and summarize the LobsterEnv outputs in the form of JSONs that are easy to interpret and process. These tools enable the estimation of (anti) bonding contributions, generation of textual descriptions, and visualization of LOBSTER computation results. Since its first release, both LobsterPy and LobsterEnv capabilities have been extended significantly. Unlike earlier versions, which could only automatically analyze Crystal Orbital Hamilton Populations (COHPs) (Dronskowski & Blöchl, 1993), both can now also analyze Crystal Orbital Overlap Populations (COOP) (Hughbanks & Hoffmann, 1983) and Crystal Orbital Bond Index (COBI) (Müller et al., 2021). Extracting the information about the most important orbitals contributing to the bonds is optional, and users can enable it as needed. Additionally, bonding-based features for machinelearning (ML) studies can be engineered via the sub-packages “featurize” and “structuregraphs”. Alongside its Python interface, it also provides an easy-to-use command line interface (CLI) that runs automatic analysis of the computations and generates a summary of results and publication-ready figures. LobsterPy has been used to produce the results in Ngo et al. (2023), Chen et al. (2024), Naik et al. (2023), and it is also part of Atomate2 (2023) bonding analysis workflow for generating bonding analysis data in a format compatible with the Materials Project (Jain et al., 2013) API. KW - Materials Science KW - Automation KW - Bonding Analysis KW - Materials Properties PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595809 DO - https://doi.org/10.21105/joss.06286 VL - 9 IS - 94 SP - 1 EP - 4 PB - The Open Journal AN - OPUS4-59580 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Musyanovych, A. A1 - Grimmer, Christoph A1 - Sadak, A. E. A1 - Heßling, L. A1 - Lüdicke, M. A1 - Bilsel, M. A1 - Horn, Wolfgang A1 - Richter, Matthias T1 - Polymer Capsules with Volatile Organic Compounds as Reference Materials for Controlled Emission N2 - Encapsulation of volatile organic compounds (VOCs) that could evaporate at a defined rate is of immense interest for application in emission reference materials (ERMs). Polyurethane/polyurea microcapsules with various VOC active ingredients (limonene, pinene, and toluene) were successfully produced by interfacial polymerization with Shirasu porous glass membrane emulsification in a size range between 10 and 50 μm. The effect of surfactant, VOC, monomer(s) type, and ratio has a great effect on the formulation process and morphology of capsules. The type of VOC played a significant role in the encapsulation efficiency. Due to the difference in vapor pressure and VOC/water interfacial tension, the formulation for encapsulation was optimized for each individual VOC. Furthermore, to achieve effective stability of the large droplets/capsules, a combination of ionic and nonionic surfactants was used. Optical and scanning electron microscopy, Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA), were used to characterize the optimized microcapsules. The results showed that the obtained microcapsules exhibited a spherical shape and core–shell morphology and featured characteristic urethane-urea bonds. The amount of encapsulated VOC ranges between 54 and 7 wt %. The emission tests were performed with the help of the emission test chamber procedure (EN 16516). The limonene-loaded polyurethane/polyurea microcapsules show a change in emission rate of less than 10% within 14 days and can be considered as a potential candidate for use as an ERM. KW - Polymer microcapsules KW - Membrane emulsification KW - Polyaddition KW - Volatile organic compound (VOC) KW - Emission testing PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-619227 DO - https://doi.org/10.1021/acsami.4c12826 SN - 1944-8252 VL - 16 IS - 50 SP - 69999 EP - 70009 PB - ACS AN - OPUS4-61922 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winkler, Nicolas P. A1 - Kotlyar, O. A1 - Schaffernicht, E. A1 - Matsukura, H. A1 - Ishida, H. A1 - Neumann, Patrick P. A1 - Lilienthal, A. J. T1 - Super-resolution for Gas Distribution Mapping N2 - Gas Distribution Mapping (GDM) is a valuable tool for monitoring the distribution of gases in a wide range of applications, including environmental monitoring, emergency response, and industrial safety. While GDM is actively researched in the scope of gas-sensitive mobile robots (Mobile Robot Olfaction), there is a potential for broader applications utilizing sensor networks. This study aims to address the lack of deep learning approaches in GDM and explore their potential for improved mapping of gas distributions. In this paper, we introduce Gas Distribution Decoder (GDD), a learning-based GDM method. GDD is a deep neural network for spatial interpolation between sparsely distributed sensor measurements that was trained on an extensive data set of realistic-shaped synthetic gas plumes based on actual airflow measurements. As access to ground truth representations of gas distributions remains a challenge in GDM research, we make our data sets, along with our models, publicly available. We test and compare GDD with state-of-the-art models on synthetic and real-world data. Our findings demonstrate that GDD significantly outperforms existing models, demonstrating a 35% improvement in accuracy on synthetic data when measured using the Root Mean Squared Error over the entire distribution map. Notably, GDD appears to have superior capabilities in reconstructing the edges and characteristic shapes of gas plumes compared to traditional models. These potentials offer new possibilities for more accurate and efficient environmental monitoring, and we hope to inspire other researchers to explore learning-based GDM. KW - Gas distribution mapping KW - Spatial interpolation KW - Sensor networks KW - Deep learning PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-607786 DO - https://doi.org/10.1016/j.snb.2024.136267 SN - 0925-4005 VL - 419 SP - 1 EP - 12 PB - Elsevier B.V. AN - OPUS4-60778 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Niebergall, Ute A1 - Marschall, Niklas A1 - Meinel, Dietmar A1 - Böhning, Martin T1 - Relation of craze to crack length during slow crack growth phenomena in high‐density polyethylene N2 - The craze‐crack mechanism occurring in high‐density polyethylene (HDPE) causing slow crack growth and environmental stress cracking is investigated in detail with respect to the relation of crack length and the related craze zone. This is essential for the understanding of the resulting features of the formed fracture surface and their interpretation in the context of the transition from crack propagation to ductile shear deformation. It turns out that an already formed craze zone does not inevitably result in formation of a propagating crack, but could also undergo ductile failure. For the examination, the full notch creep test (FNCT) was employed with a subsequent advanced fracture surface analysis that was performed using various imaging techniques: light microscopy, laser scanning microscopy, scanning electron microscopy, and X‐ray micro computed tomography scan. FNCT specimens were progressively damaged for increasing durations under standard test conditions applying Arkopal, the standard surfactant solution, and biodiesel as test media were used to analyze the stepwise growth of cracks and crazes. From considerations based on well‐established fracture mechanics approaches, a theoretical correlation between the length of the actual crack and the length of the preceding craze zone was established that could be evidenced and affirmed by FNCT fracture surface analysis. Moreover, the yield strength of a HDPE material exposed to a certain medium as detected by a classic tensile test was found to be the crucial value of true stress to induce the transition from crack propagation due to the craze‐crack mechanism to shear deformation during FNCT measurements. Highlights - Progress of crack formation in high‐density polyethylene is analyzed by different imaging techniques - Determined growth rates depend on distinction between craze zone and crack - The ratio of the present crack to the anteceding craze zone is validated theoretically - The transition from crack propagation to ductile shear deformation is identified - An already formed craze zone may still fail by ductile mechanisms KW - Craze-crack mechanism KW - Environmental stress cracking (ESC) KW - Full notch creep test (FNCT) KW - Laser scanning microscopy (LSM) KW - Slow crack growth (SCG) KW - X-ray computed tomography (CT) PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601831 DO - https://doi.org/10.1002/pen.26698 SN - 1548-2634 VL - 64 IS - 6 SP - 2387 EP - 2403 PB - Wiley AN - OPUS4-60183 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emamverdi, Farnaz A1 - Huang, J. A1 - Mosane Razavi, Negar A1 - Bojdys, M. J. A1 - Forster, A. B. A1 - Budd, P. M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Molecular Mobility and Gas Transport Properties of Mixed Matrix Membranes Based on PIM‑1 and a Phosphinine Containing Covalent Organic Framework N2 - Polymers with intrinsic microporosity (PIMs) are gaining attention as gas separation membranes. Nevertheless, they face limitations due to pronounced physical aging. In this study a covalent organic framework containing λ5-phosphinine moieties, CPSF-EtO were incorporated as a nanofiller (concentration range 0-10 wt%) into a PIM-1 matrix forming dense films with a thickness of ca. 100 μm. The aim of the investigation was to investigate possible enhancements of gas transport properties and mitigating effects on physical aging. The incorporation of the nanofiller occurred on aggregate level with domains up to 100 nm as observed by T-SEM and confirmed by X-ray scattering. Moreover, the X-ray data show that the structure of the microporous network of the PIM-1 matrix is changed by the nanofiller. As the molecular mobility is fundamental for gas transport as well as for physical aging, the study includes dielectric investigations of pure PIM-1 and PIM-1/CPSF-EtO mixed matrix membranes to establish a correlation between the molecular mobility and the gas transport properties. Using the time-lag method the gas permeability and the permselectivity were determined for N2, O2, CH4 and CO2 for samples with variation in filler content. A significant increase in the permeability of CH4 and CO2 (50 % increase compared to pure PIM-1) was observed for a concentration of 5 wt% of the nanofiller. Furthermore, the most pronounced change in the permselectivity was found for the gas pair CO2/N2 at a filler concentration of 7 wt%. KW - Polymers of Intrinsic Microporosity KW - Nanocomposites PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595031 DO - https://doi.org/10.1021/acs.macromol.3c02419 SN - 0024-9297 VL - 57 IS - 4 SP - 1829 EP - 1845 PB - ACS Publications AN - OPUS4-59503 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emamverdi, Farnaz A1 - Huang, J. A1 - Szymoniak, Paulina A1 - Bojdys, M. J. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Structure and molecular mobility of phosphinine-based covalent organic frameworks – glass transition of amorphous COFs N2 - Two-dimensional covalent organic frameworks (COFs) based on phosphinine and thiophene building blocks have been synthesized with two different side groups. The materials are denoted as CPSF-MeO and CPSF-EtO where CxxF correspond to the covalent framework, whereas P and S are related to heteroatoms phosphorous and sulfur. MeO and EtO indicate the substituents, i.e. methoxy and ethoxy. Their morphologies were studied by scanning electron microcopy and X-ray scattering. The absence of crystalline reflexes in the X-ray pattern reveal that both materials are amorphous and can be considered as glasses. Furthermore, N2 adsorption measurements indicate substantial Brunauer–Emmett–Teller (BET) surface area values pointing to the formation of three-dimensional pores by stacking of the aromatic 2D layer. An analysis of the porosity of both COFs showed a mean radius of the pores to be of ca. 4 nm, consistent with their chemical structure. The COFs form nanoparticles with a radius of around 100 nm. The thermal behavior of the COFs was further investigated by fast scanning calorimetry. These investigations showed that both COFs undergo a glass transition. The glass transition temperature of CPSF-EtO is found to be ca. 100 K higher than that for CPSF-MeO. This large difference in the glass transition is discussed to be due to a change in the interaction of the COF sheets induced by the longer ethoxy group. It might be assumed that for CPSF-EtO more individual COF sheets assemble to larger stacks than for CPSF-MeO. This agrees with the much larger surface area value found for CPSF-EtO compared to CPSF-MeO. To corroborate the results obtained be fast scanning calorimetry dielectric measurements were conducted which confirm the occurrence of a dynamic glass transition. The estimated temperature dependence of the relaxation rates of the dielectric relaxation and their absolute values agrees well with the data obtained by fast scanning calorimetry. Considering the fragility approach to the glass transition, it was further found that CPSF-MeO is a fragile glass former whereas CPSF-EtO behaves as a strong glass forming material. This difference in the fragility points also to distinct differences in the interaction between the 2D COF molecules in both materials. KW - Covalent Organic frameworks PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-596770 DO - https://doi.org/10.1039/d3ma01123b SP - 1 EP - 10 PB - Royal Society of Chemistry (RSC) AN - OPUS4-59677 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tang, Chi-Long A1 - Seeger, Stefan T1 - Measurement of sub-4 nm particle emission from FFF-3D printing with the TSI Nano Enhancer and the Airmodus Particle Size Magnifier N2 - The emission of ultrafine particles from small desktop Fused Filament Fabrication (FFF) 3D printers has been frequently investigated in the past years. However, the vast majority of FFF emission and exposure studies have not considered the possible occurrence of particles below the typical detection limit of Condensation Particle Counters and could have systematically underestimated the total particle emission as well as the related exposure risks. Therefore, we comparatively measured particle number concentrations and size distributions of sub-4 nm particles with two commercially available diethylene glycol-based instruments – the TSI 3757 Nano Enhancer and the Airmodus A10 Particle Size Magnifier. Both instruments were evaluated for their suitability of measuring FFF-3D printing emissions in the sub-4 nm size range while operated as a particle counter or as a particle size spectrometer. For particle counting, both instruments match best when the Airmodus system was adjusted to a cut-off of 1.5 nm. For size spectroscopy, both instruments show limitations due to either the fast dynamics or rather low levels of particle emissions from FFF-3D printing in this range. The effects are discussed in detail in this article. The findings could be used to implement sub-4 nm particle measurement in future emission or exposure studies, but also for the development of standard test protocols for FFF-3D printing emissions. KW - Air pollution KW - Ultrafine particles KW - Sub-4nm particles KW - FFF-3D printing KW - Emission testing PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595952 DO - https://doi.org/10.1080/02786826.2024.2320430 SN - 0278-6826 VL - 58 IS - 6 SP - 644 EP - 656 PB - Taylor & Francis CY - London AN - OPUS4-59595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gugin, Nikita A1 - Yusenko, Kirill A1 - King, Andrew A1 - Meyer, Klas A1 - Al-Sabbagh, Dominik A1 - Villajos Collado, José Antonio A1 - Emmerling, Franziska T1 - Lighting up industrial mechanochemistry: Real-time in situ monitoring of reactive extrusion using energy-dispersive X-ray diffraction N2 - Mechanochemistry is an environmentally friendly synthetic approach that enables the sustainable production of a wide range of chemicals while reducing or eliminating the need for solvents. Reactive extrusion aims to move mechanochemistry from its conventional gram-scale batch reactions, typically performed in laboratory ball mills, to a continuous, large-scale process. Meeting this challenge requires in situ monitoring techniques to gain insights into reactive extrusion and its underlying processes. While the effectiveness of in situ Raman spectroscopy in providing molecular-level information has been demonstrated, our study uses energy-dispersive X-ray diffraction to monitor reactive extrusion in real time at the crystalline level. Our results provide previously unavailable control over the reactive extrusion process, promoting its perception as an industrially feasible green alternative to traditional solvent-based syntheses. KW - Mechanochemistry KW - Reactive extrusion KW - Green chemistry KW - In situ studies KW - Time-resolved in situ KW - TRIS KW - Synchrotron radiation KW - Scalable synthesis KW - Solid-state reactions KW - Reaction mechanisms PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613969 DO - https://doi.org/10.1016/j.chempr.2024.07.033 VL - 10 IS - 11 SP - 1 EP - 16 PB - Elsevier B.V. AN - OPUS4-61396 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohring, Wencke A1 - Karafiludis, Stephanos A1 - Manzoni, Anna Maria A1 - Laplanche, G. A1 - Schneider, M. A1 - Stephan-Scherb, Christiane T1 - High-Temperature Corrosion of High- and Medium-Entropy Alloys CrMnFeCoNi and CrCoNi Exposed to a Multi-Oxidant Atmosphere H2O–O2–SO2 N2 - AbstractThe high-temperature corrosion behaviors of the equimolar CrCoNi medium-entropy alloy and CrMnFeCoNi high-entropy alloy were studied in a gas atmosphere consisting of a volumetric mixture of 10% H2O, 2% O2, 0.5% SO2, and 87.5% Ar at 800 °C for up to 96 h. Both alloys were initially single-phase fcc with a mean grain size of ~ 50 μm and a homogeneous chemical composition. The oxide layer thickness of CrMnFeCoNi increased linearly with exposure time while it remained constant at ~ 1 μm for CrCoNi. A Cr2O3 layer and minor amounts of (Co,Ni)Cr2O4 developed on the latter while three oxide layers were detected on the former, i.e., a thin and continuous chromium rich oxide layer at the oxide/alloy interface, a dense (Mn,Cr)3O4 layer in the center and a thick and porous layer of Mn3O4 and MnSO4 at the gas/oxide interface. Additionally, a few metal sulfides were observed in the CrMnFeCoNi matrix. These results were found to be in reasonable agreement with thermodynamic calculations. KW - high entropy alloys KW - corrosion KW - oxidation KW - scanning electron microscopy KW - sulfidation KW - CrMnFeCoNi PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594189 DO - https://doi.org/10.1007/s44210-023-00026-8 SP - 1 EP - 17 PB - Springer Science and Business Media LLC AN - OPUS4-59418 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sun, Yijuan A1 - Gawlitza, Kornelia A1 - Valderrey, Virginia A1 - Bhattacharya, Biswajit A1 - Rurack, Knut T1 - Ratiometric Molecularly Imprinted Particle Probes for Reliable Fluorescence Signaling of Carboxylate-Containing Molecules N2 - In addition to sensitivity, selectivity, and portability, chemical sensing systems must generate reliable signals and offer modular configurability to address various small molecule targets, particularly in environmental applications. We present a versatile, modular strategy utilizing ratiometric molecularly imprinted particle probes based on BODIPY indicators and dyes for recognition and internal referencing. Our approach employs polystyrene core particles doped with a red fluorescent BODIPY as an internal standard, providing built-in reference for environmental influences. A molecularly imprinted polymer (MIP) recognition shell, incorporating a green-fluorescent BODIPY indicator monomer with a thiourea binding site for carboxylate containing analytes, is grafted from the core particles in the presence of the analyte as the template. The dual-fluorescent MIP probe detects fexofenadine as the model analyte with a change in green emission signal referenced against a stable red signal, achieving a detection limit of 0.13 μM and a broad dynamic range from 0.16 μM to 1.2 mM, with good discrimination against other antibiotics in acetonitrile. By selecting a versatile dye scaffold and recognition element, this approach can be extended to other carboxylate-containing analytes and/or wavelength combinations, potentially serving as a robust multiplexing platform. KW - Core-shell particles KW - Molecular imprinting KW - Pharmaceutical contaminants KW - Self-referenced measurements KW - Fluorescence PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-609385 DO - https://doi.org/10.1021/acsami.4c09990 SP - 1 EP - 13 PB - American Chemical Society (ACS) AN - OPUS4-60938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Russo, Francesco F. A1 - Nowatzky, Yannek A1 - Jaeger, Carsten A1 - Parr, Maria K. A1 - Benner, Philipp A1 - Muth, Thilo A1 - Lisec, Jan T1 - Machine learning methods for compound annotation in non‐targeted mass spectrometry—A brief overview of fingerprinting, in silico fragmentation and de novo methods N2 - Non‐targeted screenings (NTS) are essential tools in different fields, such as forensics, health and environmental sciences. NTSs often employ mass spectrometry (MS) methods due to their high throughput and sensitivity in comparison to, for example, nuclear magnetic resonance–based methods. As the identification of mass spectral signals, called annotation, is labour intensive, it has been used for developing supporting tools based on machine learning (ML). However, both the diversity of mass spectral signals and the sheer quantity of different ML tools developed for compound annotation present a challenge for researchers in maintaining a comprehensive overview of the field.In this work, we illustrate which ML‐based methods are available for compound annotation in non‐targeted MS experiments and provide a nuanced comparison of the ML models used in MS data analysis, unravelling their unique features and performance metrics. Through this overview we support researchers to judiciously apply these tools in their daily research. This review also offers a detailed exploration of methods and datasets to show gaps in current methods, and promising target areas, offering a starting point for developers intending to improve existing methodologies. KW - Mass Spectrometry KW - Spectra annotation KW - Machine learning PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608732 DO - https://doi.org/10.1002/rcm.9876 VL - 38 IS - 20 SP - 1 EP - 15 PB - Wiley AN - OPUS4-60873 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peter, Elisa K. A1 - Jaeger, Carsten A1 - Lisec, Jan A1 - Peters, R. Sven A1 - Mourot, Rey A1 - Rossel, Pamela E. A1 - Tranter, Martyn A1 - Anesio, Alexandre M. A1 - Benning, Liane G. T1 - Endometabolic profiling of pigmented glacier ice algae: the impact of sample processing N2 - Introduction Glacier ice algae, mainly Ancylonema alaskanum and Ancylonema nordenskiöldi, bloom on Greenland Ice Sheet bare ice surfaces. They significantly decrease surface albedo due to their purple-brown pigmentation, thus increasing melt. Little is known about their metabolic adaptation and factors controlling algal growth dynamics and pigment formation. A challenge in obtaining such data is the necessity of melting samples, which delays preservation and introduces bias to metabolomic analysis. There is a need to evaluate the physiological response of algae to melting and establish consistent sample processing strategies for metabolomics of ice microbial communities. Objectives To address the impact of sample melting procedure on metabolic characterization and establish a processing and analytical workflow for endometabolic profiling of glacier ice algae. Methods We employed untargeted, high-resolution mass spectrometry and tested the effect of sample melt temperature (10, 15, 20 °C) and processing delay (up to 49 h) on the metabolome and lipidome, and complemented this approach with cell counts (FlowCam), photophysiological analysis (PAM) and diversity characterization. Results and Conclusion We putatively identified 804 metabolites, with glycerolipids, glycerophospholipids and fatty acyls being the most prominent superclasses ( 50% of identified metabolites). Among the polar metabolome, carbohydrates and amino acid-derivatives were the most abundant. We show that 8% of the metabolome is affected by melt duration, with a pronounced decrease in betaine membrane lipids and pigment precursors, and an increase in phospholipids. Controlled fast melting at 10 °C resulted in the highest consistency, and is our recommendation for future supraglacial metabolomics studies. KW - Metabolic profiling KW - Mass Spectrometry KW - Ice algae PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-607921 DO - https://doi.org/10.1007/s11306-024-02147-6 VL - 20 IS - 5 SP - 1 EP - 15 PB - Springer Science and Business Media LLC AN - OPUS4-60792 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tobias, Charlie A1 - López-Puertollano, Daniel A1 - Abad-Somovilla, Antonio A1 - Mercader, J. V. A1 - Abad-Fuentes, A. A1 - Rurack, Knut T1 - Development of Simple and Rapid Bead-Based Cytometric Immunoassays Using Superparamagnetic Hybrid Core−Shell Microparticles N2 - Flow cytometry-based immunoassays are valuable in biomedical research and clinical applications due to their high throughput and multianalyte capability, but their adoption in areas such as food safety and environmental monitoring is limited by long assay times and complex workflows. Rapid, simplified bead-based cytometric immunoassays are needed to make these methods viable for point-of-need applications, especially with the increasing accessibility of miniaturized cytometers. This work introduces superparamagnetic hybrid polystyrene-silica core−shell microparticles as promising alternatives to conventional polymer beads in competitive cytometric immunoassays. These beads, featuring high specificity, sensitivity, and excellent handling capabilities via magnetic separation, were evaluated with three different antibodies and binding methods, showing variations in signal intensity based on the antibody and its attachment method. The optimal performance was achieved through a secondary antibody binding approach, providing strong and consistent signals with minimal uncertainty. The optimized protocol made it possible to achieve a detection limit of 0.025 nM in a total assay time of only 15 min and was successfully used to detect ochratoxin A (OTA) in raw flour samples. This work highlights the potential of these beads as versatile tools for flow cytometry-based immunoassays, with significant implications for food safety, animal health, environmental monitoring, and clinical diagnostics. KW - Immunoassays KW - Bead-based KW - Core-shell particles KW - Cytometry KW - Mycotoxins PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-610593 DO - https://doi.org/10.1021/acsmeasuresciau.4c00038 SP - 1 EP - 11 PB - American Chemical Society CY - Washington, D.C. AN - OPUS4-61059 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gadelmeier, C. A1 - Agudo Jácome, Leonardo A1 - Suárez Ocano, Patricia A1 - Glatzel, U. T1 - Effect of stacking fault energy (SFE) of single crystal, equiatomic CrCoNi and Cantor alloy on creep resistance N2 - Compared to mechanisms like solid solution strengthening, the stacking fault energy (SFE) should be considered as a further factor that influences the material properties. The effect of SFE of alloys or individual elements on strength and resistance can vary considerably. In the high-temperature regime above 700 ◦C, there are still significant gaps in the knowledge about the effect of the SFE on the mechanical properties of single-phase alloys. The effect of SFE on creep resistance of two face-entered cubic equiatomic medium and high entropy alloys, CrCoNi and CrMnFeCoNi, respectively, is evaluated to fill parts of these gaps. Using the Bridgman solidification process, the alloys were produced as single crystals and crept under vacuum at 700 ◦C up to 1100 ◦C. This work shows a significant impact of the lower SFE of CrCoNi on the creep behavior compared to the results of previous investigations of CrMnFeCoNi. The creep resistance of the former is higher over the complete temperature range. At very high temperatures, the strengthening effect of the stacking faults is significantly present. The formation of tetragonal stacking faults and extended dislocation nodes can be identified as the reason for this effect. KW - Medium entropy alloy KW - MEA KW - HEA KW - Single crystal KW - CrCoNi PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-602620 DO - https://doi.org/10.1016/j.msea.2024.146779 SN - 0921-5093 VL - A 908 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-60262 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mansurova, Maria A1 - Johann, Sergej A1 - Kohlhoff, Harald A1 - Rurack, Knut A1 - Bartholmai, Matthias A1 - Bell, Jérémy T1 - On-Site Analytical Tool Based on Crude Oil Fluorescence and Chemometrics for the Rapid Determination of the Nature and Essential Properties of Oil Spills N2 - With the reduction of large oil spills because of stricter regulations and safety measures, the question of how to manage smaller oil spills arises. Few on-site analytical tools are available for first responders or other law enforcement personnel to rapidly test for crude oil in the early management of localized polluted areas. The approach reported here relies on well-described computer-assisted multivariate data analysis of the intrinsic fluorescence fingerprints of crude oils to build a multivariate model for the rapid classification of crude oils and the prediction of their properties. Thanks to a dedicated robust portable reader, the method allowed classification and accurate prediction of various properties of crude oil samples like density (according to API, the American Petroleum Institute and viscosity as well as composition parameters such as volume fractions of paraffins or aromatics. In this way, autonomous operation in on-site or in-the-field applications becomes possible based on the direct (undiluted and untreated) measurement of samples and a rapid, tablet-operated readout system to yield a robust and simple analytical test with superior performance. Testing in real-life scenarios allowed the successful classification and prediction of a number of oil spill samples as well as weathered samples that closely resemble samples collected by first responders. KW - Oil spills KW - Fluorescence KW - PCA KW - Petroleum KW - Rapid test KW - Portable PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595442 DO - https://doi.org/10.1021/acsestwater.3c00648 VL - 4 IS - 2 SP - 621 EP - 627 PB - American Chemical Society (ACS) AN - OPUS4-59544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -