TY - CONF A1 - Bonse, Jörn T1 - Funktionalisierung durch laser-induzierte periodische Oberflächenstrukturen N2 - Der Vortrag gibt einen Überblick über die vielfältigen Möglichkeiten der Oberflächenfunktionalisierung mittels Mikro- und Nanostrukturierung durch Ultrakurzpuls-Lasermaterialbeabeitung. Dies schließt eine Diskussion des Phänomens der Laser-induzierten periodischen Oberflächenstrukturen (LIPSS, engl.: Laser-induced Periodic Surface Structures, Ripples), sowie deren Klassifikation und Bildungsmechanismen mit ein. Ein Schwerpunkt der Präsentation liegt auf der Diskussion verschiedener Anwendungsmöglichkeiten der LIPSS in Bereichen der Optik, Fluidik, Tribologie und Medizin, sowie auf einem Ausblick auf die industrielle Skalierbarkeit der LIPSS-Technologie. T2 - 1. Netzwerktreffen 2024 des UKPL-Innovationsnetzwerks CY - Rostock, Germany DA - 11.03.2024 KW - Laser-induced Periodic Surface Structures (LIPSS) KW - Oberflächenfunktionalisierung KW - Mikrostrukturen KW - Nanostrukturen KW - Ultrakurzpuls-Laserbearbeitung PY - 2024 AN - OPUS4-59657 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Omar, Hassan A1 - Szymoniak, Paulina A1 - Hertwig, Andreas A1 - Schönhals, Andreas T1 - Investigations of Ultrathin Polymer Films Supported on Inorganic Substrates N2 - Interactions between a polymer and a substrate interface play a vital role in understanding the improvement in thin film material properties as well as serving as a model for nanocomposites. For any non-repulsive polymer-substrate interactions, polymer segments form an irreversibly adsorbed layer and show a slowdown in the glassy dynamics and thus an increase in the thermal glass transition temperature compared to the bulk-like values. The growth kinetics of the adsorbed layer showed a deviation for both poly (bisphenol-A carbonate) (PBAC) and polysulfone (PSU), two bulky polymers containing a functional group (phenyl ring) in the backbone. T2 - Royal Society of Chemistry (RSC) Online Poster Conference CY - Online meeting DA - 05.03.2024 KW - Adsorbed Layer KW - Thin Films KW - Atomic Force Microscopy KW - Ellipsometry PY - 2024 AN - OPUS4-59625 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hodoroaba, Vasile-Dan T1 - Delivering Impact - A new ISO standard on the identification of nanoparticles N2 - Nanoparticles (NPs) are tiny – around 1 to 100 billionths of a meter – and can have different chemistries and behaviours than the same material of larger size. This property has led to advances in a wide range of industries, but it can also confer toxicity. Size measurements are the main way NPs are identified but a lack of standardised methods for identifying ones with complex shapes has hindered evaluation of their potential harm. KW - Nanoparticles KW - Standardisation KW - Particle size distribution KW - nPSize KW - ISO 21363 PY - 2024 UR - https://www.euramet.org/casestudies/casestudiesdetails/news/default-c3b26209e8 SP - 1 EP - 2 PB - EURAMET CY - Braunschweig AN - OPUS4-59626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emamverdi, Farnaz A1 - Huang, J. A1 - Szymoniak, Paulina A1 - Bojdys, M. J. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Structure and molecular mobility of phosphinine-based covalent organic frameworks – glass transition of amorphous COFs JF - Materials Advances N2 - Two-dimensional covalent organic frameworks (COFs) based on phosphinine and thiophene building blocks have been synthesized with two different side groups. The materials are denoted as CPSF-MeO and CPSF-EtO where CxxF correspond to the covalent framework, whereas P and S are related to heteroatoms phosphorous and sulfur. MeO and EtO indicate the substituents, i.e. methoxy and ethoxy. Their morphologies were studied by scanning electron microcopy and X-ray scattering. The absence of crystalline reflexes in the X-ray pattern reveal that both materials are amorphous and can be considered as glasses. Furthermore, N2 adsorption measurements indicate substantial Brunauer–Emmett–Teller (BET) surface area values pointing to the formation of three-dimensional pores by stacking of the aromatic 2D layer. An analysis of the porosity of both COFs showed a mean radius of the pores to be of ca. 4 nm, consistent with their chemical structure. The COFs form nanoparticles with a radius of around 100 nm. The thermal behavior of the COFs was further investigated by fast scanning calorimetry. These investigations showed that both COFs undergo a glass transition. The glass transition temperature of CPSF-EtO is found to be ca. 100 K higher than that for CPSF-MeO. This large difference in the glass transition is discussed to be due to a change in the interaction of the COF sheets induced by the longer ethoxy group. It might be assumed that for CPSF-EtO more individual COF sheets assemble to larger stacks than for CPSF-MeO. This agrees with the much larger surface area value found for CPSF-EtO compared to CPSF-MeO. To corroborate the results obtained be fast scanning calorimetry dielectric measurements were conducted which confirm the occurrence of a dynamic glass transition. The estimated temperature dependence of the relaxation rates of the dielectric relaxation and their absolute values agrees well with the data obtained by fast scanning calorimetry. Considering the fragility approach to the glass transition, it was further found that CPSF-MeO is a fragile glass former whereas CPSF-EtO behaves as a strong glass forming material. This difference in the fragility points also to distinct differences in the interaction between the 2D COF molecules in both materials. KW - Covalent Organic frameworks PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-596770 DO - https://doi.org/10.1039/d3ma01123b SP - 1 EP - 10 PB - Royal Society of Chemistry (RSC) AN - OPUS4-59677 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Glimpses of the future: Systematic investigations of 1200 mofs using a highly automated, full-stack materials research laboratory N2 - By automatically recording as much information as possible in automated laboratory setups, reproducibility and traceability of experiments are vastly improved. This presentation shows what such an approach means for the quality of experiments in an X-ray scattering laboratory and an automated synthesis set-up. T2 - Winter School on Metrology and Nanomaterials for Clean Energy CY - Claviere, Italy DA - 28.01.2024 KW - Digitalization KW - Automation KW - Digital laboratory KW - Scattering KW - Synthesis KW - Nanomaterials KW - Holistic science PY - 2024 AN - OPUS4-59621 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - The Dark Side of Science (2024 edition) N2 - This presentation highlights ongoing scientific misconduct as found in academic literature. This includes data- and image manipulation, and paper mills. Starting with an expose of examples, it delves deeper into the causes and metrics driving this phenomenon. Finally a range of possible tools is presented, that the young researcher can use to prevent themselves from sliding into the dark scientific methods. T2 - Winter School on Metrology and Nanomaterials for Clean Energy CY - Claviere, Italy DA - 28.01.2024 KW - Scientific misconduct KW - Data manipulation KW - Image manipulation KW - Paper mills KW - Causes leading to scientific misconduct KW - Tools to combat scientific misconduct KW - Metrics PY - 2024 AN - OPUS4-59622 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lindemann, Franziska T1 - Bestimmung der spezifischen Oberfläche mittels Gasadsorption (BET-Verfahren) N2 - Im Rahmen des 2. BAM-Akademie Info-Tages "Nano or not Nano" wurde die OECD TG 124 "Volume Specific Surface Area of Manufactured Nanomaterials" vorgestellt. Der Vortrag beschreibt die Bestimmung der spezifischen Oberfläche von dispersen und/oder porösen Pulvern mittels Gasadsorption nach dem BET-Verfahren. Es wird auf die Anwendbarkeit der Methode eingegangen und es werden praktische Hinweise zur Probenvorbereitung und Messung von Nanomaterialien gegeben. T2 - BAM Akademie II: Info-Tage "Nano or not Nano" CY - Online meeting DA - 25.01.2024 KW - OECD TG 124 KW - Nanopulver KW - VSSA KW - Nano powder KW - BET KW - Spezifische Oberfläche PY - 2024 AN - OPUS4-59623 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Hörmann, Anja T1 - Trinamic TMCL IOC for exposing Trinamics motor controllers to EPICS CA N2 - Trinamic TMCL IOC is a Python package designed for controlling stepper motors connected to a Trinamic board using the TMCL language (all boards supported by PyTrinamic should now work, has been tested on the TMCM 6110 and the TMCM 6214). Since it is implementing the TMCL protocol, it should be easy to adapt to other Trinamic motor controller boards. This package assumes the motor controller is connected over a machine network via a network-to-serial converter, but the underlying PyTrinamic package allows for other connections too. This allows the control of attached motors via the EPICS Channel-Access virtual communications bus. If EPICS is not desired, plain Pythonic control via motion_control should also be possible. An example for this will be provided in the example.ipynb Jupyter notebook. This package leverages Caproto for EPICS IOCs and a modified PyTrinamic library for the motor board control, and interfaces between the two via an internal set of dataclasses. Configuration for the motors and boards are loaded from YAML files (see tests/testdata/example_config.yaml). The modifications to PyTrinamic involved extending their library with a socket interface. This was a minor modification that should eventually find its way into the official package (a pull request has been submitted). KW - Instrumentation KW - Motor controller KW - EPICS KW - Channel access KW - Instrument control KW - Laboratory automation PY - 2024 DO - https://doi.org/10.5281/zenodo.10792593 PB - Zenodo CY - Geneva AN - OPUS4-59624 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Moeez, A. A1 - Hörmann, Anja A1 - Breßler, Ingo T1 - Example configurations and test cases for the Python HDF5Translator framework. N2 - This is a set of use examples for the HDF5Translator framework. This framework lets you translate measurement files into a different (e.g. NeXus-compatible) structure, with some optional checks and conversions on the way. For an in-depth look at what it does, there is a blog post here. The use examples provided herein are each accompanied by the measurement data necessary to test and replicate the conversion. The README.md files in each example show the steps necessary to do the conversion for each. We encourage those who have used or adapted one or more of these exampes to create their own conversion, to get in touch with us so we may add your example to the set. KW - Measurement data conversion KW - Data conversion KW - HDF5 KW - NeXus KW - NXsas KW - Framework KW - Python PY - 2024 DO - https://doi.org/10.5281/zenodo.10925971 PB - Zenodo CY - Geneva AN - OPUS4-59796 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Hörmann, Anja A1 - Moeez, Abdul A1 - Breßler, Ingo T1 - BAMresearch/HDF5Translator: A Framework for translating and transforming data between HDF5 files N2 - HDF5Translator is a Python framework for translating and transforming data between HDF5 files. It supports operations like unit conversion, dimensionality adjustments, and subtree copying, making it suitable for managing and manipulating a wide range of scientific datasets. KW - Measurement data conversion KW - Data conversion KW - HDF5 KW - NeXus KW - NXsas KW - Framework KW - Python KW - Methodology PY - 2024 DO - https://doi.org/10.5281/zenodo.10927639 PB - Zenodo CY - Geneva AN - OPUS4-59797 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Omar, Hassan A1 - Szymoniak, Paulina A1 - Hertwig, Andreas A1 - Schönhals, Andreas T1 - Growth Kinetics and Molecular Mobility of the Adsorbed Layer of Poly(bisphenol-A Carbonate) (PBAC), Polysulfone (PSU), and Poly (2-Vinyl Pyridine) (P2VP) N2 - Interactions between a polymer and a substrate interface play a vital role in understanding the improvement in thin film material properties as well as serving as a model for nanocomposites. For any non-repulsive polymer-substrate interactions, polymer segments form an irreversibly adsorbed layer and show a slowdown in the glassy dynamics and thus an increase in the thermal glass transition temperature compared to the bulk-like values. The growth kinetics of the adsorbed layer showed a deviation for both poly (bisphenol-A carbonate) (PBAC) and polysulfone (PSU), two bulky polymers containing a functional group (phenyl ring) in the backbone, compared to conventional polymers previously studied like poly-2-vinyl pyridine (P2VP). This deviation was attributed to the bulkiness of the phenyl rings. . Further investigations into the influence of the adsorbed layer on glassy dynamics were conducted. The molecular mobility and glass transition for thin films of PBAC and PSU were compared to bulk samples of each polymer. Broadband dielectric spectroscopy, atomic force microscopy, and ellipsometry were primarily used and additionally supported by sum frequency generation spectroscopy. T2 - Deutsche Physikalische Gesellschaft (DPG) Tagung CY - Berlin, Germany DA - 17.03.2024 KW - Thin films KW - Adsorbed Layer KW - Atomic Force Microscopy KW - Ellipsometry KW - Dielectric Spectroscopy PY - 2024 AN - OPUS4-59821 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Feng, Wen A1 - Gemming, Thomas A1 - Giebeler, Lars A1 - Qu, Jiang A1 - Weinel, Kristina A1 - Agudo Jácome, Leonardo A1 - Büchner, Bernd A1 - González-Martínez, Ignacio T1 - Influence of magnetic field on electron beam-induced Coulomb explosion of gold microparticles in transmission electron microscopy JF - Ultramicroscopy N2 - In this work we instigated the fragmentation of Au microparticles supported on a thin amorphous carbon film by irradiating them with a gradually convergent electron beam inside the Transmission Electron Microscope. This phenomenon has been generically labeled as “electron beam-induced fragmentation” or EBIF and its physical origin remains contested. On the one hand, EBIF has been primarily characterized as a consequence of beam-induced heating. On the other, EBIF has been attributed to beam-induced charging eventually leading to Coulomb explosion. To test the feasibility of the charging framework for EBIF, we instigated the fragmentation of Au particles under two different experimental conditions. First, with the magnetic objective lens of the microscope operating at full capacity, i.e. background magnetic field B = 2 T, and with the magnetic objective lens switched off (Lorenz mode), i.e. B = 0 T. We observe that the presence or absence of the magnetic field noticeably affects the critical current density at which EBIF occurs. This strongly suggests that magnetic field effects play a crucial role in instigating EBIF on the microparticles. The dependence of the value of the critical current density on the absence or presence of an ambient magnetic field cannot be accounted for by the beam-induced heating model. Consequently, this work presents robust experimental evidence suggesting that Coulomb explosion driven by electrostatic charging is the root cause of EBIF. KW - Electron beam-induced fragmentation KW - Coulomb explosion KW - X-ray diffraction KW - Lorenz transmission electron microscopy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600247 DO - https://doi.org/10.1016/j.ultramic.2024.113978 SN - 0304-3991 VL - 262 SP - 1 EP - 8 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-60024 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fareed, Adnan A1 - Rosalie, Julian M. A1 - Kar, Satyakam A1 - Fähler, Sebastian A1 - Maaß, Robert T1 - Small-scale functional fatigue of a Ni-Mn-Ga Heusler alloy JF - Acta Materialia N2 - Functional fatigue of shape-memory alloys is a considerable threat to the reliable service of actuation devices. Here, we demonstrate the essentially degradation-free cyclic phase-transformation behavior of Ni-Mn-Ga microcrystals up to one million stress-driven superelastic cycles. Cyclic dissipation amounts to about 1/5 of the bulk counterpart and remains unaffected during cycling, even after the introduction of dislocation structures via plastic straining. Plastic yielding and the transformation stress largely exceed the known bulk values. However, the transformation-stress is found to depend on plastic pre-straining, which suggests that the size-affected transformation stress is sensitive to the initial defect structure and that it can be tuned by a targeted introduction of dislocations. These findings demonstrate the high suitability of Ni-Mn-Ga as a robust shape-memory alloy in small-scale functional device engineering. KW - Superelasticity KW - Shape-memory alloys KW - Functional fatigue KW - Ni-Mn-Ga PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600695 DO - https://doi.org/10.1016/j.actamat.2024.119988 VL - 274 SP - 1 EP - 10 PB - Elsevier B.V. AN - OPUS4-60069 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tokarski, T. A1 - Nolze, Gert T1 - Exploring Unconventional Uses of Kikuchi Pattern Analysis N2 - The characterization of really unknown phases typically uses 70 to 150 reflectors for lattice metric calculation. The determination of the lattice parameters follows with 4% accuracy. Including a Z correction up to 1% can be reached. The precision of the lattice parameters ratios (a:b:c) is, however, better than 0.1%. T2 - Oxford Users Meeting 2024 CY - Krakow, Poland DA - 14.05.2024 KW - EBSD KW - Kikuchi KW - Lattice parameters KW - Ratio refinement PY - 2024 AN - OPUS4-60086 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wojciak, K. A1 - Tokarski, T. A1 - Cios, G. A1 - Nolze, Gert T1 - Precision and accuracy during standard-less mapping of local lattice distortions using ebsd and calm technique N2 - Electron Back Scatter Diffraction (EBSD) is a very versatile analytical technique allowing for the characterization of material structure. Historically, diffraction images (Kikuchi patterns) registered during EBSD analysis were solved using Hough/Radon transformation. The last decade brought several novel techniques of experimental pattern analysis, focusing entirely on image analysis routines such as pattern matching, or various variants of High-Resolution EBSD. However, all the above-mentioned techniques require prior knowledge of the material structure to perform orientation analysis. The recently presented algorithm employed in Crystallographic Analysis of Lattice Metric (CALM) software, effectively removes this limitation enabling a standard-less analytical approach in EBSD systems. At its core, the CALM technique couples accurate detection of the Kikuchi bands position, with a rigid construction of reciprocal lattice resulting from translational crystal symmetry. A unique characteristic of the methodology also gives an opportunity for application in the analysis of continuous lattice changes, for example tetragonality mapping. During mapping, however, the geometry of the gnomonic projection (represented by the projection center) is continuously altered decreasing overall algorithm efficiency. The work presents an analysis of the projection center in terms of precision and accuracy. T2 - Oxford User Meeting 2024 CY - Krakow, Poland DA - 14.05.2024 KW - EBSD KW - Kikuchi KW - Lattice parameters KW - Ratio refinement PY - 2024 AN - OPUS4-60087 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fiedler, Saskia A1 - Frenzel, Florian A1 - Würth, Christian A1 - Tavernaro, Isabella A1 - Grüne, M. A1 - Schweizer, S. A1 - Engel, A. A1 - Resch-Genger, Ute T1 - Interlaboratory Comparison on Absolute Photoluminescence Quantum Yield Measurements of Solid Light Converting Phosphors with Three Commercial Integrating Sphere Setups JF - American Chemical Society N2 - Scattering luminescent materials dispersed in liquid and solid matrices and luminescent powders are increasingly relevant for fundamental research and industry. Examples are luminescent nano- and microparticles and phosphors of different compositions in various matrices or incorporated into ceramics with applications in energy conversion, solid-state lighting, medical diagnostics, and security barcoding. The key parameter to characterize the performance of these materials is the photoluminescence/fluorescence quantum yield (Φf), i.e., the number of emitted photons per number of absorbed photons. To identify and quantify the sources of uncertainty of absolute measurements of Φf of scattering samples, the first interlaboratory comparison (ILC) of three laboratories from academia and industry was performed by following identical measurement protocols. Thereby, two types ofcommercial stand-alone integrating sphere setups with different illumination and detection geometries were utilized for measuring the Φf of transparent and scattering dye solutions and solid phosphors, namely, YAG:Ce optoceramics of varying surface roughness, used as converter materials for blue light emitting diodes. Special emphasis was dedicated to the influence of the measurement geometry, the optical properties of the blank utilized to determine the number of photons of the incident excitation light absorbed by the sample, and the sample-specific surface roughness. While the Φf values of the liquid samples matched between instruments, Φf measurements of the optoceramics with different blanks revealed substantial differences. The ILC results underline the importance of the measurement geometry, sample position, and blank for reliable Φf data of scattering the YAG:Ce optoceramics, with the blank’s optical properties accounting for uncertainties exceeding 20%. KW - Nano KW - Fluorescence KW - Reference material KW - Luminescence KW - Quantitative spectroscopy KW - Particle KW - Quantum yield KW - Quality assurance KW - Phosphor KW - Converter material KW - Lifetime KW - Interlaboratory comparison KW - Method KW - Uncertainty PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600945 DO - https://doi.org/10.1021/acs.analchem.4c00372 SN - 0003-2700 SP - 6730 EP - 6737 PB - ACS Publications AN - OPUS4-60094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hodoroaba, Vasile-Dan A1 - Fontanges, Richard T1 - A new deep-learning AI tool for analysing images of complex nanoparticles N2 - A thousand times thinner than a human hair, nanoparticles (NPs) are finding applications in a range of modern products. However, as some can affect human health or the environment, knowing the types present is essential. Electron microscopy is the ‘gold standard’ for NP analysis, allowing identification based on manual size analysis, but a new method was required to analyse these particles quickly, accurately and in a consistent way. KW - Nanoparticles KW - Imaging KW - AI tool KW - Particle size and shape distribution PY - 2024 UR - https://www.euramet.org/casestudies/casestudiesdetails/news/a-new-deep-learning-ai-tool-for-analysing-images-of-complex-nanoparticles SP - 1 EP - 2 PB - EURAMET CY - Braunschweig AN - OPUS4-60095 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Ongoing VAMAS ILC s on Nanoparticles and Graphene Oxide N2 - This contributions shows the first results of the ongoing interlaboratory comparisons under VAMAS/TWA 34 Nanoparticle populations related on the determination of pasrticle size distribution and relative concentration of nanoparticles and an example of an ILC running under VAMAS/TWA 41 Graphene and Related 2D Materials on the determination of the lateral diemsnions of graphene oxide flakes by Scanning Electron Microscopy. The link to related standardisation projects at ISO/TC Nanotechnologies are explained. T2 - Webinar Building the Foundation: Interlaboratory Comparisons and Reference Products for Advanced Materials CY - Berlin, Germany DA - 16.05.2024 KW - Nanoparticles KW - VAMAS KW - Interlaboratory comparison KW - Standardisation KW - Electron microscopy KW - AFM KW - SAXS PY - 2024 AN - OPUS4-60097 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - About Interlaboratory Comparisons (ILCs) and VAMAS N2 - Advanced materials, such as nanomaterials, 2D materials, or thin films, play a crucial role in driving economic development and addressing major challenges in the coming years. These challenges include mitigating the impact of climate change, advancing lightweight engineering, enhancing catalysis, and improving medical applications. To comprehend the performance of these materials and ensure their acceptance across various sectors as safe and sustainable for both humans and the environment, the availability of reference procedures, materials, and data is essential. One versatile tool for establishing such references and evaluating the proficiency of individual laboratories and their competencies is through (international) interlaboratory comparisons (ILC). Notably, initiatives like the Versailles Project on Advanced Materials and Standards (VAMAS) provide a platform for conducting ILCs. This webinar will showcase various examples of interlaboratory comparisons, illustrating their impact on the development of reference products. T2 - Webinar Building the Foundation: Interlaboratory Comparisons and Reference Products for Advanced Materials CY - Berlin, Germany DA - 16.05.2024 KW - Interlaboratory comparison KW - Reference products KW - VAMAS KW - Standardisation PY - 2024 AN - OPUS4-60096 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wegner, Karl David A1 - Coro, A. A1 - Le Guevel, X. A1 - Juarez, B. H. A1 - Resch-Genger, Ute T1 - SWIR luminescent nanomaterials – key chemical parameters for bright probes for in vivo bioimaging N2 - A current challenge for studying physio-pathological phenomena and diseaserelated processes in living organisms with non-invasive optical bioimaging is the development of bright optical reporters that enable deep tissue penetration, a high detection sensitivity, and a high spatial and temporal resolution. The focus of this project are nanomaterials, which absorb and emit in the shortwave infrared (SWIR) between ~900–2500 nm where scattering, absorption, and autofluorescence of the tissue are strongly reduced compared to the visible and NIR. T2 - QD2024 - 12th International Conference on Quantum Dots CY - Munich, Germany DA - 18.03.2024 KW - Quantum dots KW - Advanced nanomaterials KW - Fluorescence KW - Quality assurance KW - Gold nanocluster KW - Shortwave infrared KW - Spectroscopy KW - Bioimaging PY - 2024 AN - OPUS4-59783 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sieg, Holger A1 - Schaar, Caroline A1 - Fouquet, Nicole A1 - Böhmert, Linda A1 - Thünemann, Andreas A1 - Braeuning, Albert T1 - Particulate iron oxide food colorants (E 172) during artificial digestion and their uptake and impact on intestinal cells JF - Toxicology in Vitro N2 - Iron oxide of various structures is frequently used as food colorant (E 172). The spectrum of colors ranges from yellow over orange, red, and brown to black, depending on the chemical structure of the material. E 172 is mostly sold as solid powder. Recent studies have demonstrated the presence of nanoscaled particles in E 172 samples, often to a very high extent. This makes it necessary to investigate the fate of these particles after oral uptake. In this study, 7 differently structured commercially available E 172 food colorants (2 x Yellow FeO(OH), 2 x Red Fe2O3, 1 x Orange Fe2O3 + FeO(OH) and 2 x Black Fe3O4) were investigated for particle dissolution, ion release, cellular uptake, crossing of the intestinal barrier and toxicological impact on intestinal cells. Dissolution was analyzed in water, cell culture medium and artificial digestion fluids. Small-angle X-ray scattering (SAXS) was employed for determination of the specific surface area of the colorants in the digestion fluids. Cellular uptake, transport and toxicological effects were studied using human differentiated Caco-2 cells as an in vitro model of the intestinal barrier. For all materials, a strong interaction with the intestinal cells was observed, albeit there was only a limited dissolution, and no toxic in vitro effects on human cells were recorded. KW - Toxicology KW - Nanoparticles KW - Small-angle X-ray scattering KW - SAXS PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593935 DO - https://doi.org/10.1016/j.tiv.2024.105772 VL - 96 SP - 1 EP - 12 PB - Elsevier BV AN - OPUS4-59393 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Maxi B. A1 - Böhmert, Linda A1 - Thünemann, Andreas A1 - Loeschner, Katrin A1 - Givelet, Lucas A1 - Fahrenson, Christoph A1 - Braeuning, Albert A1 - Sieg, Holger T1 - Influence of artificial digestion on characteristics and intestinal cellular effects of micro-, submicro- and nanoplastics JF - Food and Chemical Toxicology N2 - The production of plastics is rising since they have been invented. Micro, submicro- and nanoplastics are produced intentionally or generated by environmental processes, and constitute ubiquitous contaminants which are ingested orally by consumers. Reported health concerns include intestinal translocation, inflammatory response, oxidative stress and cytotoxicity. Every digestive milieu in the gastrointestinal tract does have an influence on the properties of particles and can cause changes in their effect on biological systems. In this study, we subjected plastic particles of different materials (polylactic acid, polymethylmethacrylate, melamine formaldehyde) and sizes (micro- to nano-range) to a complex artificial digestion model consisting of three intestinal fluid simulants (saliva, gastric and intestinal juice). We monitored the impact of the digestion process on the particles by performing Dynamic Light Scattering, Scanning Electron Microscopy and Asymmetric Flow Field-Flow Fractionation. An in vitro model of the intestinal epithelial barrier was used to monitor cellular effects and translocation behavior of (un)digested particles. In conclusion, artificial digestion decreased cellular interaction and slightly increased transport of all particles across the intestinal barrier. The interaction with organic matter resulted in clear differences in the agglomeration behavior. Moreover, we provide evidence for polymer-, size- and surface-dependent cellular effects of the test particles. KW - Toxicology KW - General Medicine KW - Food Science KW - Nanoplastics KW - Nanoparticle KW - Dynamic Light Scattering KW - DLS PY - 2024 DO - https://doi.org/10.1016/j.fct.2023.114423 VL - 184 SP - 1 EP - 16 PB - Elsevier AN - OPUS4-59298 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Maxi B. A1 - Böhmert, Linda A1 - Thünemann, Andreas A1 - Loeschner, Katrin A1 - Givelet, Lucas A1 - Fahrenson, Christoph A1 - Braeuning, Albert A1 - Sieg, Holger T1 - Influence of artificial digestion on characteristics and intestinal cellular effects of micro-, submicro- and nanoplastics JF - Food and Chemical Toxicology N2 - The production of plastics is rising since they have been invented. Micro, submicro- and nanoplastics are produced intentionally or generated by environmental processes, and constitute ubiquitous contaminants which are ingested orally by consumers. Reported health concerns include intestinal translocation, inflammatory response, oxidative stress and cytotoxicity. Every digestive milieu in the gastrointestinal tract does have an influence on the properties of particles and can cause changes in their effect on biological systems. In this study, we subjected plastic particles of different materials (polylactic acid, polymethylmethacrylate, melamine formaldehyde) and sizes (micro- to nano-range) to a complex artificial digestion model consisting of three intestinal fluid simulants (saliva, gastric and intestinal juice). We monitored the impact of the digestion process on the particles by performing Dynamic Light Scattering, Scanning Electron Microscopy and Asymmetric Flow Field-Flow Fractionation. An in vitro model of the intestinal epithelial barrier was used to monitor cellular effects and translocation behavior of (un)digested particles. In conclusion, artificial digestion decreased cellular interaction and slightly increased transport of all particles across the intestinal barrier. The interaction with organic matter resulted in clear differences in the agglomeration behavior. Moreover, we provide evidence for polymer-, size- and surface-dependent cellular effects of the test particles. KW - Toxicology KW - Nanoparticles KW - Dynamic Light Scattering KW - Nanoplastics KW - Microplastics KW - Reference Method KW - Reference Material PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593947 DO - https://doi.org/10.1016/j.fct.2023.114423 VL - 184 SP - 1 EP - 16 PB - Elsevier BV AN - OPUS4-59394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geißler, Daniel A1 - Wegner, Karl David A1 - Fischer, C. A1 - Resch-Genger, Ute T1 - Exploring Simple Particle-Based Signal Amplification Strategies in a Heterogeneous Sandwich Immunoassay with Optical Detection JF - Analytical Chemistry N2 - Heterogeneous sandwich immunoassays are widely used for biomarker detection in bioanalysis and medical diagnostics. The high analyte sensitivity of the current “gold standard” enzyme-linked immunosorbent assay (ELISA) originates from the signal-generating enzymatic amplification step, yielding a high number of optically detectable reporter molecules. For future point-of-care testing (POCT) and point-of-need applications, there is an increasing interest in more simple detection strategies that circumvent time-consuming and temperature-dependent enzymatic reactions. A common concept to aim for detection limits comparable to those of enzymatic amplification reactions is the usage of polymer nanoparticles (NP) stained with a large number of chromophores. We explored different simple NP-based signal amplification strategies for heterogeneous sandwich immunoassays that rely on an extraction-triggered release step of different types of optically detectable reporters. Therefore, streptavidinfunctionalized polystyrene particles (PSP) are utilized as carriers for (i) the fluorescent dye coumarin 153 (C153) and (ii) hemin (hem) molecules catalyzing the luminol reaction enabling chemiluminescence (CL) detection. Additionally, (iii) NP labeling with hemin-based microperoxidase MP11 was assessed. For each amplification approach, the PSP was first systematically optimized regarding size, loading concentration, and surface chemistry. Then, for an immunoassay for the inflammation marker C- eactive protein (CRP), the analyte sensitivity achievable with optimized PSP ystems was compared with the established ELISA concept for photometric and CL detection. Careful optimization led to a limit of detection (LOD) of 0.1 ng/mL for MP11-labeled PSP and CL detection, performing similarly well to a photometric ELISA (0.13 ng/mL), which demonstrates the huge potential of our novel assay concept. KW - Nanoparticle KW - Fluorescence KW - Immunoassay KW - Quality assurance KW - Antibody KW - Polymer KW - Dye KW - Signal enhancement KW - CRP KW - Biosensing PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597853 DO - https://doi.org/10.1021/acs.analchem.3c03691 SN - 1520-6882 VL - 96 IS - 13 SP - 5078 EP - 5085 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-59785 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wegner, Karl David A1 - Resch-Genger, Ute T1 - The 2023 Nobel Prize in Chemistry: Quantum dots JF - Analytical and Bioanalytical Chemistry N2 - The 2023 Nobel Prize in Chemistry was awarded to Aleksey I. Ekimov (prize share 1/3), Louis E. Brus (prize share 1/3), and Moungi G. Bawendi (prize share 1/3) for groundbreaking inventions in the field of nanotechnology, i.e., for the discovery and synthesis of semiconductor nanocrystals, also termed quantum dots, that exhibit size-dependent physicochemical properties enabled by quantum size effects. This feature article summarizes the main milestones of the discoveries and developments of quantum dots that paved the road to their versatile applications in solid-state lighting, display technology, energy conversion, medical diagnostics, bioimaging, and image-guided surgery. KW - Quantum dots KW - Semiconductor nanocrystals KW - Luminescence KW - Quantitative spectroscopy KW - Quantum yield KW - Advanced nanomaterials KW - Quality assurance KW - Energy transfer PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597843 DO - https://doi.org/10.1007/s00216-024-05225-9 VL - 2024 SP - 1 EP - 11 PB - Springer CY - Cham AN - OPUS4-59784 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oskolkova, Tatiana O. A1 - Matiushkina, Anna A. A1 - Borodina, Lyubov' N. A1 - Smirnova, Ekaterina S. A1 - Dadadzhanova, Antonina I. A1 - Sewid, Fayza A. A1 - Veniaminov, Andrey V. A1 - Moiseeva, Ekaterina O. A1 - Orlova, Anna O. T1 - FRET‐Amplified Singlet Oxygen Generation by Nanocomposites Comprising Ternary AgInS2/ZnS Quantum Dots and Molecular Photosensitizers JF - ChemNanoMat N2 - Antibacterial photodynamic therapy (a‐PDT) has emerged as a promising non‐invasive therapeutic modality that utilizes the combination of a photosensitive agent, molecular oxygen, and excitation light to generate reactive oxygen species (ROS), demonstrating remarkable activity against multidrug‐resistant bacterial infections. However, the effective use of conventional photosensitizers is significantly limited by a number of their shortcomings, namely, poor water solubility and low selectivity. Herein, we present a novel biocompatible water‐soluble nanocomposite based on hydrophobic tetraphenylporphyrin (TPP) molecules and hydrophilic ternary AgInS2/ZnS quantum dots incorporated into a chitosan matrix as an improved photosensitizer for a‐PDT. We demonstrated that TPP molecules could be successfully transferred into chitosan solution while remaining primarily in the form of monomers, which are capable of singlet oxygen generation. We performed a detailed analysis of the Förster resonance energy transfer (FRET) between quantum dots and TPP molecules within the nanocomposite and proposed the mechanism of the singlet oxygen efficiency enhancement via FRET. KW - Nano KW - Particle KW - Quantum dot KW - Fluorescence KW - Synthesis KW - Optical spectroscopy KW - Energy transfer KW - Quality assurance KW - Lifetime KW - Quantum yield PY - 2024 DO - https://doi.org/10.1002/cnma.202300469 SN - 2199-692X VL - 10 IS - 3 SP - 1 EP - 11 PB - Wiley AN - OPUS4-59728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Minenkov, Alexey A1 - Hollweger, Sophia A1 - Duchoslav, Jiri A1 - Erdene-Ochir, Otgonbayar A1 - Weise, Matthias A1 - Ermilova, Elena A1 - Hertwig, Andreas A1 - Schiek, Manuela T1 - Monitoring the Electrochemical Failure of Indium Tin Oxide Electrodes via Operando Ellipsometry Complemented by Electron Microscopy and Spectroscopy JF - ACS Applied Materials & Interfaces N2 - Transparent conductive oxides such as indium tin oxide (ITO) are standards for thin film electrodes, providing a synergy of high optical transparency and electrical conductivity. In an electrolytic environment, the determination of an inert electrochemical potential window is crucial to maintain a stable material performance during device operation. We introduce operando ellipsometry, combining cyclic voltammetry (CV) with spectroscopic ellipsometry, as a versatile tool to monitor the evolution of both complete optical (i.e., complex refractive index) and electrical properties under wet electrochemical operational conditions. In particular, we trace the degradation of ITO electrodes caused by electrochemical reduction in a pH-neutral, water-based electrolyte environment during electrochemical cycling. With the onset of hydrogen evolution at negative bias voltages, indium and tin are irreversibly reduced to the metallic state, causing an advancing darkening, i.e., a gradual loss of transparency, with every CV cycle, while the conductivity is mostly conserved over multiple CV cycles. Post-operando analysis reveals the reductive (loss of oxygen) formation of metallic nanodroplets on the surface. The reductive disruption of the ITO electrode happens at the solid–liquid interface and proceeds gradually from the surface to the bottom of the layer, which is evidenced by cross-sectional transmission electron microscopy imaging and complemented by energy-dispersive X-ray spectroscopy mapping. As long as a continuous part of the ITO layer remains at the bottom, the conductivity is largely retained, allowing repeated CV cycling. We consider operando ellipsometry a sensitive and nondestructive tool to monitor early stage material and property changes, either by tracing failure points, controlling intentional processes, or for sensing purposes, making it suitable for various research fields involving solid–liquid interfaces and electrochemical activity. KW - General Materials Science PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597625 DO - https://doi.org/10.1021/acsami.3c17923 SN - 1944-8252 VL - 16 IS - 7 SP - 9517 EP - 9531 PB - American Chemical Society (ACS) AN - OPUS4-59762 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hertwig, Andreas T1 - New analytic ways to characterise mesoporous thin layers used in electrocatalytic water splitting N2 - Mesoporous materials are needed in many applications where a high specific surface area and adsorptive behaviour is needed. Important examples are separation techniques and barrier layers and catalysts. Electrochemical water splitting is the key technology for producing green hydrogen and there is no foreseeable alternative to this process for producing elementary hydrogen from green electrical power. Water electrolysis can be divided into the anodic Oxygen Evolution Reaction (OER) and the cathodic Hydrogen Evolution Reaction (HER). Both processes have to be heavily optimised to a large extent to avoid energy losses caused by overvoltage. The development of electrodes for these processes is especially difficult due to the many boundary conditions. Water splitting is a catalytic as well as electrochemical process. The contact area between the electrolyte and the electrode must be maximised maintaining the stability of the surface. Side reactions must be suppressed, and effective gas transport must be ensured. The whole process has to be tolerant with respect to temperature, harsh chemical conditions from the electrolyte as well as high current densities. We present a hybrid analytical method combining several analytical techniques for determining the properties of thin layers of mixed oxides of the general composition Ir:TiOx. These materials are promising candidates for electrocatalytical top coatings of OER electrodes. To lower the costs of the electrolysers, the main goal is to lower the Ir content retaining the system efficiency. The main properties which are hard to determine are the porous volume fraction and the Ir:Ti element ratio. By a combination of electron microscopy, spectroscopic operando ellipsometry, ellipsometric porosimetry, and other techniques, we can determine key features of mesoporous thin layer materials. We aim to develop operando capable techniques used in process monitoring as well as measurement techniques optimised for accuracy. By developing reference materials, we support long term uptake of our methodology. This work can directly be used for optimising electrocatalytic layers and is a good example for the power of hybrid metrology for improving materials design. T2 - International Conference on Resource Chemistry CY - Alzenau, Germany DA - 11.03.2024 KW - Ellipsometry KW - Electrocatalytic Water Splitting KW - Mesoporous Materials KW - Electron Probe Microanalysis KW - Hydrogen Generation PY - 2024 AN - OPUS4-59764 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schiek, Manuela A1 - Minenkov, Alexey A1 - Hollweger, Sophia A1 - Duchoslav, Jiri A1 - Erdene-Ochir, Otgonbayar A1 - Weise, Matthias A1 - Ermilova, Elena A1 - Hertwig, Andreas T1 - Optical constants of In2O3-SnO2 (Indium tin oxide, ITO) N2 - Optical constants of In2O3-SnO2 (Indium tin oxide, ITO) Minenkov et al. 2024: on glass; n,k 0.191–1.69 µm Optical constants of In2O3-SnO2 (Indium tin oxide, ITO) Minenkov et al. 2024: on Si wafer, top; n,k 0.191–1.69 µm Optical constants of In2O3-SnO2 (Indium tin oxide, ITO) Minenkov et al. 2024: on Si wafer, bottom; n,k 0.191–1.69 µm KW - Indium Tin Oxide KW - Optical constants KW - Magnetron Sputtering KW - Electrochemical Degradation KW - Spectroscopic Ellipsometry PY - 2024 UR - https://refractiveindex.info/?shelf=other&book=In2O3-SnO2&page=Minenkov-glass UR - https://refractiveindex.info/?shelf=other&book=In2O3-SnO2&page=Minenkov-wafer-top UR - https://refractiveindex.info/?shelf=other&book=In2O3-SnO2&page=Minenkov-wafer-bottom PB - Refractiveindex.info AN - OPUS4-59766 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Knapic, D. A1 - Mardare, A. I. A1 - Voss, Heike A1 - Bonse, Jörn A1 - Hassel, A. W. T1 - Corrosion study of picosecond-laser structured and anodized Ti6Al4V for bone screws JF - Physica Satus Solidi A N2 - A corrosion study is performed on six variations of titanium grade 5 (Ti6Al4V) samples. Samples are prepared in different conditions by variation of preanodization, postanodization, and picosecond-laser (ps-laser) surface treatment, while polished and anodized samples serve as reference. Microcones and nanosized periodic surface features are successfully produced on Ti6Al4V samples. The morphology and topography of the structures are visualized by scanning electron microscopy and white light interference microscopy. Furthermore, the relative electrochemically active surface area (ECSA) is determined for the ps-laser-treated samples. It is determined that the preanodized and laser-treated sample has 3.5 times larger ECSA than a polished sample, and that the laser-treated sample has 4.1 times larger area. Moreover, Tafel analysis is performed to determine the corrosion properties of the samples. It is shown that the corrosion resistance improves for both laser-structured samples after the anodization. To further study the surface of the samples, electrochemical impedance spectroscopy measurements are conducted. The study indicates that the ps-laser-treated and anodized Ti6Al4V is suitable to be used for the fabrication of bone screws and plates due to its improved corrosion resistance as compared to nonanodized samples. KW - Laser-induced periodic surface structures (LIPSS) KW - Anodization KW - Bone screws KW - Implant material KW - Titanium alloys PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597890 DO - https://doi.org/10.1002/pssa.202300609 SN - 1862-6319 VL - 221 SP - 1 EP - 8 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-59789 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Herausforderungen bei der Granulometrie von (technischen) Nano-Pulvern N2 - Einführungsvortrag im Rahmen der Veranstaltung der BAM-Akademie zur Anwendung der OECD TG 124 "Volume Specific Surface Area of Manufactured Nanomaterials" zu Herausforderungen bei der Granulometrie von Nanopulvern. Es werden die Einflüsse von Partikelform, Breite der Partikelgrößenverteilung und Agglomeration/ Aggregation auf das Messergebnis sowie die Vergleichbarkeit der Ergebnisse verschiedener Messverfahren dargelegt. T2 - BAM Akademie II: Info-Tage "Nano or not Nano" CY - Online meeting DA - 25.01.2024 KW - Nanopulver KW - Granulometrie KW - Partikelgröße KW - VSSA KW - OECD TG 124 PY - 2024 AN - OPUS4-59558 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emamverdi, Farnaz A1 - Huang, J. A1 - Mosane Razavi, Negar A1 - Bojdys, M. J. A1 - Forster, A. B. A1 - Budd, P. M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Molecular Mobility and Gas Transport Properties of Mixed Matrix Membranes Based on PIM‑1 and a Phosphinine Containing Covalent Organic Framework JF - Macromolecules N2 - Polymers with intrinsic microporosity (PIMs) are gaining attention as gas separation membranes. Nevertheless, they face limitations due to pronounced physical aging. In this study a covalent organic framework containing λ5-phosphinine moieties, CPSF-EtO were incorporated as a nanofiller (concentration range 0-10 wt%) into a PIM-1 matrix forming dense films with a thickness of ca. 100 μm. The aim of the investigation was to investigate possible enhancements of gas transport properties and mitigating effects on physical aging. The incorporation of the nanofiller occurred on aggregate level with domains up to 100 nm as observed by T-SEM and confirmed by X-ray scattering. Moreover, the X-ray data show that the structure of the microporous network of the PIM-1 matrix is changed by the nanofiller. As the molecular mobility is fundamental for gas transport as well as for physical aging, the study includes dielectric investigations of pure PIM-1 and PIM-1/CPSF-EtO mixed matrix membranes to establish a correlation between the molecular mobility and the gas transport properties. Using the time-lag method the gas permeability and the permselectivity were determined for N2, O2, CH4 and CO2 for samples with variation in filler content. A significant increase in the permeability of CH4 and CO2 (50 % increase compared to pure PIM-1) was observed for a concentration of 5 wt% of the nanofiller. Furthermore, the most pronounced change in the permselectivity was found for the gas pair CO2/N2 at a filler concentration of 7 wt%. KW - Polymers of Intrinsic Microporosity KW - Nanocomposites PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595031 DO - https://doi.org/10.1021/acs.macromol.3c02419 SN - 0024-9297 VL - 57 IS - 4 SP - 1829 EP - 1845 PB - ACS Publications AN - OPUS4-59503 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Sokolowski‐Tinten, Klaus T1 - Probing Laser‐Driven Structure Formation at Extreme Scales in Space and Time JF - Laser & Photonics Reviews N2 - Irradiation of solid surfaces with high intensity, ultrashort laser pulses triggers a variety of secondary processes that can lead to the formation of transient and permanent structures over a large range of length scales from mm down to the nano‐range. One of the most prominent examples are LIPSS – Laser‐Induced Periodic Surface Structures. While LIPSS have been a scientific evergreen for of almost 60 years, experimental methods that combine ultrafast temporal with the required nm spatial resolution have become available only recently with the advent of short pulse, short wavelength free electron lasers. Here, the current status and future perspectives in this field are discussed by exploiting the unique possibilities of these 4th‐generation light sources to address by time‐domain experimental techniques the fundamental LIPSS‐question, namely why and how laser irradiation can initiate the transition of a “chaotic” (rough) surface from an aperiodic into a periodic structure. KW - Laser-induced periodic surface structures (LIPSS) KW - Free electron laser KW - Pump-probe experiments KW - Time-resolved scattering KW - Capillary waves PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595048 DO - https://doi.org/10.1002/lpor.202300912 SN - 1863-8899 VL - 18 SP - 1 EP - 11 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-59504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn A1 - Schwibbert, Karin A1 - Richter, Anja M. A1 - Krüger, Jörg T1 - Laserstrukturierte Oberflächen Ein Weg zur Kontrolle der Biofilmbildung? N2 - Bakterielle Biofilme stellen in medizinischen und industriellen Bereichen ein ernsthaftes Problem dar. Eine der größten gesellschaftlichen Herausforderungen liegt in der zunehmenden Resistenz von Bakterien gegen Biozide, die bei antimikrobiellen Behandlungen eingesetzt werden, z.B. durch übermäßigen Einsatz in Medizin, Industrie und Landwirtschaft oder durch Reinigung und Desinfektion in Privathaushalten. Daher sind neue effiziente bakterienabweisende Strategien, die den Einsatz von Bioziden vermeiden, dringend erforderlich. Ein vielversprechender Weg zur Erzielung bakterienabweisender Oberflächen liegt in der berührungslosen und aseptischen großflächigen Laserbearbeitung von technischen Oberflächen. Maßgeschneiderte Oberflächentexturen, ermöglicht durch verschiedene Laserbearbeitungsstrategien, die zu topographischen Skalen im Bereich von Nanometern bis Mikrometern führen, können eine Lösung für diese Herausforderung darstellen. In dem Vortrag wird ein Überblick über den aktuellen Stand der Technik bei der subtraktiven Texturierung von Laseroberflächen zur Kontrolle der Biofilmbildung bei verschiedenen Bakterienstämmen und in unterschiedlichen Umgebungen gegeben. Auf der Grundlage spezifischer Eigenschaften von Bakterien und laserbearbeiteten Oberflächen werden die Herausforderungen antimikrobieller Oberflächendesigns erörtert und zukünftige Richtungen aufgezeigt. T2 - GRAVOSeminar, GRAVOmer Kompetenznetzwerk CY - Online meeting DA - 28.02.2024 KW - Laser-Materialbearbeitung KW - Ultrakurzpuls-Laser KW - Biofilme KW - Antibakterielle Oberflächen KW - Oberflächenfunktionalisierung PY - 2024 UR - https://gravomer.de/veranstaltungen-anzeigen/laserstrukturierte-oberflaechen-ein-weg-zur-kontrolle-der-biofilmbildung AN - OPUS4-59594 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Einführung: Volume Specific Surface Area (VSSA) N2 - Im Rahmen der 2. BAM-Akademie-Veranstaltung "Nano or not Nano" wurde die OECD TG 124 "Volume Specific Surface Area of Manufactured Nanomaterials" vorgestellt. Der Vortrag enthält ein Einführung zur VSSA mit Definitionen, Vorteilen und Einschränkungen. T2 - BAM Akademie II: Info-Tage "Nano or not Nano" CY - Online meeting DA - 25.01.2024 KW - Nano powder KW - VSSA KW - Specific surface KW - OECD TG PY - 2024 AN - OPUS4-59560 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Bestimmung der Skelettdichte mittels Gaspyknometrie N2 - Im Rahmen des 2. BAM-Akademie Info-Tages "Nano or not Nano" wurde die OECD TG 124 "Volume Specific Surface Area of Manufactured Nanomaterials" vorgestellt. Der Vortrag beschreibt detailliert das Messverfahren der He-Gaspyknometrie zur Bestimmung der Skelettdichte von Pulvern und geht auf Anwendbarkeit, Besonderheiten bei Nanopulvern und wichtige Einstellparameter für die Messung ein. T2 - BAM Akademie II: Info-Tage "Nano or not Nano" CY - Online meeting DA - 25.01.2024 KW - Pycnometry KW - Density KW - Nano powder PY - 2024 AN - OPUS4-59561 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn T1 - Erzeugung und Charakterisierung anisotroper Nanostrukturen durch Ultrakurzpulslaser N2 - Der Vortrag gibt einen Überblick über die Erzeugung und Charakterisierung anisotroper Nanostrukturen mittels ultrakurzgepulster Laserstrahlung. Besonderes Augenmerk liegt dabei auf dem Phänomen der sogenannten Laser-induzierten periodischen Oberflächen-Nanostrukturen auf dielektrischen Werkstoffen und ihrer zeitlichen Dynamik. Weitere Beispiele von Volumen-Nanostrukturen aus der Literatur werden diskutiert. T2 - 21. Treffen des DGG-DKG Arbeitskreises „Glasig-kristalline Multifunktionswerkstoffe“ CY - Mainz, Germany DA - 22.02.2024 KW - Laser-induzierte periodische Oberflächen-Nanostrukturen KW - Quarzglas KW - Saphir KW - Bessel-Strahlen PY - 2024 AN - OPUS4-59565 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Kun A1 - Carrod, Andrew J. A1 - Del Giorgio, Elena A1 - Hughes, Joseph A1 - Rurack, Knut A1 - Bennet, Francesca A1 - Hodoroaba, Vasile-Dan A1 - Harrad, Stuart A1 - Pikramenou, Zoe T1 - Luminescence Lifetime-Based Sensing Platform Based on Cyclometalated Iridium(III) Complexes for the Detection of Perfluorooctanoic Acid in Aqueous Samples JF - Analytical Chemistry N2 - Luminescence lifetimes are an attractive analytical method for detection due to its high sensitivity and stability. Iridium probes exhibit luminescence with long excited-state lifetimes, which are sensitive to the local environment. Perfluorooctanoic acid (PFOA) is listed as a chemical of high concern regarding its toxicity and is classified as a “forever chemical”. In addition to strict limits on the presence of PFOA in drinking water, environmental contamination from industrial effluent or chemical spills requires rapid, simple, accurate, and cost-effective analysis in order to aid containment. Herein, we report the fabrication and function of a novel and facile luminescence sensor for PFOA based on iridium modified on gold surfaces. These surfaces were modified with lipophilic iridium complexes bearing alkyl chains, namely, IrC6 and IrC12, and Zonyl-FSA surfactant. Upon addition of PFOA, the modified surfaces IrC6-FSA@Au and IrC12-FSA @Au show the largest change in the red luminescence signal with changes in the luminescence lifetime that allow monitoring of PFOA concentrations in aqueous solutions. The platform was tested for the measurement of PFOA in aqueous samples spiked with known concentrations of PFOA and demonstrated the capacity to determine PFOA at concentrations >100 μg/L (240 nM). KW - Perfluorooctanoic Acid (PFOA) KW - Cyclometalated iridium (III) complexes KW - Luminescent lifetime KW - Optically active surfaces KW - ToF-SIMS PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594535 UR - https://pubs.acs.org/doi/10.1021/acs.analchem.3c04289 DO - https://doi.org/10.1021/acs.analchem.3c04289 VL - 96 IS - 4 SP - 1565 EP - 1575 PB - American Chemical Society (ACS) AN - OPUS4-59453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mrkwitschka, Paul A1 - Rühle, Bastian A1 - Kuchenbecker, Petra A1 - Löhmann, Oliver A1 - Lindemann, Franziska A1 - Hodoroaba, Vasile-Dan T1 - Embedding and cross-sectioning as a sample preparation procedure for accurate and representative size and shape measurement of nanopowders JF - Scientific Reports N2 - Reliable measurement of the size of polydisperse, complex-shaped commercial nanopowders is a difficult but necessary task, e.g., for regulatory requirements and toxicity risk assessment. Suitable methods exist for the accurate characterization of the size of non-aggregated, stabilized, spherical and monodisperse nanoparticles. In contrast, industrial nanoscale powders usually require dedicated sample preparation procedures developed for the analysis method of choice. These nano-powders tend to agglomerate and/or aggregate, a behavior which in combination with an innate broad particle size distribution and irregular shape often significantly alters the achievable accuracy of the measured size parameters. The present study systematically tests two commercially available nanoscale powders using different sample preparation methods for correlative analysis by scanning electron microscopy, dynamic light scattering, Brunauer–Emmet–Teller method and differential mobility analysis. One focus was set on the sample preparation by embedding nanoparticles in carbon-based hot-mounting resin. Literature on this topic is scarce and the accuracy of the data extracted from cross sections of these particles is unclearly stated. In this paper systematic simulations on the deviation of the size parameters of well-defined series of nanoparticles with different shapes from the nominal value were carried out and the contributing factors are discussed. KW - Nanopowder KW - Electron microscopy KW - Sample preparation KW - Cross-sectioning KW - Cerium oxide KW - Zinc oxide PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593289 DO - https://doi.org/10.1038/s41598-023-51094-0 SN - 2045-2322 VL - 14 SP - 1 EP - 10 PB - Springer Nature CY - London AN - OPUS4-59328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liu, Y. A1 - Gruner, A. A1 - Aboud, D. G. K. A1 - Bonse, Jörn A1 - Schille, J. A1 - Loeschner, U. A1 - Kietzig, A.-M. T1 - Polarization effects on laser-inscribed angled micro-structures JF - Applied Surface Science N2 - The polarization of the laser beam exhibits more substantial differences in laser micromachining as the angle of incidence deviates from zero. In the reported work, our focus was to explore the effects of circularly, p- and s-polarized laser on angled ultrashort pulse laser micromachining of micropillar arrays. The examination encompassed laser process factors, including angles of incidence, microstructure dimensions, and inter-pillar spacing. A comparison between the resulting structures demonstrated that p-polarized laser beam was the most efficient in material removal in angled laser micromachining, followed by circularly polarized laser. While the s-polarized beam exhibited the lowest ablation efficiency among the three. Such distinction is mainly attributed to the distinguishing reflectivity of the three states of polarization on tilted planes. The development of structural heights during ablation processes was examined, and potential defects in laser processing methodologies were interpreted. The dependency of structural heights on inter-pillar spacing was analyzed. This study bridges the gap between existing studies on angled ultrashort pulse laser machining and the influences of polarization on laser machining. The comparison between structures produced using laboratory-scale and industrial-scale laser systems also yielded pertinent recommendations for facilitating a smooth transition of angled laser micromachining from laboratory-scale research to industrial applications. KW - Laser processing KW - Laser-induced periodic surface structures (LIPSS) KW - Microstructures KW - Nanostructures PY - 2024 UR - https://www.sciencedirect.com/science/article/pii/S0169433223028714 DO - https://doi.org/10.1016/j.apsusc.2023.159191 SN - 0169-4332 VL - 649 SP - 1 EP - 15 PB - Elsevier AN - OPUS4-59329 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinekamp, Christian A1 - Kneiske, Sönke A1 - Guilherme Buzanich, Ana A1 - Ahrens, Mike A1 - Braun, Thomas A1 - Emmerling, Franziska T1 - A fluorolytic sol-gel route to access an amorphous Zr fluoride catalyst: A useful tool for C-F bond activation JF - Catalysis Science & Technology N2 - A route to a ZrF4 catalyst active in room temperature Friedel–Crafts and dehydrofluorination reactions was developed via a fluorolytic sol–gel route, which was followed by a postfluorination step using a stream of CHClF2. The behaviour of different Zr(IV) precursors in a sol–gel reaction with anhydrous isopropanol/HF solution was investigated. The subsequent post-fluorination step was optimised in its temperature ramp and confirmed the necessity of a fluorination of the generated xerogels to obtain catalytic activity. The process is discussed in the context of the analysis of the materials using Brunauer–Emmett–Teller analysis (BET), powder X-ray diffraction (XRD), infrared spectroscopy (IR), thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The local structure of the amorphous catalyst was elucidated by extended X-ray absorption fine structure spectroscopy (EXAFS). KW - Catalysis KW - Heterogeneous catalysis KW - C-F bond activation KW - Postfluorination PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593433 DO - https://doi.org/10.1039/D3CY01439H SN - 2044-4761 SP - 1 EP - 8 PB - Royal Society of Chemistry (RSC) AN - OPUS4-59343 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sun, Yijuan A1 - Gawlitza, Kornelia A1 - Valderrey, Virginia A1 - Bell, Jérémy A1 - Rurack, Knut T1 - Polymerizable BODIPY probe crosslinker for the molecularly imprinted polymer-based detection of organic carboxylates via fluorescence JF - Materials Advances N2 - This contribution reports the development of a polymerizable BODIPY-type fluorescent probe targeting small-molecule carboxylates for incorporation into molecularly imprinted polymers (MIPs). The design of the probe crosslinker includes a urea recognition site p-conjugated to the 3-position of the BODIPY core and two methacrylate moieties. Titration experiments with a carboxylate-expressing antibiotic, levofloxacin (LEVO), showed a blue shift of the absorption band as well as a broadening and decrease in emission, attributed to hydrogen bonding between the probe’s urea group and the carboxylate group of the antibiotic. Using this probe crosslinker, core–shell particles with a silica core and a thin MIP shell were prepared for the detection of LEVO. The MIP exhibited highly selective recognition of LEVO, with an imprinting factor of 18.1 compared to the non-imprinted polymer. Transmission electron microscopy confirmed the core–shell structure and spectroscopic studies revealed that the receptor’s positioning leads to a unique perturbation of the polymethinic character of the BODIPY chromophore, entailing the favourable responses. These features are fully preserved in the MIP, whereas no such response was observed for competitors such as ampicillin. The sensory particles allowed to detect LEVO down to submicromolar concentrations in dioxane. We have developed here for the first time a BODIPY probe for organic carboxylates and incorporated it into polymers using the imprinting technique, paving the way for BODIPY-type fluorescent MIP sensors. KW - Fluorescence KW - BODIPY probe KW - Molecularly Imprinted Polymers KW - Sensor Materials KW - Dyes KW - Water analysis KW - Advanced materials PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-598629 DO - https://doi.org/10.1039/D3MA00476G SP - 1 EP - 11 PB - Royal Society of Chemistry (RSC) AN - OPUS4-59862 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn A1 - Krüger, Jörg A1 - Florian, C. A1 - Sokolowski-Tinten, K. A1 - Gräf, S. T1 - Advances in ultrafast laser manufacturing: nanostructures, thin films, and scaling perspectives N2 - Advanced ultrafast laser technology is a rapidly growing field that currently enables many new industrial and scientific applications. During the last decades, this has been significantly driven by the availability of high-repetition-rate laser sources and novel beam delivery concepts. At the laser side, Moore’s law equally manifests for ultrafast laser technologies, since the average output power of such lasers doubles approximately every two years. This development is mainly driven by the increase of the pulse repetition rates of energetic laser pulses, currently enforcing the development of smart beam control and novel scanning strategies for preventing heat-accumulation and plasma-shielding effects during laser-based materials processing. This keynote presentation addresses the advantages, recent developments, and perspectives of laser processing with ultrashort laser pulses. A special focus is laid on the tailored structuring of thin films as well as the manufacturing and probing of sub-diffraction surface nanostructures – an ongoing race to extreme scales. Current limitations are identified and an outlook to future scaling perspectives will be provided. T2 - SPIE Photonics Europe 2024 Conference, Symposium "Lasers and Photonics for Advanced Manufacturing" CY - Strasbourg, France DA - 07.04.2024 KW - Ultrafast laser processing KW - Laser-induced periodic surface structures (LIPSS) KW - Surface functionalization KW - Laser technology KW - Time-resolved analysis PY - 2024 UR - https://spie.org/photonics-europe/presentation/Advances-in-ultrafast-laser-manufacturing--nanostructures-thin-films-and/13005-36#_=_ AN - OPUS4-59852 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grundmann, Jana A1 - Bodermann, Bernd A1 - Ermilova, Elena A1 - Weise, Matthias A1 - Hertwig, Andreas A1 - Klapetek, Petr A1 - Rafighdoost, Jila A1 - Pereira, Silvania F. T1 - Optical and tactile measurements on SiC sample defects JF - Journal of Sensors and Sensor Systems N2 - Abstract. In power electronics, compound semiconductors with large bandgaps, like silicon carbide (SiC), are increasingly being used as material instead of silicon. They have a lot of advantages over silicon but are also intolerant of nanoscale material defects, so that a defect inspection with high accuracy is needed. The different defect types on SiC samples are measured with various measurement methods, including optical and tactile methods. The defect types investigated include carrots, particles, polytype inclusions and threading dislocations, and they are analysed with imaging ellipsometry, coherent Fourier scatterometry (CFS), white light interference microscopy (WLIM) and atomic force microscopy (AFM). These different measurement methods are used to investigate which method is most sensitive for which type of defect to be able to use the measurement methods more effectively. It is important to be able to identify the defects to classify them as critical or non-critical for the functionality of the end product. Once these investigations have been completed, the measurement systems can be optimally distributed to the relevant defects in further work to realize a hybrid analysis of the defects. In addition to the identification and classification of defects, such a future hybrid analysis could also include characterizations, e.g. further evaluation of ellipsometric data by using numerical simulations. KW - Compound semiconductors KW - Hybrid metrology KW - Material defects KW - Spectroscopic Ellipsometry KW - Scanning Probe Microscopy KW - White-light Interference Microscopy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601220 DO - https://doi.org/10.5194/jsss-13-109-2024 SN - 2194-878X VL - 13 IS - 1 SP - 109 EP - 121 PB - Copernicus GmbH AN - OPUS4-60122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - López-Iglesias, C. A1 - Markovina, A. A1 - Nirmalananthan-Budau, N. A1 - Resch-Genger, Ute A1 - Klinger, D. T1 - Optically monitoring the microenvironment of a hydrophobic cargo in amphiphilic nanogels: influence of network composition on loading and release JF - Nanoscale N2 - Amphiphilic nanogels (ANGs) are promising carriers for hydrophobic cargos such as drugs, dyes, and catalysts. Loading content and release kinetics of these compounds are controlled by type and number of hydrophobic groups in the amphiphilic copolymer network. Thus, understanding the interactions between cargo and colloidal carrier is mandatory for a tailor-made and cargo-specific ANG design. To systematically explore the influence of the network composition on these interactions, we prepared a set of ANGs of different amphiphilicity and loaded these ANGs with varying concentrations of the solvatochromic dye Nile Red (NR). Here, NR acts as a hydrophobic model cargo to optically probe the polarity of its microenvironment. Analysis of the NR emission spectra as well as measurements of the fluorescence quantum yields and decay kinetics revealed a decrease in the polarity of the NR microenvironment with increasing hydrophobicity of the hydrophobic groups in the ANG network and dye–dye interactions at higher loading concentrations. At low NR concentrations, the hydrophobic cargo NR is encapsulated in the hydrophobic domains. Increasing NR concentrations resulted in probe molecules located in a more hydrophilic environment, i.e., at the nanodomain border, and favored dye–dye interactions and NR aggregation. These results correlate well with release experiments, indicating first NR release from more hydrophilic network locations. Overall, our findings demonstrate the importance to understand carrier–drug interactions for efficient loading and controlled release profiles in amphiphilic nanogels. KW - Particle KW - Energy transfer KW - Limit of detection KW - Polymer KW - Luminescence KW - Quantitative spectroscopy KW - Nano KW - Quantum yield KW - Lifetime KW - Quality assurance KW - Dye KW - Probe KW - Sensor KW - Nile Red PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601603 DO - https://doi.org/10.1039/d4nr00051j SN - 2040-3364 IS - 16 SP - 9525 EP - 9535 PB - The Royal Society of Chemistry AN - OPUS4-60160 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Salzmann, Christoph A1 - Heilmann, Maria T1 - Ongoing VAMAS interlaboratory comparisons on nanoparticles size and shape as pre standardisation projects for harmonized measurements N2 - Traceable morphological and chemical characterization of nanomaterials with respect to the various possible sizes, size distributions, shapes, and concentrations of real-world nanoparticles (NPs) is a challenging task. Particularly for the nonspherical, non-monodisperse nanoparticles – as typically for most of the commercial particles, including their strong tendency to agglomerate, there is a lack of standard operation procedures providing accurate nanoparticle characterisation. In the framework of the pre-standardisation framework of VAMAS (Versailles Project on Advanced Materials and Standards, www.vamas.org) two interlaboratory comparison (ILC) studies are being carried out under the Technical Working Area (TWA) 34 “Nanoparticle Populations”:i) Project #15 addresses the analysis of the size and shape distribution of TiO2 bipyramidal NPs by traceable imaging methods such as TEM, SEM, STEM-in-SEM, AFM as well as with SAXS as an ensemble method. This ILC is thought as the next level development of the case studies exemplified in the published ISO standards ISO 21363 and ISO 19749. It was agreed to complete the first ILC with the NPs already prepared according to the same procedure on a TEM grid, and, at a later stage, to carry out second ILCs with the same NPs distributed to the participants as liquid suspensions together with protocols for the uniform NP deposition on suited substrates - as developed and optimized within the European project nPSize. Once having good deposition protocols available, the door for automated image analysis gets opened. Corresponding image analysis protocols and reporting templates have been distributed to the ILC participants, too. ii) Project #16: two spherical SiO2 NP samples with bi-modal size distributions in two nominal relative number concentrations were prepared and distributed also as liquid suspensions accompanied by sample preparation, measurement, and image analysis protocols and reporting templates. Here, the NP concentration is the primary parameter to be measured. For the imaging methods it is targeted to measure the relative nanoparticle concentrations (relative populations of the two modes). The results of all the participating laboratories, in both ILCs, compiled in comparative representations will be shown and discussed for the first time. The reduction of the measurement uncertainties associated to the size, shape and number-concentration results induced by the significant improvement of the sample preparation on substrates (as single particles with a high-density coverage), combined with welldefined image analysis procedures will be highlighted. T2 - 2024 Spring Meeting of the European Materials Research Society (E-MRS) CY - Strasbourg, France DA - 27.05.2024 KW - VAMAS KW - Interlaboratory comparison KW - Electron microscopy KW - Particle size distribution KW - Article concentration PY - 2024 AN - OPUS4-60184 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Sachse, René A1 - Kotil, L. A1 - Matjacic, L. A1 - McMahon, G. A1 - Bernicke, M. A1 - Bernsmeier, D. A1 - Kraehnert, R. A1 - Hertwig, Andreas T1 - Morphological and chemical analysis of mesoporous mixed IrOx-TiOy thin films as electrode materials N2 - Porous films play an important role particularly in energy applications like photovoltaics, electrolysis or batteries. Thin film properties such as thickness, chemical composition, crystallinity of the framework, and porosity define the activity of the porous films. The accurate morpho-chemical characterisation of mesoporous thin films is a challenging analytical task which requires the consideration of new analytical approaches based on the combination of data of different methods able to address the structure and chemical composition at the nanoscale. In this contribution we characterise thin mesoporous iridium-titanium mixed oxide film properties by Electron Probe Microanalysis (EPMA) with Energy-Dispersive X-ray Spectroscopy (EDS) at an SEM applied in a dedicated “thin film analysis” approach (1). Thus, the film mass deposition, film thickness and the film density can be determined. Further, by dividing the measured film density to an assumed (theoretical) metal oxide framework (skeletal) density, the thin film porosity can be extracted, too. In order to assess the homogeneity of the thin film properties like the chemical composition, Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) and Auger Electron Spectrometry are applied in the depth profiling mode, so that possible in-depth gradients are detected. Lateral inhomogeneities in the chemical composition and structure of the thin mesoporous films are also identified by applying the same methods in the line-scan or mapping mode, which can be further combined with in-depth sputtering for 3D information. The role of the spatial resolution of the analytical methods considered, which can go down well below 100 nm, will be highlighted. T2 - 2024 Spring Meeting of the European Materials Research Society (E-MRS) CY - Strasbourg, France DA - 27.05.2024 KW - Mesoporous KW - Thin films KW - Iridium oxide KW - Titanium oxide KW - Thin film analysis KW - Porosity KW - SIMS KW - Auger electron spectroscopy PY - 2024 AN - OPUS4-60185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hertwig, Andreas A1 - Ermilova, Elena T1 - On the use of spectroscopic imaging ellipsometry for quantification and characterisation of defects in thin films for power electronics N2 - Compound semiconductors (CS) are promising materials for the development of high-power electrical applications. They have low losses, can withstand high temperatures and can operate at very high voltages and currents. This makes them a key technology for the electrification of many high energy applications, especially electromobility and HVDC power lines. The challenge with CS technology is that most of the process technology has to be developed anew to the high standards required by electronic applications. Today, compound semiconductors can be produced in thin layers on top of substrates fabricated from classical crystal growth processes that are already well established. A promising method for this is metal organic vapour phase epitaxy (MOVPE). With this method, many different compounds with semiconducting properties can be synthesized. Additionally, this process technology is a direct thin layer deposition method. Therefore, complex multilayer systems can be generated directly by the deposition process and without the need of doping after growing. There are a number of critical defects that can originate from the deposition process of these thin film devices. Within this project, we intend to develop new correlative imaging and analysis techniques to determine defect types, to quantify defect size and number density, as well as to characterise defects for process optimisation. We report here on the use of spectroscopic ellipsometry and imaging ellipsometry to investigate defects in several different compound semiconductor materials used in high-power electronic devices. The materials we investigated are β-Ga2O3, SiC, GaN, AlN, and AlGaN materials as well as oxidised SiC surfaces. All of these materials have their typical defects and require optimised measurement and analysis schemes for reliable detection and analysis. Spectroscopic ellipsometry is a highly sensitive method for determining the thicknesses and dielectric function of thin layers, yielding potentially a high number of microscopic properties. The combined method between ellipsometry and optical microscopy is called imaging ellipsometry and is especially powerful for the large amount of data it produces. We have analysed defects in SiC- and AlN-based thin film semiconductors as well as characterised the properties of different types of SiO2 layers created on top of SiC monocrystals. We developed ellipsometric models for the data analysis of the different semiconductor materials. If the defects have geometric features, it is useful to combine the ellipsometric analysis with topometry method like interference microscopy and scanning probe microscopy. We have successfully characterised function-critical defects in MOVPE SiC layers and correlated the findings with topography from WLIM measurements. We have developed an imaging ellipsometric measurement methodology that allows to estimate the relative defect area on a surface by a statistical raw data analysis. Compound semiconductors (CS) are promising materials for the development of high-power electrical applications. They have low losses, can withstand high temperatures and can operate at very high voltages and currents. This makes them a key technology for the electrification of many high energy applications, especially electromobility and HVDC power lines. The challenge is that most of the process technology has to be developed specifically and tailored to the high standards required by electronic applications. Today, many different CS materials can be produced in thin layers on top of substrates fabricated from classical crystal growth processes that are already well established. A promising method for this is metal organic vapour phase epitaxy (MOVPE). This technology is a direct thin layer deposition method capable of producing complex multilayer systems directly from one deposition process without the need of doping after growing. There are a number of critical defects that can originate from the deposition process when targeting electronic thin film devices. Within this project, we intend to develop new correlative imaging and analysis techniques to determine defect types, to quantify defect size and density, as well as to characterise defects for further process optimisation. We report here on the use of spectroscopic and multispectral imaging ellipsometry to investigate defects in several different compound semiconductor materials used in high-power electronic devices. The materials we investigated are β-Ga2O3, SiC, GaN, AlN, and AlGaN as well as oxidised SiC. All of these materials have their typical defects and require optimised measurement and analysis schemes for reliable detection and analysis. Spectroscopic ellipsometry is a highly sensitive method for determining the thicknesses and dielectric function of thin layers, yielding potentially a high number of microscopic properties. The combined method between ellipsometry and optical microscopy is known as imaging ellipsometry and is especially powerful for the large amount of data it produces. We have analysed defects in SiC- and AlN-based thin film semiconductors as well as characterised the properties of different types of SiO2 layers created on top of SiC monocrystals. We developed ellipsometric models for the data analysis of the different semiconductor materials. If the defects have geometric features, it is useful to combine the ellipsometric analysis with topometry methods like interference microscopy and scanning probe microscopy. We have successfully characterised function-critical defects in MOVPE SiC layers and correlated the findings with topography from WLIM measurements. We have developed an imaging ellipsometric measurement methodology that allows to estimate the relative defect area on a surface by a statistical raw data analysis. T2 - EMRS Spring Meeting 2024 - ALTECH 2024 CY - Strasbourg, France DA - 27.05.2024 KW - Ellipsometry KW - Power Electronics KW - Layer Materials KW - Defect Analysis PY - 2024 AN - OPUS4-60266 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ermilova, Elena A1 - Weise, Matthias A1 - de Preville, Sophie A1 - Hoffmann, Johannes A1 - Morán-Meza, José A1 - Hertwig, Andreas A1 - Piquemal, François T1 - Ellipsometry as optical metrology method for analysis of reference materials for nanoelectronics N2 - Electrical properties of materials at the nanoscale can be characterized using scanning microwave microscopes (SMM) and conductive atomic force microscopes (C AFM). However, the measurement results are difficult to compare since different setups and different reference standards are used. The development of new “out-of-lab” reference standards can contribute to the traceability and reliability of these scanning probe microscopy methods (SPM) and facilitate their broader industrial application. In this study, we discuss the capability of optical methods such as ellipsometry for the characterization of existing and the development of new reference calibration samples for scanning microwave microscopy. Ellipsometry is a fast and non-destructive method, which enables very accurate determination of the layer thickness and the dielectric functions of the materials. Imaging ellipsometry is suitable for spatially resolved measurements when analyzing thin layers in microstructured samples. We show how the electrical resistivity of indium tin oxide (ITO) layers in newly designed resistive calibration samples can be obtained from spectroscopic ellipsometric measurements. The extension of the measurement range into the mid-infrared region was necessary when analyzing ITO layers with low conductivity. This parameter was obtained by fitting a Drude function describing the absorption of the free carriers. The impact of the coating process conditions on the layer properties is discussed. Imaging ellipsometry was applied for the characterisation of thin ITO and SiO2 layers in microstructured resistive and capacitance calibration kits. The uncertainties of determined layer thicknesses were specified according to standardized practice guides used in ellipsometry. We show how statistical fingerprint analysis of the measured ellipsometric transfer quantities can be used to validate the quality of potential reference materials for nano-electronics and to monitor the processing of structured samples. T2 - L. ALTECH 2024 - Analytical techniques for accurate nanoscale characterization of advanced materials CY - Strasbourg, France DA - 27.05.2024 KW - Ellipsometry KW - Reference materials KW - Transparent conductive Oxides KW - Scannig probe microscope KW - Metrology KW - Nanoelectronics PY - 2024 AN - OPUS4-60268 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ciornii, Dmitri A1 - Knigge, Xenia A1 - Radnik, Jörg A1 - Thünemann, Andreas A1 - Hodoroaba, Vasile-Dan A1 - Altmann, Korinna T1 - Identification of toxicologically relevant functional groups on micro- and nanoplastic particles’ surface by means of X-Ray photoelectron spectroscopy N2 - Microplastic and nanoplastic particles (MNP) are spread all over the world in various types, shapes and sizes making it very challenging to accurately analyse them. Each sampling procedure, sample preparation method and detection technique needs suitable reference materials to validate the method for accurate results. Furthermore, the effects of these MNPs should be evaluated by risk and hazard assessment with test particles close to reality. To better understand MNP behavior and aid in clarification of their interactions with organisms, we produced several MNP materials by top-down procedure and characterized their properties. Since surface properties mostly determine particles’ toxicity, the aim of the present study was to determine which functional groups are present on MNPs and how the surface can be affected by the production process and particle’s environment. T2 - SETAC 34th Meeting CY - Seville, Spain DA - 05.05.2024 KW - Microplastics KW - Nanoplastics KW - Polypropylene KW - XPS KW - SEM PY - 2024 AN - OPUS4-60037 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -