TY - JOUR A1 - Kolmangadi, Mohamed A. A1 - Raab, A. R. A1 - Szymoniak, Paulina A1 - Li, Z. A1 - Huber, P. A1 - Laschat, S. A1 - Schönhals, Andreas T1 - Molecular mobility and electrical conductivity of amino acid-based (DOPA) ionic liquid crystals in the bulk state and nanoconfinement N2 - This study explores the molecular mobility, phase behavior, and electrical conductivity of dihydroxyphenylalanine-based ionic liquid crystals (DOPAn, with alkyl side chains n = 12, 14, 16) featuring cyclic guanidiniumchloride headgroups, in both bulk and nanoconfined states. Using broadband dielectric spectroscopy, differential scanning calorimetry, and fast scanning calorimetry, the research uncovers a complex interplay between molecular structure, self-assembly, and molecular mobility. In bulk, DOPAn shows a phase sequence from plastic crystalline to hexagonal columnar and isotropic phases, driven by superdisc formation and columnar organization. Multiple relaxation processes are identified: localized side-chain dynamics (γ-relaxation), ionic headgroup or core motions (α1-relaxation), and cooperative alkyl domain fluctuations (α2-relaxation). Conductivity decreases with increasing side chain length. Under nanoconfinement in anodic aluminum oxide membranes, phase behavior changes: the Colh–Iso transition is suppressed, and a new α3-relaxation appears, linked to dynamics in an adsorbed interfacial layer. DC conductivity drops by up to four orders of magnitude due to confinement effects, altered molecular orientation, and phase transitions—especially the emergence of a nematic-like state in DOPA16. These findings highlight the importance of molecular design, pore geometry, and surface chemistry in tuning ionic liquid crystal properties for advanced applications in nanofluidics, ion transport, and responsive materials. KW - Ionic Liquid Crystals PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639657 DO - https://doi.org/10.1039/d5cp02406d SN - 1463-9084 SP - 1 EP - 17 PB - Royal Society of Chemistry (RSC) AN - OPUS4-63965 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Szymoniak, Paulina T1 - Bio-Based Vitrimers: Cracking the Code of Recyclability, Exchange Reactions and Flame Retardancy N2 - Vitrimers are a promising class of sustainable materials that offer an alternative to traditional epoxy thermosets in line with circular economy principles. Built on covalent adaptive networks (CANs), they can rearrange their chemical bonds in response to external stimuli, giving them properties like recyclability, shape-memory, and self-healing. These materials combine the strength of thermosets with the reprocessability of thermoplastics, making them attractive for next-generation applications. This study focuses on a bio-based vitrimer made from glycerol triglycidyl ether (GTE) and a vanillin-derived imine hardener (VA), which reacts through catalyst-free imine metathesis. To better understand the recyclability mechanisms of such systems, especially the dynamic bond exchange, we apply a comprehensive suite of techniques including dielectric spectroscopy, neutron scattering, mechanical analysis, and calorimetry. By linking molecular dynamics with macroscopic performance, the work aims to support the development of vitrimers as practical, recyclable materials. T2 - EPF2025 - European Polymer Congress CY - Groningen, The Netherlands DA - 22.06.2025 KW - Polymer recycling PY - 2025 AN - OPUS4-63859 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hülagü, Deniz A1 - Ermilova, Elena A1 - Weise, Matthias A1 - de Préville, Sophie A1 - Hoffmann, Johannes A1 - Morán‐Meza, José A1 - Piquemal, François A1 - Hertwig, Andreas T1 - Multimethod Electrical Characterization of Thin Indium Tin Oxide Films: Structuring and Calibration Sample Development for Scanning Probe Microscopy N2 - Indium tin oxide (ITO), a transparent conductive oxide, is widely used in optoelectronic applications due to its electrical conductivity, optical transparency, and chemical stability. This study employs spectroscopic ellipsometry (SE) to analyze ITO layers, enabling nondestructive determination of film thickness, dielectric functions, and bulk conductivity. Electrical properties derived from SE are compared with those obtained using the four‐point probe method (4PM) to improve metrological tools for nanotechnology applications and optimize deposition process monitoring for better control of film properties. This work also investigates the chemical stability of ITO layers under etching conditions and explores the development of new sheet resistance standards for scanning microwave microscopy (SMM). The results show that ITO resistivity, calculated from fitted SE data, increases with oxygen flow rate up to 5 cm3(STP) min−1. Good agreement is observed between sheet resistance values obtained by SE and 4PM up to 3 cm3(STP) min−1. Additionally, the sheet resistance values of a distinct set of microstructured ITO samples with different ITO layer thicknesses are determined by SMM, which are highly consistent with those obtained by the 4PM. KW - Ellipsometry KW - Indium tin oxide (ITO) KW - Scanning microwave microscopy (SMM) KW - Sheet resistance calibration standards KW - ITO wet etching PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626242 DO - https://doi.org/10.1002/pssa.202400871 SN - 1862-6300 VL - 222 IS - 14 SP - 1 EP - 18 PB - Wiley CY - Hoboken, New Jersey, USA AN - OPUS4-62624 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Szymoniak, Paulina T1 - Nanoscale Confinement Effects in Thin Films of Rigid-Backbone Polymers N2 - Thin polymer films play a crucial role in modern technologies, with applications spanning flexible electronics, membranes, coatings, and nanodevices. Their reduced dimensions result in unique physical behavior, often deviating significantly from bulk properties due to confinement and interfacial effects. In this study, we investigate how nanoscale confinement and polymer–substrate interactions influence the structural and dynamic properties of supported thin films of two rigid-backbone polymers: poly(bisphenol A carbonate) (PBAC) and polysulfone (PSU). Emphasis was placed on the development of adsorbed interfacial layers, molecular mobility, and the glass transition behavior as functions of film thickness and thermal history. Using a multimodal experimental approach—including Atomic Force Microscopy (AFM), Broadband Dielectric Spectroscopy (BDS), Differential and Fast Scanning Calorimetry (DSC, FSC), and Ellipsometry—we characterized adsorption kinetics, desorption processes, and segmental dynamics across a wide range of thicknesses and annealing conditions. Special attention was given to the formation and growth regimes of the adsorbed polymer layers, including a newly observed pre-growth stage, and their effect on thermal and dielectric relaxation behavior. To probe dynamics in ultrathin films, two dielectric electrode configurations—crossed electrode capacitors and nanostructured electrodes—were employed, enabling measurements down to 10 nm and isolated adsorbed layer. This comprehensive analysis provides insight into how one-dimensional confinement and interfacial interactions modulate macromolecular behavior, which is critical for the design of functional nanostructured polymeric systems in advanced applications. T2 - 10th International Discussion Meeting on Relaxations in Complex Systems (10thIDMRCS) CY - Barcelona, Spanien DA - 20.06.2025 KW - Thin films PY - 2025 AN - OPUS4-63858 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 - Strommer, Bettina A1 - Schulze, Dietmar A1 - Schartel, Bernhard A1 - Böhning, Martin T1 - Networking Skills: The Effect of Graphene on the Crosslinking of Natural Rubber Nanocomposites with Sulfur and Peroxide Systems N2 - Tailored crosslinking in elastomers is crucial for their technical applications. The incorporation of nanoparticles with high surface-to-volume ratios not only leads to the formation of physical networks and influences the ultimate performance of nanocomposites, but it also affects the chemical crosslinking reactions. The influence of few-layer graphene (FLG) on the crosslinking behavior of natural rubber is investigated. Four different curing systems, two sulfur-based with different accelerator-to-sulfur ratios, and two peroxide-based with different peroxide concentrations, are combined with different FLG contents. Using differential scanning calorimetry (DSC), vulcametry (MDR) and swelling measurements, the results show an accelerating effect of FLG on the kinetics of the sulfur-based curing systems, with an exothermic reaction peak in DSC shifted to lower temperatures and lower scorch and curing times in the MDR. While a higher accelerator-to-sulfur ratio in combination with FLG leads to reduced crosslinking densities, the peroxide crosslinkers are hardly affected by the presence of FLG. The good agreement of crosslink densities obtained from the swelling behavior confirms the suitability of vulcameter measurements for monitoring the complex vulcanization process of such nanocomposite systems in a simple and efficient way. The reinforcing effect of FLG shows the highest relative improvements in weakly crosslinked nanocomposites. KW - Nanocomposite KW - Elastomers KW - Graphene KW - Crosslinking KW - Network KW - Rubber KW - Vulcanization PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560409 DO - https://doi.org/10.3390/polym14204363 VL - 14 IS - 20 PB - MDPI AN - OPUS4-56040 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 - Kamoun, E. A1 - Afifi, K. A1 - Szymoniak, Paulina A1 - Schönhals, Andreas A1 - Fahmy, Alaa T1 - Structure-property relationship of cross-linked chitosan-ethyl cellulose membranes N2 - Intensive research is focused on creating cost-effective, high-performance polyelectrolyte membranes (PEMs) for electrochemical devices designed to generate and/or store electrical energy. On the other hand, biopolymer materials have been utilized in a wide range of applications across medical and engineering fields, as well as in the textile and energy sectors. Therefore, in this study, chemically cross-linked chito-san/ethyl cellulose-citric acid (CS-EC-CA) membranes were prepared by a casting technique. The structure-property relationship of CS-EC/CA has been discussed based on the molar ratio of CS. The structural properties of the resultant membrane were characterized using Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy, thermal stability was assessed using thermogravimetric analysis. Moreover, the ion exchange capacity (IEC) and water uptake of the membrane were studied. FTIR analysis revealed a significant broadening of absorption peaks in the range of 3200–3500 cm-1 , corresponding to -OH groups, presence of CA. A new peak at 1725 cm-1 confirmed the formation of chemical linkages between CA and CS-EC. The results of the thermal analysis revealed that a thermally stable membrane was obtained when it was chemically cross-linked compared to non-cross-linked membranes. The IEC values of the modified membranes were enhanced significantly, increasing from 0.08 mmol/g for pure CS to 0.5 mmol/g for CS (50%) and 0.8 mmol/g for CS (50%) cross-linked withCA. Furthermore, the cross-linked membranes demonstrated the lowest water and ethanol uptake values, emphasizing their suitability for fuel cell applications. KW - Polyelectrolyte membranes PY - 2025 DO - https://doi.org/10.1063/5.0279022 SN - 1089-7666 VL - 37 IS - 8 SP - 1 EP - 11 PB - AIP Publishing AN - OPUS4-63890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kolmangadi, Mohamed Aejaz T1 - Molecular Dynamics of Janus Polynorbornenes: Glass Transitions and Nanophase separation N2 - We report the dielectric and calorimetric investigations of an homologous series of Janus polynorbornenes with rigid main backbone and flexible -Si(OR)3 side groups, of differing length alkyl chains (R = Propyl, Butyl, Hexyl, Octyl, Decyl). Dielectric dispersion reveals two active processes at low temperatures, denoted as β- and α- relaxation. The former can be assigned to localized fluctuations, whilst the latter relates to the glassy dynamics of the flexible -Si(OR)3 side groups, that creates a nanophase separation in both the alkyl chain rich and backbone rich domains. Temperature modulated DSC measurements and X-ray scattering experiment confirm the nanophase separation. Fast Scanning Calorimetry employing both fast heating and cooling rates detects the glass transition temperatures of the backbone rich domains, which are beyond or near to their degradation temperatures in terms of conventional DSC. The cooperative length scale of glass transition and the size of the alkyl chain rich domains increases with chain length. Alongside these results, a significant conductivity contribution was observed for all Poly(tricyclononenes) with Si(OR)3 side groups, which is interpreted in terms of a percolation model. T2 - Chemical Engg Seminar CY - Columbia University, NY, USA DA - 14.03.2023 KW - Glass transition KW - Conductivity KW - Fast Scanning Calorimetry KW - Dynamics PY - 2023 AN - OPUS4-57343 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT ED - Tuma, Dirk ED - Weide, T. ED - Rasmusson, H. T1 - MefHySto - Metrology for advanced hydrogen storage solutions N2 - The “Metrology for Advanced Hydrogen Storage Solutions” (MefHySto) project is a European initiative addressing the need for large-scale energy storage solutions, that is crucial for the successful transition to renewable energy sources. The main objective of this project was to develop and provide metrological standards and validated techniques for the storage and utilization of hydrogen. Hydrogen is increasingly recognized as an important component in the future energy system due to its ability to store and supply energy during peak demand periods when renewable sources, such as solar and wind, are not generating power. KW - Water electrolysis KW - Thermophysical properties KW - Fuel cell KW - Hydrogen storage PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625952 DO - https://doi.org/10.5281/zenodo.12684898 SP - 1 EP - 40 PB - ERIG European Research Institute for Gas and Energy Innovation a.i.s.b.l. CY - Bruxelles AN - OPUS4-62595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pu, Y. A1 - Lawrence, M. J. A1 - Celorrio, V. A1 - Wang, Q. A1 - Gu, M. A1 - Sun, Z. A1 - Agudo Jácome, Leonardo A1 - Russell, A. E. A1 - Huang, L. A1 - Rodriguez, P. T1 - Nickel confined in 2D earth-abundant oxide layers for highly efficient and durable oxygen evolution catalysts N2 - Low cost, high-efficiency catalysts towards water splitting are urgently required to fulfil the increasing demand for energy. In this work, low-loading (<20 wt%) Ni-confined in layered metal oxide anode catalysts (birnessite and lepidocrocite titanate) have been synthesized by facile ion exchange methodology and subjected to systematic electrochemical studies. It was found that Ni-intercalated on K-rich birnessite (Ni-KMO) presents an onset overpotential (ηonset) as low as 100 mV and overpotential at 10 mA cm−2 (η10) of 206 mV in pH = 14 electrolyte. By combining electrochemical methods and X-ray absorption and emission spectroscopies (XAS and XES), we demonstrate Ni sites are the active sites for OER catalysis and that the Mn3+ sites facilitate Ni intercalation during the ion-exchange process, but display no observable contribution towards OER activity. The effect of the pH and the nature of the supporting electrolyte on the electrochemical performance was also evaluated. KW - Confined catalyst KW - Low-loading KW - Layered manganese oxide KW - Oxygen evolution reaction KW - Transmission electron microscopy (TEM) PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515027 DO - https://doi.org/10.1039/D0TA04031B SN - 2050-7496 SN - 2050-7488 VL - 8 IS - 26 SP - 13340 EP - 13350 PB - Royal Society of Chemistry CY - London AN - OPUS4-51502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Weinel, Kristina A1 - Hahn, Marc Benjamin A1 - Lubk, Axel A1 - Feng, Wen A1 - Martinez, Ignacio Gonzalez A1 - Büchner, Bernd A1 - Agudo Jácome, Leonardo T1 - Electron-beam-induced modification of gold microparticles in an SEM N2 - Electron-beam-induced conversion of materials in a transmission electron microscope uses the high power density of a localized electron beam of acceleration voltages above 100 kV as an energy source to transform matter at the sub-micron scale. Here, the e-beam-induced transformation of precursor microparticles employing a low-energy e-beam with an acceleration voltage of 30 kV in a scanning electron microscope is developed to increase the versatility and efficiency of the technique. Under these conditions, the technique can be classified between e-beam lithography, where the e-beam is used to mill holes in or grow some different material onto a substrate, and e-beam welding, where matter can be welded together when overcoming the melting phase. Modifying gold microparticles on an amorphous SiOx substrate reveals the dominant role of inelastic electron-matter interaction and subsequent localized heating for the observed melting and vaporization of the precursor microparticles under the electron beam. Monte-Carlo scattering simulations and thermodynamic modeling further support the findings. KW - Scanning electron microscopy KW - Electron-beam-induced modification KW - Heat transfer KW - Gold microparticles KW - Nanoparticles synthesis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-609513 UR - https://arxiv.org/html/2408.02409v1 SP - 1 EP - 9 AN - OPUS4-60951 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Feng, Wen A1 - Gemming, Thomas A1 - Giebeler, Lars A1 - Qu, Jiang A1 - Weinel, Kristina A1 - Agudo Jácome, Leonardo A1 - Büchner, Bernd A1 - González-Martínez, Ignacio T1 - Influence of magnetic field on electron beam-induced Coulomb explosion of gold microparticles in transmission electron microscopy N2 - In this work we instigated the fragmentation of Au microparticles supported on a thin amorphous carbon film by irradiating them with a gradually convergent electron beam inside the Transmission Electron Microscope. This phenomenon has been generically labeled as “electron beam-induced fragmentation” or EBIF and its physical origin remains contested. On the one hand, EBIF has been primarily characterized as a consequence of beam-induced heating. On the other, EBIF has been attributed to beam-induced charging eventually leading to Coulomb explosion. To test the feasibility of the charging framework for EBIF, we instigated the fragmentation of Au particles under two different experimental conditions. First, with the magnetic objective lens of the microscope operating at full capacity, i.e. background magnetic field B = 2 T, and with the magnetic objective lens switched off (Lorenz mode), i.e. B = 0 T. We observe that the presence or absence of the magnetic field noticeably affects the critical current density at which EBIF occurs. This strongly suggests that magnetic field effects play a crucial role in instigating EBIF on the microparticles. The dependence of the value of the critical current density on the absence or presence of an ambient magnetic field cannot be accounted for by the beam-induced heating model. Consequently, this work presents robust experimental evidence suggesting that Coulomb explosion driven by electrostatic charging is the root cause of EBIF. KW - Electron beam-induced fragmentation KW - Coulomb explosion KW - X-ray diffraction KW - Lorenz transmission electron microscopy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600247 DO - https://doi.org/10.1016/j.ultramic.2024.113978 SN - 1879-2723 VL - 262 SP - 1 EP - 8 PB - Elsevier CY - Amsterdam AN - OPUS4-60024 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Straße, Anne T1 - Preliminary study to investigate the applicability of optical strain measurement technique for the detection of hot cracks in laser metal deposited layers N2 - Laser metal deposition (LMD) as an additive manufacturing technique became increasingly important in recent years and thus the demand for component safety. This is the reason, for the need for reliable in-situ defect detection techniques. For laser beam weld seams an optical measurement technique based on an optical flow algorithm was successfully used to define the critical straining conditions that lead to hot cracking. This algorithm was adapted for bead-on-plate weld seams on LMD deposited layers of IN718 alloy while performing external strain on the specimen in an externally loaded hot cacking test facility. The resulting transversal hot cracks along the weld seam were localized via X-Ray inspection and the type of cracking confirmed by Scanning Electron Microscopy (SEM). The strain distribution was measured in the vicinity of the solidification front and correlated to the detected hot cracks. Based on the results this technique could be adopted for LMD experiments. T2 - 12th CIRP Conference on Photonic Technologies [LANE 2022] CY - Fürth, Germany DA - 04.09.2022 KW - Strain measurement KW - Optical flow KW - Laser Metal Deposition (LMD) KW - Critical strain PY - 2022 AN - OPUS4-55642 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nicolai, Marcel A1 - Bulling, Jannis A1 - Narayanan, M.M. A1 - Zeipert, Henning A1 - Prager, Jens A1 - Henning, Bernd T1 - Dynamic interface behavior in coupled plates: Investigating Lamb wave mode repulsion with a spring-based model N2 - This study investigates the phenomenon of mode repulsion in Lamb waves propagating through two coupled plates with an elastic interface. Using a spring-based coupling model and the Scaled Boundary Finite Element Method, the dispersion curves of the coupled system are analyzed under various interface conditions—weak coupling, sliding boundary, and perfect coupling. This research highlights how the mechanical stiffness of the interface influences the separation of modes and the emergence of repulsion regions. A novel focus on interface displacements reveals a unique dynamic behavior within the repulsion regions, driven by in-phase and out-of-phase oscillations of the coupled plates. The findings provide a physically grounded explanation of mode repulsion, linking it to the strain patterns in the interface. This insight lays the theoretical groundwork for future applications in material characterization and non-destructive evaluation, enabling more precise selection of Lamb wave modes for scientific and industrial purposes. KW - Lamb waves KW - Mode repulsion KW - Coupled plates KW - Elastic interface KW - Dispersion curves PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-642245 DO - https://doi.org/10.1016/j.ultras.2025.107799 SN - 0041-624X VL - 158 SP - 1 EP - 9 PB - Elsevier BV AN - OPUS4-64224 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nicolai, Marcel T1 - Investigating Lamb wave mode repulsion with a spring-based model N2 - Lamb waves are widely utilized in material characterization, non-destructive testing (NDT), and structural health monitoring (SHM). A unique feature of Lamb waves is mode repulsion, where dispersion curves approach each other but do not cross. This phenomenon is observed in both single and multilayer plates and is influenced by wave coupling. While mode repulsion in single plates has been linked to symmetry-breaking effects, its underlying mechanism in multilayer systems remains unclear. This study investigates mode repulsion in a coupled aluminum-polycarbonate plate system using a spring-based interface model. Dispersion curves are computed via the Scaled Boundary Finite Element Method, and time-domain simulations are used to analyze the interface dynamics. Results indicate that repulsion depends on interface stiffness, distinguishing between opening and closing repulsion regions. The study further reveals that mode repulsion corresponds to distinct oscillatory behaviors in the interface, where certain wave modes induce increased coupling spring elongation, leading to localized strain. A coupled harmonic oscillator model effectively explains opening repulsion regions but does not fully capture closing regions. Findings suggest that mode repulsion could be leveraged for non-destructive evaluation of adhesive interfaces, offering insights into bond strength characterization. This research contributes to a deeper understanding of wave interactions in multilayer structures and provides a theoretical foundation for advancing NDT and SHM techniques. T2 - ICU2025 - International Congress on Ultrasonics 2025 CY - Paderborn, Germany DA - 21.09.2025 KW - Lamb waves KW - Mode repulsion KW - Coupled plates KW - Dispersion curves KW - Elastic Interfaces PY - 2025 AN - OPUS4-64225 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Przyklenk, A. A1 - Balsamo, A. A1 - O'Connor, D. A1 - Evans, Alexander A1 - Yandayan, T. A1 - Akgöz, S. A1 - Flys, O. A1 - Zeleny, V. A1 - Czułek, D. A1 - Meli, F. A1 - Ragusa, C. A1 - Bosse, H. T1 - New European Metrology Network for advanced manufacturing N2 - Advanced manufacturing has been identified as one of the key enabling technologies with applications in multiple industries. The growing importance of advanced manufacturing is reflected by an increased number of publications on this topic in recent years. Advanced manufacturing requires new and enhanced metrology methods to assure the quality of manufacturing processes and the resulting products. However, a high-level coordination of the metrology community is currently absent in this field and consequently this limits the impact of metrology developments on advanced manufacturing. In this article we introduce the new European Metrology Network (EMN) for Advanced Manufacturing within EURAMET, the European Association of National Metrology Institutes (NMIs). The EMN is intended to be operated sustainably by NMIs and Designated Institutes in close cooperation with Stakeholders interested in advanced manufacturing. The objectives of the EMN are to set up a permanent stakeholder dialogue, to develop a Strategic Research Agenda for the metrology input required for advanced manufacturing technologies, to create and maintain a knowledge sharing programme and to implement a web-based service desk for stakeholders. The EMN development is supported by a Joint Network Project within the European Metrology Programme for Innovation and Research. KW - Stakeholder KW - Advanced manufacturing KW - Metrology KW - European Metrology Networks (EMNs) KW - Strategic Research Agenda (SRA), PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-530618 DO - https://doi.org/10.1088/1361-6501/ac0d25 VL - 32 IS - 11 SP - 111001 PB - IOP Publishing AN - OPUS4-53061 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Azimzada, Agil A1 - Meermann, Björn T1 - AF4/ICP-ToF-MS for the investigation of species-specific adsorption of organometallic contaminants on natural colloidal particles N2 - Organotin (OT) compounds, while crucial in many industrial applications, pose substantial risks to the environment and human health. The toxicity and environmental behaviour of OTs depend on their chemical form, i.e., the type and number of organic substituents. Each species thus exhibits distinct toxicity profiles and varying binding affinities to environmental colloids, which influence their mobility, bioavailability, and environmental impacts. To date, however, most studies addressed speciation and colloidal characterization separately, leaving the combined determinations of organometallics along with their carrier colloids largely elusive. Here, we develop and validate an on-line measurement system to quantify the adsorption dynamics of 10 OT species on natural colloidal particles (<500 nm). The approach integrates a versatile fractionation technique (AF4), with a state-of-the-art multi-element analyzer (ICP-ToF-MS), achieving Sn detection limits as low as 6.0 ng/L. The method separates colloid-free OT species from those bound to colloids and enables the determination of OT interactions with distinct colloidal fractions. Validated in both fractionation and detection, the method provides reliable data that could elucidate the species-specific and temporal aspects of species-colloids adsorption processes. The results feature comparative studies of 10 OT species, offering critical insights into OT mobility and distribution in environmental systems. KW - Fractionation KW - Speciation KW - Adsorption KW - Colloids KW - Organotin KW - AF4 KW - Nanoparticle characterization PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625244 DO - https://doi.org/10.1016/j.jhazmat.2025.137320 SN - 1873-3336 VL - 488 SP - 1 EP - 11 PB - Elsevier B.V. AN - OPUS4-62524 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Monavari, Mahshid A1 - Homaeigohar, Shahin A1 - Medhekar, Rucha A1 - Nawaz, Qaisar A1 - Monavari, Mehran A1 - Zheng, Kai A1 - Boccaccini, Aldo R. T1 - A 3D-Printed Wound-Healing Material Composed of Alginate Dialdehyde–Gelatin Incorporating Astaxanthin and Borate Bioactive Glass Microparticles N2 - In this study, a wound dressing composed of an alginate dialdehyde−gelatin (ADA-GEL) hydrogel incorporated by astaxanthin (ASX) and 70B (70:30 B2O3/CaO in mol %) borate bioactive glass (BBG) microparticles was developed through 3D printing. ASX and BBG particles sti.ened the composite hydrogel construct and delayed its in vitro degradation compared to the pristine hydrogel construct, mainly due to their cross-linking role, likely arising from hydrogen bonding between the ASX/BBG particles and ADA-GEL chains. Additionally, the composite hydrogel construct could hold and deliver ASX steadily. The composite hydrogel constructs codelivered biologically active ions (Ca and B) and ASX, which should lead to a faster, more e.ective wound-healing process. As shown through in vitro tests, the ASX-containing composite hydrogel promoted fibroblast (NIH 3T3) cell adhesion, proliferation, and vascular endothelial growth factor expression, as well as keratinocyte (HaCaT) migration, thanks to the antioxidant activity of ASX, the release of cell-supportive Ca2+ and B3+ ions, and the biocompatibility of ADA-GEL. Taken together, the results show that the ADA-GEL/BBG/ASX composite is an attractive biomaterial to develop multipurposed wound-healing constructs through 3D printing. KW - General Materials Science PY - 2023 DO - https://doi.org/10.1021/acsami.2c23252 SP - 1 EP - 12 PB - American Chemical Society (ACS) AN - OPUS4-58548 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Engelhard, Carsten T1 - On ICP-MS with Nanosecond Time Resolution: From Nanoparticles to Microplastics N2 - In this presentation, recent developments in inductively coupled plasma mass spectrometry (ICP-MS) instrumentation for particle characterization in complex mixtures will be reviewed. The current state-of-the-art in single-particle (sp) ICP-MS instrumentation for the detection and characterization of nanoparticles (NP) and microplastics (MPs) as well as remaining challenges will be discussed. While millisecond dwell times were used in the advent of spICP-MS, the use of microsecond dwell times helped to improve nanoparticle data quality and particle size detection limits. We could show that a custom-built high-speed data acquisition unit with microsecond time resolution (μsDAQ) can be used to successfully address issues of split-particle events and particle coincidence, to study the temporal profile of individual ion clouds, and to extend the linear dynamic range by compensating for dead time related count losses. Our latest development is an in-house built data acquisition system with nanosecond time resolution (nanoDAQ). Recording of the SEM signal by the nanoDAQ is performed on the nanosecond time scale with a dwell time of approximately 2 ns and enables detection of gold nanoparticles (AuNP) as small as 7.5 nm with a commercial single quadrupole ICP-MS instrument. [1] Analysis of acquired transient data is based on the temporal distance between detector events and a derived ion event density. It was shown that the inverse logarithm of the distance between detector events is proportional to particle size. Also, the number of detector events per particle can be used to calibrate and determine the particle number concentration (PNC) of a nanoparticle dispersion. In addition to inorganic nanoparticles, first results on the detection of microplastics with spICP-MS will be discussed. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Nano KW - Microplastics KW - Nanoparticle Characterization KW - ICP-MS KW - Instrumentation PY - 2025 AN - OPUS4-63580 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Engelhard, Carsten T1 - From Particles to PFAS: Recent Advances in Plasma-based Instrumentation Development N2 - In this presentation, recent advances in plasma spectrochemistry with hot and cold plasma sources for the direct detection of nanoparticles as well as per- and polyfluoroalkyl substances (PFAS) will be discussed. In the first part, single-particle inductively coupled plasma mass spectrometry (spICP-MS) with an in-house built data acquisition system with nanosecond time resolution (nanoDAQ) will be presented. In the second part, we turn to a cooler plasma source. Specifically, a flowing atmospheric-pressure afterglow source (FAPA) and its application for the direct mass spectrometric analysis of PFAS will be discussed. T2 - 20th European Winter Conference on Plasma Spectrochemistry CY - Berlin, Germany DA - 02.03.2025 KW - ICP-MS KW - Instrumentation KW - Nano KW - Nanoparticle Characterization KW - PFAS PY - 2025 AN - OPUS4-63581 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmitt, Johannes T1 - Data acquisition system for single particle inductively coupled plasma mass spectrometry (spICP-MS) with nanosecond time resolution N2 - This study presents our data acquisition system prototype for single particle inductively coupled plasma mass spectrometry (spICP-MS) with nanosecond time resolution (nanoDAQ) and a matching data processing approach for time-resolved data in the nanosecond range. The system continuously samples the secondary electron multiplier (SEM) detector signal with a dwell time of approximately 2 ns and enables detection of gold nanoparticles (AuNP) as small as 7.5 nm with a commercial single quadrupole ICP-MS instrument. [1] Analysis of acquired transient data is based on the temporal distance between detector events and a derived ion event density. It was shown that the inverse logarithm of the distance between detector events is proportional to particle size. Also, the number of detector events per particle can be used to calibrate and determine the particle number concentration (PNC) of a nanoparticle dispersion. [1] Particle-by-particle-based analysis of ion event density and other parameters derived from nanosecond time resolution show promising results. High data acquisition frequency of the systems allows recording of a statistically significant number of data points in 60 s or less, which leaves only the sample uptake and rinsing steps as remaining factors for limiting the total measurement time. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - ICP-MS KW - Instrumentation KW - Nano KW - Nanoparticle Characterization PY - 2025 AN - OPUS4-63603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Favres, Georges T1 - European Metrology Network (EMN) for Advanced Manufacturing N2 - The European Commission has identified Advanced Manufacturing and Advanced Materials as two of six Key Enabling Technologies (KETs). By fully utilizing these KETs, advanced and sustainable economies will be created. It is considered that Metrology is a key enabler for the advancement of these KETs. EURAMET, the association of metrology institutes in Europe, has strengthened the role of Metrology for these KETs by enabling the creation of a European Metrology Network for Advanced Manufacturing. The EMN is made up of National Metrology Institutes (NMIs) and Designated Institutes (DIs) from across Europe and was formally established in October 2021. The EMN aims to provide a high-level coordination of European metrology activities for the Advanced Materials and Advanced Manufacturing community. The EMN itself is organized in three sections representing the major stages of the manufacturing chain: 1) Advanced Materials, 2) Smart Manufacturing Systems, and 3) Manufactured Components & Products. The EMN for Advanced Manufacturing is engaging with stakeholders in the field of Advanced Manufacturing and Advanced Materials (Large companies & SMEs, industry organisations, existing networks, and academia), as well as the wider metrology community (including TCs) to provide input for the preparation of a Strategic Research Agenda (SRA) for Metrology for Advanced Manufacturing. This presentation will describe the progress in the development of the SRA by the EMN for Advanced Manufacturing. The metrology challenges identified across the various key industrial sectors, which utilise Advanced Materials and Advanced Manufacturing will be presented. The EMN for Advanced Manufacturing is supported by the project JNP 19NET01 AdvManuNet. T2 - 21st International Metrology Congress, CIM 2023 CY - Lyon (Chassieu), France DA - 07.03.2023 KW - Advanced Materials KW - EMN KW - European Metrology Network for Advanced Manufacturing, Strategic Research Agenda KW - SRA PY - 2023 AN - OPUS4-59208 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - O'Connor, Daniel A1 - Evans, Alexander A1 - Balsamo, Alessandro A1 - Favres, Georges A1 - Przyklenk, Anita A1 - Bosse, Harald A1 - Phillips, Dishi T1 - European Metrology Network (EMN) for Advanced Manufacturing ─ Development of the Strategic Research Agenda (SRA) N2 - The European Commission has identified Advanced Manufacturing and Advanced Materials as two of six Key Enabling Technologies (KETs). It is considered that Metrology is a key enabler for the advancement of these KETs. Consequently, EURAMET, the association of metrology institutes in Europe, has strengthened the role of Metrology for these KETs by enabling the creation of a European Metrology Network (EMN) for Advanced Manufacturing. The EMN is comprised of National Metrology Institutes (NMIs) and Designated Institutes (DIs) from across Europe and was formally established in October 2021. The aim of the EMN is to provide a high-level coordination of European metrology activities for the Advanced Manufacturing community. The EMN itself is organized in three sections representing the major stages of the manufacturing chain: 1) Advanced Materials, 2) Smart Manufacturing Systems, and 3) Manufactured Components & Products. The EMN for Advanced Manufacturing is engaging with stakeholders in the field of Advanced Manufacturing (large companies & SMEs, industry organisations, existing networks, and academia), as well as the wider Metrology community, including Technical Committees, to provide input for the Strategic Research Agenda (SRA) on Metrology for Advanced Manufacturing. This contribution will give an overview about the first version of the SRA prepared by the EMN for Advanced Manufacturing T2 - Euspen, 23rd International Conference & Exhibitio CY - Copenhagen, Danmark DA - 12.06.2023 KW - European Metrology Network (EMN) KW - Advanced Manufacturing KW - Metrology KW - Strategic Research Agenda (SRA) PY - 2023 SP - 363 EP - 364 AN - OPUS4-59196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Characterization of hydrogen trapping in a CoCrFeMnNi high-entropy alloy charged up to 1000 bar high-pressure hydrogen N2 - First studies on the mechanical behavior of high-entropy alloys (HEAs) in high-pressure hydrogen environment are available. In contrast, the underlying hydrogen absorption, diffusion and trapping in these HEAs like the Cantor-alloy was less in the scientific scope so far. For that reason, the CoCrFeMnNi-HEA was compared to a conventional AISI 316L austenitic steel, by exposing to high-pressure hydrogen charging at 200 bar and very-high pressure at 1,000 bar. Thermal desorption analysis (TDA) was applied with different heating rates (0.125 K/s to 0.500 K/s), see Fig. 1a to d. The underlying TDA spectra were analyzed in terms of a reasonable peak deconvolution to into a defined number of peaks and the calculation of the activation energies for the respective and predominant hydrogen trap sites. Both materials show a comparable hydrogen diffusivity. The obtained activation energies suggest that in case of the CoCrFeMnNi-HEAs an interaction of the austenitic phase as well as the direct atomic bonding of hydrogen to the metal atoms are the dominant traps, since “impurities” such as carbides or inclusions are only present in trace amounts. Available literature suggests that the Cr and Mn-content is here of special interest for the direct hydrogen bonding at solute atoms. In addition, the trap occupancy rate must be considered in terms of a pressure-related hydrogen absorption. The derived apparent hydrogen solubility was in the order: 316L < CoCrFeMnNi-HEA for both charging pressures. Especially, the 1,000 bar values lead to noteworthy results with > 70 wt.ppm for the AISI 316L and >130 wt.ppm for the CoCrFeMnNi. In fact, both the hydrogen diffusion and trapping data on gaseous high-pressure hydrogen charged HEAs are rare so far. The results of the present study allow a deeper understanding of hydrogen trapping in the regarded CoCrFeMnNi-system. T2 - 78th IIW Annual Assembly and International Conference CY - Genoa, Italy DA - 26.06.2025 KW - Hydrogen KW - Thermal desorption analysis KW - High-pressure charging KW - Trapping KW - Diffusion PY - 2025 AN - OPUS4-63542 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schilling, Markus T1 - Data-Driven Materials Science: Reproducibility and Standardization N2 - Advancing development and digitalization in materials science requires to focus on quality assurance, interoperability, and compliance with FAIR principles. Semantic technologies offer effective solutions for these challenges by enabling the storage, processing, and contextualization of data in machine-actionable and human-readable formats – essential for robust data management. This presentation highlights the PMD Core Ontology 3.0 (PMDco 3.0), developed specifically for the field of materials science and engineering, and its implementation within generic knowledge representation frameworks. Demonstrators such as standardized mechanical testing, material processing workflows, and the Orowan Demonstrator exemplify the ontology’s practical applications. The use of graph patterns, able to be compiled into rule-based semantic shapes, supports a unified and automated approach to managing heterogeneous experimental data across domains. T2 - Persson Group Seminar CY - Berkeley, CA, USA DA - 23.06.2025 KW - Semantic Data KW - Data Integration KW - Digitalization KW - Data Interoperability KW - PMD Core Ontology KW - Graph Patterns PY - 2025 AN - OPUS4-63484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Monavari, M. A1 - Homaeigohar, S. A1 - Fuentes-Chandía, M. A1 - Nawaz, Q. A1 - Monavari, Mehran A1 - Venkatraman, A. A1 - Boccaccini, A. T1 - 3D printing of alginate dialdehyde-gelatin (ADA-GEL) hydrogels incorporating phytotherapeutic icariin loaded mesoporous SiO2-CaO nanoparticles for bone tissue engineering N2 - 3D printing enables a better control over the microstructure of bone restoring constructs, addresses the challenges seen in the preparation of patient-specific bone scaffolds, and overcomes the bottlenecks that can appear in delivering drugs/growth factors promoting bone regeneration. Here, 3D printing is employed for the fabrication of an osteogenic construct made of hydrogel nanocomposites. Alginate dialdehyde-gelatin (ADA-GEL) hydrogel is reinforced by the incorporation of bioactive glass nanoparticles, i.e. mesoporous silica-calcia nanoparticles (MSNs), in two types of drug (icariin) loading. The composites hydrogel is printed as superhydrated composite constructs in a grid structure. The MSNs not only improve the mechanical stiffness of the constructs but also induce formation of an apatite layer when the construct is immersed in simulated body fluid (SBF), thereby promoting cell adhesion and proliferation. The nanocomposite constructs can hold and deliver icariin efficiently, regardless of its incorporation mode, either as loaded into the MSNs or freely distributed within the hydrogel. Biocompatibility tests showed that the hydrogel nanocomposites assure enhanced osteoblast proliferation, adhesion, and differentiation. Such optimum biological properties stem from the superior biocompatibility of ADA-GEL, the bioactivity of the MSNs, and the supportive effect of icariin in relation to cell Proliferation and differentiation. Taken together, given the achieved structural and biological properties and effective drug delivery capability, the hydrogel nanocomposites show promising potential for bone tissue engineering. KW - 3D printed hydrogel KW - ADA-GEL KW - Drug delivery KW - Mesoporous SiO2-CaO nanoparticles KW - Bone tissue engineering PY - 2021 DO - https://doi.org/10.1016/j.msec.2021.112470 VL - 131 SP - 1 EP - 11 PB - Elsevier B.V. AN - OPUS4-53848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Evans, Alexander T1 - The European Metrology Network (EMN) for Advanced Manufacturing N2 - Advanced Manufacturing and Advanced Materials have been identified by the European Commission as one of six Key Enabling Technologies (KETs), the full exploitation of which will create advanced and sustainable economies. Metrology is a key enabler for progress of these KETs. EURAMET, which is the association of metrology institutes in Europe, has addressed the vital importance of Metrology for these KETs through the support for the creation of a European Metrology Network for Advanced Manufacturing. The EMN for Advanced Manufacturing (AdvanceManu) was approved in June 2021 and held the formal kick-of meeting in October 2022. The EMN comprises both National Metrology Institutes (NMIs) from across Europe and other designated Institutes (Dis). The EMN is organized in three sections; Advanced Materials, Smart Manufacturing Systems and Manufactured components and products. The aim of the EMN is to engage with stakeholders in the field of Advanced Manufacturing and Advanced Materials (Large & SMEs, industry organisations, existing networks and academia) with the aim to prepare a Strategic Research Agenda (SRA) for Metrology for Advanced Manufacturing. In the shorter term, an orientation paper is aimed to be produce to in the context of the European Partnership for Metrology. In addition to the SRA, the EMN will establish knowledge and technology transfer and promotion plan. This includes leveraging the existing research results from the completed and running EMPIR JRP projects funded through EURAMET. This presentation will outline the EMN for Advanced Manufacturing, describing the structures and goals, the route to the production of the SRA and the progress made to date identifying the key metrology challenges across the related Key Industrial Sectors (KICs). In particular, the presentation aims to inform the community on how to be involved in the shaping of the strategic research agenda for the future of Metrology for Advanced Manufacturing and Advanced Materials. T2 - 3D Metrology Conference (3DMC) CY - Online meeting DA - 08.11.2021 KW - Advanced manufacturing KW - Metrology KW - European Metrology Network (EMN) KW - Strategic Research Agenda (SRA) KW - JNP PY - 2021 AN - OPUS4-54099 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Przyklenk, A. T1 - Progress of the European Metrology Network for Advanced Manufacturing N2 - The European Metrology Network (EMN) for Advanced Manufacturing has been established in June 2021. Currently nine EMNs focussing on different important topics of strategic importance for Europe exist and form an integral part of EURAMET, the European Association of National Metrology Institutes (NMI). EMNs are tasked to ▪ develop a high-level coordination of the metrology community in Europe in a close dialogue with the respective stakeholders (SH) ▪ develop a strategic research agenda (SRA) within their thematic areas ▪ provide contributions to the European Partnership on Metrology research programme Based on the analysis of existing metrology infrastructures and capabilities of NMIs, the metrology research needs for advanced manufacturing are identified in close cooperation with academic, governmental and industrial stakeholders. Here, we report on the progress of the EMN for Advanced Manufacturing. T2 - Euspen 22nd International Conference & Exhibition (Euspen 2022) CY - Genf, Switzerland DA - 30.05.2022 KW - JNP AdvManuNet KW - Metrology KW - Advanced manufacturing KW - European Metrology Network KW - EMN PY - 2022 AN - OPUS4-55805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sprachmann, J. A1 - Grabicki, N. A1 - Möckel, Anna A1 - Maltitz, J. A1 - del Refugio Monroy Gómez, J. A1 - Smales, Glen Jacob A1 - Dumele, O. T1 - Substituted Benzophenone Imines for COF Synthesis via Formal Transimination N2 - Covalent organic frameworks (COFs) are a prominent class of organic materials constructed from versatile building blocks via reversible reactions. The quality of imine-linked COFs can be improved by using amine monomers protected with benzophenone forming benzophenone imines. Here, we present a study on substituted benzophenones in COF synthesis via formal transimination. 12 para-substituted N-aryl benzophenone imines, with a range of electron-rich to electron-poor substituents, were prepared and their hydrolysis kinetics were studied spectroscopically. All substituted benzophenone imines can be employed in COF synthesis and lead to COFs with high crystallinity and high porosity. The substituents act innocent to COF formation as the substituted benzophenones are cleaved off. Imines can be tailored to their synthetic demands and utilized in COF formation. This concept can make access to previously unattainable, synthetically complex COF monomers feasible. KW - Materials Chemistry KW - Metals and Alloys KW - Surfaces, Coatings and Films KW - General Chemistry KW - Ceramics and Composites KW - Electronic, Optical and Magnetic Materials KW - Catalysis PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586449 DO - https://doi.org/10.1039/D3CC03735E SN - 1359-7345 SP - 1 EP - 4 PB - Royal Society of Chemistry (RSC) AN - OPUS4-58644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dal Molin, E. S. A1 - Henning, L. M. A1 - Müller, J. T. A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Bekheet, M. F. A1 - Gurlo, A. A1 - Simon, U. T1 - Robocasting of ordered mesoporous silica‐based monoliths: Rheological, textural, and mechanical characterization N2 - Hierarchically porous, high‐surface‐area silica materials are excellent candidates for multiple applications like catalysis and environmental remediation. Shaping these materials with additive manufacturing (AM) techniques, like robocasting, could enable their use with the benefit of on‐demand, customized shaping and maximizing performance. Herein, ordered mesoporous silica COK‐12 slurries were robocasted into monoliths, containing different ratios of uncalcined COK‐12 and sodium bentonite (0–25 wt.%). The rheology of the mixed slurries is characterized by lower flow indexes (0.69 vs. 0.32) and higher yield stresses (96 vs. 259 Pa) compared to pure COK‐12 ones. Monoliths were printed in woodpile structures and calcined at 600°C. Micro‐CT measurements showed a linear shrinkage of 25% after calcination. Mechanical characterization showed increased uniaxial strength (0.20 ± 0.07 to 1.0 ± 0.3 MPa) with increasing binder/solids ratio from 13 to 25%. The amorphous, mesoporous structure of COK‐12 was retained. The structures exhibited open porosities of 52 ± 4% and showed higher specific mesopore volumes, and increased average mesopore size (6 vs. 8 nm) compared to COK‐12. Small‐angle x‐ray scattering analysis revealed an increased lattice parameter (10.3 vs. 11.0 nm) and reduced wall thickness (3.1 nm vs. 4.1 nm) of the COK‐12 in the monoliths. These properties indicate suitability for their application as porous supports and adsorbents. KW - Industrial and Manufacturing Engineering KW - Additive manufacturing KW - OMS KW - Porous materials KW - Robocasting KW - X-ray scattering KW - MOUSE PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-582503 DO - https://doi.org/10.1002/nano.202300109 VL - 4 IS - 11-12 SP - 615 EP - 631 PB - Wiley-VCH GmbH AN - OPUS4-58250 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hayward, E. C. A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Takeguchi, M. A1 - Kulak, A. A1 - Hunter, R. D. A1 - Schnepp, Z. T1 - The effect of catalyst precursors on the mechanism of iron-catalysed graphitization of cellulose N2 - Iron-catalysed graphitization of biomass is a simple and sustainable route to carbons with high graphitic content. It uses abundant precursors and moderate processing temperatures and generates carbons with high porosity. Recently, it has been demonstrated that the choice of biomass precursor can have a significant impact on the textural and compositional properties of the resulting carbon. In this paper, we demonstrate that the choice of catalyst is also critical to the carbon structure. Aqueous iron(III) nitrate and iron(III) chloride convert cellulose to carbons with very different textural properties. This is due to the choice of iron catalyst changing the mechanism of cellulose decomposition and also the nature of the active graphitization catalyst. KW - Catalyst KW - Carbon materials KW - Cellulose KW - Small-angle scattering KW - Green energy KW - Graphitic carbon KW - Green synthesis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-614800 DO - https://doi.org/10.1039/D4SU00365A SP - 1 EP - 10 PB - Royal Society of Chemistry (RSC) AN - OPUS4-61480 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hallier, Dorothea C. A1 - Smales, Glen Jacob A1 - Seitz, H. A1 - Hahn, Marc Benjamin T1 - Bio-SAXS of single-stranded DNA-binding proteins: Radiation protection by the compatible solute ectoine N2 - Small-angle X-ray scattering (SAXS) can be used for structural determination of biological macromolecules and polymers in their native states (e.g. liquid phase). This means that the structural changes of (bio-)polymers, such as proteins and DNA, can be monitored in situ to understand their sensitivity to changes in chemical environments. In an attempt to improve the reliability of such experiments, the reduction of radiation damage occurring from exposure to X-rays is required. One such method, is to use scavenger molecules to protect macromolecules against radicals produced during radiation exposure, such as reactive oxygen species (ROS). In this study we investigate the feasibility of applying the compatible solute, osmolyte and radiation protector Ectoine (THP(B)), as a scavenger molecule during SAXS measurements of the single-stranded DNA-binding protein Gene-V Protein (G5P/GVP). In this case, we monitor the radiation induced changes of G5P during bio-SAXS measurments and the resulting microscopic energy-damage relation was determined from microdosimetric calculations by Monte-Carlo based particle scattering simulations with TOPAS/Geant4 and a custom target-model. This resulted in a median-lethal energy deposit of pure G5P at 4 mg mL−1 of E1/2 = 7 ± 5 eV, whereas a threefold increase of energy-deposit was needed under the presence of Ectoine to reach the same level of damage. This indicates that Ectoine increases the possible exposure time before radiation-damage to G5P is observed. Furthermore, the dominant type of damage shifted from aggregation in pure solutions towards a fragmentation for solutions containing Ectoine as a cosolute. These results are interpreted in terms of indirect radiation damage by reactive secondary species, as well as post-irradiation effects, related to preferential-exclusion of the cosolute from the protein surface. Hence, Ectoine is shown to provide a non-disturbing way to improve structure-determination of proteins via bio-SAXS in future studies. KW - BioSAXS KW - Bio-SAXS KW - Cosolute KW - Ectoine KW - G5P KW - GVP KW - Radiation damage KW - Radical Scavenger KW - Single-stranded DNA-binding proteins KW - X-ray scattering KW - DNA KW - ssDNA KW - Protein KW - SAXS KW - Small-angle xray scattering KW - McSAS3 KW - Dosimetry KW - Microdosimetry KW - Geant4 KW - Geant4-DNA KW - Topas KW - Topas-MC KW - Monte-Carlo simulations KW - Particle scattering simulations KW - Topas-nBio KW - OH Radical KW - OH radical scavenger KW - LEE KW - Ionizing radiation damage KW - Protein unfolding KW - Ectoin PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568909 DO - https://doi.org/10.1039/d2cp05053f SN - 1463-9076 SN - 1463-9084 VL - 25 IS - 7 SP - 5372 EP - 5382 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-56890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hallier, Dorothea C. A1 - Smales, Glen Jacob A1 - Seitz, H. A1 - Hahn, Marc Benjamin T1 - Inside back cover for the article "Bio-SAXS of single-stranded DNA-binding proteins: Radiation protection by the compatible solute ectoine" N2 - Showcasing research from the Federal Institute for Material Research and Testing Berlin and Fraunhofer Institute for Celltherapy and Immunology Branch Bioanalytics and Bioprocesses Potsdam. Bio-SAXS of single-stranded DNA-binding proteins: Radiation protection by the compatible solute ectoine. We aimed to increase the possible undisturbed exposure time during bio-SAXS measurements of single-stranded DNA-binding proteins. Therefore small angle X-ray scattering was performed on Gene-V Protein (G5P/GVP), which is involved in DNA repair processes. To achieve this, irradiations were performed in presence and absence of the hydroxyl-radical scavenger and osmolyte Ectoine, which showed efficient radiation protection and prevented protein aggregation, thus allows for a non-disturbing way to improve structure-determination of biomolecules. KW - Bio-SAXS KW - BioSAXS KW - Cosolute KW - DNA KW - Dosimetry KW - Ectoin KW - Ectoine KW - G5P KW - GVP KW - Geant4 KW - Geant4-DNA KW - Ionizing radiation damage KW - LEE KW - McSAS3 KW - Microdosimetry KW - Monte-Carlo simulations KW - OH Radical KW - OH radical scavenger KW - Protein KW - Protein unfolding KW - Radiation damage KW - Radical Scavenger KW - SAXS KW - Single-stranded DNA-binding proteins KW - Small-angle xray scattering KW - Topas-MC KW - Topas-nBio KW - TopasMC KW - X-ray scattering KW - Particle scatterin simulations KW - ssDNA PY - 2023 DO - https://doi.org/10.1039/D3CP90056H SN - 1463-9076 SN - 1463-9084 VL - 25 IS - 7 SP - 5889 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-57006 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hunter, R. D. A1 - Hayward, E. C. A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Kulak, A. A1 - Guan, S. A1 - Schnepp, Z. T1 - The effect of nitrogen on the synthesis of porous carbons by iron-catalyzed graphitization N2 - This paper reports a systematic study into the effect of nitrogen on iron-catalyzed graphitization of biomass. Chitin, chitosan, N-acetylglucosamine, gelatin and glycine were selected to represent nitrogen-rich saccharides and amino-acid/polypeptide biomass precursors. The materials were pyrolyzed with an iron catalyst to produce carbons with a wide range of chemical and structural features such as mesoporosity and nitrogen-doping. Many authors have reported the synthesis of nitrogen-doped carbons by pyrolysis and these have diverse applications. However, this is the first systematic study of how nitrogen affects pyrolysis of biomass and importantly the catalytic graphitization step. Our data demonstrates that nitrogen inhibits graphitization but that some nitrogen survives the catalytic graphitization process to become incorporated into various chemical environments in the carbon product. KW - Graphitization KW - Nanoparticles KW - Nanocomposite KW - Porous carbon KW - Nitrogen KW - Scattering PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575351 DO - https://doi.org/10.1039/d3ma00039g VL - 4 SP - 2070 EP - 2077 PB - Royal Society of Chemistry AN - OPUS4-57535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kolmangadi, Mohamed Aejaz T1 - Confinement induced Relaxations and phase behvaiour of nanoconfined Ionic Liquid Crystal N2 - Ionic Liquid Crystals (ILCs) are materials that combine the properties of liquid crystals together with ionic conduction. It is known that liquid crystal mesophases in confinement exhibit anomalous dynamics and phase behavior. However, similar studies about factors that control the macroscopic properties of ILCs in confinement are limited. Here, Broadband Dielectric Spectroscopy (BDS), X-ray scattering, and calorimetry were applied to study the molecular dynamics, and phase behavior of a guanidinium based columnar ionic liquid crystal confined in self-ordered alumina oxide nanopores of pore sizes ranging from 180 nm down to 25 nm. It is aimed to understand how pore size and pore surface wettability (hydrophilic or hydrophobic) influence the molecular dynamics, and phase behavior for this system which are crucial for applications. The DSC measurements show: (i) the crystalline-liquid crystalline transition temperature has non-monotonic dependence on inverse pore diameter and (ii) the liquid crystalline-isotropic transition is completely suppressed for all the confined samples. This thermally suppressed transition was detected by BDS and X-ray scattering and is considered as a continuous phase transition instead of a discontinuous first order transition. BDS investigations reveal several relaxation processes for the bulk and confined scenarios. The relaxation modes are suppressed and become slower for the confined scenarios compared to the bulk. Possible molecular origins for these relaxation processes are discussed, and it is shown that the self-assembly of these ILCs is dynamic in nature. T2 - CONFIT 2022 CY - Grenoble, France DA - 10.10.2022 KW - Ionic Liquid crystals KW - Nanoconfinement KW - Conductivity PY - 2022 AN - OPUS4-57339 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Extending Bio-SAXS measurements of Single-Stranded DNA-Binding Proteins: Radiation Protection of G5P by Cosolutes N2 - Small-angle X-ray scattering (SAXS) can be used for structural de- termination of biological macromolecules and polymers in their na- tive states. To improve the reliability of such experiments, the re- duction of radiation damage occurring from exposure to X-rays is needed.One method, is the use of scavenger molecules that protect macromolecules against radicals produced by radiation exposure.In this study we investigate the feasibility to apply the compatible solute, osmolyte and radiation protector Ectoine (THP(B)) as a scavenger throughout SAXS measurements of single-stranded DNA-binding protein Gene-V Protein (G5P/GVP). Therefore we monitor the radiation induced changes of G5P during bio-SAXS. The resulting microscopic energy-damage relation was determined by particle scattering simu- lations with TOPAS/Geant4. The results are interpreted in terms of radical scavenging as well as post-irradiation effects, related to preferential-exclusion from the protein surface. Thus, Ectoine provides an non-disturbing way to improve structure-determination of proteins via bio-SAXS in future studies. T2 - MultiChem Conference 2023 CY - Prague, Czech Republic DA - 26.04.2023 KW - Bio-SAXS KW - BioSAXS KW - Compatible solute KW - Cosolute KW - DNA KW - Dosimetry KW - Ectoin KW - Ectoine KW - Ectoin KW - G5P KW - GVP KW - Geant4 KW - Geant4-DNA KW - Gene five protein KW - Hydroxyectoine KW - Ionizing radiation damage KW - LEE KW - McSAS3 KW - Microdosimetry KW - Monte-Carlo simulations KW - OH Radical KW - OH radical scavenger KW - Osmolyte KW - Particle scattering simulations KW - Protein KW - Protein unfolding KW - Proteins KW - ROS KW - Radiation damage KW - Radical Scavenger KW - Radical scavenger KW - SAXS KW - Single-stranded DNA-binding proteins KW - Small-angle xray scattering KW - Topas KW - Topas-MC KW - Topas-nBio KW - X-ray scattering KW - ssDNA KW - Median lethal energy deposit PY - 2023 AN - OPUS4-57407 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob T1 - Electric Safety Interlock N2 - This interlock is designed to prevent electrical shock from high voltage (>60V) equipment. While the general safety interlock can be generically applied, this particular example employs an external vacuum-activated switch. It is for safeguarding human operations inside a vacuum sample chamber while the chamber doors are open. The circuit is closed (output is active) when a sufficient level of vacuum is reached, i.e. when all accessible openings are necessarily closed. The initial application is to interrupt power to a 220V, 250W heating cartridge (itself mounted inside a small sample holder with potentially exposed contacts) when the sample chamber is open. The external circuit can be modified to use different interlock mechanisms as needed. Note that the external interlock circuit is only a single circuit (with two signal lines) and thus is not protected against external shorts. To accomodate a range of safety interlocks, the 4-pin M12 connector is wired as follows: Pin 1 (Brown): +24V for power supply, max current 0.6A Pin 2 (White): Safety interlock system signal 1 (0 or 24V) Pin 3 (Blue) : Safety interlock system signal 2 (0 or 24V) Pin 4 (Black): 0V for power supply The safety is interlocked (output active) when both signal pins are set high (24V), with sufficient current to activate the two relays. Pin 1 and 4 can be used to power safety hardware (such as light curtains or proximity detectors) with 24VDC up to a current of 0.6A. A larger power supply can be installed when higher currents are needed, while staying within the current limits imposed by the wiring cross-section. KW - Electric Safety Interlock KW - MOUSE KW - 60-230V PY - 2023 DO - https://doi.org/10.6084/m9.figshare.22265920.v1 PB - Digital Science CY - Cambridge, MA, USA AN - OPUS4-57138 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - X-ray Scattering USAXS/SAXS/WAXS (/XRD/PDF) N2 - A ten minute introduction to the technique of X-ray scattering. This talk discusses the foundation and the resulting morphological parameters that can be obtained from the technique. The talk is prepared for discussion within the framework of the OECD REACH guideline for nanomaterials. T2 - Digitaler Info-Tag "Nano or not Nano" CY - Berlin, Germany DA - 16.02.2023 KW - X-ray scattering KW - BAM Academy KW - SAXS KW - XRD KW - WAXS KW - Nanomaterial KW - REACH KW - OECD KW - Guideline PY - 2023 AN - OPUS4-57013 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Reimagining user-driven science N2 - The materials scientists we work with do not want (or need) to learn the ways of the scatterer; they are primarily interested in obtaining trustworthy, authoritative answers. In particular, they need structural understanding in light of the wider framework of their experiment(s). Our interest, therefore, lies in helping them attain this this interconnected understanding, while using such investigations to further hone our methodology to approximate perfection. While perfection is by definition an unattainable goal, we have spent the last 15+ years exploring and expanding on many of its constituent aspects (often together with likeminded people) [1]. These aspects include: developing various visualization and simulation tools, deconstructing data corrections and uncertainty estimation, advancing analysis methods, quantifying questions on traceability, documentation, reproducible automation of synthesis-, measurement- and data pipelines, data visualization, exploration and education, and many more… As we explored these individual aspects, it has become clear that high quality output demands involving ourselves in the entire experimental workflow, with all associated aspects. This allows you to establish trustworthy links between parameters, structure, and performance. Through multiple cross-checks and validations, we can furthermore assign a degree of confidence to our findings. This is what we call the holistic approach. This talk will briefly define perfection in scattering experiments, expand on the holistic approach, and show examples to demonstrate its benefits. T2 - Invited talk - special event CY - Trieste, Italy DA - 15.05.2025 KW - X-ray scattering KW - Holistic experiments KW - Laboratory management KW - Laboratory automation KW - Data stewardship KW - User support PY - 2025 AN - OPUS4-63372 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - and now it's bigger…: setting up for large scale experimentation N2 - In our laboratory, we rely heavily on automation for synthesis and measurement. Done right, automation can deliver reliable quantities of excruciatingly detailed data, produced in a reproducible and traceable way. This data then needs sorting and organising, and a good structure of metadata is a good start to long-lasting data. This metadata collection is an essential part of our “holistic experimentation”-approach. In this approach, we try to ensure that all aspects of the experimental chain are performed to a high standard, so that experimental integrity is maintained. In other words: as a failure in one of the components of the chain can make an entire experiment worthless, we must ensure each component is done (and documented) well. In this talk, we show how we 1) synthesise well-documented sample series, 2) apply a complete end-to-end X-ray scattering characterisation methodology to those samples, and 3) can link the data from the synthesis to the structural details obtained from the scattering experiments in a visual dashboard. Furthermore, we will show examples on how data can be organised in hierarchical structures in HDF5-based datafiles, and how this helps move towards more trustworthy, traceable science. T2 - Future Labs Live 2025 CY - Basel, Switzerland DA - 27.05.2025 KW - Lab automation KW - Holistic experiments KW - Synthesis KW - Traceability KW - Data stewardship PY - 2025 AN - OPUS4-63373 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Monroy, José del Refugio A1 - Deshpande, Tejas A1 - Schlecht, Joël A1 - Douglas, Clara A1 - Stirling, Robbie A1 - Grabicki, Niklas A1 - Smales, Glen Jacob A1 - Kochovski, Zdravko A1 - Fabozzi, Filippo Giovanni A1 - Hecht, Stefan A1 - Feldmann, Sascha A1 - Dumele, Oliver T1 - Homochiral versus racemic 2D covalent organic frameworks N2 - The synthesis of homochiral two-dimensional covalent organic frameworks (2D COFs) from chiral π-conjugated building blocks is challenging, as chiral units often lead to misaligned stacking interactions. In this work, we introduce helical chirality into 2D COFs using configurationally stable enantiopure and racemic [5]helicenes as linkers in the backbone of 2D [5]HeliCOFs as powders and films. Through condensation with 1,3,5-triformylbenzene (TFB) or 1,3,5-triformylphloroglucinol (TFP), our approach enables the efficient formation of a set of homochiral and racemic 2D [5]HeliCOFs. The resulting carbon-based crystalline and porous frameworks exhibit distinct structural features and different properties between homochiral and racemic counterparts. Propagation of helical chirality into the backbone of the crystalline frameworks leads to the observation of advanced chiroptical properties in the far-red visible spectrum, along with a less compact structure compared with the racemic frameworks. Homogeneous thin films of [5]HeliCOFs disclosed photoluminescent properties arising from the controlled growth of highly ordered π-conjugated lattices. The present study offers insight into general chiral framework formation and extends the Liebisch−Wallach rule to 2D COFs. KW - Chirality KW - Covalent organic frameworks KW - Diffraction KW - Lattices KW - Thin films PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-633755 DO - https://doi.org/10.1021/jacs.5c01004 SN - 0002-7863 VL - 147 IS - 21 SP - 17750 EP - 17763 PB - American Chemical Society (ACS) CY - Washington, DC AN - OPUS4-63375 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aliyah, K. A1 - Prehal, C. A1 - Diercks, J. S. A1 - Diklić, N. A1 - Xu, L. A1 - Ünsal, S. A1 - Appel, C. A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Guizar-Sicairos, M. A1 - Herranz, J. A1 - Gubler, L. A1 - Büchi, F. N. A1 - Eller, J. T1 - Quantification of PEFC Catalyst Layer Saturation via In Silico, Ex Situ, and In Situ Small-Angle X-ray Scattering N2 - The complex nature of liquid water saturation of polymer electrolyte fuel cell (PEFC) catalyst layers (CLs) greatly affects the device performance. To investigate this problem, we present a method to quantify the presence of liquid water in a PEFC CL using small-angle X-ray scattering (SAXS). This method leverages the differences in electron densities between the solid catalyst matrix and the liquid water filled pores of the CL under both dry and wet conditions. This approach is validated using ex situ wetting experiments, which aid the study of the transient saturation of a CL in a flow cell configuration in situ. The azimuthally integrated scattering data are fitted using 3D morphology models of the CL under dry conditions. Different wetting scenarios are realized in silico, and the corresponding SAXS data are numerically simulated by a direct 3D Fourier transformation. The simulated SAXS profiles of the different wetting scenarios are used to interpret the measured SAXS data which allows the derivation of the most probable wetting mechanism within a flow cell electrode. KW - Polymer electrolyte fuel cell KW - Water management KW - Catalyst layer KW - Representative morphology modeling KW - Small-angle X-ray scattering KW - MOUSE KW - SAXS PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575973 DO - https://doi.org/10.1021/acsami.3c00420 SN - 1944-8244 VL - 15 IS - 22 SP - 26538 EP - 26553 PB - ACS Publications AN - OPUS4-57597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob T1 - Small-angle scattering data analysis round robin dataset - Original for participants N2 - These are four datasets that were made available to the participants of the Small-angle Scattering data analysis round robin. The intent was to find out how comparable results from different researchers are, who analyse exactly the same processed, corrected dataset. In this repository, there are: 1) a PDF document with more details for the study, 2) the datasets for people to try and fit, 3) an Excel spreadsheet to document the results. Datasets 1 and 2 were modified from: Deumer, Jerome, & Gollwitzer, Christian. (2022). npSize_SAXS_data_PTB (Version 5) [Data set]. Zenodo. https://doi.org/10.5281/zenodo.5886834 Datasets 3 and 4 were collected in-house on the MOUSE instrument. KW - Round robin KW - SAXS KW - Small angle scattering KW - SANS KW - X-ray KW - Neutron KW - Human factor KW - Data analysis KW - Data fitting KW - Human influence PY - 2023 DO - https://doi.org/10.5281/zenodo.7506365 PB - Zenodo CY - Geneva AN - OPUS4-56799 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard T1 - McSAS3 N2 - McSAS3 is a refactored version of the original McSAS (see DOI 10.1107/S1600576715007347). This software fits scattering patterns to obtain size distributions without assumptions on the size distribution form. The refactored version has some neat features: - Multiprocessing is included, spread out over as many cores as number of repetitions! - Full state of the optimization is stored in an organized HDF5 state file. - Histogramming is separate from optimization and a result can be re-histogrammed as many times as desired. - SasModels allow a wide range of models to be used - If SasModels does not work (e.g. because of gcc compiler issues on Windows or Mac), an internal sphere model is supplied - Simulated data of the scattering of a special shape can also be used as a McSAS fitting model. Your models are infinite! - 2D fitting also works. KW - X-ray scattering KW - Polydispersity KW - Monte carlo KW - Scattering pattern analysis KW - Analysis approach KW - Neutron scattering KW - Automation KW - Command line PY - 2023 DO - https://doi.org/10.6084/m9.figshare.21814128.v1 PB - Digital Science CY - Cambridge, MA, USA AN - OPUS4-56787 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob T1 - X-ray scattering Datasets of gold and silver nanoparticle composites, relating to the publication "Gold and silver dichroic nanocomposite in the quest for 3D printing the Lycurgus cup" N2 - Wide-range X-ray scattering datasets and analyses for all samples described in the 2020 publication "Gold and silver dichroic nanocomposite in the quest for 3D printing the Lycurgus cup". These datasets are composed by combining multiple small-angle x-ray scattering and wide-angle x-ray scattering curves into a single dataset. They have been analyzed using McSAS to extract polydispersities and volume fractions. They have been collected using the MOUSE project (instrument and methodology). KW - X-ray scattering KW - MOUSE KW - Saxs KW - Waxs KW - Analyses KW - Datasets PY - 2022 DO - https://doi.org/10.5281/zenodo.7193859 PB - Zenodo CY - Geneva AN - OPUS4-55979 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - The human factor: A round robin study on the variation in data analyses N2 - How much do we, the small-angle scatterers, influence the results of an investigation? What uncertainty do we add by our human diversity in thoughts and approaches, and is this significant compared to the uncertainty from the instrumental measurement factors? After our previous Round Robin on data collection, we know that many laboratories can collect reasonably consistent small-angle scattering data on easy samples. To investigate the next, human component, we compiled four existing datasets from globular (roughly spherical) scatterers, each exhibiting a common complication, and asked the participants to apply their usual methods and toolset to the quantification of the results (https://lookingatnothing.com/index.php/archives/3274). Accompanying the datasets was a modicum of accompanying information to help with the interpretation of the data, similar to what we normally receive from our collaborators. More than 30 participants reported back with volume fractions, mean sizes and size distribution widths of the particle populations in the samples, as well as information on their self-assessed level of experience and years in the field. While the Round Robin is still underway (until the 25th of April, 2022), the initial results already show significant spread in the results. Some of these are due to the variety in interpretation of the meaning of the requested parameters, as well as simple human errors, both of which are easy to correct for. Nevertheless, even after correcting for these differences in understanding, a significant spread remains. This highlights an urgent challenge to our community: how can we better help ourselves and our colleagues obtain more reliable results, how could we take the human factor out of the equation, so to speak? In this talk, we will introduce the four datasets, their origins and challenges. Hot off the press, we will summarize the anonymized, quantified results of the Data Analysis Round Robin. (Incidentally, we will also see if a correlation exists between experience and proximity of the result to the median). Lastly, potential avenues for improving our field will be offered based on the findings, ranging from low-effort yet somehow controversial improvements, to high-effort foundational considerations. T2 - International Small-Angle Scattering Conference (SAS2022) CY - Campinas, Brazil DA - 11.09.2022 KW - Round robin KW - Data analysis KW - Small angle scattering KW - Nanomaterials KW - MOUSE KW - Interlaboratory comparison KW - Intercomparability KW - Reliability KW - Data analysis round robin KW - Large number of participants PY - 2022 AN - OPUS4-55762 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - X-ray scattering for nanostructure quantification, and the quest for the perfect experiment N2 - Measuring an X-ray scattering pattern is relatively easy, but measuring a steady stream of high-quality, useful patterns requires significant effort and good laboratory organization. Such laboratory organization can help address the reproducibility crisis in science, and easily multiply the scientific output of a laboratory, while greatly elevating the quality of the measurements. We have demonstrated this for small- and wide-angle X-ray scattering in the MOUSE project (Methodology Optimization for Ultrafine Structure Exploration). With the MOUSE, we have combined a comprehensive and highly automated laboratory workflow with a heavily modified X-ray scattering instrument. This combination allows us to collect fully traceable scattering data, within a well-documented, FAIR-compliant data flow (akin to what is found at the more automated synchrotron beamlines). With two full-time researchers, our lab collects and interprets thousands of datasets, on hundreds of samples, for dozens of projects per year, supporting many users along the entire process from sample selection and preparation, to the analysis of the resulting data. This talk will briefly introduce the foundations of X-ray scattering, present the MOUSE project, and will highlight the proven utility of the methodology for materials science. Upgrades to the methodology will also be discussed, as well as possible avenues for transferring this holistic methodology to other instruments T2 - SNI 2022 CY - Berlin, Germany DA - 05.09.2022 KW - Methodology KW - X-ray scattering KW - Laboratory management KW - Instrumentation utilization KW - MOUSE KW - SAXS KW - WAXS KW - Automation PY - 2022 AN - OPUS4-55760 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Smales, Glen Jacob A1 - Hahn, Marc Benjamin A1 - Hallier, Dorothea C. A1 - Seitz, H. T1 - X-ray scattering datasets and simulations associated with the publication "Bio-SAXS of single-stranded DNA-binding proteins: Radiation protection by the compatible solute ectoine" N2 - This dataset contains the processed and analysed small-angle X-ray scattering data associated with all samples from the publications "Bio-SAXS of Single-Stranded DNA-Binding Proteins: Radiation Protection by the Compatible Solute Ectoine" (https://doi.org/10.1039/D2CP05053F). Files associated with McSAS3 analyses are included, alongside the relevant SAXS data, with datasets labelled in accordance to the protein (G5P), its concentration (1, 2 or 4 mg/mL), and if Ectoine is present (Ect) or absent (Pure). PEPSIsaxs simulations of the GVP monomer (PDB structure: 1GV5 ) and dimer are also included. TOPAS-bioSAXS-dosimetry extension for TOPAS-nBio based particle scattering simulations can be obtained from https://github.com/MarcBHahn/TOPAS-bioSAXS-dosimetry which is further described in https://doi.org/10.26272/opus4-55751. This work was funded by the Deutsche Forschungsgemeinschaft (DFG, German Research Foundation) under grant number 442240902 (HA 8528/2-1 and SE 2999/2-1). We acknowledge Diamond Light Source for time on Beamline B21 under Proposal SM29806. This work has been supported by iNEXT-Discovery, grant number 871037, funded by the Horizon 2020 program of the European Commission. KW - SAXS KW - Radiation protection KW - Microdosimetry KW - G5P KW - Ectoine KW - DNA-Binding protein PY - 2023 DO - https://doi.org/10.5281/zenodo.7515394 PB - Zenodo CY - Geneva AN - OPUS4-56811 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Khropost, Diana A1 - Riethmüller, Franziska A1 - Döhring, Thorsten A1 - Flachs, Dennis A1 - Hülagü, Deniz A1 - Hertwig, Andreas A1 - Cotroneo, Vincenzo A1 - gibertini, eugenio T1 - Polydopamine – a bio-inspired polymer for X-ray mirror coatings and other technical applications N2 - Although the organic molecule dopamine (3,4-dihydroxyphenethylamine) is commonly known as one of the “hormones of happiness”, thin polymer films of polydopamine (PDA) also have interesting technical properties. PDA is a very strong glue that sticks on almost everything, even under water. In nature, PDA is found in the byssal thread cuticles of mussels. When produced by dip-coating, the self-organizing PDA layers grow in a reproducible thickness of single or multiple molecule monolayers of a few nanometres thickness only. Here we present an optimized preparation regime as derived from polymerization analysis through absorption spectroscopy. One application is the use of thin PDA overcoatings to increase the soft X-ray reflectivity of astronomical X-ray mirrors. Furthermore, we give an outlook to other technical applications for this interesting material, presenting this bio-inspired organic polymer as an innovative technical solution for the future, with applications such as PDA-based super-capacitors and its promising role in enhancing separator materials for batteries. T2 - SPIE Optics + Optoelectronics 2025 CY - Prague, Czech Republic DA - 07.04.2025 KW - X-ray mirrors KW - Reflectivity KW - Polydopamine KW - Ellipsometry PY - 2025 DO - https://doi.org/10.1117/12.3056298 VL - 13531 SP - 1 EP - 11 PB - SPIE AN - OPUS4-63630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Khropost, Diana A1 - Riethmüller, Franziska A1 - Stanik, Eva A1 - Döhring, Thorsten A1 - Hertwig, Andreas A1 - Hülagü, Deniz T1 - Polydopamine -a bionic material and its potential applications for batteries N2 - Polydopamine (PDA) recently came into focus as an innovative material for applications in various technical fields. It is a very strong glue that sticks on almost everything, even under water: In nature, PDA is found in the byssal thread cuticles of mussels. In 2007, Lee et al. first showed that dipping substrates into a solution of dopamine results in the formation of thin PDA films on numerous materials. The simple preparation and the high durability of these coatings have stimulated growing research interest and a wide variety of applications in energy, biomedical and environmental science, and other fields. We have investigated thin layers of PDA with different methods including ellipsometry, tactile measurements of the layer thickness and in situ absorption measurements during the polymerization process. During polymerization the dopamine solution shows a progressive colour change from transparent to brown that has been monitored by spectrometric measurements. The increasing absorption of the cuvette with dopamine solution can be seen in figure 1. The absorption levels off after approximately 2,5 h of polymerization time, thus indicating termination of the primary formation of the PDA film. This data shows that for homogeneous layer growth it is advantageous to interrupt the process after two hours. To generate a higher layer thickness, the samples need to be cleaned and immersed in a fresh dopamine solution subsequently. In addition, ellipsometry measurements on polydopamine layers could determine the corresponding coating thickness as well as its complex refractive index over a broad wavelength range. T2 - Materials Week 2025 CY - Frankfurt am Main, Germany DA - 02.04.2025 KW - Polydopamine KW - Ellipsometry KW - Leyer thickness PY - 2025 AN - OPUS4-63636 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -