TY - CONF A1 - Huber, Norbert T1 - Testing and analysis of materials and components ‒ an expedition from lab to field in a digitally transforming world N2 - In an era where digital transformation is reshaping every facet of our lives, the field of material science and engineering is no exception. This presentation delves into the exciting journey of material and component testing, tracing its path from the confines of the laboratory to the vast expanse of real-world applications, with a particular focus on enhancing safety and reliability. We will explore how modern techniques are pushing the boundaries of conventional material testing, revealing new dimensions of material behavior and performance that are crucial for ensuring safety. The integration of in situ quality control within production processes is revolutionizing manufacturing, ensuring unparalleled precision and reliability, which are essential for maintaining high safety standards. As we venture into the realm of Structural Health Monitoring (SHM), discover how cutting-edge technologies are being deployed in field applications, from infrastructure to renewable energy sectors, to monitor and ensure the safety and integrity of critical systems. The presentation will also offer a glimpse into the future, where centralized systems for research data management and innovative digital initiatives promise to transform the landscape of material testing and analysis, further bolstering safety measures. Join us to uncover how these advancements are not only enhancing safety and reliability but also paving the way for a digitally interconnected world. T2 - MaterialsWeek 2025 CY - Frankfurt am Main, Germany DA - 02.04.2025 KW - Characterization KW - Materials testing KW - In situ quality control KW - Digitalization PY - 2025 AN - OPUS4-63918 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lemiasheuski, Anton A1 - Wehrkamp, F. A1 - Bajer, Evgenia A1 - Sonnenburg, Elke A1 - Göbel, Artur A1 - Porohovoj, Ilja A1 - Bettge, Dirk A1 - Pfennig, Anja T1 - Practical application of an automated 3D metallography system for the reconstruction and microstructural analysis of porosity in a sintered steel N2 - In the 3D microstructural analysis of a digital twin of porosity in the sintered steel Astaloy CrA, pore shape, average pore size as well as pore distribution will be analyzed. Porosity plays a major role in powder-metallurgical materials since it greatly impacts the mechanical properties of these materials and therefore represents a key parameter in their characterization. Based on the robot-assisted automated serial sectioning and imaging (RASI) system of the Federal Institute for Materials Research and Testing (BAM, Bundesanstalt für Materialforschung und Prüfung) in Berlin, the technique of metallographic serial sectioning will be used to image the microstructure and reconstruct a digital 3D twin from the stack of images obtained. Compared with an individual 2D microsection, the quantitative microstructural analysis of this 3D twin will enable more accurate conclusions on the shape, size and distribution of pores. This paper will detail the key steps in 3D microstructural analysis, including the metallographic preparation routine, the imaging technique, image alignment as well as the segmentation of pores. After the methodology has been described, the results of the quantitative microstructural analysis will be presented and the validity of quantitative parameters of 3D and 2D images will be compared and discussed. The analysis of more than 10,000 pores revealed a correlation between pore shape and pore size. It was also found that a 2D representation of the material surface is insufficient for a precise quantitative characterization of porosity. N2 - In der 3D-Gefügeanalyse eines digitalen Zwillings von Poren in einem Sinterstahl des Typs Astaloy CrA werden sowohl die Porenform als auch die durchschnittliche Porengröße und -verteilung analysiert. Die Porosität spielt in pulvermetallurgischen Werkstoffen eine große Rolle, da sie erheblich die mechanischen Eigenschaften beeinflusst und daher bei der Charakterisierung dieser Werkstoffe ein wichtiger Parameter ist. Basierend auf der Verwendung des Robot-Assisted Automated Serial-Sectioning and Imaging (RASI)-Systems der Bundesanstalt für Materialforschung und Prüfung (BAM) in Berlin, wird das metallographische Serienschnittverfahren genutzt, um das Gefüge aufzunehmen und aus dem Bildstapel einen digitalen 3D-Zwilling zu rekonstruieren. Verglichen zu einem 2D-Einzelschliff ermöglicht die quantitative Gefügeanalyse dieses 3D-Zwillings präzisere Aussagen zu Porenform, -größe und -verteilung. Diese Arbeit beschreibt die wesentlichen Schritte, die für eine 3D-Gefügeanalyse nötig sind, darunter die metallografische Präparationsroutine, das Bildgebungs-Verfahren, das Alignment der Bilder sowie die Segmentierung der Poren. Im Anschluss an die methodische Darstellung werden die Ergebnisse der quantitativen Gefügeanalyse präsentiert und ein Vergleich zwischen der Aussagekraft der quantitativen Parameter von 3D- und 2D-Abbildungen diskutiert. Bei der Analyse von über 10.000 Poren konnte eine Korrelation zwischen der Form und der Porengröße aufgezeigt werden. Weiterhin konnte aufgezeigt werden, dass eine 2D-Abbildung der Werkstoffoberfläche nicht ausreichend für eine eindeutige quantitative Beschreibung der Porosität ist. KW - 3D Metallographie KW - RASI KW - Porenstruktur PY - 2025 DO - https://doi.org/10.1515/pm-2025-0049 SN - 2195-8599 VL - 62 IS - 8 SP - 516 EP - 535 PB - De Gruyter Brill AN - OPUS4-63930 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ruehle, Bastian T1 - Nano- and Advanced Materials Synthesis in a Self-Driving Lab (SDL) N2 - Nano- and advanced materials have been recognized as a key enabling technology of the 21st century, due to their high potential of driving innovations in new clean energy technologies, sustainable manufacturing by substitution of critical raw materials and replacement of hazardous substances, breakthroughs in energy conversion and storage, improvement of the environmental performance of products and processes, and facilitation of circularity. Consequently, improving tools that enhance the development and optimization cycle of nano- and advanced materials is crucial. In this contribution, we present our Self-Driving Lab (SDL) for Nano and Advanced Materials [1], that integrates robotics for batched autonomous synthesis – from molecular precursors to fully purified nanomaterials – with automated characterization and data analysis, for a complete and reliable nanomaterial synthesis workflow. By fully automating these three process steps for seven different materials from five representative, completely different classes of nano- and advanced materials (metal, metal oxide, silica, metal organic framework, and core–shell particles) that follow different reaction mechanisms, we demonstrate the great versatility and flexibility of the platform. The system also exhibits high modularity and adaptability in terms of reaction scales and incorporates in-line characterization measurement of hydrodynamic diameter, zeta potential, and optical properties (absorbance, fluorescence) of the nanomaterials. We discuss the excellent reproducibility of the various materials synthesized on the platform in terms of particle size and size distribution, and the adaptability and modularity that allows access to a diverse set of nanomaterial classes. These features underscore the SDL’s potential as a transformative tool for advancing and accelerating the development of nano- and advanced materials, offering solutions for a sustainable and environmentally responsible future. T2 - Accelerate 2025 CY - Toronto, Canada DA - 11.08.2025 KW - Nanomaterials KW - Advanced Materials KW - Automation KW - SDL KW - MAP PY - 2025 AN - OPUS4-63934 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Walter, Keven A1 - Hoch, Dominik P. A1 - Hertweck, Leon A1 - Balasubramanian, Kannan A1 - Geisler, Jonas A1 - Röllig, Mathias A1 - Neubert, Tilmann J. A1 - Börner, Hans G. T1 - Unlocking the Essence of Lignin: High‐Performance Adhesives That Bond via Thiol‐Catechol Connectivities and Debond on Electrochemical Command N2 - AbstractThe next generation of adhesives requires effective debonding capabilities that can be triggered on demand to enable advanced circular repair and recycling strategies. A new class of lignin‐inspired, two‐component (2K) structural adhesives offers bonding strengths of up to 20 MPa and clean, on‐command electrochemical debonding within 5–30 min. The debonding is induced by a distinct electrochemical oxidation of thiol‐catechol connectivities (TCCs) within the entire adhesive network, enforcing rapid and clean adhesive failure on the cathodic substrate side. The TCC‐functionalities are formed during curing by a thiol‐quinone Michael‐type polyaddition, reacting polyester‐based trithiols with tris‐quinones as lignin‐inspired minimal building blocks. The structural adhesive can be fine‐tuned by adjusting the formulation. The addition of carbon black and ionic liquids facilitates the desired electrochemical transformation of TCC‐catechols to TCC‐quinones. Applying only 9 V for 5–30 min, leads to clean debonding with 72–86% loss of shear strength. A comprehensive study of curing, bonding, and debonding behavior by rheological, spectroscopic, and electrochemical investigations reveals the debonding mechanism by correlating catechol oxidation to adhesive performance. The electrochemical debonding capability of TCC‐structural adhesives is demonstrated in a functional prototype, where on‐command detachment of a cover glass from a display device is achieved within 6.5 min. KW - Lignin-inspired KW - Electrochemical-Debonding KW - Thiol-Catechol-Connectivity (TCC) KW - Michael-Type Polyaddition KW - On-Demand Adhesive Failure PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639674 DO - https://doi.org/10.1002/adma.202510463 SN - 0935-9648 SP - 1 EP - 10 PB - Wiley VHC-Verlag CY - 69451 Weinheim AN - OPUS4-63967 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yildirim, Arda A1 - Haug, T. C. V. A1 - Fröba, M. A1 - Huber, P. A1 - Schönhals, Andreas T1 - Molecular fluctuations in mixed-metal MOF-74: influence of the metal composition N2 - A selected series of metal–organic frameworks M-MOF-74 (M = Mg, Co, Ni) and mixed metal MM-MOF-74 (Mg/Co or Mg/Ni) with different compositions of metal atoms have been prepared and further investigated by broadband dielectric spectroscopy (BDS) in a wide temperature range. The dielectric spectra show at least two relaxation processes. Process-A is observed only for the Ni-containing MOFs and is attributed to localized fluctuations of the metal oxide corners. Relaxation processes-B and -C are observed for all prepared MOFs, except that process-B is not observed for Ni-MOF-74. Large-angle fluctuations such as free rotations of the linkers can be excluded due to the structure of MOF-74, but small-angle fluctuations such as torsions are possible. According to numerical simulations carried out for MOF-74, process-B can be attributed to inward and outward fluctuations of the linkers relative to the pore center. Process-C is related to small-angle rotational fluctuations of the linker together with co-rotations of the metal nodes. The latter interpretation is supported by the dependence of the activation energy of the relaxation rate of process-C on the metal composition of the MOFs, which is discussed in terms of the bond lengths between the metal atoms and the linker which decrease in the sequence Mg, Co and Ni. KW - Metal Organic Frameworks PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639378 DO - https://doi.org/10.1039/d5ra05357a SN - 2046-2069 VL - 15 IS - 35 SP - 29109 EP - 29118 PB - Royal Society of Chemistry (RSC) AN - OPUS4-63937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - "Ultima Ratio": Multi-scale, high-resolution 3D-FFT scattering pattern simulations N2 - This talk highlights a proof-of-concept that demonstrates the ability to calculate high-resolution Fourier transforms. These can be combined with multi-scale modeling to simulate scattering over a wide range, from small-angle scattering to XRD and PDF. T2 - Shapespyer/MuSSIC Launch Workshop CY - Didcot, UK DA - 20.02.2023 KW - X-ray scattering KW - Simulation KW - Fourier Transform KW - 3D KW - High resolution KW - Multi-scale PY - 2023 AN - OPUS4-57031 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Laskina, Sofya A1 - Naik, Aakash A1 - Smales, Glen Jacob A1 - George, Janine A1 - Breßler, Ingo A1 - Benner, Philipp T1 - Jupyter notebook and VASP calculation details accompanying the manuscript: "Ultima Ratio: Simulating wide-range X-ray scattering and diffraction" N2 - Summary: This notebook and associated datasets (including VASP details) accompany a manuscript available on the ArXiv (https://doi.org/10.48550/arXiv.2303.13435) and hopefully soon in a journal as short communication as well. Most of the details needed to understand this notebook are explained in that paper with the same title as above. For convenience, the abstract is repeated here: Paper abstract: We demonstrate a strategy for simulating wide-range X-ray scattering patterns, which spans the small- and wide scattering angles as well as the scattering angles typically used for Pair Distribution Function (PDF) analysis. Such simulated patterns can be used to test holistic analysis models, and, since the diffraction intensity is presented coupled to the scattering intensity, may offer a novel pathway for determining the degree of crystallinity. The "Ultima Ratio" strategy is demonstrated on a 64-nm Metal Organic Framework (MOF) particle, calculated from $Q<0.01$\,$\mathrm{nm}^{-1}$ up to $Q\approx150$\,$\mathrm{nm}^{-1}$, with a resolution of 0.16\,\AA. The computations exploit a modified 3D Fast Fourier Transform (3D-FFT), whose modifications enable the transformations of matrices at least up to $8000^3$ voxels in size. Multiple of these modified 3D-FFTs are combined to improve the low-$Q$ behaviour. The resulting curve is compared to a wide-range scattering pattern measured on a polydisperse MOF powder. While computationally intensive, the approach is expected to be useful for simulating scattering from a wide range of realistic, complex structures, from (poly-)crystalline particles to hierarchical, multicomponent structures such as viruses and catalysts. KW - X-ray KW - Simulation KW - Scattering KW - MOUSE KW - Nanomaterials KW - XRD KW - SAXS KW - PDF KW - Total scattering KW - 3D Fourier transform KW - High resolution KW - FFT PY - 2023 DO - https://doi.org/10.5281/zenodo.7764044 PB - Zenodo CY - Geneva AN - OPUS4-57207 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 - CONF A1 - Gugin, Nikita T1 - Advancing Industrial Mechanochemistry: Real-Time Insights for Sustainable, Solvent-Free Manufacturing N2 - Mechanochemistry is an environmentally friendly synthetic approach that enables the sustainable production of a wide range of chemicals while reducing or eliminating the need for solvents. Reactive extrusion aims to move mechanochemistry from its conventional gram-scale batch reactions, typically performed in laboratory ball mills, to a continuous, large-scale process. Meeting this challenge requires in situ monitoring techniques to gain insights into reactive extrusion and its underlying processes. While the effectiveness of in situ Raman spectroscopy in providing molecular-level information has been demonstrated, our study uses energy-dispersive X-ray diffraction to monitor reactive extrusion in real time at the crystalline level. Our results provide previously unavailable control over thereactiveextrusion process, promoting its perception as an industrially feasible green alternative to traditional solventbased syntheses. T2 - #RSCPoster 2025 CY - Online meeting DA - 04.03.2025 KW - Mechanochemistry PY - 2025 AN - OPUS4-63803 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gugin, Nikita T1 - Advancing Industrial Mechanochemistry: Real-Time Insights for Sustainable, Solvent-Free Manufacturing N2 - Reactive extrusion has emerged as a continuous approach for conducting mechanochemical reactions on a large scale. However, the use of this method under industrial conditions is hindered by limited understanding. In this study, we unveil the black box of reactive extrusion by employing energy-dispersive X-ray diffraction (EDXRD) to collect time- and spatially resolved in situ data. Our findings demonstrate the EDXRD method’s applicability to a range of chemical transformations and conditions associated with reactive extrusion. T2 - Chemie-Kolloquium & IfC Science Day CY - Berlin, Germany DA - 22.01.2025 KW - Mechanochemistry PY - 2025 AN - OPUS4-63801 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Costa, Elena A1 - Climent Terol, Estela A1 - Ast, S. A1 - Weller, Michael G. A1 - Canning, J. A1 - Rurack, Knut T1 - Development of a lateral flow test for rapid pyrethroid detection using antibody-gated indicator-releasing hybrid materials N2 - The employment of type-I pyrethroids for airplane disinfection in recent years underlines the necessity to develop sensing schemes for the rapid detection of these pesticides directly at the point-of-use. Antibody-gated indicator-releasing materials were thus developed and implemented with test strips for lateral-flow assay-based analysis employing a smartphone for readout. Besides a proper matching of pore sizes and gating macromolecules, the functionalization of both the material's outer surface as well as the strips with PEG chains enhanced system performance. This simple assay allowed for the detection of permethrin as a target molecule at concentrations down to the lower ppb level in less than 5 minutes. KW - Lateral flow test KW - Gated hybrid material KW - Fluorescence KW - Smartphone readout device KW - Pyrethroid KW - Pesticide KW - Insecticide KW - SBA-15 KW - Permethrin PY - 2020 DO - https://doi.org/10.1039/d0an00319k SN - 0003-2654 SN - 1364-5528 VL - 145 IS - 10 SP - 3490 EP - 3494 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-50756 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -