TY - JOUR A1 - Giannakopoulos, Antonios E. A1 - Zisis, Athanasios A1 - Zervaki, Anna D. A1 - Dimopoulos, Christos D. A1 - Platypodis, Efstathios A1 - Eberwein, Robert T1 - Effective elastic moduli and failure mechanisms of a random assembly of thin walled glass microbubbles N2 - In this work a methodology is presented to estimate the elastic properties and failure mechanisms of an assembly of random, brittle microbubbles. The approach is based on the mechanics of frictionless micro-contact between hollow spherical shells by employing relations from classical shell theory and verified by two dimensional axisymmetric Finite Elements. The estimated values are in agreement with available experimental values. Moreover, a granular type analytical homogenization model provides an isotropic elastic constitutive law to be used for the macroscopic deformation of an assembly of glass micro-bubbles when it is compressed by external loads. In addition, approximate estimates are also proposed for two important micro-failure mechanisms of such assemblies that relate either to the splitting or to the buckling of a brittle spherical shell, prior its complete crushing. The results are novel and are expected to enhance the application of glass microbubbles directly in acute thermal insulation problems such as liquid hydrogen storage. KW - LH2 KW - Cryogenic Vessels KW - Insulation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634354 DO - https://doi.org/10.1016/j.ijsolstr.2025.113528 SN - 0020-7683 VL - 320 SP - 1 EP - 11 PB - Elsevier BV CY - Amsterdam AN - OPUS4-63435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shasmal, Nilanjana T1 - Effects of Direct femtosecond laser writing on chloroborosilicate glasses doped with Eu3+/Eu2+ and CdS quantum dots N2 - Femtosecond (fs) direct laser writing (DLW) is a promising technique for developing nano-inhomogeneous materials with advanced optical properties and for fabricating novel photonic devices such as integrated waveguides, ultrafast optical switches, phase plates, and 3D optical memory. In this study, DLW was applied to chloroborosilicate glasses that were singly and co-doped with Eu and CdS quantum dots (QDs). The glasses were laser-treated within a very narrow range of experimental conditions, resulting in laser-inscribed sites exhibiting enhanced emission, similar to the glass-ceramics crystallized from the as-prepared glass. In the regions crystalized by DLW a significant reduction of Eu3+ to Eu2+ was verified by photoluminescence spectroscopy. However, the characteristics of the emission bands of Eu2+ changed markedly in the laser-treated sites as compared to the emission spectra of the same glass crystallized by heat treatment. A considerable redshift and splitting of the emission band were observed, attributed to changes in the surrounding environment of the rare earth (RE) ions which was, in turn, attributed to an alteration in the coordination number of Ba2 + and/or Eu2+ as a result of the high-power laser treatment. Although there was an issue with homogeneity of the glass in the micro-level, which restricts some of the aspects of the DLW, these findings suggest the potential for structural modifications through laser treatment, which could be harnessed to create new functionalities for advanced optical applications. T2 - ICG 2025 (27th International Congress on Glass) CY - Kolkata, India DA - 20.01.2025 KW - Femtosecond direct laser writing KW - DLW KW - CdS quantum dots KW - Eu/CdS co-doped glass PY - 2025 AN - OPUS4-65285 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ruehle, Bastian T1 - A Self-Driving Lab for Nano and Advanced Materials Synthesis 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, new tools that enhance the development and optimization cycle of nano- and advanced materials are 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 the processing 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). 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. We also present several key aspects of the central backend that orchestrates the (parallelized) syntheses workflows. One key feature is the resource management or “traffic control” for scheduling and executing parallel reactions in a multi-threaded environment. Another is the interface with data analysis algorithms from in-line, at-line, and off-line measurements. Here, we will give examples of how automatic image segmentation of electron microscopy images with the help of AI [2] can be used for reducing the “data analysis bottleneck” from an off-line measurement. We will also discuss various machine learning (ML) algorithms that are currently implemented in the backend and can be used for ML-guided, closed-loop material optimization in our SDL. Lastly, we will show our recent efforts [3] in making the workflow generation on SDLs more user-friendly by using large language models to generate executable workflows automatically from synthesis procedures given in natural language and user-friendly graphical user interfaces based on node editors that also allow for knowledge graph extraction from the workflows. In this context, we are currently also working on a common description or ontology for representing the process steps and parameters of the workflows, which will greatly facilitate the semantic description and interoperability of workflows between different SDL hardware and software platforms. 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 - MRS Fall Meeting 2025 CY - Boston, MA, USA DA - 30.11.2025 KW - Self-Driving Labs KW - Materials Acceleration Platforms KW - Advanced Materials KW - Nanomaterials KW - Automation PY - 2025 AN - OPUS4-65129 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ankli, P. P. A1 - Abdelwahab, A. A. A1 - Logachov, A. A1 - Bugiel, R. A1 - Drobne, D. A1 - Novak, S. A1 - Kranjc, E. A1 - Saje, S. A1 - Pellegrino, F. A1 - Alladio, E. A1 - Sordello, F. A1 - Corrao, E. A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg A1 - Mrkwitschka, Paul A1 - Madbouly, Loay Akmaal A1 - Akdemir, Yücel A1 - Gulumian, M. A1 - Wepener, V. A1 - Andraos, C. A1 - Boodhia, K. A1 - Jones, E. A1 - Doolin, A. A1 - Leuchtenberg, K. A1 - Valsami Jones, E. A1 - Rocca, C. A1 - Ibrahim, B. A1 - Singh, D. A1 - Chakraborty, S. A1 - Jurkschat, K. A1 - Johnston, C. A1 - Van Der Zande, M. A1 - Fernandez, D. A1 - Queipo, P. A1 - Clifford, C. A1 - Hardy, B. T1 - Knowledge Infrastructure supporting image-based characterisation of 2D graphene materials N2 - As part of the European Horizon ACCORDs project, advanced methods are being developed for the image-based characterisation of 2D nanomaterials. Given the complexity of this task, robust nd wellorganised data management is critical to ensuring high-quality outcomes. To support this, we have established a knowledge infrastructure that serves as the central repository for protocols, images and experimental data which are stored in a standardised, harmonised manner and in accordance with the FAIR principles – Findable, Accessible, Interoperable and Reusable and open science. This machine-readable framework enables the systematic and computationally automated correlation of image features with experimental descriptors, facilitating accurate material characterisation and transparent reporting which is all integrated in the ACCORDs KI. KW - Graphene-related 2D materials (GR2M) KW - 2D materials KW - Knowledge infrastructure KW - Characterisation PY - 2025 DO - https://doi.org/10.1016/j.toxlet.2025.07.660 SN - 0378-4274 VL - 411 SP - S281 EP - S282 PB - Elsevier B.V. AN - OPUS4-65061 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ciornii, Dmitri A1 - Hodoroaba, Vasile-Dan A1 - Wachtendorf, Volker A1 - Fengler, Petra A1 - Altmann, Korinna T1 - Interlaboratory Comparison Reveals State of the Art in Microplastic Detection and Quantification Methods N2 - In this study, we investigate the current accuracy of widely used microplastic (MP) detection methods through an interlaboratory comparison (ILC) involving ISO-approved techniques. The ILC was organized under the prestandardization platform of VAMAS (Versailles Project on Advanced Materials and Standards) and gathered a large number (84) of analytical laboratories across the globe. The aim of this ILC was (i) to test and to compare two thermo-analytical and three spectroscopical methods with respect to their suitability to identify and quantify microplastics in a water-soluble matrix and (ii) to test the suitability of the microplastic test materials to be used in ILCs. Two reference materials (RMs), polyethylene terephthalate (PET) and polyethylene (PE) as powders with rough size ranges between 10 and 200 μm, were used to press tablets for the ILC. The following parameters had to be assessed: polymer identity, mass fraction, particle number concentration, and particle size distribution. The reproducibility, SR, in thermo-analytical experiments ranged from 62%−117% (for PE) and 45.9%−62% (for PET). In spectroscopical experiments, the SR varied between 121% and 129% (for PE) and 64% and 70% (for PET). Tablet dissolution turned out to be a very challenging step and should be optimized. Based on the knowledge gained, development of guidance for improved tablet filtration is in progress. Further, in this study, we discuss the main sources of uncertainties that need to be considered and minimized for preparation of standardized protocols for future measurements with higher accuracy. KW - Microplastics KW - Interlaboratory comparison KW - PlasticsFatE KW - PET KW - PE KW - Reference materials KW - VAMAS KW - Thermo-analytical methods KW - Spectroscopical methods PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630462 DO - https://doi.org/10.1021/acs.analchem.4c05403 SN - 1520-6882 VL - 97 SP - 8719 EP - 8728 PB - ACS Publications AN - OPUS4-63046 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Reliable physico–chemical characterisation of graphene-related and other 2D materials: present and future N2 - In the path of commercialisation of graphene-related and other 2D materials the consolidation has begun. In this phase, it is important to build trust between the individual partners in the product value chain. This requires trustworthy statements based on reliable and reproducible material characterisation. The first steps have been taken to measure graphene and other related 2D materials (GR2Ms) under well-defined conditions. Measurands and protocols for key methods were made available for this purpose. But there are still some challenges to overcome such as (i) reference materials, (ii) reference data, (iii) reproducibility throughout the workflow, (iv) credible structure-activity relationships, bringing the standards to (v) the factory floor and to (vi) real-word products. In addition, 2D materials beyond graphene should also be considered exploiting the knowledge gained from the characterisation of GR2M. KW - 2D Materials KW - Commercialisation KW - Standardisation KW - Trust PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638122 DO - https://doi.org/10.1088/2053-1583/aded9d SN - 2053-1583 VL - 12 IS - 4 SP - 1 EP - 8 PB - IOP Publishing AN - OPUS4-63812 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wolf, M. E. A1 - Vickery, W. M. A1 - Swift-Ramirez, W. A1 - Arnold, A. M. A1 - Orlando, J. D. A1 - Schmidt, S. J. A1 - Liu, Y. A1 - Er, Jasmin A1 - Schusterbauer, Robert A1 - Ahmed, R. A1 - Nickl, Philip A1 - Radnik, Jörg A1 - Donskyi, Ievgen A1 - Sydlik, S. A. T1 - The Mitsunobu reaction for the gentle covalent attachment of biomolecules to graphene oxide N2 - Graphene oxide (GO) has emerged as a promising biomaterial as it is easily and cheaply synthesized, strong, cytocompatible, osteoinductive, and has a well-characterized aqueous degradation pathway. It is also a great substrate for functionalization with biomolecules such as proteins, peptides, and small molecules that can enhance or add bioactivity. Covalent chemical linkages as opposed to typical noncovalent association methods are preferable so that the biomolecules do not quickly diffuse away or face replacement by other proteins, which is critical in long time scale applications like bone regeneration. However, covalent chemistry tends to carry a drawback of harsh reaction conditions that can damage the structure, conformation, and therefore function of a delicate biomolecule like a protein. Here, the Mitsunobu reaction is introduced as a novel method of covalently attaching proteins to graphene oxide. It features gentle reaction conditions and has the added benefit of utilizing the plentiful basal plane alcohol functionalities on graphene oxide, allowing for high yield protein functionalization. The amino acid Glycine (G), the protein bovine serum albumin (BSA), and the small molecule SVAK-12 are utilized to create the three Mitsunobu Graphene (MG) materials G-MG, BSA-MG, and SVAK-MG that demonstrate the wide applicability of this functionalization method. KW - Graphene oxide KW - Mitsunobu reaction KW - Covalent attachment KW - Bovine serum albumin KW - Macrophage polarization KW - Osteogenesis PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630483 DO - https://doi.org/10.1016/j.carbon.2025.120221 VL - 238 SP - 1 EP - 15 PB - Elsevier Ltd. AN - OPUS4-63048 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chemello, Giovanni A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - XPS–SEM/EDS Tandem Analysis for the Elemental Composition of Functionalized Graphene Nanoplatelets N2 - Over the past decade, energy-dispersive X-ray spectrometry (EDS) with scanning electron microscopy (SEM) has advanced to enable the accurate analysis of light elements such as C, N, or O. For this reason, EDS is becoming increasingly interesting as an analytical method for the elemental analysis of functionalized graphene and could be an attractive alternative to Xray photoelectron spectroscopy (XPS), which is considered the most important method for elemental analysis. In this study, comparative XPS and EDS investigations under different excitation conditions are carried out on commercially available powders containing graphene particles with different morphologies. The slightly different XPS/HAXPES and EDS results can be explained by the different information depths of the methods and the functionalization of the particle surfaces. For the material with smaller graphene particles and higher O/C ratios, all methods reported a lower O/C ratio in pellets compared with the unpressed powder samples. This clearly shows that sample preparation has a significant influence on the quantification results, especially for such a type of morphology. Overall, the study demonstrates that EDS is a reliable and fast alternative to XPS for the elemental quantification of functionalized graphene particles, provided that differences in the information depth are taken into account. Particle morphology can be examined in parallel with quantitative element analysis, since EDS spectrometers are typically coupled with SEM, which are available in a huge number of analytical laboratories. KW - Graphene oxide KW - SEM/EDS KW - XPS/HAXPES KW - Elemental composition KW - Functionalization PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647294 DO - https://doi.org/10.1021/acsomega.5c07830 SN - 2470-1343 SP - 1 EP - 7 PB - American Chemical Society (ACS) AN - OPUS4-64729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mrkwitschka, Paul A1 - Sahre, Mario A1 - Zurutuza, Amaia A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Standardized Chemical Composition Analysis of Graphene Oxide Flakes with SEM/EDS and XPS Works Reliably N2 - Suspensions of graphene-related 2D materials (GR2M) are broadly used for further applications like printable electronics. The reliable quantification of the composition of graphene-related 2D materials as liquid suspensions is still a challenging task, which can hinder the commercialisation of the products. Specific parameters to be measured are defined, e.g. the oxygen-to-carbon (O/C) concentration ratio, the trace metal impurities, or the functional groups present, but reference protocols are still missing. One of the central methods for the quantification is X-ray photoelectron spectroscopy (XPS) as a rather expensive method. Therefore, the development of cheaper alternatives is highly desired. One attractive alternative of XPS is energy-dispersive spectroscopy (EDS) which is usually coupled with scanning electron microscopy (SEM). This combination is one of the most widely used methods in analytical laboratories. In this contribution the results of a systematic study on the capability of SEM/EDS to reliably quantify the O/C ratio in a well-defined and well-characterized graphene oxide material are presented. The robustness of the SEM/EDS results obtained at various measurement conditions (various excitation energies) is tested by comparing the results to the established XPS analysis, which has been carried out on the same samples. It is demonstrated that for samples prepared by drop-casting on a substrate, both surface-sensitive XPS analysis and bulk-characterising EDS result in very similar elemental composition of oxygen and carbon for thick spots. Further, the effect of untight deposited material enabling co-analysis of the (silicon) substrate, is evaluated for both methods, XPS and EDS. The last results clearly show the influence of the substrate on the analysis of the results and stressed out the importance of the sample preparation. KW - EDS KW - Light elements KW - XPS/HAXPES KW - Graphene oxide KW - Quantification KW - Standardisation PY - 2025 DO - https://doi.org/10.1093/mam/ozaf048.267 VL - 31 IS - 7 SP - 531 EP - 532 PB - Oxford Aacademic AN - OPUS4-63792 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Reusable data: putting the “Arr” in FAIR N2 - This talk demonstrates how to apply FAIR principles to data from actual scientific investigations. The reasons and practical benefits of FAIR data are highlighted. Several levels of reusability are discussed, i.e. the “trust me”-level, the “I’ll not need to repeat my measurement”-level, and the “you’ll not need to repeat my measurements”-level. Practical FAIR datafiles are explored and their information content highlighted. T2 - Reusability of Scientific Data for Matter CY - Online meeting DA - 13.11.2025 KW - Methodology KW - Metadata KW - FAIR KW - Reusability KW - X-ray scattering KW - Traceability PY - 2025 AN - OPUS4-65309 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Standardized Chemical Characterisation of Graphene Oxide Flakes by X-Ray Photoelectron Spectroscopy and Energy-Dispersive X-Ray Spectroscopy N2 - Reliable quantification of the chemical composition of graphene-related 2D materials as powders and liquid suspensions is a challenging task. Analytical methods such as XPS, ICP-MS, TGA and FTIR are recommended to be used in ongoing projects at standardisation bodies. The specific parameters to be measured are also defined, e.g. the oxygen-to-carbon (O/C) concentration ratio, the trace metal impurities, or the functional groups present [1]. In this contribution, for the first time, the results of a systematic study on the capability of SEM/EDS to reliably quantify the O/C ratio in a well-defined and well-characterized graphene oxide material [2] are presented. It is expected that the quantitative EDS analysis of light elements emitting characteristic X-ray lines below 1 keV to be provided with significantly larger measurement uncertainties than the analysis of elements with an atomic number of 11 (Na) or above [3]. The robustness of the SEM/EDS results obtained at various measurement conditions (various excitation energies) is tested by comparing the results to the established XPS analysis [4], which has been carried out on the same samples. A crucial step in sample preparation from liquid suspension with graphene oxides flakes onto a substrate for analysis with both XPS and EDS. It is demonstrated that if a closed and enough thick drop-cast deposited spot is succeeded to be deposited on a substrate, both surface-sensitive XPS analysis and bulk-characterising EDS result in very similar elemental composition of oxygen and carbon. Hence, theoretical, expected O/C atomic ratio values for pure graphene oxide of ~0.5 [1] are achieved (with both methods), see Figure 1. Further, the effect of untight deposited material enabling co-analysis of the (silicon) substrate, is evaluated for both methods, XPS and EDS. To note that all the EDS results in this study have been quantified standardless. The results of this study demonstrate the reliability of the reference measurement protocol for SEM/EDS to be introduced into ISO/DTS 23359, including the dedicated sample preparation, particularly for the cases when the concentration of the GO flakes in stock liquid suspension is low. Further, also the consideration of this GO material as one of the very few available as a commercial material on the market as the very first GO reference material with regard to its morphology as well as chemical composition. Both the standard measurement procedure and the candidate reference material will immensely contribute to characterise reliably the chemical composition of graphene-related 2D materials with SEM/EDS as one of the most widely used methods in analytical laboratories T2 - EMAS 2025 Workshop CY - Mataró, Spain DA - 11.05.2025 KW - Advanced Materials KW - Graphene KW - Chemical Quantification KW - EDX KW - XPS PY - 2025 AN - OPUS4-64082 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Wire-print procedure for accurate morphological and Chemical characterization of graphene-related 2D-materials N2 - One of the biggest challenges in the physico-chemical characterization of particulate nanomaterials pertains to the sample preparation. Particularly the imaging methods require suitable deposition of the sample on a substrate. ‘Suitable’ sample preparation of a particulate (nano)material on a substrate means to make visible the constituent particles to a microscopy technique able to analyze the nanoscale (AFM, SEM, TEM, etc). The particles deposited on a substrate either directly as a powder or from liquid suspension must be ideally isolated (de-agglomerated), without particle losses, homogeneously distributed in a high density of particles per substrate area for efficient analysis, with good statistics of the counted particles. Various sample preparation approaches to meet the latter requirements have been reported in the literature, e.g. electrospray, substrate surface treatment, embedding the particulate material and polishing the cross-section, or addition of ligands to the suspended nanostructures to enhance their hydrophilicity [1], [2], [3], [4]. In this study we have systematically tested the efficacy of a new deposition procedure for graphene-related 2D materials (GR2M’s) from liquid suspension onto a substrate for quantitative analysis of their size and shape distribution with electron microscopy. The technique is an extension of the conventional drop-casting method, and we have designated it “wire-print” deposition. It consists of two steps, first one being usual drop-casting on a copper substrate and second one involving a thin copper wire with a sub-mm diameter being dipped into the deposited droplet and retracted with a corresponding half-spherical droplet attached on its tip and final deposition of this entire nL-amount of suspension onto e.g. a silicon wafer for microscopical, detailed analysis. The result of 11 series of such a wire-print deposition for a graphene-based ink is shown in Figure 1 (labeled A-L), where various conditions (treatment of the starting suspension) have been experimented with a repetition of up to 10 times per condition, all together 86 spots on a silicon wafer of 10 mm x 10 mm. The result of one series of 8 repeated wire-print depositions is shown in Figure 2, where the deposited spots are visualized with SEM. Note the weak presence of coffee-rings, irregular spot shape, and presence of agglomerates. The results for the measured flake size distribution expressed as ECD (equivalent circular diameter) are represented in Fig. 3 for all the eight depositions. Both the mean value of the 8 ECD distributions and the total number of flakes deposited in each spot show a variance in the range of 17% and 22%, respectively, see Table 1. In the context of accurate analysis of such challenging complex materials these numbers can be considered as excellent and demonstrate the high benefit of the wire-print deposition for accurate morphological measurements on GR2M’s. T2 - Microscopy and Microanalysis 2025 CY - Salt Lake City, UTAH, USA DA - 27.07.2025 KW - Sample preparation KW - Graphene KW - Electron Microscopy KW - Morphology PY - 2025 AN - OPUS4-64083 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Waqfi, R. A. A1 - Khan, C. J. A1 - Irving, O. J. A1 - Matthews, Lauren A1 - Albrecht, T. T1 - Crowding Effects during DNA Translocation in Nanopipettes N2 - Quartz nanopipettes are an important emerging class of electric single-molecule sensors for DNA, proteins, their complexes, as well as other biomolecular targets. However, in comparison to other resistive pulse sensors, nanopipettes constitute a highly asymmetric environment and the transport of ions and biopolymers can become strongly directiondependent. For double-stranded DNA, this can include the characteristic translocation time and tertiary structure, but as we show here, nanoconfinement can also unlock capabilities for biophysical and bioanalytical studies at the single-molecule level. To this end, we show how the accumulation of DNA inside the nanochannel leads to crowding effects, and in some cases reversible blocking of DNA entry, and provide a detailed analysis based on a range of different DNA samples and experimental conditions. Moreover, using biotin-functionalized DNA and streptavidinmodified gold nanoparticles as target, we demonstrate in a proof-of-concept study how the crowding effect, and the resulting increased residence time in nanochannel, can be exploited by first injecting the DNA into the nanochannel, followed by incubation with the nanoparticle target and analysis of the complex by reverse translocation. We thereby integrate elements of sample processing and detection into the nanopipette, as an important conceptual advance, and make a case for the wider applicability of this device concept. KW - DNA translocation KW - Transport KW - Resistive-pulse sensing KW - Nanopores KW - Nanopipettes KW - Crowding KW - Confinement PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630448 DO - https://doi.org/10.1021/acsnano.5c01529 SN - 1936-086X VL - 19 IS - 17 SP - 1 EP - 9 PB - ACS Publications AN - OPUS4-63044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pellegrino, F. A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - Unveiling Order in Graphene Oxide Synthesis Through A Design of Experiment and Chemometric Strategy Based on Tour’s Method N2 - Graphene oxide (GO), a derivative of graphene containing oxygen functional groups, shows significant potential for a wide range of applications due to its unique electrical, mechanical, and chemical properties. Traditional synthesis methods, such as Tour's method, often rely on trial-and-error, leading to variations in product quality and yield. To address these challenges, we applied Design of Experiments (DoE) to systematically investigate the effects of key synthesis parameters, including reaction temperature, reaction time, and oxidant concentration. We identified the most significant factors influencing GO characteristics using a Plackett-Burman design and chemometric analysis. Our results highlight that the oxidation level is the most critical factor, impacting outcomes observed through various characterization techniques, such as UV-Vis spectroscopy and X-Ray Diffraction. Principal Component Analysis (PCA) and Multiple Linear Regression (MLR) provided insights into the synthetic parameters most strongly affecting material properties. While some findings aligned with expectations, others were counterintuitive. For instance, oxidation temperature had a minimal effect on the final material characteristics and may not need to be prioritized in the synthesis process. On the other hand, stirring was found to enhance the homogeneity of the material and promote more uniform oxidation. This study demonstrates the effectiveness of DoE in the controlled production of graphene oxide, offering a reliable framework for manufacturing high-quality GO tailored to specific applications. By minimizing time and resource consumption, this approach is increasingly relevant in the context of materials science, which demands higher quality, safety and sustainability standards. T2 - Joint Regulatory Risk Assessors Summit – Advancing Safety & Sustainability Assessments of Advanced Materials CY - Paris, France DA - 19.06.2025 KW - Graphene oxide KW - Chemometry KW - UV-Vis KW - XRD KW - XPS KW - EDX PY - 2025 UR - https://macrame-project.eu/macrame-meetings-workshops/jointrras/#Agenda AN - OPUS4-63676 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Xing, Na A1 - Er, Jasmin A1 - Vidal, Ricardo M. A1 - Khadka, Sandhya A1 - Schusterbauer, Robert A1 - Rosentreter, Maik A1 - Etouki, Ranen A1 - Ahmed, Rameez A1 - Page, Taylor A1 - Nickl, Philip A1 - Bawadkji, Obida A1 - Wiesner, Anja A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan A1 - Ludwig, Kai A1 - Trimpert, Jakob A1 - Donskyi, Ievgen T1 - Scalable covalently functionalized black phosphorus hybrids for broadspectrum virucidal activity N2 - At the onset of viral outbreaks, broad-spectrum antiviral materials are crucial before specific therapeutics become available. We report scalable, biodegradable black phosphorus (BP) hybrids that provide mutation-resilient virucidal protection. BP sheets, produced via an optimized mechanochemical process, are covalently functionalized with 2-azido-4,6-dichloro- 1,3,5-triazine to form P=N bonds. Fucoidan, a sulfated polysaccharide with intrinsic antiviral activity, and hydrophobic chains are then incorporated to achieve irreversible viral deactivation. The material exhibits strong antiviral inhibition and complete virucidal activity against multiple viruses, including recent severe acute respiratory syndrome coronavirus-2 (SARS-CoV-2) variants. It maintains high biocompatibility, remains effective against viral mutations, and is shelf stable for at least five month. The combination of biodegradability, scalable synthesis, and synergistic antiviral and virucidal mechanisms establishes BP-conjugates as a new class of highly efficient antivirals. They offer a broad spectrum antiviral solutions that could bridge the gap between antiviral medicines and general antiseptics. KW - Black phosphorus KW - Antiviral materials KW - Functionalization KW - Biodegradability KW - Sheets PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652941 DO - https://doi.org/10.48550/arXiv.2510.12854 SN - 2331-8422 SP - 1 EP - 22 PB - Cornell University CY - Ithaca, NY AN - OPUS4-65294 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - The role of Critical Raw Materials in Advanced Materials for the Energy Transition N2 - The energy transition needs advanced materials, especially for batteries, solar cells, and fuel cells. Therefore, critical raw materials are necessary. In this presentation the use of critcal raw materials and strategies for the optimisation of their use are discussed. T2 - Critical Raw Material Workshop during VAMAS Annual Meeting CY - Teddington, United Kingdom DA - 17.09.2025 KW - Advanced solar cells KW - Iridium oxide KW - Aerogels KW - Advanced carbon materials PY - 2025 AN - OPUS4-64290 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mrkwitschka, Paul A1 - Mühlbauer, Michaela A1 - Rossi, Andrea A1 - Pellegrino, Francesco A1 - Zurutuza, Amaia A1 - Radnik, Jörg A1 - Meier, Florian A1 - Hodoroaba, Vasile-Dan T1 - Morphological Analysis of Graphene Oxide by Scanning Electron Microscopy and Correlative Field-flow Fractionation Coupled with Multi-angle Light Scattering N2 - In this paper graphene related 2D materials (GR2M) arre investigated by centrifugal field flow fractioning (CF3) and SEM. Three materials were selected as case studies (CS): graphene „HD-G (CS I), graphene oxide UniTo“ (CS II), and graphene oxide „Graphenea“ (CS III). For CS I particles were evaluated as constituent particles in agglomerates, for the other two materials only isolated (non aggregated/agglomerated) flakes were considered for determination of the area equivalent circular diameter (ECD). Size analysis of all three materials was carried out by CF3 coupled with MALS (Multi-Angle Light Scattering). For evaluation, it was found that the data obtained was best suited to a disc model. Results are in good agreement when compared to the sizes obtained before CF3 analysis. CS II material is too heterogenous to accurately determine flake size by imaging. CF3 coupled with MALS enables to assess fractions within the highly heterogenous material of CS II. Imaging of the material in CS III after CF3 measurement indicates that the procedure is non-destructive. This could not be verified for the CS‘s I & II As a next step we plan to analyse the fractionated samples by imaging them within a SEM wet-cell. KW - 2D Materials KW - SEM KW - Centrifugal field flow fractionation (CF3) KW - Imaging KW - Size distribution PY - 2025 DO - https://doi.org/10.1093/mam/ozaf048.222 VL - 31 IS - 7 SP - 442 EP - 443 PB - Oxford Academic AN - OPUS4-63804 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Methodologies implemented to measure key properties of graphene and other 2D materials N2 - The key properties and suitable measurement methods for the characterization of graphene-related 2D materials are presented. A case study will be discussed about the chemical characterisation of functionalised graphene used in inks along the production chain. T2 - European-African Graphene Workshop CY - Parys, South Africa DA - 26.11.2025 KW - X-ray photoelectron spectroscoyp KW - Raman spectroscopy KW - Defects KW - Surface Chemistry PY - 2025 AN - OPUS4-64959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Liaison Report ISO/TC 229 Nanotechnology for ISO/TC 202 Microbeam Analysis and vice-versa N2 - The liaison between the ISO technical committees TC 229 Nanotechnologies and TC 202 Microbeam analysis is described in detail with highlight on the projects under development and published since 2024 and which involve input /knowledge from ISO/TC 202. T2 - 32nd Plenary Meeting of ISO/TC 202 Microbeam Analysis CY - London, United Kingdom DA - 28.10.2025 KW - Nanotechnology KW - Microabeam analysis KW - Standardisation KW - ISO PY - 2025 AN - OPUS4-64551 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Energy-Dispersive X-Ray Spectrometry (EDS) on GR2Ms for Routine/Standardized Elemental Analysis N2 - The elemental analysis of solid matter by means of the Energy-Dispersive X-Ray Spectrometry (EDS) is meanwhile posible as a quick (seconds!) and more and more accurate analysis via standardsless (instantaneous) quantification. The sensitivity & quantification accuracy for light elements (C, O,..) has significantly increased in the recent years. The availability via table-top SEMs with incorporated EDS is also enhanced. Further, the EDS analysis at an SEM is well-standardized, see ISO/TC 202 Microbeam Analysis & VAMAS/ TWA 37 Quantitative Microstructural Analysis in good liaisonships with ISO/TC 229 Nanotechnologies. It is demostrated that key parameters such as oxygen-to-carbon atomic-% ratio and impurities can be realibly measured, with XPS as a reference method. Various EDS spectrometers and analysis conditions are tested and the validity of the EDS quantification of an ionic liquid of well-defined chemical composition is demonstrated. Next steps are: launch of a corresponding VAMAS interlaboratory comparison and discussions within ISO/TC 202 Microbeam Analysis. T2 - 32nd Plenary Meeting of ISO/TC 202 Microbeam Analysis CY - London, United Kingdom DA - 28.10.2025 KW - GR2M KW - EDS KW - Quantification KW - XPS KW - Light elements KW - 2D materials PY - 2025 AN - OPUS4-64553 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Methodologies implemented to measure key properties of graphene and other 2D materials - EDX N2 - The elemental analysis of solid matter by means of the Energy-Dispersive X-Ray Spectrometry (EDS) is meanwhile posible as a quick (seconds!) and more and more accurate analysis via standardsless (instantaneous) quantification. The sensitivity & quantification accuracy for light elements (C, O,..) has significantly increased in the recent years. The availability via table-top SEMs with incorporated EDS is also enhanced. It is demostrated that key parameters such as oxygen-to-carbon atomic-% ratio and impurities can be realibly measured, with XPS as a reference method. Various EDS spectrometers and analysis conditions are tested and the validity of the EDS quantification of an ionic liquid of well-defined chemical composition is demonstrated. T2 - Advanced Materials Graphene: The implementation of SbD and SSbD CY - Parys, South Africa DA - 26.11.2025 KW - Light elements KW - EDS KW - Quantification KW - Oxygen-to-carbon ratio KW - XPS KW - Graphene-realted 2D materials PY - 2025 AN - OPUS4-64943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Energy Dispersive X Ray Spectrometry (EDS) on GR2Ms for Routine/Standardized Elemental Analysis N2 - The elemental analysis of solid matter by means of the Energy-Dispersive X-Ray Spectrometry (EDS) is meanwhile posible as a quick (seconds!) and more and more accurate analysis via standardsless (instantaneous) quantification. The sensitivity & quantification accuracy for light elements (C, O,..) has significantly increased in the recent years. The availability via table-top SEMs with incorporated EDS is also enhanced. Further, the EDS analysis at an SEM is well-standardized, see ISO/TC 202 Microbeam Analysis & VAMAS/ TWA 37 Quantitative Microstructural Analysis in good liaisonships with ISO/TC 229 Nanotechnologies. It is demostrated that key parameters such as oxygen-to-carbon atomic-% ratio and impurities can be realibly measured, with XPS as a reference method. Various EDS spectrometers and analysis conditions are tested and the validity of the EDS quantification of an ionic liquid of well-defined chemical composition is demonstrated. Next steps are: launch of a corresponding VAMAS interlaboratory comparison and discussions within ISO/TC 202 Microbeam Analysis. T2 - ISO/TC 229 Nanotechnologies Meeting Week CY - Stockholm, Sweden DA - 19.05.2025 KW - Graphene-related 2D materials (GR2M) KW - Energy-Dispersive X-Ray Spectrometry (EDS) KW - Elemental analysis KW - Quantification KW - ISO/TC 229 Nanotechnologies PY - 2025 AN - OPUS4-63190 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Report VAMAS/TWA 37 "Quantitative Microstructural Analysis" & Liaison with ISO/TC 202 "Microbeam Analysis" N2 - The progress in activities on Quantitative MicroStructural Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 Microbeam Analysis is presented and discussed with respect to the identification and launching corresponding VAMAS projects. The ongoing projects "Development of guidelines for reproducible TEM specimen preparation by FIB processing", "Measurement of dislocation density in metallic materials by Transmission Electron Microscope (TEM)", "Repeatability of high angular resolution electron backscatter diffraction (HR-EBSD) analysis for elastic strain measurements", "Measurement of grain size and distribution of nanocrystalline nickel by using Transmission Kikuchi Diffraction (TKD) in SEM" and the just started project "Evaluation Method of Surface Layer Quality of TEM Specimen Prepared by focused Ion Beam Processing" are presented in detail. T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 50th Steering Committee Meeting CY - London, United Kingdom DA - 15.09.2025 KW - VAMAS KW - Interlaboratory comparison KW - Microbeam Analysis KW - Electron Microscopy KW - ISO/TC 202 KW - Sample preparation PY - 2025 AN - OPUS4-64231 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Deep Insights into Functionalised Nanoparticles with Photoelectron Spectroscopy N2 - Modern instrumentation X-ray photoelectron instrumentation combines soft and hard X-rays. Additonally, in the last years methods were developed for the analysis of the measurement data to elucidate the composition and thickness of coatings of nanoparticles. In this presentation four examples will be presented: quantum dots, silica-coated iron-oxide nanoparticles, mixed Fe-Ni-O nanoparticles and amine-functionalized silica nanoparticles. These different nanoparticles are used for displays, for biomedicine, for water splitting, and as additives and fillers. T2 - United Kingdom Surface Analysis Forum Meeting 2025 CY - Teddington, UK DA - 15.07.2025 KW - Simulation KW - Oxygen evolution reaction KW - Transmission electron microscopy KW - Quantitative nuclear magnetic resonance (qNMR) PY - 2025 AN - OPUS4-63733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Analysis of Nanoparticles N2 - The determination of the thickness and composition of the coating is crucial for the understanding of the properties of nanoparticles. Four different approaches will be presented: (i) numerical methods, (ii) descriptive formulae, (iii) the simulation of spectra with Monte-Carlo methods, and (iv) inelastic background analysis. The advantages and limits of these methods will be discussed. T2 - XPS Workshop CY - Teddington, United Kingdom DA - 14.07.2025 KW - Numerical simulation KW - Emperical formulae KW - Simulation KW - Inelastic background analysis PY - 2025 AN - OPUS4-63732 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Interlaboratory comparisons for validated measurements of the surface chemistry of nanomaterials N2 - Interlaboratory comparisons are essential tools for validating new protocols or methods. The properties of advanced materials are largely determined by surface chemistry. Using a VAMAS interlaboratory comparison on the surface functionalization of GR2DM, it is explained what insights can be gained from such a comparison.” T2 - Nanomesure France Journee technique CY - Paris, France DA - 04.11.2025 KW - VAMAS KW - Functionalized graphene KW - X-ray photoelectron spectroscopy PY - 2025 AN - OPUS4-65002 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altmann, Korinna A1 - Wimmer, Lukas A1 - Alcolea-Rodriguez, Victor A1 - Waniek, Tassilo A1 - Wachtendorf, Volker A1 - Matzdorf, Kay A1 - Ciornii, Dmitri A1 - Fengler, Petra A1 - Milczewski, Frank A1 - Otazo-Aseguinolaza, Itziar A1 - Ferrer, Manuel A1 - Bañares, Miguel A. A1 - Portela, Raquel A1 - Dailey, Lea Ann T1 - Quality-by-design and current good practices for the production of test and reference materials for micro- and nano-plastic research N2 - Understanding the environmental and human health impacts of micro- and nanoplastic pollutants is currently a high priority, stimulating intensive methodological research work in the areas of sampling, sample preparation and detection as well as intensive monitoring and testing. It is challenging to identify and quantify microplastics in complex organic matrices and concepts for nanoplastic detection are still in their infancy. All analytical techniques employed in studying micro- and nanoplastics require suitable reference materials for validation measurements, with requirements as diverse as the analytical tools used, ranging from different polymer types, size distributions and shapes of the material to the concentrations employed in different experimental set ups (ng to g amounts). The aim of this manuscript is to outline current good practices for small-scale laboratory production and characterization of suitable test and reference materials. The focus is placed on top-downfragmentation methods as well as bottom-up precipitation methods. Examples using polyethylene, polypropylene, polystyrene and polyethylene terephthalate with size distribution classes of mainly 10–1000, 1–10 and <1 μm particles will be provided. Experiences and suggestions on how to produce well-characterized micro- and nano-plastics for internal research needs will ensure that studies using the materials have robust and informative outcomes. KW - Mmicroplastics KW - Nanoplastics KW - Reference materials KW - Standard validation method PY - 2025 DO - https://doi.org/10.1016/j.jhazmat.2025.139595 SN - 0304-3894 VL - 497 SP - 1 EP - 20 PB - Elsevier B.V. AN - OPUS4-63958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cosimi, Andrea A1 - Stöbener, Daniel D. A1 - Nickl, Philip A1 - Schusterbauer, Robert A1 - Donskyi, Ievgen A1 - Weinhart, Marie T1 - Interfacial nanoengineering of hydrogel surfaces via block copolymer self-assembly N2 - Synthetic polymer hydrogels are valuable matrices for biotransformations, drug delivery, and soft implants. While the bulk properties of hydrogels depend on chemical composition and network structure, the critical role of interfacial features is often underestimated. This work presents a nanoscale modification of the gel−water interface using polymer brushes via a straightforward “grafting-to” strategy, offering an alternative to more cumbersome “grafting-from” approaches. Functional block copolymers with photoreactive anchor blocks are successfully self-assembled and UV-immobilized on hydrogel substrates despite their low solid content (<30 wt %). This versatile technique works on both bulk- and surface-immobilized hydrogels, demonstrated on poly(hydroxypropyl acrylate), poly(N-isopropylacrylamide), and alginate gels, allowing precise control over grafting density. X-ray photoelectron spectroscopy and time-of-flight secondary ion mass spectrometry revealed a homogeneous bilayered architecture. By “brushing-up”, the hydrogels’ interface can be tailored to enhance protein adsorption, improve cell adhesion, or impair the diffusive uptake of small molecules into the bulk gels. This effective interfacial nanoengineering method is broadly applicable for enhancing hydrogel performance across a wide range of applications. KW - Brushing-up KW - Benzophenone KW - LCTS-type polymer KW - Poly(glycidyl ether) (PGE) KW - Fibroblast adhesion KW - XPS KW - ToF-SIMS PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652966 DO - https://doi.org/10.1021/acsami.4c18632 SN - 1944-8244 VL - 17 IS - 6 SP - 10073 EP - 10086 PB - American Chemical Society (ACS) CY - Washington, DC AN - OPUS4-65296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Standardized Chemical Composition Analysis of Graphene Oxide Flakes with SEM/EDS and XPS Works Reliably N2 - Reliable quantification of the chemical composition of graphene-related 2D materials (GR2M) as powders and liquid suspensions is a challenging task. Analytical methods such as XPS, ICP-MS, TGA and FTIR are recommended in projects at standardization bodies. The parameters to be measured are also defined, e.g. the oxygen-to-carbon (O/C) concentration ratio, the trace metal impurities, or the functional groups present. In this contribution, for the first time, the capability of SEM/EDS to reliably quantify the O/C ratio in a well-characterized graphene oxide (GO) material is evaluated. The robustness of the SEM/EDS results under various measurement conditions is tested by comparison to the established XPS analysis. A crucial step is the sample preparation from liquid suspension with GO flakes onto a substrate for analysis with both EDS and XPS. It is demonstrated that if a closed and enough thick drop-cast spot is deposited on a substrate, both surface-sensitive XPS analysis and bulk-characterizing EDS result in very similar elemental composition of oxygen and carbon. Hence, the theoretical, expected O/C atomic ratio values for pure GO of ~0.5 are achieved with both methods. Further, the effect of untight deposited material causing co-analysis of the silicon substrate, is evaluated for both methods, XPS and EDS. Note that all the EDS results in this study have been quantified standardless. The standard measurement procedure including the GO material considered here as a candidate reference material will make a significant contribution to analyse reliably the chemical composition of GR2M with SEM/EDS as one of the most widely used methods in analytical laboratories. T2 - Graphene Week 2025 CY - Vicenza, Italy DA - 22.09.2025 KW - EDX KW - Graphene-related 2D materials KW - O/C ratio KW - Standardisation KW - Samle preparation KW - XPS PY - 2025 AN - OPUS4-64261 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mrkwitschka, Paul A1 - Sahre, Mario A1 - Corrao, Elena A1 - Pellegrino, Francesco A1 - Hodoroaba, Vasile-Dan T1 - Wire-Print as a Sample Preparation Procedure Suitable for Accurate Morphological Characterization of Constituent Particles for Graphene-Related 2D-Materials N2 - In this study we have systematically tested the efficacy of a new deposition procedure for graphene-related 2D materials (GR2M’s) from liquid suspension onto a substrate for quantitative analysis of their size and shape distribution with electron microscopy. The technique is an extension of the conventional drop-casting method, and we have designated it “wire-print” deposition. It consists of two steps, first one being usual drop-casting on a copper substrate and second one involving a thin copper wire with a sub-mm diameter being dipped into the deposited droplet and retracted with a corresponding half-spherical droplet attached on its tip and final deposition of this entire nL-amount of suspension onto e.g. a silicon wafer for microscopical, detailed analysis. 11 series of such a wire-print deposition for a graphene-based ink have been considered, whereby various conditions (treatment of the starting suspension) have been experimented with a repetition of up to 10 times per condition, all together 86 spots on a silicon wafer of 10 mm x 10 mm. The evaluation of one series of 8 repeated wire-print depositions reveal that the deposited spots are visualized with SEM. The weak presence of coffee-rings, irregular spot shape, and presence of agglomerates should be noticed. Both the mean value of the 8 ECD distributions and the total number of flakes deposited in each spot show a variance in the range of 17% and 22%, respectively. In the context of accurate analysis of such challenging complex materials these numbers can be considered as excellent and demonstrate the high benefit of the wire-print deposition for accurate morphological measurements on GR2M’s. KW - Sample preparation KW - Imaging KW - 2D materials KW - Morphology KW - Size distribution PY - 2025 DO - https://doi.org/10.1093/mam/ozaf048.219 VL - 31 IS - 7 SP - 436 EP - 437 PB - Oxford Academic AN - OPUS4-63821 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Habibimarkani, Heydar A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan A1 - John, Elisabeth T1 - Probing Surface Changes in Fe–Ni Oxide Nanocatalysts with a ToF-SIMS-Coupled Electrochemistry Setup and Principal Component Analysis N2 - Understanding catalyst surface dynamics under operating conditions is essential for improving electrocatalytic performance. Here, we present a novel approach combining electrochemical treatment with contamination-free transfer to Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS), followed by principal component analysis (PCA), to probe surface and interfacial changes in Ni–Fe oxide nanoparticles stabilized by polyvinylpyrrolidone (PVP) during the oxygen evolution reaction (OER). The surface analysis at three distinct treatment stages revealed distinct chemical fingerprints across pristine nanoparticles, after exposure to 1 M KOH electrolyte, and after cyclic voltammetry treatment. The results highlight a progressive transition from ligand-rich to ligand-depleted interfaces, with PVP-related fragments dominant in the early stages and metal- and electrolyte-derived species emerging after activation. Complementary ToF-SIMS analysis of electrolyte deposited on Si wafers after each treatment step confirms the concurrent leaching of PVP and Fe–Ni-based fragments during OER. These findings underscore the dynamic nature of catalyst–electrolyte interfaces and demonstrate a robust strategy for monitoring surface-sensitive chemical changes associated with the nanoparticles, especially during the initial cycles of the OER. KW - Fe-Ni oxide KW - Nanocatalysts KW - ToF-SIMS KW - Electrochemistry KW - PCA (principal component analysis) KW - OER PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652667 DO - https://doi.org/10.1021/acs.analchem.5c03894 SN - 0003-2700 SP - 1 EP - 8 PB - American Chemical Society (ACS) AN - OPUS4-65266 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Harald T1 - Nano and Advanced Materials - Competences at BAM and perspectives N2 - This presentation gives an overview about the competencies and the characterization possibilities of nanoparticles at BAT, based on this the development of the OECD TG 125 at BAM. It further describes research activities at BAM concerning the characterization of nanoparticles and the way to the digital representation of these characterization possibilities. It concludes with the challenges of a digital product passport (DPP) for nanomaterial based products and the need of a digital materials passport (DMP). Finally, the activities of BAM are presented which address the former mentioned challenges from ESRP and DPP. T2 - Austausch Helmholtz Hereon / Digipass & BAM CY - Berlin, Germany DA - 07.07.2025 KW - Nanomaterials KW - ESPR KW - DPP KW - Nano KW - Advanced Materials PY - 2025 AN - OPUS4-64974 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Campos de Oliveira, Paula A1 - Markötter, Henning A1 - Zhang, Wen A1 - Eddah, Mustapha A1 - Widjaja, Martinus Putra A1 - Remacha, Clément A1 - Bruno, Giovanni T1 - Enhanced image segmentation of refractories using synchrotron X-ray computed tomography and machine learning techniques N2 - The microstructure of refractory materials is complex, featuring a variety of mineral phases, agglomerates, defects, and controlled porosity. The behavior of refractories at high temperatures adds another layer of complexity, as phase transitions and particle rearrangements can strongly affect their properties. To analyze such intricate microstructure, advanced imaging techniques such as Synchrotron X-ray Computed Tomography (SXCT) allow detailed 3D visualization and quantification of features up to 1 μm. However, the intricacy of these microstructures makes phase identification (known as image segmentation) in digital images a challenging process. X-ray images often contain noise and image artifacts, making the analysis more difficult. Therefore, this work describes image segmentation and artifact reduction methods to characterize refractories using X-ray imaging. We studied refractory ceramics used in the aerospace industry, primarily composed of fused silica. For image segmentation, the traditional approach of greyscale thresholding was compared with machine learning. Greyscale thresholding relies on predefined algorithms to assign phases based on intensity values. In contrast, machine learning extracts patterns from large datasets, enabling more adaptive and accurate segmentation. By combining high-resolution SXCT and machine learning analysis algorithms, we successfully segmented previously uncharacterized 3D microstructural key features of refractories, including agglomerates, grain boundaries, pore size distribution and interconnectivity. Compared to traditional methods, the machine learning-enhanced segmentation presented a more accurate quantification of porosity and defects. The integration of advanced imaging techniques with machine learning segmentation significantly improves the characterization of refractory materials, providing a more precise understanding of the relationship between microstructure and material performance, supporting the development of innovative industrial solutions. T2 - The 19th Biennial International Technical Conference on Refractories (UNITECR 2025) CY - Cancún, Mexiko DA - 27.10.2025 KW - Synchrotron X-ray Tomography KW - Machine learning KW - Image segmentation KW - Ceramics KW - Refractories PY - 2025 SP - 478 EP - 481 AN - OPUS4-64803 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ren, L. A1 - Pollard, A. A1 - Hodoroaba, Vasile-Dan T1 - Measurement of Lateral Size of Graphene Oxide Flakes by SEM - An Update of the VAMAS TWA 41 Project P13 N2 - The progress of the VAMAS interlaboratory comparison Project P13 "Lateral size of graphene oxide flakes by SEM" within the Technical Working Area 41 "Graphene and Related 2D Materials" is presented. The challenges at sample preparation on substrates for accurate measurement and image analysis as well as two different image analysis approaches, containing exact guidance how to measure the main descriptors for the lateral size measurement of the imaged graphene oxide flakes with Scanning Electron Microscopy are described. Discrepancies are explained. The inclusion of the results into the corresponding ISO technical specification CD/TS 23879 is also discussed and planned, in relation with the AFM part. T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 50th Steering Committee Meeting CY - London, United Kingdom DA - 15.09.2025 KW - VAMAS KW - Interlaboratory comparison KW - Electron microscopy KW - Lateral size KW - Graphene oxide flakes PY - 2025 UR - https://www.vamas.org/twa41/documents/2023_vamas_twa41_project13_GO_SEM.pdf AN - OPUS4-64228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul A1 - Hodoroaba, Vasile-Dan T1 - Wire-Print as a Novel Sample Preparation Approach for Accurate Morphological Characterization of Constituent Particles of Graphene-Related 2D-Materials N2 - Graphene and graphene-oxide (GO) are used for instance in catalysis, biomedical applications, in inks and as composite materials. To ensure product quality and safe-by-design principles within the various application fields, the commercial material must be characterized and specified through well-known and standardized procedures. The accurate morphological characterization of 2D materials is a challenging task, requiring careful sample preparation on a substrate either as a powder or from liquid suspension. These must be isolated, homogeneously distributed, with good statistics of the counted particles. Various sample preparation approaches have been reported in the literature, e.g. electrospray, substrate surface treatment, embedding the particulate material and polishing the cross-section, or addition of ligands to the suspended nanostructures. In this study, a novel deposition procedure for graphene-related 2D materials (GR2Ms) was systematically tested for its efficacy. The quantitative analysis of the size and shape distribution of the materials was conducted using electron microscopy and was successfully tested in XPS and EDS experiments. The technique is an extension of the conventional drop-casting method and has been designated "wire-print" deposition. The result of such a wire-print deposition for a graphene-based suspension is shown in Figure, where various treatment conditions have been tested with a repetition of up to 10 times per condition, all together 86 spots on a silicon wafer of 10 mm². T2 - Graphene Week 2025 CY - Vicenza, Italy DA - 22.09.2025 KW - Graphene-related 2D materials (GR2M) KW - Sample peparation KW - Imaging KW - Electron Microscopy KW - Wire-print deposition method PY - 2025 AN - OPUS4-64248 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Florian, Camilo T1 - Optical thickness-profiling for fs-laserinduced superficial amorphization and oxide removal on silicon N2 - Amorphization and re-crystallization of polished silicon wafers cut in <111> and <100> orientation were studied after irradiation by single Ti:sapphire femtosecond laser pulses (790 nm, 30 fs) using optical imaging, topographic characterization, and transmission electron microscopy. Spectroscopic imaging ellipsometry (SIE) enabled fast data acquisition at multiple wavelengths and provided experimental data for calculating the amorphous layer thickness profiles with lateral resolution in the micrometer and vertical resolution in the nanometer range based on a thin-film layer model including the topmost native oxide. For a radially Gaussian shaped laser beam and at moderate peak laser fluences above the melting but below the ablation threshold, laterally parabolic amorphous layer profiles with maximum thicknesses of some tens of nanometers were quantitatively derived. Moreover, the threshold fluence of the native oxide removal was quantified. At laser peak fluences closely below the ablation threshold of silicon, SIE is capable to reveal even the laser-induced removal and formation of the native oxide covering the Si wafers under ambient air conditions. The accuracy of these all-optical, non-destructive SIE-based layer thickness assessments is verified experimentally through high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray spectroscopy (STEM-EDX). Along with topographic information obtained by atomic force microscopy (AFM), a comprehensive picture of the oxide removal and superficial re-solidification of silicon after local melting by femtosecond laser pulses can be drawn. T2 - E-MRS Spring Meeting 2025 CY - Strasbourg, France DA - 26.05.2025 KW - Femtosecond laser KW - Laser-induced amorphization KW - Native oxide layer KW - Spectroscopic imaging ellipsometry KW - Transmission electron microscopy PY - 2025 AN - OPUS4-63275 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn T1 - Bacterial adhesion on ultrashort pulse laser processed surfaces ― more than size matters! N2 - Bacterial biofilms are aggregates of bacterial cells, often attached to a surface and enclosed by a self-produced extracellular matrix which confers increased stress tolerance and resistance to cleaning. Biofilm formation leads to biofouling which gives rise to high costs in numerous technical settings due to biocorrosion and biodegradation. However, biofilms can also be attractive for industrial settings such as wastewater treatment systems or for soil bioremediation processes. Hence, the control of bacterial adhesion to a surface is of major concern. Surface topography strongly influences bacterial adhesion. Therefore, one promising way to achieve bacteria-guiding surfaces lies in the contactless and aseptic large-area laser processing of technical surfaces. We used short and ultrashort pulsed laser systems to generate different surface textures, mainly high-spatial-frequency and low-spatial-frequency laser-induced periodic surface structures, LIPSS (HFSL and LFSL), on Ti, Ti-alloy, steel, and polymers (PET and PE). Pristine (polished) and laser processed samples were subjected to bacterial adhesion experiments with two different Escherichia coli strains and Staphylococcus aureus as test organisms. The bacterial strains differed in their cell wall structure (grampositive vs. gramnegative strains), in size, shape, the occurrence of cell appendages, and in their biofilm forming capabilities. Adhesion patterns were analyzed microscopically and compared regarding the respective test strain and surface topography. Our results revealed that adhesion behavior strongly depends not only on the material’s topography and chemistry, but also on the specific bacterial strain, the presence of cell appendages, and ambient growth conditions. T2 - 13th International Conference on Photoexcited Processes and Applications, ICPEPA-13 CY - Lecce, Italy DA - 14.09.2025 KW - Biofilm KW - Bacterial adhesion KW - Laser-induced periodic surface structures (LIPSS) KW - Ultrashort laser pulses PY - 2025 AN - OPUS4-64166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martínez, E. A1 - Lejeune, N. A1 - Frechilla, J. A1 - Porta-Velilla, L. A1 - Forneau, E. A1 - Angurel, L. A. A1 - de la Fuente, G. F. A1 - Bonse, Jörn A1 - Silhanek, A. V. A1 - Badía-Majós, A. T1 - Laser engineered architectures for magnetic flux manipulation on superconducting Nb thin films N2 - Custom shaped magnetic flux guiding channels have been fabricated on superconducting Nb thin films by laser nanopatterning of their surface. Preferential pathways are defined by suitable combination of imprinted anisotropic pinning domains through laser-induced periodic surface structures (LIPSS). Generated by the selective energy deposition of femtosecond UV laser pulses, quasi-parallel ripple structures are formed under optimized irradiation conditions. On average, each domain is formed by grooves with a lateral period of 260–270 nm and a depth about 80 nm. By combination of scanning and transmission electron microscopy, magneto-optical imaging, and conductive atomic force microscopy techniques, we conclude that the boundaries of the LIPSS-covered domains play a prominent role in the magnetic flux diversion process within the film. This is confirmed by dedicated modeling of the flux dynamics, combined with the inversion of the magneto-optical signal. The created metasurfaces enable control of the flux penetration process at the microscale. KW - Laser-induced periodic surface structures (LIPSS) KW - Magnetic flux KW - Magneto-optical imaging (MOI) KW - Critical current density PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611243 UR - https://www.sciencedirect.com/science/article/pii/S0169433224019287 DO - https://doi.org/10.1016/j.apsusc.2024.161214 SN - 1873-5584 (Online) SN - 0169-4332 (Print) VL - 679 SP - 1 EP - 12 PB - Elsevier AN - OPUS4-61124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wonneberger, R. A1 - Gräf, S. A1 - Bonse, Jörn A1 - Wisniewski, W. A1 - Freiberg, K. A1 - Hafermann, M. A1 - Ronning, C. A1 - Müller, F. A. A1 - Undisz, A. T1 - Tracing the Formation of Femtosecond Laser-Induced Periodic Surface Structures (LIPSS) by Implanted Markers N2 - The generation of laser-induced periodic surface structures (LIPSS) using femtosecond lasers facilitates the engineering of material surfaces with tailored functional properties. Numerous aspects of their complex formation process are still under debate, despite intensive theoretical and experimental research in recent decades. This particularly concerns the challenge of verifying approaches based on electromagnetic effects or hydrodynamic processes by experiment. In the present study, a marker experiment is designed to conclude on the formation of LIPSS. Well-defined concentration depth profiles of 55Mn+- and 14N+-ions were generated below the polished surface of a cast Mn- and Si-free stainless steel AISI 316L using ion implantation. Before and after LIPSS generation, marker concentration depth profiles and the sample microstructure were evaluated by using transmission electron microscopy techniques. It is shown that LIPSS predominantly formed by material removal through locally varying ablation. Local melting and resolidification with the redistribution of the material occurred to a lesser extent. The experimental design gives quantitative access to the modulation depth with a nanometer resolution and is a promising approach for broader studies of the interactions of laser beams and material surfaces. Tracing LIPSS formation enables to unambiguously identify governing aspects, consequently guiding the path to improved processing regarding reproducibility, periodicity, and alignment. KW - Laser-induced periodic surface structures (LIPSS) KW - Femtosecond laser processing KW - Ion implantation KW - Transmission Electron Microscopy (TEM) KW - Stainless steel PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623990 DO - https://doi.org/10.1021/acsami.4c14777 SN - 1944-8244 (Print) SN - 1944-8252 (Online) VL - 17 IS - 1 SP - 2462 EP - 2468 PB - ACS Publications AN - OPUS4-62399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn T1 - Laser Nanotexturierung von Metalloberflächen zur Reduktion von Reibung und Verschleiß N2 - Die Reduktion von Reibung und Verschleiß in technischen Systemen bietet ein großes Potenzial zur Reduktion von CO2-Emissionen. Dieser Beitrag diskutiert die Erzeugung und tribologische Charakterisierung von Ultrakurzpuls-generierten Nanostrukturen auf Metallen (Stahl, Titan). Besonderes Augenmerk wird dabei auf die Rolle der laserinduzierten Oxidschicht im Zusammenspiel mit verschleißreduzierenden Additiven in ölbasierten Schmiermitteln gerichtet. T2 - Online Abendvortrag beim AWT Härterei- und Werkstoffkreis Bodensee der Arbeitsgemeinschaft Wärmebehandlung + Werkstofftechnik e.V. CY - Online meeting DA - 16.01.2025 KW - Additive KW - Laser-induzierte periodische Nanostrukturen KW - Reibungsreduktion KW - Verschleißreduktion PY - 2025 AN - OPUS4-62432 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Voss, Heike T1 - Morphology and regularity of high-spatial frequency laser-induced periodic surface structures (HSFL) on titanium materials N2 - Titanium and its alloys are known to allow the straightforward laser‐based manufacturing of ordered surface nanostructures, so‐called high spatial frequency laser‐induced periodic surface structures (HSFL). These structures exhibit sub‐100 nm spatial periods – far below the optical diffraction limit. The resulting surface functionalities are usually enabled by both, topographic and chemical alterations of the nanostructured surfaces. For exploring these effects, HSFL were processed on different titanium materials (bulk, film) upon irradiation with near‐infrared ps‐laser pulses (1030 nm wavelength, ≈ 1 ps pulse duration) under different laser scan processing conditions. Here we extend our previous work on chemical analyses of HSFL on titanium materials towards a more detailed morphological and topographical surface characterization. For that, scanning electron and atomic force microscopic images are subjected to a regularity analysis using our self-developed ReguΛarity software. The regularity of the HSFL is assessed with respect to the influences of sample- and laser-related parameters, as well as the imaging method used. T2 - 13th International LIPSS Workshop CY - Enschede, Netherlands DA - 29.10.2025 KW - Laser-induced periodic surface structures (LIPSS) KW - Titanium KW - Ultrashort laser pulses KW - Laser processing PY - 2025 AN - OPUS4-64631 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn T1 - Laser Nanotexturierung von Metalloberflächen zur Reduktion von Reibung und Verschleiß N2 - Die Reduktion von Reibung und Verschleiß in technischen Systemen bietet ein großes Potenzial zur Reduktion von CO2-Emissionen. Dieser Beitrag diskutiert die Erzeugung und tribologische Charakterisierung von Ultrakurzpuls-generierten Nanostrukturen auf Metallen (Stahl, Titan). Besonderes Augenmerk wird dabei auf die Rolle der laserinduzierten Oxidschicht im Zusammenspiel mit verschleißreduzierenden Additiven in ölbasierten Schmiermitteln gerichtet. T2 - Internationale Bodensee Fachtagung „Wärmebehandlung und Oberflächentechnik zur Verbesserung von Tribologie und Verschleissbeständigkeit" CY - Feldkirch, Austria DA - 20.03.2025 KW - Additive KW - Laser-induzierte periodische Nanostrukturen KW - Reibungsreduktion KW - Verschleißreduktion PY - 2025 AN - OPUS4-62757 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn T1 - Generation and characterization of anisotropic nanostructures using ultrashort pulsed lasers N2 - The lecture gives an overview of the generation and characterization of anisotropic nanostructures using ultrashort pulsed laser radiation. Special attention will be paid to the phenomenon of so-called laser-induced periodic surface structures (LIPSS) on various materials. One focus will be on dielectrics and the dynamics of nanostructure formation. Further examples of bulk nanostructures from the literature will be discussed. T2 - 8th UKP-Workshop: Ultrafast Laser Technology CY - Aachen, Germany DA - 08.04.2025 KW - Laser-induced Periodic Surface Structures (LIPSS) KW - Dielectrics KW - Surface Nanostructures KW - Volume Nanostructures PY - 2025 AN - OPUS4-62947 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn T1 - Ultrafast optical probing of laser-induced formation of periodic surface nanostructures N2 - Laser-induced Periodic Surface Structures (LIPSS, ripples) are a universal phenomenon and can be generated in a contactless, single-step process on almost any type of solid upon irradiation with intense laser pulses. They represent a (quasi-)periodic modulation of the surface topography in the form of a linear grating and are typically formed in a “self-ordered” way in the focus of a coherent laser beam. Thus, they are often accompanying laser material processing applications. The structural sizes of LIPSS typically range from several micrometers down to less than 100 nanometers – far beyond the optical diffraction limit – while their orientations exhibit a clear correlation with the local polarization direction of the laser radiation. From a theoretical point of view, a controversial debate has emerged during the last decades, whether LIPSS originate from electromagnetic effects (seeded already during the laser irradiation) – or whether they emerge from matter-reorganization processes (distinctly after the laser irradiation). From a practical point of view, however, LIPSS represent a simple and robust way for the nanostructuring of solids that allows creating a wide range of different surface functionalities featuring applications in optics, tribology, medicine, energy technologies, etc. The presentation provides an overview of current theories on LIPSS and the quest to achieve ever smaller surface nanostructures. The historical development of the fundamental ideas behind LIPSS is presented, together with experimental approaches that make it possible to distinguish between the various LIPSS formation scenarios. Time-resolved experimental methods are required to investigate the dynamics of their formation. The presentation focuses on ultrafast time-resolved optical (pump-probe) techniques that can be used for localized point measurements or microscopic imaging, utilizing the reflection, diffraction, or coherent scattering of the probe radiation at the emerging LIPSS, while simultaneously capturing information about rapid melting, ablation, and solidification phenomena. However, given the sub-micrometric spatial periods of LIPSS, their analysis using optical radiation employed in far-field techniques remained a challenge. Therefore, short wavelengths of the probe beam in the UV range or even below are required to overcome the diffraction limit imposed in the optical spectral range. Fourth-generation light sources, namely short-wavelength (XUV or X-ray) short-pulse free-electron lasers (FELs), offer new and fascinating possibilities for resolving laser-induced structure formation on surfaces in the sub-micrometer to nanometer range and in time domains from picoseconds to several nanoseconds with a resolution in the sub-picosecond regime. On laser-irradiated semiconductor surfaces, this unique spatio-temporal resolution enables the detection of early signs of coherent/plasmonic electromagnetic scattering effects, followed by the excitation of hydrodynamic capillary waves – providing new insights into the above-mentioned debate. Recent experiments at the European XFEL used fs-time-resolved small-angle X-ray scattering (fs-SAXS) and even fs-time-resolved grazing incidence small-angle X-ray scattering (fs-GISAXS), combined with grazing-incidence diffraction (fs-GID), to reveal the dynamics of the formation of nanometric LIPSS on metals. T2 - CINSaT Herbstkolloquium 2025 CY - Kassel, Germany DA - 05.11.2025 KW - Laser-induced periodic surface structures (LIPSS) KW - Ultrashort laser pulses KW - Pump-probe measurements KW - Free-electron laser KW - Small angle X-ray scattering (SAXS) PY - 2025 AN - OPUS4-64633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hassenstein, Christian T1 - Robotergestützte Ultraschallprüfung von Objekten mit komplexen Geometrien N2 - Durch den Einsatz moderner digitaler Design- und Fertigungsmethoden wachsen einerseits die Komplexität von Bauteilen, andererseits der Bedarf an Informationen über deren Qualität und Zustand. Damit steigen auch die Anforderungen an die zerstörungsfreie Prüfung, die im Zuge von ZfP 4.0 automatisierte und flexible, innovative Prüfmethoden erfordert. Das gilt insbesondere für Objekte, deren Oberflächengeometrien über plane Flächen und eindimensionale Krümmungen hinausgehen. Um zu zeigen, wie eine Ultraschallprüfung von Objekten mit komplexer Oberflächengeometrie realisiert werden kann, wurde an der BAM eine roboterbasierte Demonstratoranlage entwickelt. Dabei führt ein Roboterarm einen Array-Prüfkopf in Tauchtechnik senkrecht über die Prüffläche. Die dafür erforderliche Prüfbahn kann entweder anhand der CAD-Geometrie oder mithilfe einer Punktewolke der Prüffläche, die vorab mit einem am Roboter angebrachten Laser-Profilometer erfasst wird, ermittelt werden. Zur Erhöhung der Genauigkeit werden der Lasersensor und der Ultraschallprüfkopf automatisiert mit dafür entwickelten Routinen am Roboter eingemessen. Durch bildgebende Verfahren und eine automatische Auswertung der Bilder kann die in Tauchtechnik auftretende Brechung des Schallbündels an der Prüfteiloberfläche berücksichtigt werden, was die ortsrichtige Rekonstruktion von Anzeigen aus dem Prüfteilinneren bzw. der Rückwand ermöglicht. Durch Rückführung der Anzeigen in ein gemeinsames Koordinatensystem entsteht eine 3D-Rekonstruktion des Prüfteils. Der vorliegende Beitrag stellt die Demonstratoranlage und die angewendeten Methoden im Detail vor und nennt Anwendungsbeispiele. T2 - DGZfP Jahrestagung 2025 CY - Berlin, Germany DA - 26.05.2025 KW - Ultraschall KW - Robotik KW - Turbinenschaufel KW - Wanddicke KW - Defekterkennung PY - 2025 AN - OPUS4-63417 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Voss, Heike T1 - ReguΛarity - A free software for the objective quantification of the regularity of periodic surface structures generated by femtosecond laser irradiation N2 - The precise laser-based surface structuring on the micro- and nanoscale allows to create functional properties for innovative applications, e.g., in medicine, optics and biology. Among the various types of surface structures, laser-induced periodic surface structures (LIPSS) are characterized by their versatility and the relatively simple manufacturing process. However, the fabrication of highly regular LIPSS patterns remains challenging. The systematic investigation of LIPSS formation, as well as of the resulting functional properties requires a precise evaluation of the surface morphology, especially with regard to periodicity and regularity. Existing quantification methods such as Fast Fourier Transformation (FFT) tend to lack automation and objectivity, especially when dealing with large data sets and multi-scale structures. Although automated approaches exist with the Gini coefficient and the P³S method, their limited availability restricts a broader scientific use. We therefore introduce ReguΛarity as an innovative open-source software solution for objective, rapid and reproducible evaluation of structured surfaces concerning their regularity. In order to provide comprehensive surface morphological analysis, our software uses advanced image-processing techniques and integrates the already developed tools such as P³S method, Gini coefficient, FFT analysis, and the calculation of DLOA (Dispersion of LIPSS Orientation Angle). The software allows to evaluate any relevant image format as provided, e.g., by standard scanning electron micrographs. An intuitive PyQt5-based interface, enhanced by multi-threading capabilities, facilitates efficient data processing. Interactive features such as region-of-interest selection and plotting provide flexible adaptation to diverse applications. ReguΛarity offers a robust analysis tool that will contribute to the further development of precise laser-based surface structuring and to the optimization of the desired functional properties in both research and industry. T2 - 13th International Conference on Photoexcited Processes and Applications, ICPEPA-13 CY - Lecce, Italy DA - 14.09.2025 KW - Laser-induced periodic surface structures (LIPSS) KW - Laser processing KW - Fourier transformation KW - Regularity PY - 2025 AN - OPUS4-64176 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rahner, E. T1 - From nightmare to numbers - A novel software tool for objective regularity analysis of LIPSS N2 - The precise laser-based surface structuring on the micro- and nanoscale allows for the creation of functional properties for innovative applications, e.g., in medicine, optics and biology. Among the various types of surface structures, laser-induced periodic surface structures (LIPSS) are distinguished by their versatility and the comparatively simple manufacturing process. Nevertheless, the fabrication of highly regular LIPSS patterns remains challenging. The systematic investigation of LIPSS formation, as well as of the resulting functional properties demands accurate and objective evaluation of surface morphology, especially regarding periodicity and regularity. Existing quantification methods such as Fast Fourier Transformation (FFT) tend to lack automation and objectivity, especially when dealing with large data sets and multi-scale structures. Although automated approaches, such as those based on the Gini coefficient or the P³S method, have been proposed, their limited availability hinders a broader scientific use. To overcome these limitations, we introduce ReguΛarity, a novel, freely available Python-based software tool featuring a graphical user interface for automated and quantitative assessment of regularity in period and (quasi-)periodic surface patterns including LIPSS. The software processes microscopic images obtained from optical, scanning electron microscopy (SEM), or atomic force microscopy (AFM), combining image segmentation with one- and two-dimensional Fourier analyses (1D-FT, 2D-FT), phase evaluation, and gradient-based orientation determination to facilitate a comprehensive regularity analysis of (quasi-)periodic surface patterns with spatial periods Λ. Regularity is quantified by the newly proposed five-dimensional regularity tuple R comprising the normalized spread of spatial periods from 2D-FT, the normalized local variation of the dominant spatial period from 1D-FT, the Gini coefficient G, the Dispersion of the LIPSS Orientation Angle (DLOA), and the mean phase deviation. The demonstration of the software’s capabilities is achieved by comparing idealized sinusoidal test patterns with SEM micrographs of fs-laser-generated LIPSS on stainless steel (AISI 316L) and aluminum alloy (AlMg5). This comparison highlights ReguΛarity’s objective differentiation between varying levels of structural regularity. The software facilitates high-throughput analysis and data-driven optimization in laser surface engineering processes. T2 - 13th International LIPSS Workshop CY - Enschede, Netherlands DA - 29.10.2025 KW - Laser-induced periodic surface structures (LIPSS) KW - Surface functionalization KW - Fourier transform KW - Gini coefficient PY - 2025 AN - OPUS4-65047 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gräf, S. T1 - Ion marker implantation as key to understand the formation of femtosecond LIPSS on steel N2 - Ultrashort laser (fs-laser) pulses can be used to generate laser-induced periodic surface structures (LIPSS, ripples) on different types of materials. A variety of potential applications of these grating-like LIPSS have already been demonstrated in the field of surface functionalization. Examples include structural colours (e.g. for optical effects or safety features), beneficial friction and wear reduction, modification of the wetting behaviour of surfaces, and antibacterial or cell adhesion promoting properties for medical implants. Despite decades of research, however, some aspects regarding the formation mechanism are still unclear and the subject of controversial debate. This involves the two main models of coherent electromagnetic scattering and matter reorganization, which are used for explaining aspects of LIPSS formation and phenomenology. One major issue is to quantify the actual amount of material removal during the fs-laser processing due to the lack of an independent depth reference and to visualize the so-called heat-affected zone accompanying intense fs-laser irradiation. In the present study, near-surface implantation of Mn and N ions into different material depth of Mn-free austenitic stainless steel alloy FeCrNiMo18-12-2 was used to create reference layers of a defined thickness containing the respective elements. LIPSS (type low-spatial frequency LIPSS, LSFL) were fabricated on the polished substrate surfaces in an air environment by fs-laser irradiation (λ = 1025 nm, τ = 300 fs, frep = 100 kHz, F = 1.5 J/cm2). The implanted layers subsequently served as a kind of coordinate system to assess the material removal during the formation process via cross-sectional Transmission Electron Microscopy (TEM) and Energy Dispersive X-ray Spectroscopy (EDXS). Using both analysis methods enabled in particular to determine the position of peaks and valleys of the LIPSS topography in relation to the initial surface before fs-laser irradiation. This confirmed the selective ablation in the LIPSS valleys. Moreover, linking changes in the material’s microstructure, e.g., the crystallinity and near surface elemental composition before and after fs-laser treatment, gave additional insights regarding the transient cooling rates, as recently shown for NiTi alloys. T2 - 13th International LIPSS Workshop CY - Enschede, Netherlands DA - 29.10.2015 KW - Energy dispersive X-ray analysis (EDX) KW - Ion implantation KW - Laser-induced periodic surface structures (LIPSS) KW - Steel KW - Transmission electron microscopy (TEM) PY - 2025 AN - OPUS4-64900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn T1 - Bacterial adhesion on ultrashort pulse laser processed surfaces ― more than size matters! N2 - Bacterial biofilms are aggregates of bacterial cells, often attached to a surface, and enclosed by a self-produced extracellular matrix which confers increased stress tolerance and resistance to cleaning. Biofilm formation leads to biofouling which gives rise to high costs in numerous technical settings due to biocorrosion and biodegradation. However, biofilms can also be attractive for industrial settings such as wastewater treatment systems or for soil bioremediation processes. Hence, the control of bacterial adhesion to a surface is of major concern. Surface topography strongly influences bacterial adhesion. Therefore, one promising way to achieve bacteria-guiding surfaces lies in the contactless and aseptic large-area laser processing of technical surfaces. We used short and ultrashort pulsed laser systems to generate different surface textures, mainly high-spatial-frequency and low-spatial-frequency laser-induced periodic surface structures, LIPSS (HFSL and LFSL), on Ti, Ti-alloy, steel, and polymers (PET and PE). Pristine (polished) and laser processed samples were subjected to bacterial adhesion experiments with two different Escherichia coli strains and Staphylococcus aureus as test organisms. The bacterial strains differed in their cell wall structure (grampositive vs. gramnegative strains), in size, shape, the occurrence of cell appendages, and in their biofilm forming capabilities. Adhesion patterns were analyzed microscopically and compared regarding the respective test strain and surface topography. Our results revealed that adhesion behavior strongly depends not only on the material’s topography and chemistry, but also on the specific bacterial strain, the presence of cell appendages, and ambient growth conditions. T2 - 13th International LIPSS Workshop CY - Enschede, Netherlands DA - 29.10.2025 KW - Bacterial adhesion KW - Biofilm KW - Laser-induced periodic surface structures (LIPSS) KW - Ultrashort laser pulses PY - 2025 AN - OPUS4-64632 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Voss, Heike T1 - Morphology and regularity of high-spatial frequency laser-induced periodic surface structures (HSFL) on titanium materials N2 - Titanium and its alloys are known to enable the straightforward laser‐based manufacturing of ordered surface nanostructures, so‐called high-spatial frequency laser‐induced periodic surface structures (HSFL). These structures exhibit sub‐100 nm spatial periods – far below the optical diffraction limit. The resulting surface functionalities are usually enabled by both, topographic and chemical alterations of the nanostructured surfaces. For exploring these effects, HSFL were processed on different titanium materials (bulk, film) upon irradiation with near‐infrared ps‐laser pulses (1030 nm wavelength, ≈1 ps pulse duration) under different laser scan processing conditions in normal air atmosphere. Here, we extend our previous work on chemical analyses of HSFL on titanium materials towards a more detailed large-area morphological and topographical surface characterization. For this purpose, scanning electron or atomic force microscopic images are subjected to a regularity analysis using our ReguΛarity software. The results are assessed with respect to the influences of sample- or laser-related parameters on the regularity of the HSFL. T2 - 13th International Conference on Photoexcited Processes and Applications, ICPEPA-13 CY - Lecce, Italy DA - 14.09.2025 KW - Laser-induced periodic surface structures (LIPSS) KW - Laser processing KW - Ulltrashort laser pulses KW - Titanium PY - 2025 AN - OPUS4-64173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gräf, S. T1 - Ion marker implantation for tracing the formation of femtosecond LIPSS on steel N2 - An ion marker experiment is conducted to investigate the formation of low spatial frequency laser-induced periodic surface structures (LIPSS) on stainless steel surfaces upon scan-processing with femtosecond laser pulses (300 fs, 1025 nm, 100 kHz) focussed to a spot diameter of ~20 µm. Defined concentration depth profiles of 14N^+- and 55Mn^+-ions were implanted below the polished surface of a cast Mn- and Si-free stainless steel AISI 316L using an acceleration energy of 380 keV. This generated two distinct “depth-tracer-layers” ~135 nm (55Mn) and ~340 nm (14N) below the sample surface. The sample morphology and microstructure were evaluated before and after LIPSS-processing using scanning and transmission electron microscopy techniques in top-view and cross-sectional geometry. Energy-dispersive X-ray spectroscopy (EDXS) allowed to visualize the depth distribution of the marker elements, the steel constituents, and of oxygen involved through the laser processing in ambient air. These experiments revealed that the LIPSS on this metal are predominantly formed by material removal through locally varying ablation and, to a lesser extent, by local melt displacement effects prior to the re-solidification. Moreover, the processing in air leads to the formation of a less than 10 nm thick laser-induced oxide layer covering the steel surface. Our new tracer ion approach contributes to the ongoing debate on the relevance of electromagnetic or hydrodynamic effects during the formation of LIPSS. T2 - E-MRS Spring Meeting 2025 CY - Strasbourg, France DA - 26.05.2026 KW - Laser-induced periodic surface structures (LIPSS) KW - Steel KW - Ion implantation KW - Transmission electron microscopy (TEM) KW - Energy dispersive X-ray analysis (EDX) PY - 2025 AN - OPUS4-63274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Obenlüneschloß, Jorit A1 - Boysen, Nils A1 - Rönnby, Karl A1 - Muriqi, Arbresha A1 - Hoffmann, Volker A1 - Abad Andrade, Carlos Enrique A1 - Rogalla, Detlef A1 - Brokmann, Ulrike A1 - Rädlein, Edda A1 - Nolan, Michael A1 - Devi, Anjana T1 - Ein seltener mononuklearer Lithium‐Carben‐Komplex für die Atomlagenabscheidung von lithiumhaltigen Dünnschichten N2 - KurzfassungLithium ist das zentrale Element moderner Batterietechnologien, und die Herstellung von lithiumhaltigen Materialien mittels Atomlagenabscheidung (engl. Atomic Layer Deposition, ALD) bietet erhebliche Vorteile bei der Kontrolle der Schichtdicke und ‐zusammensetzung. In dieser Studie wird ein neuer mononuklearer, durch ein N‐heterocyclisches Carben (NHC) stabilisierter Lithiumkomplex, [Li(tBuNHC)(hmds)], als vielversprechender Präkursor für die ALD von lithiumhaltigen Dünnschichten vorgestellt. Die strukturelle Charakterisierung erfolgt durch den Vergleich von Dichtefunktionaltheorie (DFT) und Einkristall‐Röntgenbeugung (engl. Single‐Crystal X‐ray Diffraction, SC‐XRD), wobei die seltene mononukleare Struktur bestätigt wird. Thermogravimetrische Analysen (TGA) zeigen vorteilhafte thermische Eigenschaften für ALD‐Anwendungen. Die Verbindung weist einen niedrigen Schmelzpunkt, saubere Verdampfung und ermutigende Volatilitätsparameter im Vergleich zu anderen Lithium‐Präkursoren auf. ALD‐Experimente mit [Li(tBuNHC)(hmds)] und Ozon zeigen dessen Effektivität bei der Abscheidung von LiSixOy‐Filmen. Der ALD‐Prozess zeigt ein gesättigtes Wachstum pro Zyklus (engl. Growth per Cycle, GPC) von 0,95 Å. Die Zusammensetzung, analysiert mittels Rutherford‐Rückstreu‐Spektrometrie/Kernreaktionsanalyse (engl. Rutherford Backscattering Spectrometry/Nuclear Reaction Analysis, RBS/NRA), Röntgenphotoelektronenspektroskopie (engl. X‐ray Photoelectron Spectroscopy, XPS) und Glimmentladungsspektroskopie (engl. Glow Discharge Optical Emission Spectrometry, GD‐OES), bestätigt das Vorhandensein von Lithium und Silizium in den erwarteten Verhältnissen. Diese Arbeit stellt nicht nur einen neuen ALD‐Präkursor vor, sondern trägt auch zum Verständnis der Lithiumchemie bei und bietet Einblicke in die faszinierende Koordinationschemie und das thermische Verhalten von durch NHC‐Liganden stabilisierten Lithiumkomplexen. KW - Atomlagenabscheidung KW - N-heterozyklischer-Carben-(NHC)-stabilisierter Lithium-Präkursor KW - Mononuklearer Li–Carben-Komplex KW - Lithiumsilicat-Dünnfilme KW - Filmanalytik/-Charakterisierung PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-644045 DO - https://doi.org/10.1002/ange.202513066 SN - 0044-8249 N1 - Es gibt eine parallele Sprachausgabe (englisch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (English), a link is in the field related identifier SP - 1 EP - 12 PB - Wiley-VCH CY - Weinheim AN - OPUS4-64404 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Obenlüneschloß, Jorit A1 - Boysen, Nils A1 - Rönnby, Karl A1 - Muriqi, Arbresha A1 - Hoffmann, Volker A1 - Abad Andrade, Carlos Enrique A1 - Rogalla, Detlef A1 - Brokmann, Ulrike A1 - Rädlein, Edda A1 - Nolan, Michael A1 - Devi, Anjana T1 - Rare Mononuclear Lithium-Carbene Complex for Atomic Layer Deposition of Lithium Containing Thin Films N2 - Lithium is the core material of modern battery technologies and fabricating the lithium‐containing materials with atomic layer deposition (ALD) confers significant benefits in control of film composition and thickness. In this work, a new mononuclear N‐heterocyclic carbene (NHC) stabilized lithium complex, [Li(tBuNHC)(hmds)], is introduced as a promising precursor for ALD of lithium‐containing thin films. Structural characterization is performed, comparing density functional theory (DFT) and single‐crystal X‐ray diffraction (SC‐XRD), confirming a rare mononuclear structure. Favorable thermal properties for ALD applications are evidenced by thermogravimetric analysis (TGA). The compound exhibits a low melting point, clean evaporation, and its volatility parameters are encouraging compared to other lithium precursors. ALD trials using [Li(tBuNHC)(hmds)] with ozone demonstrate its effectiveness in depositing LiSixOy films. The ALD process exhibits a saturated growth per cycle (GPC) of 0.95 Å. Compositional analysis using Rutherford backscattering spectrometry/nuclear reaction analysis (RBS/NRA), X‐ray photoelectron spectrometry (XPS), and glow discharge optical emission spectrometry (GD‐OES), confirms the presence of lithium and silicon in the expected ratios. This work not only presents a new ALD precursor but also contributes to the understanding of lithium chemistry, offering insights into the intriguing coordination chemistry and thermal behavior of lithium complexes stabilized by NHC ligands. KW - Atomic layer deposition (ALD) KW - N-heterocyclic carbene (NHC) ligands KW - Lithium ALD precursor chemistry KW - Mononuclear Li–carbene complex [Li(tBuNHC)(hmds)] KW - Li-silicate thin films (LiSixOy) KW - Thermal properties & TGA/volatility KW - Compositional analysis (RBS/NRA, XPS, GD-OES) PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643790 DO - https://doi.org/10.1002/anie.202513066 SN - 1433-7851 N1 - Es gibt eine parallele Sprachausgabe (deutsch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (German), a link is in the field related identifier SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim AN - OPUS4-64379 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Campos de Oliveira, Paula T1 - Advancing microstructural characterisation of ceramic cores for aerospace: from state-of-the-art to in-situ synchrotron X-ray computed tomography N2 - Ceramic cores are crucial for manufacturing turbine blades in aircraft engines, creating intricate cooling channels that improve engine efficiency and reduce emissions. During high-temperature casting, the cores undergo significant microstructural changes, including phase transitions, particle rearrangements, and porosity transformations, which can affect their properties and must be carefully controlled. State-of-the-art characterisation techniques for ceramic cores mostly rely on 2D methods, such as scanning and transmission electron microscopy. While valuable, these methods are limited in capturing the 3D complexity of the material. Advances in X-ray computed tomography (XCT) offer a more comprehensive perspective on 3D microstructures, but conventional XCT often lacks the resolution and in-situ capabilities to study microstructural evolution under casting conditions. Synchrotron XCT (SXCT) addresses these limitations, offering high spatial and temporal resolution with features down to 1 µm, enabling in-situ investigations. This study highlights the potential of SXCT, revealing previously unseen 3D microstructural features in ceramic cores, such as agglomeration, porosity evolution, surface reactions, microcracking, and particle orientation. These findings provide a more realistic view of dynamic changes during casting, advancing the understanding of core behaviour. Despite its advantages, SXCT is still rarely used in the field due to challenges such as limited access to synchrotron facilities and sample movement artifacts. Future developments, including high-temperature and vacuum compatible CT setups, could enhance this technique, leading to a better optimisation of ceramics performance. T2 - XIXth Conference of the European Ceramic Society (ECERS 2025) CY - Dresden, Germany DA - 31.08.2025 KW - Synchrotron KW - X-ray Computed Tomography KW - Ceramic core KW - Aerospace KW - Microstructure PY - 2025 AN - OPUS4-64050 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Habibimarkani, Heydar A1 - Prinz, Carsten A1 - Sahre, Mario A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - CV, TEM, XRD and XPS/HAXPES datasets of FeNi-based nanoparticles for the oxygen evolution reaction N2 - The datasets from Cyclic Voltammetry, Transmision Electron Microscopy, X-ray Diffraction, and (Hard Energy) X-ray Photoelectron Spectroscopy are related to the publication H. Habibimarkani, S.-L. Abram, A. Guilherme Buzanich, C. Prinz, M. Sahre, V.-D. Hodoroaba and J. Radnik "In-depth analysis of FeNi-based nanoparticles for the oxygen evolution reaction" Scientific Reports (2025), https://doi.org/10.1038/s41598-025-92720-3 Details of the materials and the experimental procedures are described in this publications. KW - Oxygen evolution reaction KW - Fe-Ni nanopartices KW - Comprehensive analysis PY - 2025 DO - https://doi.org/10.5281/zenodo.14975964 PB - Zenodo CY - Geneva AN - OPUS4-63335 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Morphological Analysis of Graphene Oxide by SEM and Correlative Field-Flow Fractionation Coupled with Multi-Angle Light Scattering N2 - Since the first free-standing monolayer graphene sheet was successfully prepared in 2004 [1], graphene and graphene oxide materials achieved the necessary technical readiness level to be considered for use in commercial products. Moreover, the focus has shifted from fundamental research towards expanding the applicability of graphene-related 2D materials (GR2M) and to improve their competitiveness with established materials [2]. Significant advances have been made especially in applications regarding optoelectronics, energy storage materials, chemical additives, sensor applications etc. [3]. Composite products containing graphene and functionalized graphene such as inks and dyes have shown enhanced performance regarding longevity, wettability, and can be tailored for specific purposes through dedicated functionalization. For accurate physico-chemical characterization, GR2M products in their raw form or as part of composites present challenges in terms of sample preparation, choice of analytical method and evaluation of data. For instance, in the context of imaging, these challenges encompass: (a) the selection of images magnifications being representative for all the flakes ranging in size from hundreds of nanometers to micrometers; (b) the selection of representative flakes for adequate statistics, which may involve the separation of overlapping/agglomerating flakes by segmentation; and (c) the classification of diverse morphologies such as irregularly shaped/crumpled flakes, porous flakes and particulate features present in the sample. The complexity of the analytical task has needed the introduction of specific ontology for 2D materials to identify the proper descriptors characterizing confidently the morphological features of interest. Regarding light scattering techniques such as Dynamic Light Scattering (DLS) and Multi-Angle Light Scattering (MALS) commonly used for process control in industry as a first measure, an alternative approach would be necessary. This is in part due to the use of the standard sphere-model for 2D materials as appearing to be inappropriate, whilst a disc-shape model potentially yields more suitable results. Standardization efforts are underway to establish a baseline for accurate characterization of aimed measurands with sufficient statistics. To date, the measurement methods recommended by standardization bodies for the morphological-structural characterization of GR2M’s are AFM, Raman Spectroscopy and SEM and/or TEM. The acquisition of statistically relevant numbers of flakes for a thorough characterization using TEM and AFM is particularly time-consuming. The size distribution of graphene oxide- and graphene-containing inks was investigated by using a correlative approach coupling Centrifugal Field-Flow Fractionation (CF3) [4] with MALS. Up to now, promising results for Field-Flow Fractionation have been achieved only with respect to the separation into size classes of GO samples as well as of graphene oxide mixed with graphene by Asymmetrical Field-Flow Fractionation (AF4) [5], [6]. Besides the online characterization by MALS, the eluting size fractions obtained by CF3 were also collected and subsequently measured by SEM. Successful separation into size fractions allows us to apply ensemble techniques such as MALS to samples that were previously not measurable according to best-practices. In this study, the following material sub-classes have been observed with SEM: (i) nano-graphite mixed with graphene flakes, (ii) graphene oxide few- and multi-layer flakes with diverse and highly complex morphology, and (iii) graphene oxide of well-defined size and shape with >95% single- and bilayer content were investigated. Data on the class size ranges was obtained by MALS after separation with CF3 and consideration of a disc-shape model. Significant effort was invested into the sample preparation for CF3 measurements to achieve a recovery rate of >80%, well above the recommended 70% by ISO/TS 21362:2018 for validation purposes. The material fractions collected after the CF3 measurement were separately deposited on a silicon wafer and the size results of the SEM analysis were correlated with the corresponding mean sizes obtained with MALS. T2 - Microscopy and Microanalysis 2025 CY - Salt Lake City, UTAH, USA DA - 27.07.2025 KW - Advanced Material KW - CF3 KW - SEM KW - Morphology PY - 2025 AN - OPUS4-64084 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Correlative chemical imaging to reveal the nature of different commercial graphene materials N2 - Different synthesis techniques were developed which led to other graphene-related materials such as graphene oxide (GO) or elemental-doped graphene. Further chemical functionalization can enhance but also alter or reduce specific properties of the graphene. To reveal the nature of these materials a proper physico‑chemical characterization with different analytical techniques is crucial. Single-layer GO flakes provided by Graphenea (Spain) were prepared for systematic image analysis. These flakes were disposed on an alignment-marked SiO2 substrate and correlatively imaged by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Raman spectroscopy. The high lateral resolution and/ or extreme surface sensitivity of the mentioned techniques is necessary to explore monolayers. The ToF-SIMS images match well with the SEM and AFM images and provide information about the chemistry. With 2D Raman spectroscopy it is possible to differentiate between the number of stacked single-layer flakes. This is visualized in a 3D image. Well-defined GO flakes could be used as a reference material for imaging of graphene-like structures but also of other types of 2D materials. In addition to these monolayer GO flakes, commercial graphene-containing inks (Haydale) with a more complex morphology were also correlatively imaged. ToF-SIMS and SEM images were merged to identify the origin of different chemical fragments. The findings correlate closely with the expectation that the specific functionalizations (with fluorine and nitrogen as marker elements) are present only on the graphene flakes as presumed from the SEM images. Energy-dispersive X-ray spectroscopy (EDX) supports these results, yet with a much lower sensitivity compared to ToF-SIMS. T2 - Joint Regulatory Risk Assessors Summit – Advancing Safety & Sustainability Assessments of Advanced Materials CY - Paris, France DA - 19.06.2025 KW - ToF-SIMS KW - Imaging KW - Graphene-related 2D materials KW - SEM/EDX KW - Auger electron spectroscopy KW - Raman spectroscopy PY - 2025 UR - https://macrame-project.eu/macrame-meetings-workshops/jointrras/#Agenda AN - OPUS4-63656 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Reliable analysis of the elemental composition of graphene oxide flakes with energy dispersive spectroscopy (SEM/EDS) and x-ray photoelectron spectroscopy (XPS) N2 - Suspensions of graphene-related 2D materials (GR2M) are broadly used for further applications like printable electronics. The reliable quantification of the composition of graphene-related 2D materials as liquid suspensions is still a challenging task, which can hinder the commercialisation of the products. Specific parameters to be measured are defined, e.g. the oxygen-to-carbon (O/C) concentration ratio, the trace metal impurities, or the functional groups present [1], but reference protocols are still missing. One of the central methods for the quantification is X-ray photoelectron spectroscopy (XPS) as a rather expensive method. Therefore, the development of cheaper alternatives is highly desired. One attractive alternative of XPS is energy-dispersive spectroscopy (EDS) which is usually coupled with scanning electron microscopy (SEM). This combination is one of the most widely used methods in analytical laboratories. In this contribution the results of a systematic study on the capability of SEM/EDS to reliably quantify the O/C ratio in a well-defined and well-characterized graphene oxide material [2] are presented. The robustness of the SEM/EDS results obtained at various measurement conditions (various excitation energies) is tested by comparing the results to the established XPS analysis [3], which has been carried out on the same samples. It is demonstrated that for samples prepared by drop-casting on a substrate, both surface-sensitive XPS analysis and bulk-characterising EDS result in very similar elemental composition of oxygen and carbon for thick spots. Further, the effect of untight deposited material enabling co-analysis of the (silicon) substrate, is evaluated for both methods, XPS and EDS. The last results clearly show the influence of the substrate on the analysis of the results and stressed out the importance of the sample preparation. T2 - E-MRS Spring Meeting CY - Strasbourg, France DA - 26.05.2025 KW - Graphene oxide KW - Reliable Analysis KW - Ionic Liquid KW - Reference Material PY - 2025 AN - OPUS4-63336 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Liaison report from VAMAS/TWA 37 Quantitative Microstructural Analysis to ISO/TC 202 Microbeam Analysis N2 - The liaison between VAMAS/TWA 37 Quantitative Microstructural Analysis and other TWAs to ISO/TC 202 Microbeam Analysis since the last Annual Meeting of ISO/TC 202 is reported. The VAMAS/TWA 37 projects initiated in the last year and the new ones in the planing phase are highlighted with technical and organisational details. Also need for more participants in 2 projects is discussed. T2 - 32nd Plenary Meeting of ISO/TC 202 Microbeam Analysis CY - London, United Kingdom DA - 28.10.2025 KW - VAMAS KW - Quantitative microstructural analysis KW - ISO KW - Standardisation KW - Interlaboratory comparisons PY - 2025 AN - OPUS4-64552 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - Knowledge Infrastructure supporting image-based characterisation of 2D graphene materials N2 - To better understand the relationship between image features and biological effects such as toxicity,we have developed a method combining image thresholding and pixel-wise segmentation to create annotated datasets. These datasets are used to train machine learning models and establish human–AI learning loops for material classification and structure detection. We employ deep learning architectures such as ResNet, EfficientNet, and U-Net to automate the classification and segmentation of SEM/TEM images of 2D nanomaterials, with targeted manual annotation focusing on key structures (graphene flakes, agglomerates, contaminants, etc.). This approach ensures reproducible, large-scale analysis, which is essential for studying the links between structure and biological response. Finally, our methodology aligns with OECD requirements and contributes to the Safe and Sustainable by Design (SSbD) framework, aiming to enhance product reliability and sustainability. T2 - Joint Regulatory Risk Assessors Summit – Advancing Safety & Sustainability Assessments of Advanced Materials CY - Paris, France DA - 19.06.2025 KW - Graphene KW - 2D materials KW - Knowledge infrastructure KW - Imaging KW - Machine learning PY - 2025 UR - https://macrame-project.eu/macrame-meetings-workshops/jointrras/#Agenda AN - OPUS4-63682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - In depth analysis of commercial functionalized graphene nanoplateles towards structure-activity relationships N2 - The analysis of commercial graphene related products from the raw material to inks is discussed and the input to structure-activity relationships. Different approaches to obtain structure-activity relationships like operando or using data mining are presented. Challenges and recommendation to obtain structure-activity relationships are given. T2 - Joint Regulator Risk Summit: Advancing Safety & Sustainability Assessments of Advanced Materials CY - Paris, France DA - 19.06.2025 KW - Functionalized graphene KW - Structure activity relationsships KW - Commercialisation PY - 2025 AN - OPUS4-63565 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chemello, Giovanni A1 - Despotelis, Konstantinos A1 - Paton, Keith A1 - Clifford, Charles A A1 - Pollard, Andrew A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Approaches for the measurement of lateral dimensions of graphene oxide flakes using scanning electron microscopy N2 - There is a practical need, especially from the industrial community, to accurately measure the size and shape of graphene oxide (GO) flakes of commercial origin, in a reliable, simple, and unambiguous way. The sample preparation is a decisive step to obtain a homogeneous distribution of flakes on a substrate, which is suitable for image analysis. A certain level of inhomogeneity was still found but could be accepted for the purpose of this lateral size measurement study. A measurement procedure for Scanning Electron Microscopy (SEM) including sample preparation, measurement, image analysis and reporting was developed and validated to be applied for the lateral size analysis of “real-world” 2D flakes. Samples were produced for analysis by drop casting GO dispersions onto Si/SiO2 substrates. After SEM imaging, the images were analysed using two approaches to derive size and shape parameters. The influence of different operators has been evaluated. A maximum difference of 10% for the size descriptor and 2% for shape descriptor was found for both image analysis approaches when different samples of the same source material are measured and analysed by the same operator, hence indicating variability caused by sample preparation and analysing different sample areas. When different laboratories/operators perform the image analysis on exactly the same images and same flakes, the deviation found for the size descriptor is 2% and 4.6% corresponding to the two approaches applied, while no difference in the shape descriptor is observed. KW - Graphene oxide KW - SEM KW - Lateral dimension KW - Standardisation KW - Imaging PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625070 DO - https://doi.org/10.1088/2632-959X/adae28 VL - 6 IS - 1 SP - 1 EP - 11 PB - IOP Publishing AN - OPUS4-62507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madbouly, Loay Akmal A1 - Mrkwitschka, Paul A1 - Stockmann, Jörg Manfred A1 - Jones, Elliot A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Comparative Elemental Analysis of Commercial Functionalized Graphene Nanoplatelets Along the Production Chain With X‐Ray Photoelectron and Energy‐Dispersive X‐Ray Spectroscopy N2 - Graphene has been commercialized for over a decade, primarily in the form of suspensions and inks. In this study, we investigate the properties of graphene nanoplatelets (GNPs) and their functionalized derivatives, incorporating fluorine or nitrogen as functional groups (FG). The analysis was conducted on three forms, that is, powders, suspensions, and inks, using X‐ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) with energy‐dispersive X‐ray spectroscopy (EDX). The objective of this work is to establish a rapid and comprehensive systematic approach for elemental analysis of commercial functionalized graphene, which can be used for quality control. Functionalization is employed to tailor the material's physical and chemical properties. In our study, graphene samples, functionalized with fluorine or ammonia in a plasma reactor, were investigated. Both XPS and EDX were applicable for all three forms and showed, in general, similar trends between the three forms, so that both XPS and EDX can be used for quality control of GNPs along the production chain. KW - Commercial graphene KW - Functionalized graphene KW - Graphene inks KW - SEM/EDS KW - XPS PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625752 DO - https://doi.org/10.1002/sia.7386 SN - 1096-9918 SP - 1 EP - 7 PB - Wiley AN - OPUS4-62575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - John, Elisabeth A1 - Weise, Matthias A1 - Radnik, Jörg A1 - Stockmann, Jörg Manfred A1 - Lange, Thorid A1 - Sahre, Mario A1 - Hodoroaba, Vasile-Dan T1 - Towards a New Reference Material—Analytical Challenges in Examining High-Entropy Alloy Thin Films N2 - A new high-entropy alloy (HEA) consisting of titanium, chromium, manganese, iron, and nickel was deposited as a thin-film on silicon substrates using magnetron sputtering from a novel segmented target composed of metal stripes. This material was explored with the goal to create a new reference material for surface analysis and evaluation of complex composite materials. The film's morphology was initially characterized by scanning electron microscopy (SEM), followed by crystallographic analysis using X-ray diffraction (XRD) and selected area electron diffraction (SAED). The two-dimensional compositional homogeneity was assessed using a combination of scanning and transmission electron microscopy (TEM) with energy-dispersive spectroscopy (EDS), X-ray fluorescence (XRF), time-of-flight secondary ion mass spectrometry (ToF-SIMS), and X-ray photoelectron spectroscopy (XPS). The in-depth chemical composition was further analysed using ToF-SIMS and Auger electron spectroscopy (AES). Our findings demonstrate that it is possible to produce thin HEA films with a homogeneous in-depth composition from a segmented target. Notably, despite the fixed composition of the target, we were able to vary the HEA's composition by exploiting inhomogeneities within the magnetrons sputter plasma. Additionally, we successfully created HEA films with significant compositional gradients. T2 - ECASIA CY - Gothenburg, Sweden DA - 10.06.2024 KW - Reference material KW - High-entropy alloy KW - Thin-films PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625777 DO - https://doi.org/10.1002/sia.7387 SN - 1096-9918 SP - 1 EP - 8 PB - Wiley AN - OPUS4-62577 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Chahal, Shweta T1 - Sustainable Synthesis of Na+ and Bi3+ - doped Cs₂AgInCl₆ Double Perovskites for Efficient White-Light Emission N2 - Double halide perovskites have emerged as promising, less-toxic alternatives to lead-based perovskites for diverse photochemical applications. Among them, Cs₂AgInCl₆ has attracted significant attention, particularly when doped with various elements, which induce self-trapped exciton (STE) states within the bandgap, resulting in efficient white-light emission and a remarkable enhancement of photoluminescence quantum yield (PL QY). While several solid-state and solution-based methods have been employed for the synthesis of double halide perovskites, many rely on toxic solvents and complex procedures, hindering scalability. In this study, we present two environmentally friendly synthesis approaches for the preparation of Cs₂AgInCl₆ doped with monovalent (Na⁺) and trivalent (Bi³⁺) cations: 1. Green solution-based method: Utilizes mild reagents and entirely replaces harsh chemicals, enabling synthesis at ambient conditions. 2. Mechanochemical approach: Employs high-energy ball milling for 62 minutes at room temperature to obtain the desired crystalline phase. These green methodologies provide sustainable and scalable alternatives to conventional routes, minimizing the environmental footprint. We systematically compare the structural and optical properties of the doped perovskites synthesized via both approaches. The resulting materials exhibit strong UV absorption, broadband white-light emission, high PL QY (up to 85%, Fig. 1), long PL lifetimes, and good thermal and environmental stability (up to 300 °C in air). These results highlight the potential of doped Cs₂AgInCl₆ double perovskites as an eco-friendly material with possible photonic applications as in white-light devices. T2 - eMRS Fall Meeting 2025 CY - Warsaw, Poland DA - 15.09.2025 KW - Fluorescence KW - Advanced material KW - Perovskite KW - Synthesis KW - Characterization KW - Fluorescence quantum yield KW - Absolute KW - Integrating sphere spectroscopy KW - Sustainable synthesis KW - Lifetime KW - Photophysics PY - 2025 AN - OPUS4-64185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dumit, Verónica I. A1 - Furxhi, Irini A1 - Nymark, Penny A1 - Afantitis, Antreas A1 - Ammar, Ammar A1 - Amorim, Monica J. B. A1 - Antunes, Dalila A1 - Avramova, Svetlana A1 - Battistelli, Chiara L. A1 - Basei, Gianpietro A1 - Bossa, Cecilia A1 - Cimpan, Emil A1 - Cimpan, Mihaela Roxana A1 - Ciornii, Dmitri A1 - Costa, Anna A1 - Delpivo, Camilla A1 - Dusinska, Maria A1 - Fonseca, Ana Sofia A1 - Friedrichs, Steffi A1 - Hodoroaba, Vasile-Dan A1 - Hristozov, Danail A1 - Isigonis, Panagiotis A1 - Jeliazkova, Nina A1 - Kochev, Nikolay A1 - Kranjc, Eva A1 - Maier, Dieter A1 - Melagraki, Georgia A1 - Papadiamantis, Anastasios G. A1 - Puzyn, Tomasz A1 - Rauscher, Hubert A1 - Reilly, Katie A1 - Jiménez, Araceli Sánchez A1 - Scott‐Fordsmand, Janeck J. A1 - Shandilya, Neeraj A1 - Shin, Hyun Kil A1 - Tancheva, Gergana A1 - van Rijn, Jeaphianne P. M. A1 - Willighagen, Egon L. A1 - Wyrzykowska, Ewelina A1 - Bakker, Martine I. A1 - Drobne, Damjana A1 - Exner, Thomas E. A1 - Himly, Martin A1 - Lynch, Iseult T1 - Challenges and Future Directions in Assessing the Quality and Completeness of Advanced Materials Safety Data for Re‐Usability: A Position Paper From the Nanosafety Community N2 - Ensuring data quality, completeness, and interoperability is crucial for progressing safety research, Safe‐and‐Sustainable‐by‐Design approaches, and regulatory approval of nanoscale and advanced materials. While the FAIR (Findable, Accessible, Interoperable, and Re‐usable) principles aim to promote data re‐use, they do not address data quality, essential for data re‐use for advancing sustainable and safe innovation. Effective quality assurance procedures require (meta)data to conform to community‐agreed standards. Nanosafety data offer a key reference point for developing best practices in data management for advanced materials, as their large‐scale generation coincided with the emergence of dedicated data quality criteria and concepts such as FAIR data. This work highlights frameworks, methodologies, and tools that address the challenges associated with the multidisciplinary nature of nanomaterial safety data. Existing approaches to evaluating the reliability, relevance, and completeness of data are considered in light of their potential for integration into harmonized standards and adaptation to advance material requirements. The goal here is to emphasize the importance of automated tools to reduce manual labor in making (meta)data FAIR, enabling trusted data re‐use and fostering safer, more sustainable innovation of advanced materials. Awareness and prioritization of these challenges are critical for building robust data infrastructures. KW - Advanced materials KW - Safety data KW - Re-usability KW - Nanosafety KW - SSbD KW - FAIR KW - Standardisation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652918 DO - https://doi.org/10.1002/adsu.202500567 SN - 2366-7486 SP - 1 EP - 18 PB - Wiley-VCH CY - Weinheim AN - OPUS4-65291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Towards Standardised Procedures for Morphology Measurement of 2D-Materials by Imaging N2 - The industry uptake of graphene-related 2D materials (GR2M) material increases, and international standardization is critical to enable commercialization. Reliable, accurate, and reproducible measurements are important due to the multiple production routes and producers of the material to maintain quality in manufacture. Several standards are under development within ISO/TC 229 ‘Nanotechnologies’, i.e. ISO/AWI TS 23879 “Structural characterization of graphene oxide flakes: thickness and lateral size measurement using AFM and SEM” or ISO DTS 23359 “Chemical characterization of graphene in powders and suspensions”, which focus on determining the dimensional and chemical properties of GR2M. Interlaboratory comparisons are required to develop best practice and understand the associated measurement uncertainties. In this contribution challenges and solutions for the accurate measurement of the lateral size of GR2M will be discussed based on the results of a recently completed interlaboratory comparison organized under the pre-standardisation platform of VAMAS (www.vamas.org/twa41/documents/2023_vamas_twa41_project13_GO_SEM.pdf). Aspects related to sample preparation, measurement conditions, and image analysis with different approaches to extract the corresponding size and shape descriptors will be presented. A discussion on the measurement uncertainty budget associated to the final result will be also included. T2 - Graphene Week 2025 CY - Vicenza, Italy DA - 22.09.2025 KW - Graphene-related 2D materials (GR2M) KW - Interlaboratory comparison KW - VAMAS KW - Lateral size KW - ISO/TC 229 Nanotechnologies PY - 2025 AN - OPUS4-64250 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eggert, Claudia A1 - Hodoroaba, Vasile-Dan T1 - Welcome and Introduction N2 - Nanotechnology has emerged over the past decade as a key field involving the design, characterization, production, and application of materials, structures, devices, and systems at the nanometer scale. Due to their large specific surface area and significant surface chemistry, nanomaterials offer enhanced material properties and product functionalities. However, alongside these advancements comes the potential risk to humans and the environment. The development of nanomaterials has provided new opportunities to understand matter at the nanoscale, accelerating the creation of innovative advanced materials and devices. The expertise gained in the standardization and regulation of nanomaterials, particularly in characterizing nanoparticulate matter, should be applied to other innovative advanced materials, such as (nano)composites, 2D structures, additive manufactured materials, gels, and foams. Initial guidance for the safe-and-sustainable-by-design (SSbD) development of advanced materials during the early innovation phase has been introduced by various groups and projects. Additionally, digital material passports (DMP) and digital product passports (DPP) need to be defined and implemented uniformly across Europe. In 2024, the Innovative Advanced Materials Initiative (IAM-I) was launched by European stakeholders to contribute to a "Research and Innovation ecosystem that will significantly accelerate the time-to-market of sustainable innovative advanced materials (IAMs) and associated technologies designed for a digital circular economy." Knowledge transfer is a crucial pillar of this ecosystem, and a future IAM-I Academy could be a valuable tool. Initially, it is essential to define "education & training needs to boost Europe’s competitiveness and sovereignty within the area of IAM." T2 - Nano and Beyond - What can we learn from Nano for other Innovative Advanced Materials? CY - Online meeting DA - 04.07.2025 KW - Advance Materials KW - Nanomaterials KW - IAM-I KW - SSbD KW - DMP KW - DPP PY - 2025 UR - https://www.bam-akademie.de/kursangebot/kurs/webinar-nano-and-beyond-55.html?lang=en AN - OPUS4-63690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Advanced physico-chemical Characterisation & Correlation of Results with different Methods for GFMs N2 - An accurate characterisation of the morphological, structural, and chemical properties of nano and advanced materials is key for the understanding of the material functionality and constitutes the basis for future optimisation or even prediction of the product performance. Further, the correlation of the physical-chemical properties with results from biological testing leads to an understanding of the potential toxicological effects so that a minimisation of the materials risks becomes possible. The presentation will highlight with examples the importance of the selection of the relevant parameters/descriptors and particularly their measurement for the reliable characterisation of the morphology, structure, and chemistry of graphene-related 2D-materials (GR2M’s) [1-3]. One crucial aspect is also one of most challenging ones in the characterisation chain: the proper sample preparation, which shall be tailored to the accurate measurement of the defined analytical parameter. Practical examples of measurement of morphological descriptors of GR2M’s, such as equivalent circular diameter (ECD), minimum and maximum Feret, and aspect ratio with electron microscopy, or of the thickness with atomic force microscopy (AFM) will be showed, together with quantitative chemical characterisation with X-ray photoelectron spectroscopy (XPS) and, newly, with energy-dispersive X-ray spectroscopy with a scanning electron microscope (SEM/EDX) [4] by evaluating accurately the elemental content as the ratio of O/C and the composition of impurities. Another relevant, but challenging part of the characterisation of GR2M’s, particularly as the final products containing mostly low amounts of GR2M’s, is the analysis of homogeneity of the chemical composition by sensitive imaging methods. Examples of successful analysis with secondary ion mass spectrometry (SIMS), even if not quantitative, will be presented. T2 - Joint online Workshop: Harmonisation & Standardisation of Test Methods for Nano- and Advanced Materials CY - Paris, France DA - 19.06.2025 KW - Physico-chemical characterisation KW - Graphene-related 2D materials KW - OECD KW - Standardisation KW - GO flakes PY - 2025 UR - https://macrame-project.eu/macrame-meetings-workshops/ws_hamonisation_standardisation_2023/ AN - OPUS4-63557 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Measurement of the Lateral Size of Graphene Oxide Flakes by SEM N2 - The progress of the VAMAS interlaboratory comparison Project P13 "Lateral size of graphene oxide flakes by SEM" within the Technical Working Area 41 "Graphene and Related 2D Materials" is presented. The challenges at sample preparation on substrates for accurate measurement and image analysis as well as two different analysis approaches, containing exact guidance how to measure the main descriptors for the lateral size measurement of the imaged graphene oxide flakes with Scanning Electron Microscopy are highlighted. The size and shape distributions as measured by 17 laboratories are showed expressed in size and shape descriptors extracted from SEM images by using two proposed measurement approaches. The implementation of the results into the corresponding ISO technical specification AWI/TS 23879 is discussed and planned, in relation with the AFM part. T2 - ISO/TC 229 Nanotechnologies Meeting Week CY - Stockholm, Sweden DA - 19.05.2025 KW - Graphene oxide KW - Interlaboratory comparison KW - SEM KW - Lateral size KW - VAMAS KW - ISO/TC 229 Nanotechnologies PY - 2025 AN - OPUS4-63189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - The next steps in the standardisation of graphene-related and other 2D materials (GR2M) N2 - The first products with graphene-related 2D material (GR2M) are on the market. In this phase trust is essential for the commercial success of these products, between the individual partners of the product value chain, and between the manufacturer and the consumer. Standards are an important tool for building this trust. The first steps have been taken in standardisation, e.g. in terminology and the characterization of raw materials. But there are still some challenges to overcome such as bringing the standards to the factory floor and real-world products. For the validation of new protocols and methods there is a need of reference data and materials. But not only the measurement should be reproducible, the whole analytical workflow from sample storage and preparation to data analysis should be reproducible. Another important issue is the establishment of credible structure-activity relationships which allows the prediction of the properties of the GR2M, but also of the biological activity including the safety for the human health and the environment. Such relationships can be used for read-across and grouping and can facilitate the regulation of the advanced materials. In addition, 2D materials beyond graphene should also be considered and can benefit from the experience from the standardisation of graphene and graphene oxide. T2 - Nanomaterials Standardization Strategy Forum - Europe - Republic of Korea CY - Online meeting DA - 08.07.2025 KW - Commercialisation KW - Product-value chain KW - Confidence building PY - 2025 AN - OPUS4-63731 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Standardized Chemical Composition Analysis of Graphene Oxide Flakes with SEM/EDS and XPS Works Reliably N2 - Reliable quantification of the chemical composition of graphene-related 2D materials as powders and liquid suspensions is a challenging task. Analytical methods such as XPS, ICP-MS, TGA and FTIR are recommended to be used in ongoing projects at standardization bodies. The specific parameters to be measured are also defined, e.g. the oxygen-to-carbon (O/C) concentration ratio, the trace metal impurities, or the functional groups present [1]. In this contribution, for the first time, the results of a systematic study on the capability of SEM/EDS to reliably quantify the O/C ratio in a well-defined and well-characterized graphene oxide material [2] are presented. It is expected that the quantitative EDS analysis of light elements emitting characteristic X-ray lines below 1 keV to be provided with significantly larger measurement uncertainties than the analysis of elements with an atomic number of 11 (Na) or above [3]. The robustness of the SEM/EDS results obtained at various measurement conditions (various excitation energies) is tested by comparing the results to the established XPS analysis [4], which has been carried out on the same samples. A crucial step in sample preparation from liquid suspension with graphene oxides flakes onto a substrate for analysis with both XPS and EDS. It is demonstrated that if a closed and enough thick drop-cast deposited spot is succeeded to be deposited on a substrate, both surface-sensitive XPS analysis and bulk-characterizing EDS result in very similar elemental composition of oxygen and carbon. Hence, theoretical, expected O/C atomic ratio values for pure graphene oxide of ~0.5 [1] are achieved (with both methods), see Figure 1. Further, the effect of untight deposited material enabling co-analysis of the (silicon) substrate, is evaluated for both methods, XPS and EDS. To note that all the EDS results in this study have been quantified standardless. The effect of the variation of beam voltage on the result of the quantification of the O/C ratio is shown in Figure 2. No clear tendency is visible by varying the kV, which is a confirmation of the quality of the standardless analysis at the used EDS spectrometer. The results of this study demonstrate the reliability of the reference measurement protocol for SEM/EDS to be introduced into ISO/DTS 23359, including the dedicated sample preparation, particularly for the cases when the concentration of the GO flakes in stock liquid suspension is low. Further, also the consideration of this GO material as one of the very few available as a commercial material on the market as the very first GO reference material with regard to its morphology as well as chemical composition. Both the standard measurement procedure and the candidate reference material will immensely contribute to characterise reliably the chemical composition of graphene-related 2D materials with SEM/EDS as one of the most widely used methods in analytical laboratories. T2 - Microscopy and Microanalysis 2025 CY - Salt Lake City, UTAH, USA DA - 27.07.2025 KW - Graphene oxide flakes KW - SEM/EDS KW - XPS KW - O/C ratio KW - Impurities PY - 2025 AN - OPUS4-64085 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Physical-chemical Characterization of Graphene-Related 2D Materials: Development of Approaches for Reliable Quantification N2 - An accurate characterisation of the morphological, structural, and chemical properties of nano and advanced materials is key for the understanding of the material functionality and constitutes the basis for future optimisation or even prediction of the product performance. Further, the correlation of the physical-chemical properties with results from biological testing leads to an understanding of the potential toxicological effects so that a minimisation of the materials risks becomes possible. The presentation will highlight with examples the importance of the selection of the relevant parameters/descriptors and particularly their measurement for the reliable characterisation of the morphology, structure, and chemistry of graphene-related 2D-materials (GR2M’s) [1-3]. One crucial aspect is also one of most challenging ones in the characterisation chain: the proper sample preparation, which shall be tailored to the accurate measurement of the defined analytical parameter. Practical examples of measurement of morphological descriptors of GR2M’s, such as equivalent circular diameter (ECD), minimum and maximum Feret, and aspect ratio with electron microscopy, or of the thickness with atomic force microscopy (AFM) will be showed, together with quantitative chemical characterisation with X-ray photoelectron spectroscopy (XPS) and, newly, with energy-dispersive X-ray spectroscopy with a scanning electron microscope (SEM/EDX) [4] by evaluating accurately the elemental content as the ratio of O/C and the composition of impurities. Another relevant, but challenging part of the characterisation of GR2M’s, particularly as the final products containing mostly low amounts of GR2M’s, is the analysis of homogeneity of the chemical composition by sensitive imaging methods. Examples of successful analysis with secondary ion mass spectrometry (SIMS), even if not quantitative, will be showed. T2 - SaferWorldbyDesign Webinars CY - Online meeting DA - 25.03.2025 KW - Graphene-related 2D materials KW - Standardisation KW - Interlaboratory comparison KW - Physico-chemical characterisation PY - 2025 UR - https://saferworldbydesign.com/webinars/ AN - OPUS4-62791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Quantitative EDS analysis on graphene related 2D materials N2 - The elemental analysis of solid matter by means of the Energy-Dispersive X-Ray Spectrometry (EDS) is meanwhile posible as a quick (seconds!) and more and more accurate analysis via standardsless (instantaneous) quantification. The sensitivity & quantification accuracy for light elements (C, O,..) has significantly increased in the recent years. The availability via table-top SEMs with incorporated EDS is also enhanced. Further, the EDS analysis at an SEM is well-standardized, see ISO/TC 202 Microbeam Analysis & VAMAS/ TWA 37 Quantitative Microstructural Analysis in good liaisonships with ISO/TC 229 Nanotechnologies. It is demostrated that key parameters such as oxygen-to-carbon atomic-% ratio and impurities can be realibly measured, with XPS as a reference method. Various EDS spectrometers and analysis conditions are tested and the validity of the EDS quantification of an ionic liquid of well-defined chemical composition is demonstrated. Next steps are to launch a corresponding VAMAS interlaboratory comparison and to discuss within ISO/TC 229 towards inclusion of EDS as a routine method for the elemental analysis of GR2M into the ISO/TS 23359 Nanotechnologies — Chemical characterization of GR2Ms in powders and suspensions. T2 - Annual Microscopy Community Meeting for the National Research Council in Canada CY - Online meeting DA - 18.11.2025 KW - Graphene-related 2D materials (GR2M) KW - Elemental analysis KW - Light elements KW - SEM/EDS KW - Standardisation PY - 2025 AN - OPUS4-64766 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Knigge, Xenia A1 - Radnik, Jörg T1 - Advanced materials for the energy transition N2 - The climate crisis is the burning issue of our time. In order to avert the impending consequences, global efforts are being made in a wide variety of social and scientific fields. This report looks at a small part of these efforts, a technical aspect, namely the question of which AdMa are currently considered in techniques to support the energy transition. AdMa, i.e. materials that are rationally designed to have new or enhanced properties, and/or targeted or enhanced structural features, are used in all sectors of the energy transition. Questions of energy generation, storage and saving are considered here. This report is based on literature research and contains a general compilation of various AdMa that are used in the energy transition or are being researched for this purpose. From this compilation, ten materials that are considered particularly relevant for various reasons were selected and examined in more detail in relation to their use. The specific question here lies in the conflicting objective that the development of technologies for the energy transition is welcomed, but the use of AdMa may entail possible challenges in view of chemical safety as well as sustainability and circular economy. KW - Energy generation KW - Energy saving KW - Eneergy storage KW - Energy transportation PY - 2025 DO - https://doi.org/10.60810/openumwelt-7853 SN - 1862-4804 VL - 83 SP - 1 EP - 64 PB - Umweltbundesamt CY - Dessau-Roßlau AN - OPUS4-63529 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schilling, Markus T1 - Towards Structured Data Spaces: Prototypical Application of Semantic Technologies as a Driver for Innovation in Materials Science N2 - In the pursuit of advancing development and digitalization within materials science, ensuring quality assurance, interoperability, and adherence to FAIR principles is significant. To address these aspects, semantic technologies are employed for storage, processing, and contextualization of data, offering machine-actionable and human-readable knowledge representations crucial for data management. This presentation showcases the prototypical application of generic approaches of knowledge representation in materials science. It includes the design and documentation of graph patterns that may be compiled into rule-based semantic shapes. The development and application of the PMD Core Ontology 3.0 (PMDco 3.0) tailored for materials science is highlighted. Its integration into daily lab life is demonstrated through its functional incorporation into electronic lab notebooks (ELN). Examples of material processing and standardized mechanical testing illustrate how knowledge graph operations enhance ELN capabilities, providing a generalizable unified approach for managing diverse experimental data from different sources with automation potentials. T2 - TMS Specialty Congress 2025 CY - Anaheim, CA, USA DA - 15.06.2025 KW - Semantic Data KW - Data Integration KW - Digitalization KW - Data Interoperability KW - Plattform MaterialDigital PY - 2025 AN - OPUS4-63401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fernandez-Poulussen, D. A1 - Hodoroaba, Vasile-Dan T1 - Holistic, reliable and practical Characterization Framework for Graphene Family Materials, a correlated approach including Imaging based techniques N2 - ACCORDs is an Horizon Europe project working in the development of an imaging-based characterization framework (ACCORDs framework) for the holistic correlative assessment of Graphene Family Materials (GFMs) as a representative of 2D nanomaterials (NMs) to assess and predict 2D NMs health and environmental risks. The ACCORDs framework will operationalise safe and sustainable by design (SSbD) strategies proposed in past or ongoing H2020 projects or within OECD by correlating low-, medium-, and high-resolution physico-chemical-biological imaging-based methods with non-imaging methods in a tiered approach. ACCORDs will deliver the ACCORDs framework and user guidance, new imaging-based characterisation methods, reference in vitro tests, new reference 2D NMs for different matrices, a new minimum information reporting guideline for FAIR data sharing and reuse of images as well as an atlas with reference images for diagnostics of compromised safety of GFMs/GFM products. The new guidelines and standard proposals will be submitted to standardisation bodies to allow creation of regulatory ready products. The novelty of ACCORDs is in translating the principles of medical imaging-based diagnostics to 2D material hazard diagnostics. ACCORDs will accelerate industrial sectors in the area of aviation, marine construction, drone production, flexible electronics, photovoltaics, photocatalytics and print inks-based sensors. The value ACCORDs proposes to the graphene industry are practical, easy, imaging-based tools for GFM quality monitoring next to the production line with a possibility to be correlated with advanced highresolution imaging characterization methods in case hazard i.e. deviation from controls (benchmark values) are diagnosed. The ACCORDs framework and tools will contribute to the European Green Deal by addressing the topic: “Graphene: Europe in the lead” and to a new European strategy on standardization, released on 2nd February, 2022 T2 - Joint Regulatory Risk Assessors Summit – Advancing Safety & Sustainability Assessments of Advanced Materials CY - Paris, France DA - 19.06.2025 KW - Graphene-related 2D materials (GR2M) KW - Imaging KW - SSbD KW - ACCORDs PY - 2025 UR - https://macrame-project.eu/macrame-meetings-workshops/jointrras/#Agenda AN - OPUS4-63660 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Investigation of Fe-Ni-O nanoparticles for water splitting N2 - This study investigates the effect of varying iron-to-nickel ratios on the catalytic performance of Fe-Ni oxide nanoparticles (NPs) for the oxygen evolution reaction (OER). Addressing the issue of high energy wastage due to large overpotentials in OER, we synthesized and characterized different NP catalysts with different Fe: Ni oxide ratios. Transmission Electron Microscopy (TEM), Energy Dispersive X-ray Spectroscopy (EDS), and X-ray Diffraction (XRD) were employed to determine the morphology, elemental and phase composition of the NPs. Furthermore, in-depth profiling with X-rayPhotoelectron Spectroscopy (XPS) and Hard X-ray Photoelectron Spectroscopy (HAXPES) revealedthat iron predominantly exists as oxide, while nickel exhibits both metallic and oxidic forms depending on the Fe content. XPS indicated an enrichment of iron at the NP surface, whereas HAXPES and EDSdata agreed on the bulk stoichiometry. T2 - PhI European User Meeting 2025 CY - Eibelstadt, Germany DA - 29.04.2025 KW - Oxygen evolution reaction KW - In depth analysis KW - (Hard) X-ray Photoelectron Spectroscopy PY - 2025 AN - OPUS4-63334 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fagan, J. A1 - Hodoroaba, Vasile-Dan T1 - VAMAS TWA 34 Nanoparticle Populations Combined Projects P15 and P16 N2 - The progress in the VAMAS Project #15 "Measurement of particle size and shape distribution of bipyramidal titania including deposition from liquid suspension" within TWA 34 Nanoparticle Populations is presented with highlight of the following points: - Determine and compare particle size and shape distribution by means of electron microscopy (SEM, TEM, STEM-in-SEM), atomic force microscopy (AFM) and small angle X-ray scattering (SAXS). - Determine uncertainty induced by deposition protocol from liquid suspension with comparison to known values from a prior ILC with already deposited nanoparticles on TEM grids. - Provide comparative validation of protocols for the techniques other than TEM. Further, the VAMAS/TWA 34 Project #16 "Measurement of (relative) number concentration of bimodal silica nanoparticles including deposition from liquid suspension" is presented. Follwowing points are discusssed: - Validate the performance of imaging methods to measure the relative number concentration by electron microscopy (SEM, TEM) and atomic force microscopy (AFM) and two modes of bimodal (30 and 60 nm) silica nanoparticles - Validate the performance of small angle X-ray scattering (SAXS) for the traceable measurement of the number concentration of the two modes. - Discussion of sample preparation issues - Publication of the results in 2026 T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 50th Steering Committee Meeting CY - London, United Kingdom DA - 14.09.2025 KW - VAMAS KW - Interlaboratory comparison KW - Particle size and shape distribution KW - Particle number concentration KW - Standardisation PY - 2025 UR - https://www.vamas.org/twa34/index.html AN - OPUS4-64234 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - VAMAS Regional Report Advanced Materials Germany 2025 N2 - Regional standardisation activities and how VAMAS can help in any way to promote activities are reported. Activities related to organisational updates, government initiatives/priorities (especially related to Advanced Materials), details of any strategy documents publicly available, networks within Germany and how we engage are presented. T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 50th Steering Committee Meeting CY - London, United Kingdom DA - 14.09.2025 KW - VAMAS KW - Interlaboratory comparison KW - Advanced materials KW - Standardisation PY - 2025 AN - OPUS4-64232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Narayanan, M.M. A1 - Nicolai, M. A1 - Prager, J. T1 - C9-a5 - Optimization of Low-Frequency Shear Wave Transducers for Guided Wave Applications N2 - Development of ultrasonic transducers for the excitation of a torsional mode T(0,1) mode in a large pipe of the material typical of actual oil/gas pipelines is discussed. Towards this,16 ultrasonic transducers are designed and fabricated using shear plates of PIC 255 material, backing mass of tungsten-epoxy composite and brass shims as wear plates. The transducers are qualified using Laser Doppler Vibrometry. Then, the transducers are embedded in a springloaded ring and tested on a pipe using a multi-channel ultrasonic system. The results show the successful excitation of T(0,1) mode and it is seen to propagate for distance of 60 m with a good SNR. T2 - 2025 ICU PADERBORN - 9th International Congress on Ultrasonics CY - Paderborn, Germany DA - 21.09.2025 KW - Ultrasonic guided waves KW - Torsional mode KW - Shear PZT plates KW - Ring array transducer design KW - Pipe testing PY - 2025 DO - https://doi.org/10.5162/Ultrasonic2025/C9-a5 SP - 223 EP - 226 PB - AMA Service GmbH AN - OPUS4-65356 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zeipert, H. A1 - Nellius, T. A1 - Schönlau, N. A1 - Wippermann, M. A1 - Claes, L. A1 - Henning, B. A1 - Nicolai, Marcel A1 - Prager, J. T1 - C6-a3 - Monitoring the curing process of adhesive bonds using selective excitation of guided ultrasonic waves N2 - A measurement setup for the selective excitation of guided ultrasonic waves in adhesively bonded plates is introduced. Changes of the dispersive behaviour of the guided waves during the curing process is known to be accompanied by a change in the propagating waves group velocities. The proposed measurement setup is used to monitor that change during the curing process of an aluminium-epoxy-polycarbonate bond. T2 - 2025 ICU PADERBORN - 9th International Congress on Ultrasonics CY - Paderborn, Germany DA - 21.09.2025 KW - Ultrasonic guided waves KW - Selective excitation KW - Non-destructive testing KW - Adhesive bonding KW - Condition monitoring PY - 2025 DO - https://doi.org/10.5162/Ultrasonic2025/C6-a3 SP - 207 EP - 210 PB - AMA Service GmbH AN - OPUS4-65357 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dudziak, Mateusz A1 - Riechers, Birte A1 - Maaß, Robert A1 - Michalchuk, Adam A1 - Schönhals, Andreas A1 - Szymoniak, Paulina T1 - Beyond conventional calorimetry: Unlocking thermal characterization with fast scanning techniques N2 - Fast scanning calorimetry (FSC) has emerged as a transformative technique in thermal analysis, enabling the investigation of rapid and kinetically driven thermal transitions that are inaccessible to conventional differential scanning calorimetry. This review highlights the capabilities enabled by FSC for studying a wide range of materials under extreme thermal conditions, including polymers, pharmaceuticals, metallic glasses, nanocomposites, and hydrogels. By employing ultrafast heating and cooling rates, FSC allows for the suppression of crystallization, resolution of weak transitions, and analysis of thermally labile or size-limited samples. The technique is particularly valuable for probing glass transitions, relaxation phenomena, and phase behavior in systems with complex morphologies or confined geometries. Case studies demonstrate the use of FSC in characterizing vitrification, physical aging, and interfacial dynamics, as well as its application in emerging fields such as additive manufacturing, supramolecular systems, and neuromorphic materials. Together, these examples underscore the role that FSC plays in advancing the understanding of structure-property relationships across diverse material classes. KW - Flash DSC KW - Calorimetry KW - Glass transition PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647405 DO - https://doi.org/10.1016/j.tca.2025.180177 VL - 754 SP - 1 EP - 14 PB - Elsevier B.V. AN - OPUS4-64740 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kossatz, Philipp A1 - Mezhov, Alexander A1 - Andresen, Elina A1 - Prinz, Carsten A1 - Schmidt, Wolfram A1 - Resch-Genger, Ute T1 - Assessing the Applicability of Lanthanide-Based Upconverting Nanoparticles for Optically Monitoring Cement Hydration and Tagging Building Materials N2 - Chemically stable, lanthanide-based photon upconversion micro- and nanoparticles (UCNPs) with their characteristic multicolor emission bands in the ultraviolet (UV), visible (vis), near-infrared (NIR), and short-wave infrared (SWIR) arepromising optical reporters and barcoding tags. To assess the applicability of UCNPs for the monitoring of early stage cement hydration processes and as authentication tags for cementitious materials, we screened the evolution of the luminescence of Selfmade core-only NaYF4:Yb,Er UCNPs and commercial μm-sized Y2O2S:Yb,Er particles during the first stages of cement hydration, which largely determines the future properties of the hardened material. Parameters explored from the UCNP side included particle size, morphology, surface chemistry or coating, luminescence properties, and concentration in different cement mixtures. From the cement side, the influence of the mineral composition of the cement matrix was representatively examined for ordinary Portland cement (OPC) and its constituents tricalcium aluminate (C3A), tricalcium silicate (C3S), and gypsum at different water to cement ratios. Based on reflection and luminescence measurements, enabling online monitoring, which were complemented by XRD and isothermal heat-flow calorimetric measurements to determine whether the incorporation of these particles could impair cement hydration processes, well suited lanthanide particle reporters could be identified as well as application conditions. In addition, thereby the reporter influence on cement hydration kinetics could be minimized while still preserving a high level of information content. The best performance for the luminescence probing of changes during early stage cement hydration processes was observed for 25 nm-sized oleate (OA)-coated UCNPs added in a concentration of 0.1 wt %. Higher UCNP amounts of 1.0 wt % delayed cement hydration processes size- and surface coatingspecifically in the first 24 h. Subsequent luminescence stability screening studies performed over a period of about one year support the applicability of UCNPs as optical authentication tags for construction materials. KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Synthesis KW - Quantum yield KW - NIR KW - Mechanism KW - Characterization KW - XRD KW - Calorimetry KW - Advanced material KW - Cement KW - Monitoring KW - Surface KW - Size KW - Lifetime KW - Barcode KW - Lanthanide KW - Upconversion KW - Encoding KW - Method PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638318 DO - https://doi.org/10.1021/acsomega.5c02236 SN - 2470-1343 VL - 10 IS - 29 SP - 31587 EP - 31599 PB - ACS Publications CY - Washington, DC AN - OPUS4-63831 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schilling, Markus T1 - Semantic Technologies in Action: Integrating Mechanical and Microstructure Data in MSE N2 - Semantic technologies (ST) are a powerful tool for storing, processing, and querying data in a contextualized and interoperable manner. They enable machine-actionable and human-readable knowledge representations essential for advanced data management, retrieval, and reuse. As one of the key factors within the frame of the collaborative project platform MaterialDigital (PMD), the establishment of a virtual material data space and the semantic modeling of hierarchical, process-dependent material data is aimed at to serve as best-practice examples of knowledge representation through ontologies and knowledge graphs. In this presentation, the application of ST to a specific use case from the field of materials sciences and engineering (MSE) is demonstrated: the integration and analysis of data related to a 2000 series age-hardenable aluminum alloy. By semantically representing mechanical and microstructural data obtained from tensile tests and dark-field transmission electron microscopy across various aging times, an expandable knowledge graph was constructed that is aligned with the PMD Core Ontology (PMDco) and enriched through the Tensile Test (TTO) and Precipitate Geometry Ontologies. This semantically integrated dataset enables advanced analytical capabilities via SPARQL queries and reveals microstructure–property relationships consistent with the well-known Orowan mechanism. The approach highlights the potential of semantic data integration to support FAIR data principles and to foster a more data-centric and interoperable research infrastructure in MSE. T2 - MSE Research Data Forum 2025 CY - Siegburg, Germany DA - 08.07.2025 KW - Semantic Data KW - Data Integration KW - Digitalization KW - Data Interoperability PY - 2025 AN - OPUS4-63666 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oskoei, Párástu A1 - Afonso, Rúben A1 - Bastos, Verónica A1 - Nogueira, João A1 - Keller, Lisa-Marie A1 - Andresen, Elina A1 - Saleh, Maysoon I. A1 - Rühle, Bastian A1 - Resch-Genger, Ute A1 - Daniel-da-Silva, Ana L. A1 - Oliveira, Helena T1 - Upconversion Nanoparticles with Mesoporous Silica Coatings for Doxorubicin Targeted Delivery to Melanoma Cells N2 - Melanoma is one of the most aggressive skin cancers and requires innovative therapeutic strategies to overcome the limitations of conventional therapies. In this work, upconversion nanoparticles coated with mesoporous silica and functionalized with folic acid (UCNP@mSiO2-FA) were developed as a targeted nanocarrier system for the delivery of doxorubicin (DOX). The UCNPs were synthesized via thermal decomposition, coated with mesoporous silica shells, and functionalized with folic acid (FA) to enable receptor-mediated targeting. DOX was then loaded into the mesoporous silica coating by adsorption, yielding UCNP@mSiO2-FA-DOX. The different UCNPs were characterized for size, composition, colloidal stability, and loading and release of DOX. This comprehensive physicochemical characterization confirmed a high DOX loading efficiency and a slightly increased drug release under acidic conditions, mimicking the tumour microenvironment. In vitro assays using four melanoma cell lines (A375, B16-F10, MNT-1, and SK-MEL-28) revealed an excellent biocompatibility of UCNP@mSiO2-FA and a significantly higher cytotoxicity of UCNP@mSiO2-FA-DOX compared to unloaded UCNPs, in a dose-dependent manner. Cell cycle analysis demonstrated G2/M phase arrest after treatment with UCNP@mSiO2-FA-DOX, confirming its antiproliferative effect. Overall, UCNP@mSiO2-FA-DOX represents a promising nanoplatform for targeted melanoma therapy, combining active tumour targeting and enhanced anticancer efficacy. KW - Fluorescence KW - Synthesis KW - Nano KW - Particle KW - Silica KW - Cell KW - Uptake KW - Drug KW - Characterization KW - DOX KW - Imaging KW - Toxicity KW - Release KW - pH PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653596 DO - https://doi.org/10.3390/molecules31010074 SN - 1420-3049 VL - 31 IS - 1 SP - 1 EP - 18 PB - MDPI AG AN - OPUS4-65359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Madbouly, Loay Akmal T1 - Chemical analysis of commercial functionalized graphene along the production process N2 - Graphene has been commercialized for over a decade. For many applications like flexible electronics, coating of different materials like paper or for textiles, it used in the form of suspensions or inks. Functionalization enables tailoring the properties of graphene, such as the sheet resistance. X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy are used to characterize the chemical composition of graphene flakes, functionalized and otherwise. In this study, we investigate the following set of commercial materials: fluorine-functionalized graphene (F-graphene) and nitrogen-functionalized graphene (N-graphene) as well as unfunctionalized graphene (G-graphene, as the starting material) in the forms of powders, suspensions, and inks, the latter as the final commercial product. Raman spectroscopy and XPS are complementary techniques. Our results obtained from Raman spectroscopy confirmed the existence of graphene structures in all samples investigated and provided a comparative insight on the structural defects between samples. XPS was used to investigate the chemical states of elements in graphene, such as sp2 and sp3 hybridization states of carbon, as well as the chemical effect of functionalization on graphene. High resolution XPS analysis was performed for C 1s, F 1s and N 1s core-levels for all the graphene samples. The XPS results showed the elemental composition and the impurities of each sample. All powders showed less presence of carboxyl groups, compared to their respective suspensions and inks. F-functionalized suspension and inks showed a significant decrease in the at-% of fluorine relative to the powder. These valuable insights, particularly when correlated, allowed the tracking of the structural and chemical changes of graphene along its production process. T2 - 3rd FUB Nano Colloquium CY - Berlin, Germany DA - 15.07.2025 KW - Functionalized graphene KW - Graphene-related 2D materials (GR2M) KW - Raman Spectroscopy KW - XPS KW - Inks PY - 2025 AN - OPUS4-64116 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Madbouly, Loay Akmal A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - Raman Spectroscopy and X-ray Photoelectron Spectroscopy of Commercial Functionalized Graphene N2 - Graphene has found widespread commercial use, particularly in flexible electronics and coatings for substrates such as paper and textiles, in the form of suspensions and inks (Zhang et al., 2017). Functionalization of graphene allows fine-tuning of properties like electrical conductivity. Structural and chemical features of graphene materials are typically analyzed by Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). While Raman spectroscopy plays a critical role in identifying the presence of graphene and characterizing its structural defects (Pollard et al., 2017), XPS examines the chemistry of graphene. This study investigates three types of graphene materials — graphene (unfunctionalized, G-graphene), fluorine-functionalized graphene (F-graphene), and nitrogen-functionalized graphene (N-graphene) — across three physical forms: powders, suspensions, and embedded in inks. Functionalization was performed via plasma treatment of G-graphene with fluorine or ammonia gases. Suspensions were obtained by dispersing powders in distilled water, while inks were formulated using diacetone alcohol, carbon black, and graphene. Raman spectroscopy analysis confirmed the graphitic nature of all materials and revealed differences in defect density across different forms. The characteristic D, G, and D’ bands varied in relative intensity, offering insight into structural integrity and functionalization effects. XPS measurements examined core-level spectra (C 1s, F 1s, N 1s), revealing chemical bonding environments and hybridization states, including the sp² and sp³ states. A notable decline in fluorine content in F-graphene suspensions and inks, relative to powders, was observed. Existence of organic fluorine and total absence of metallic fluorine were observed. Raman spectroscopy and XPS data provided a correlated view of structural and chemical evolution through the graphene production chain. T2 - Joint Regulatory Risk Assessors Summit – Advancing Safety & Sustainability Assessments of Advanced Materials CY - Paris, France DA - 19.06.2025 KW - Graphene-related 2D materials (GR2M) KW - Inks KW - Raman Spectroscopy KW - XPS KW - Functionalized graphene PY - 2025 UR - https://macrame-project.eu/macrame-meetings-workshops/jointrras/#Agenda AN - OPUS4-63661 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Tamang, S. A1 - Wegner, Karl David A1 - Reiss, P. ED - Alivisatos, P. ED - Jang, E. ED - Ma, R. T1 - Quantum Dot Material Systems, Compositional Families N2 - Following the discovery of the quantum confinement effect in the early 1980s, it took more than 10 years to be able to synthesize monodisperse colloidal quantum dots (QDs) using organometallic chemistry approaches. The researchers behind these pioneering works, Alexey Ekimov, Louis Brus, and Moungi Bawendi, were awarded the Nobel Prize in Chemistry in 2023, exactly 30 years after the seminal report on the preparation of cadmium chalcogenide QDs. From the synthetic point of view, this approach, relying on the fast injection of a chalcogenide precursor dissolved in a tertiary phosphine into a hot solution of the cadmium precursor in a coordinating solvent (trioctylphosphine oxide, TOPO) acting at the same time as surface ligand, was revolutionary. It enabled the fast synthesis of wellcrystallized CdS, CdSe, and CdTe QDs of low size dispersion and high colloidal stability, whose size and hence optical and electronic properties could be conveniently tuned with the reaction time. Due to the comparable ease of this method and the later developed shelling procedures with ZnS, ZnSe, CdS, and mixtures or alloys of these materials, CdSe has become the workhorse for the entire QD field, covering the whole visible range of absorption and emission. Meanwhile, several breakthroughs have been achieved, which enabled us to bring QDs to their maturity of today and integrate them in several applications, in particular those relying on their exceptional luminescence properties, such as biological imaging as well as displays and screens. For such real-life applications, the quest for less toxic, safer-to-use, and environmentally friendly materials is of utmost importanceand a highly active research field. The use of cadmium- and lead-based materials is severely restricted by regulations such as the RoHS directive of the European Union: the maximum concentrations of lead and cadmium are 0.1 and 0.01% by weight, respectively, in all homogeneous materials in electrical and electronicequipment. Several families of alternative materials have been explored, with the most important ones for display technologies being indium phosphide (InP)- and ternary chalcopyrite-type QDs. KW - Quantum dots KW - Photoluminescence KW - LED KW - Display technology PY - 2025 SN - 978-1-394-18187-2 SP - 23 EP - 62 PB - John Wiley & Sons Ltd. AN - OPUS4-64675 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Döring, Sarah A1 - Wulfes, Birte S. A1 - Atanasova, Aleksandra A1 - Jaeger, Carsten A1 - Walzel, Leopold A1 - Tscheuschner, Georg A1 - Flemig, Sabine A1 - Gawlitza, Kornelia A1 - Feldmann, Ines A1 - Konthur, Zoltán A1 - Weller, Michael G. T1 - Corundum Particles as Trypsin Carrier for Efficient Protein Digestion N2 - Reusable enzyme carriers are valuable for proteomic workflows, yet many supports are expensive or lack robustness. This study describes the covalent immobilization of recombinant trypsin on micrometer-sized corundum particles and assesses their performance in protein digestion and antibody analysis. The corundum surface was cleaned with potassium hydroxide, silanized with 3-aminopropyltriethoxysilane and activated with glutaraldehyde. Recombinant trypsin was then attached, and the resulting imines were reduced with sodium cyanoborohydride. Aromatic amino acid analysis (AAAA) estimated an enzyme loading of approximately 1 µg/mg. Non-specific adsorption of human plasma proteins was suppressed by blocking residual aldehydes with a Tris-glycine-lysine buffer. Compared with free trypsin, immobilization shifted the temperature optimum from 50 to 60 °C and greatly improved stability in 1 M guanidinium hydrochloride. Activity remained above 80 % across several reuse cycles, and storage at 4 °C preserved functionality for weeks. When applied to digesting the NISTmAb, immobilized trypsin provided peptide yields and sequence coverage comparable to soluble enzyme and outperformed it at elevated temperatures. MALDI-TOF MS analysis of Herceptin digests yielded fingerprint spectra that correctly identified the antibody and achieved >60 % sequence coverage. The combination of low cost, robustness and analytical performance makes corundum-immobilized trypsin an attractive option for research and routine proteomic workflows. KW - Aluminum oxide KW - Mass spectrometry KW - Enzyme immobilization KW - Antibodies KW - Protein quantification PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647944 DO - https://doi.org/10.20944/preprints202510.2002.v1 SP - 1 EP - 22 PB - Preprints.org AN - OPUS4-64794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ahmed, A. A. A. A1 - Alegret, N. A1 - Almeida, B. A1 - Alvarez-Puebla, R. A1 - Andrews, A. M. A1 - Ballerini, L. A1 - Barrios-Capuchino, J. J. A1 - Becker, C. A1 - Blick, R. H. A1 - Bonakdar, S. A1 - Chakraborty, I. A1 - Chen, X. A1 - Cheon, J. A1 - Chilla, G. A1 - Conceicao, A. L. C. A1 - Delehanty, J. A1 - Dulle, M. A1 - Efros, A. L. A1 - Epple, M. A1 - Fedyk, M. A1 - Feliu, N. A1 - Feng, M. A1 - Fernandez-Chacon, R. A1 - Fernandez-Cuesta, I. A1 - Fertig, N. A1 - Förster, S. A1 - Garrido, J. A. A1 - George, M. A1 - Guse, A. H. A1 - Hampp, N. A1 - Harberts, J. A1 - Han, J. A1 - Heekeren, H. R. A1 - Hofmann, U. G. A1 - Holzapfel, M. A1 - Hosseinkazemi, H. A1 - Huang, Y. A1 - Huber, P. A1 - Hyeon, T. A1 - Ingebrandt, S. A1 - Ienca, M. A1 - Iske, A. A1 - Kang, Y. A1 - Kasieczka, G. A1 - Kim, D.-H. A1 - Kostarelos, K. A1 - Lee, J.-H. A1 - Lin, K.-W. A1 - Liu, S. A1 - Liu, X. A1 - Liu, Y. A1 - Lohr, C. A1 - Mailänder, V. A1 - Maffongelli, L. A1 - Megahed, S. A1 - Mews, A. A1 - Mutas, M. A1 - Nack, L. A1 - Nakatsuka, N. A1 - Oertner, T. G. A1 - Offenhäusser, A. A1 - Oheim, M. A1 - Otange, B. A1 - Otto, F. A1 - Patrono, E. A1 - Peng, B. A1 - Picchiotti, A. A1 - Pierini, F. A1 - Pötter-Nerger, M. A1 - Pozzi, M. A1 - Pralle, A. A1 - Prato, M. A1 - Qi, B. A1 - Ramos-Cabrer, P. A1 - Resch-Genger, Ute A1 - Ritter, N. A1 - Rittner, M. A1 - Roy, S. A1 - Santoro, F. A1 - Schuck, N. W. A1 - Schulz, F. A1 - Seker, E. A1 - Skiba, M. A1 - Sosniok, M. A1 - Stephan, H. A1 - Wang, R. A1 - Wang, T. A1 - Wegner, Karl David A1 - Weiss, P. S. A1 - Xu, M. A1 - Yang, C. A1 - Zargarin, S. S. A1 - Zeng, Y. A1 - Zhou, Y. A1 - Zhu, D. A1 - Zierold, R. A1 - Parak, W. J. T1 - Interfacing with the Brain: How Nanotechnology Can Contribute N2 - Interfacing artificial devices with the human brain is the central goal of neurotechnology. Yet, our imaginations are often limited by currently available paradigms and technologies. Suggestions for brain−machine interfaces have changed over time, along with the available technology. Mechanical levers and cable winches were used to move parts of the brain during the mechanical age. Sophisticated electronic wiring and remote control have arisen during the electronic age, ultimately leading to plug-and-play computer interfaces. Nonetheless, our brains are so complex that these visions, until recently, largely remained unreachable dreams. The general problem, thus far, is that most of our technology is mechanically and/or electrically engineered, whereas the brain is a living, dynamic entity. As a result, these worlds are difficult to interface with one another. Nanotechnology, which encompasses engineered solid-state objects and integrated circuits, excels at small length scales of single to a few hundred nanometers and, thus, matches the sizes of biomolecules, biomolecular assemblies, and parts of cells. Consequently, we envision nanomaterials and nanotools as opportunities to interface with the brain in alternative ways. Here, we review the existing literature on the use of nanotechnology in brain−machine interfaces and look forward in discussing perspectives and limitations based on the authors’ expertise across a range of complementary disciplines from neuroscience, engineering, physics, and chemistry to biology and medicine, computer science and mathematics, and social science and jurisprudence. We focus on nanotechnology but also include information from related fields when useful and complementary. KW - Nanoneuro interface KW - Brain-on-a-chip KW - Nanostructured interface KW - Electrode arrays KW - Neuro-implants KW - Advanced nanomaterials KW - Quality assurance PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634893 DO - https://doi.org/10.1021/acsnano.4c10525 SN - 1936-086X VL - 19 IS - 11 SP - 10630 EP - 10717 PB - ACS Publications AN - OPUS4-63489 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - El-Dahshan, O. A1 - Deniaud, A. A1 - Ling, W. L. A1 - Wegner, Karl David A1 - Proux, O. A1 - Veronesi, G. A1 - Reiss, P. T1 - Hydrothermal microwave synthesis of water soluble NIR-II emitting Ag2S quantum dots N2 - Hydrothermal-based synthetic methods of quantum dots allow for the exploration of reaction parameters normally inaccessible to typical aqueous-based batch reactions, such as elevated reaction temperatures (>100 °C) and reaction pressures above atmospheric pressure. Coupled with microwave heating, new instantaneously bio-compatible quantum dots (QDs) with enhanced opitcal properties can be yielded. As of today, aqueous-based synthetic methods often lag behind their organic analogues in terms of the photophysical properties of the QDs obtained and the ease of modulation of both the emission wavelength and crystallite size. Using a novel microwave-assisted hydrothermal approach, the synthesis of silver sulphide (Ag2S) QDs exhibiting NIR emission spanning the biological transparency windows via modulation of the reaction parameters has been developed. The intrinsic link between their optical and structural properties is explored via laboratory and synchrotron-based structural analysis techniques. Their toxicity towards a hepatic cell line was assessed, and related back to their structure and size. Overall this work aims to not only further develop the repertoire of synthetic methods for the synthesis of Ag2S QDs, but also paves the way for the development of safer QDs suitable for future clinical applications. KW - Quantum dots KW - Microwave synthesis KW - Quality assurance KW - NIR-II emission KW - PL quantum yield KW - Ag2S PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634825 DO - https://doi.org/10.1039/d5nr00052a SN - 2040-3372 VL - 17 IS - 24 SP - 14637 EP - 14646 PB - RSC AN - OPUS4-63482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nakadi, Flavio V. T1 - Single-event analysis of discrete entities using microwave-induced nitrogen plasma–mass spectrometry N2 - ICP-MS has become a standard for (ultra)trace elemental analysis due to its excellent sensitivity and multi-element capabilities. However, its widespread use is hampered by spectral interferences—especially in the low mass range (<81 amu)—primarily arising from Ar-based polyatomic ions, such as ArO+ and Ar2+, which compromise the accurate quantification of key elements like Fe and Se.1 Over the years, improvements such as collision/reaction cells and sector-field configurations have helped mitigate these interferences, albeit often at the cost of instrument complexity and increased operational burden.The microwave-induced nitrogen plasma (MINP) source, sustained by microwaves at atmospheric pressure and using nitrogen as the plasma gas, offers a fundamentally different plasma environment. Nitrogen is not only more economical (40-60%) and readily available than Ar, but also avoids the generation of problematic Ar-based interferences. While MINP had been previously applied in optical emission and bulk mass spectrometry,2 its implementation in single-event detection had not yet been demonstrated. This study pioneers the application of MINP-MS in single-event mode for real-time, high-throughput characterization of NPs, cells, and MPs. The evaluation began with Fe2O3 NPs monitoring the 56Fe nuclide, with a limit of detection of 8.6 ag for Fe, equivalent to a particle size threshold of 19 nm—surpassing the detection capabilities of quadrupole-based ICP-MS systems. Size distribution results obtained by SP-MINP-MS for Fe2O3 NPs (20–70 nm) matched closely with transmission electron microscopy (TEM) and dynamic light scattering (DLS), confirming the method’s accuracy. For Se, despite its high ionization energy, metallic SeNPs (150 and 250 nm) were reliably quantified by monitoring 80Se. A calibration curve constructed using SeNP standards yielded excellent linearity (R2 = 0.9994). This approach was further extended to single-cell analysis, using Se-enriched yeast (SELM-1 CRM) as a model. A transport efficiency-independent calibration strategy was employed, relying on SeNPs to determine Se content per cell. The results showed strong agreement with data from conventional SC-ICP-MS, with average Se masses of ~65 fg per cell, validating the performance of SC-MINP-MS for biological systems. Additionally, the instrument's capability to handle large, low atomic number particles was demonstrated via the analysis of polystyrene (PS) and polytetrafluoroethylene (PTFE) MPs. These MPs (2.5–3.0 µm) were quantified by monitoring 12C+ signals and applying a calibration strategy using citric acid as a standard. The resulting size distributions closely matched nominal sizes, reinforcing the system’s robustness for micrometer-sized polymeric materials. Event durations ranging from 470 to over 900 µs were consistent with literature values for single-entity ICP-MS and correlated well with particle size. These findings establish single-event MINP-MS as a promising analytical platform for analyzing discrete entities. It provides significant advantages over conventional Ar-based ICP-MS, including reduced interferences, lower operational cost, and comparable or superior sensitivity for analytes such as Fe and Se. By avoiding the limitations of Ar-based plasmas and enabling accurate quantification across a wide range of particle types and sizes, MINP-MS in single-event mode opens new avenues for high-resolution, interference-free elemental analysis at the individual entity level. T2 - 17th Rio Symposium on Atomic Spectrometry (17th RSAS) CY - São Pedro City, Brazil DA - 09.11.2025 KW - MICAP-MS KW - Nitrogen plasma KW - Nanoparticles KW - Cells KW - Microplastic KW - Single particle KW - Single event KW - ICP-MS PY - 2025 AN - OPUS4-64954 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Döring, Sarah T1 - Corundum Particles as Trypsin Carrier for Efficient Protein Digestion N2 - This dataset contains raw LC–MS/MS files of trypsin-digested NISTmAb acquired on a SCIEX TripleTOF 6600 mass spectrometer in DIA (SWATH) mode for antibody quantification. In addition, it includes MALDI-TOF MS peptide mass fingerprints of trypsin-digested Herceptin as well as reference spectra that can be used for antibody identification using the open-source software ABID 2.0 (https://bam.de/ABID). The data were generated within a study demonstrating the applicability of corundum-immobilized trypsin for antibody digestion and its suitability for peptide-based LC–MS/MS quantification and MALDI-TOF MS fingerprinting–based antibody identification. KW - NISTmAb KW - Herceptin KW - MALDI-TOF MS peptide mass fingerprint KW - ABID 2.0 PY - 2025 DO - https://doi.org/10.5281/zenodo.17416536 PB - Zenodo CY - Geneva AN - OPUS4-65365 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madbouly, Loay Akmal A1 - Sturm, Heinz A1 - Doolin, Alexander A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - Chemical Analysis of Commercial Functionalized Graphene Nanoplatelets along the Production Process with Raman Spectroscopy and X-ray Photoelectron Spectroscopy N2 - Commercial applications increasingly rely on functionalized graphene nanoplatelets (GNPs) supplied as powders, aqueous suspensions, and printable inks, yet their process−structure−property relationships across the production chain remain to be fully mapped. Here we apply a correlative Raman spectroscopy (Raman) and X-ray photoelectron spectroscopy (XPS) workflow to nine independent industrial graphene batches spanning three surface chemistries, raw (R), fluorinated (F), and nitrogen-functionalized (N), in all three physical forms which are powders, suspensions, and inks. Raman mapping (with a 532 nm excitation laser) showed that I2D/IG is highest for N samples and lowest for R-ink. A 2D-vs-G correlation places all samples on a trajectory parallel to the pure-doping vector, which can correlate to holes in the graphene lattice. The mean point-defect spacing is LD = 8.4−10.0 nm. High-resolution XPS resolves the accompanying chemical changes: F-powder exhibits distinct C−F (289 eV), C−F2 (292 eV), and C−F3 (293 eV) components and loses roughly half its F content upon dispersion in deionized water or ink formulation; inks of all chemistries show a pronounced O−C=O peak near 289−290 eV originated from the ink compounds. N-functionalized samples showed a prominent C−N (285.5 eV) only for the ink formulated N-functionalized sample. This study establishes a process-aware blueprint linking the functionalization route and formulation step to lattice disorder and surface chemistry, offering transferable quality-control metrics for graphene supply chains in industrial products/applications such as coatings, storage devices, and printed electronics. KW - Functionalized graphene KW - Raman Spectroscopy KW - XPS KW - Chemical analysis PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652548 DO - https://doi.org/10.1021/acs.jpcc.5c06820 SN - 1932-7447 VL - 129 IS - 50 SP - 22033 EP - 22040 PB - American Chemical Society (ACS) AN - OPUS4-65254 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Madbouly, Loay Akmal T1 - Chemical analysis of commercial functionalized graphene along the production process N2 - Graphene has found widespread commercial use, particularly in flexible electronics and coatings for substrates such as paper and textiles, in the form of suspensions and inks (Zhang et al., 2017). Functionalization of graphene allows fine-tuning of properties like electrical conductivity. Structural and chemical features of graphene materials are typically analyzed by Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). While Raman spectroscopy plays a critical role in identifying the presence of graphene and characterizing its structural defects (Pollard et al., 2017), XPS examines the chemistry of graphene. This study investigates three types of graphene materials — graphene (unfunctionalized, G-graphene), fluorine-functionalized graphene (F-graphene), and nitrogen-functionalized graphene (N-graphene) — across three physical forms: powders, suspensions, and embedded in inks. Functionalization was performed via plasma treatment of G-graphene with fluorine or ammonia gases. Suspensions were obtained by dispersing powders in distilled water, while inks were formulated using diacetone alcohol, carbon black, and graphene. Raman spectroscopy analysis confirmed the graphitic nature of all materials and revealed differences in defect density across different forms. The characteristic D, G, and D’ bands varied in relative intensity, offering insight into structural integrity and functionalization effects. XPS measurements examined core-level spectra (C 1s, F 1s, N 1s), revealing chemical bonding environments and hybridization states, including the sp² and sp³ states. A notable decline in fluorine content in F-graphene suspensions and inks, relative to powders, was observed. Existence of organic fluorine and total absence of metallic fluorine were observed. Raman spectroscopy and XPS data provided a correlated view of structural and chemical evolution through the graphene production chain (Figure 1). T2 - RamanFest 2025 CY - Frankfurt, Germany DA - 02.07.2025 KW - Functionalized graphene KW - Graphene-related 2D materials (GR2M) KW - Raman Spectroscopy KW - XPS KW - Inks PY - 2025 AN - OPUS4-64114 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Madbouly, Loay Akmal T1 - Raman Spectroscopy and X-ray Photoelectron Spectroscopy of Commercial Functionalized Graphene N2 - Graphene has been commercialized for over a decade. For many applications like flexible electronics, coating of different materials like paper or for textiles, it used in the form of suspensions or inks [1]. Graphene powders are typically used as the starting material for the synthesize of graphene suspensions and graphene inks. Functionalization enables tailoring the properties of graphene, such as the sheet resistance. X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, along other techniques are used to characterize graphene flakes, functionalized and otherwise. Raman spectroscopy is necessary as a primary step to validate the existence of graphene structure in graphene powders [2]. XPS is commonly used to investigate the elemental composition, including impurities, and the chemical structure of graphene. In this study, we investigate the following set of commercial materials: fluorine-functionalized graphene (F-graphene) and nitrogen-functionalized graphene (N-graphene) as well as unfunctionalized graphene (G-graphene) in the forms of powders, suspensions, and inks. The functionalization process for the graphene powder was carried out in a plasma reactor by purging fluorine and ammonia gases, in separate processes, over the G-graphene powder. The suspensions were prepared by adding distilled water to the powders. The inks consist of diacetone alcohol, carbon black, and graphene powders. Raman spectroscopy and XPS are complementary techniques. Our results obtained from Raman spectroscopy confirmed the existence of graphene structures in all samples and provided a comparative insight on the structural defects between samples. XPS was used to investigate the chemical states of elements in graphene, such as sp2 and sp3 hybridization states of carbon, as well as the chemical effect of functionalization on graphene. High resolution XPS analysis was performed for C 1s, F 1s and N 1s core-levels for all the graphene samples: G-graphene, F-graphene, and N-graphene, in all forms. The XPS results showed the elemental composition and the impurities of each sample. All powders showed less presence of carboxyl groups, compared to their respective suspensions and inks. F-functionalized suspension and inks showed a significant decrease in the at% of fluorine relative to the powder. These valuable insights, independent and when correlated, allowed the tracking of the structural and chemical changes of graphene along its production process. T2 - E-MRS 2025 CY - Strasbough, France DA - 26.05.2025 KW - Functionalized graphene inks PY - 2025 AN - OPUS4-64113 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholtz, Lena T1 - Luminescent, Semiconductor Nanoparticle-Loadedpolymer Microbeads–Comparingparticlearchitectures N2 - Luminescent polymer microparticles (PMPs) are applied in various (bio)analytical and diagnostic processes.[1] The staining of these beads is important for the realization of optically distinguishable barcodes that can be read out, e.g., by a flow cytometer or fluorescence microscope. Typically, luminescent semiconductor nanoparticles (NPs) absorb in a broad wavelength range and show narrow emission bands, which enables simultaneous excitation of differently colored luminophores and facilitates a spectral discrimination.[1] This makes them ideal candidates for this purpose and encouraged us to explore and develop a simple, effective approach to luminescent semiconductor NP encoding of polystyrene PMPs and identify suitable synthesis conditions.[2] Until now, mainly semiconductor quantum dots (QDs) have been used for the synthesis of luminescent PMPs, although NPs with different shapes could introduce beneficial new features. Aiming for the application of our developed procedure to non-spherical NPs, we systematically investigated the luminescence properties of the resulting NP-stained beads using fluorescence and integrating sphere spectroscopy as well as fluorescence and electron microscopy. These studies showed that the suitability of semiconductor NPs for the synthesis of luminescent PMPs depends not only on their shape, but also heavily on their surface chemistry.[3] The successful incorporation of nonspherical NPs opens the path to include even more NPs, and the results can help to deduce future applications for the beads which best suit their specific properties. T2 - E-MRS Fall Meeting 2025 CY - Warsaw, Poland DA - 15.09.2025 KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Synthesis KW - Quantum dot KW - Quantum rod KW - Platelet KW - Quantum yield KW - Polymer particle KW - Encoding KW - Surface chemistry KW - Mechanism KW - Characterization KW - Lifetime KW - Barcode KW - Polymerization KW - Method PY - 2025 AN - OPUS4-64242 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wegner, Karl David T1 - Ag₂S nanocrystals as next-generation, heavy-metal free SWIR emitter for biomedical imaging and sensing applications N2 - There is a growing interest in the exploitation of the short-wave infrared (SWIR), which refers to the wavelength band of light between 900 nm and 2500 nm. Luminophores that emit in the SWIR are used in various areas of telecommunications, photovoltaics, security systems (night vision), and in biomedicine. In particular for biomedical applications, the SWIR range is highly promising because light scattering, absorption, and autofluorescence of tissue and biological compounds are strongly reduced compared to the visible (400–700 nm) and NIR (~700–900 nm). The benefits of SWIR-emissive QDs have been demonstrated for a variety of applications, such as in thermal sensing, as photoelectrochemical biosensor, in in vivo vascular imaging, and for fluorescence-guided surgery. Full exploitation of SWIR photoluminescence (PL) imaging and sensing is currently hampered by i.) a lack of suitable advanced nanomaterials with a high PL quantum yield (PL QY) and a high brightness, that can be used safely in vivo and ii.) a lack of quantitative and reliable data on the optical properties of many SWIR emitters. Promising nanomaterials for the SWIR are heavy metal-free Ag2S quantum dots (QDs). Aiming for the development of SWIR advanced nanomaterials with optimum performance, we have dived deeper into the photophysical processes occurring in these nanomaterials, thereby exploring in depth how the environment such as temperature, surface ligand composition, and the incorporation of transition metals influence the optical properties Ag2S QDs. We observed a strong enhancement of the SWIR emission of upon addition of metal ions such as Zn2+, yielding PL quantum yields of about 10% and thus making them highly suitable for non-invasive deep imaging of vascular networks and 3D fluid flow mapping. T2 - Shining a light on biomedical and energy applications (Shift) CY - Tenerife, Spain DA - 13.10.2025 KW - Quantum dots KW - Short-wave infrared KW - SWIR KW - Spectroscopy KW - Photoluminescence KW - Quantum yield PY - 2025 AN - OPUS4-64673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nicolai, Marcel T1 - Investigation of 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 - 2025 ICU PADERBORN - 9th International Congress on Ultrasonics CY - Paderborn, Germany DA - 21.09.2025 KW - Lamb waves KW - Mode repulsion KW - Coupled plates KW - Elastic interface KW - Dispersion curves PY - 2025 AN - OPUS4-65531 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -