TY - CONF A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob T1 - The Meticulous Approach: Fully traceable X-ray scattering data via a comprehensive lab methodology N2 - To find out if experimental findings are real, you need to be able to repeat them. For a long time, however, papers and datasets could not necessarily include sufficient details to accurately repeat experiments, leading to a reproducibility crisis. It is here, that the MOUSE project (Methodology Optimization for Ultrafine Structure Exploration) tries to implement change – at least for small- and wide-angle X-ray scattering (SAXS/WAXS). In the MOUSE project, we have combined: a) a comprehensive laboratory workflow with b) a heavily modified, highly automated Xenocs Xeuss 2.0 instrumental component. This combination allows us to collect fully traceable scattering data, with a well-documented data flow (akin to what is found at the more automated beamlines). With two full-time researchers, the lab collects and interprets thousands of datasets, on hundreds of samples for dozens of projects per year, supporting many users along the entire process from sample selection and preparation, to the analysis of the resulting data. While these numbers do not light a candle to those achieved by our hardworking compatriots at the synchrotron beamlines, the laboratory approach does allow us to continually modify and fine-tune the integral methodology. So for the last three years, we have incorporated e.g. FAIR principles, traceability, automated processing, data curation strategies, as well as a host of good scattering practices into the MOUSE system. We have concomitantly expanded our purview as specialists to include an increased responsibility for the entire scattering aspect of the resultant publications, to ensure full exploitation of the data quality, whilst avoiding common pitfalls. This talk will discuss the MOUSE project1 as implemented to date, and will introduce foreseeable upgrades and changes. These upgrades include better pre-experiment sample scattering predictions to filter projects on the basis of their suitability, exploitation of the measurement database for detecting long-term changes and automated flagging of datasets, and enhancing MC fitting with sample scattering simulations for better matching of odd-shaped scatterers. T2 - S4SAS CY - Online meeting DA - 01.09.2021 KW - X-ray scattering KW - Methodology KW - MOUSE KW - Data organization KW - Automation KW - Traceability PY - 2021 AN - OPUS4-53273 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Friedrich, Sebastian A1 - Cappella, Brunero T1 - Friction and mechanical properties of AFM-scan-induced ripples in polymer films N2 - In the present paper, friction and mechanical properties of AFM-Scan-Induced ripple structures on films of polystyrene and poly-n-(butyl methacrylate) are investigated. Force volume measurements allow a quantitative analysis of the elastic moduli with nanometer resolution, showing a contrast in mechanical response between bundles and troughs. Additionally, analysis of the lateral cantilever deflection shows a clear correlation between friction and the sample topography. Those results support the theory of crack propagation and the formation of voids as a mechanism responsible for the formation of ripples. This paper also shows the limits of the presented measuring methods for soft, compliant, and small structures. KW - AFM KW - Polymer KW - Ripples KW - Mechanical properties KW - Friction PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532772 DO - https://doi.org/10.3389/fmech.2021.672898 SN - 2297-3079 VL - 7 SP - 1 EP - 8 PB - Frontiers Media CY - Lausanne AN - OPUS4-53277 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella A1 - Nirmalananthan-Budau, Nithiya A1 - Rühle, Bastian A1 - Geißler, Daniel A1 - Resch-Genger, Ute T1 - Quantification of surface functional groups on inorganic and organic nanomaterials using cleavable reporters N2 - Engineered nanomaterials (NM) with their unique size-dependent properties are of increasing relevance for current and future developments in various fields such as medical and pharmaceutical industry, computing and electronics or food and consumer products. The performance and safety of NM are determined by the sum of their intrinsic physicochemical properties. Especially, the particle surface chemistry, which is largely controlled by the chemical nature and density of functional groups and ligands, is an important key driver for the performance, stability, and processibility of NM, as well as their interaction with the environment. Thus, methods for functional group quantification can foster the sustainable development of functional and safe(r) NM. Aiming at the development of simple, versatile and multimodal tools for the quantification of common bioanalytically relevant functional groups, we designed a catch-and-release assay based on cleavable probes that enable the quantification of the cleaved-off reporters in the supernatant after particle separation. Thus, the approach circumvents interferences resulting from particle light scattering and sample-inherent absorption or emission. To study the potential of the assay, commercially available and in-house synthesized aminated and carboxylated polymer and silica nanoparticles of different functional group densities were tested. Our cleavable probe strategy can be easily adapted to other analytical techniques requiring different reporters, or to different types of linkers that can be cleaved thermally, photochemically, or by variation of pH, utilizing well-established chemistry. In addition, it can contribute to the development of multi-method characterization strategies to provide a more detailed picture of the intrinsic physicochemical property - performance/safety relationships and thus can support the design of tailored nanomaterials with better controlled properties. T2 - E-MRS Spring Meeting 2021 / ALTECH 2021 - Analytical techniques for precise characterization of nanomaterials CY - Online meeting DA - 31.05.2021 KW - Surface modified nano- and microparticles KW - Optical assays KW - Particle surface analysis KW - Surface functional group quantification PY - 2021 AN - OPUS4-55596 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Bonse, Jörn A1 - Kirner, Sabrina V. A1 - Krüger, Jörg ED - Sugioka, K. T1 - Laser-induced periodic surface structures (LIPSS) N2 - Laser-induced periodic surface structures (LIPSS) are a universal phenomenon and can be generated on almost any material by irradiation with linearly polarized radiation. This chapter reviews the current state in the field of LIPSS, which are formed in a “self-ordered” way and are often accompanying materials processing applications. LIPSS can be produced in a single-stage process and enable surface nanostructuring and, in turn, adaption of optical, mechanical, and chemical surface properties. Typically, they feature a structural size ranging from several micrometers down to less than 100 nm and show a clear correlation with the polarization direction of the light used for their generation. Various types of LIPSS are classified, relevant control parameters are identified, and their material-specific formation mechanisms are analyzed for different types of inorganic solids, i.e., metals, semiconductors, and dielectrics. Finally, technological applications featuring surface functionalization in the fields of optics, fluidics, medicine, and tribology are discussed. KW - Femtosecond laser KW - Laser ablation KW - Laser-induced periodic surface structures (LIPSS) KW - Microstructures KW - Nanostructures PY - 2021 SN - 978-3-319-69537-2 DO - https://doi.org/10.1007/978-3-319-69537-2_17-2 SP - 1 EP - 59 PB - Springer Nature CY - Cham, Switzerland ET - 2 AN - OPUS4-51493 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hodoroaba, Vasile-Dan A1 - Hörenz, Christoph T1 - Improving nanoparticle size measurement accuracy for safety assessment N2 - Nanomaterials and nanoparticles are finding applications across a wide range of technology sectors, from medicine and food to transportation and construction. In order to assess these new materials for potential risks to health and the environment, they need to be well-characterised. The measurement of constituent nanoparticle size, shape, and size distribution are important factors for the risk evaluation process. EMPIR project Improved traceability chain of nanoparticle size measurements (17NRM04, nPSize) is working to assess a range of traceable nanoparticle measurement approaches, including Scanning Electron Microscopy (also in Transmission Mode), Atomic Force Microscopy and Small Angle X-ray Scattering, and deliver improved calibration methods to users. For the techniques under investigation, physical models of their response to a range of nanoparticle types are developed. Validated reference materials will also be used for an inter-comparison of measurement systems, with an evaluation of the associated measurement uncertainty. With project contributions to standards development work, manufacturers will be better placed to assess the human and environmental risks posed by nanomaterials across a whole range of products. KW - Nanoparticles KW - Particle size distribution KW - Traceability KW - Electron microscopy KW - AFM KW - SAXS PY - 2021 UR - https://www.euramet.org/?L=0&news=40%3A1159 SP - 1 PB - EURAMET e.V. CY - Braunschweig AN - OPUS4-52129 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sun, C. A1 - Schäferling, Michael A1 - Resch-Genger, Ute A1 - Gradzielski, M. T1 - Solvothermal Synthesis of Lanthanide-doped NaYF4 Upconversion N2 - Lanthanide-doped NaYF4 upconversion nano- and microcrystals were synthesized via a facile solvothermal approach. Thereby, the influence of volume ratios of ethylene glycol (EG)/H2O, molar ratios of NH4F/RE3+ (RE3+ represents the total amount of Y3+ and rare-earth dopant ions), Gd3+ ion contents, types of activator dopant ions, and different organic co-solvents on the crystal phase, size, and morphology of the resulting particles were studied systematically. A possible formation mechanism for the growth of crystals of different morphology is discussed. Our results show that the transition from the α- to the β-phase mainly depends on the volume ratio of EG/H2O and the molar ratio of NH4F/RE3+, while the morphology and size could be controlled by the type of organic co-solvent and Gd3+ dopant ions. Furthermore, the reaction time has to be long enough to convert α-NaYF4 into β-NaYF4 during the growth process to optimize the upconversion luminescence. The formation of larger β-NaYF4 crystals, which possess a higher upconversion luminescence than smaller particles, proceeds via intermediates of smaller crystals of cubic structure. In summary, our synthetic approach presents a facile route to tailor the size, Crystal phase, morphology, and luminescence features of upconversion materials. KW - Nano KW - Nanomaterial KW - Upconversion nanoparticle KW - Photoluminescence KW - Lanthanide KW - Quantum yield KW - Photophysics KW - Lifetime KW - Surface chemistry KW - Single particle KW - Brightness KW - NIR KW - Synthesis PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520307 DO - https://doi.org/10.1002/cnma.202000564 VL - 7 IS - 2 SP - 174 EP - 183 PB - Wiley AN - OPUS4-52030 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Szymoniak, Paulina A1 - Omar, Hassan A1 - Schönhals, Andreas A1 - Qu, Xintong T1 - Spatial Inhomogeneity, Interfaces and Complex Vitrification Behavior of Epoxy-based Materials by Broadband Dielectric Spectroscopy and Calorimetry N2 - Although in the last decades epoxy-based nanocomposites have been successfully adopted by the marine, automotive and aerospace industries they are still rarely studied on a fundamental level. This work deals with an in-depth comparative investigation of the structure, molecular mobility and vitrification kinetics of three bisphenol A diglycidyl ether (DGEBA)-based materials with different nanofillers: I) taurine-modified layered double hydroxide (T-LDH), II) boehmite (BNPs) and III) halloysite nanotubes (HNTs). Moreover, the effect of different hardeners (diethylene triamine and methyl tetrahydrophtalic acid anhydride) on the unfilled epoxy matrix is addressed as well. The chosen methodology comprises I) small – and wide – angle X-ray scattering (SAXS/WAXS) II) calorimetry in the forms of a) conventional DSC and b) static fast scanning calorimetry (FSC), III) broadband dielectric spectroscopy (BDS), as well as IV) specific heat spectroscopy in the forms of a) temperature modulated DSC, and b) temperature modulated FSC. The combination of these techniques proved an intrinsic spatial heterogeneity of epoxy-based materials, evidenced by two separate segmental relaxation processes. Although, depending on the hardener the response of the systems to calorimetric and dielectric investigations was different, in a broader sense similar conclusions can be extracted on the structural heterogeneity. As expected from the two distinct α-processes, it was shown that, in parallel to the main glass transition, epoxy-based materials can exhibit an additional low temperature vitrification mechanism, which was not discussed in prior studies for an unfilled network former. Furthermore, the interfacial region (so-called rigid amorphous fraction) was qualitatively and quantitatively addressed, in dependence of the employed nanofiller structure. T2 - Webinar University of Southern Denmark CY - Online meeting DA - 20.01.2021 KW - BDS KW - Nanocomposites KW - Epoxy KW - Rigid amorphous fraction KW - TMDSC KW - Flash DSC PY - 2021 AN - OPUS4-52036 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Schmitt, M. T1 - EMPIR nPSize - Improved Traceability Chain of Nanoparticle Size Measurement; What nPSize can offer to CEN/TC 352? N2 - The main outcomes of the EMPIR project nPSize are presented and the suitability of the new capabilities (e.g. reference materials, measurement procedures, inter-laboratory comparisons) as pertinent contributions to normative projects within CEN/TC 352 Nanotechnologies are discussed. E.g. the first technical report of nPSize on full algorithm sequences for nanoparticle detection and size measurement as developed on both a physical basis (SEM, TSEM, AFM and SAXS) and by machine learning is put at disposal. T2 - 29th Meeting of CEN/TC 352 Nanotechnologies CY - Online meeting DA - 25.03.2021 KW - Nanoparticles KW - Electron microscopy KW - CEN/TC 352 Nanotechnologies KW - Particle size distribution KW - Modelling KW - Machine learning PY - 2021 AN - OPUS4-52464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kuchenbecker, Petra T1 - Granulometry of Nano Powders - a Challenge Especially for the Dispersion Process N2 - The use of increasingly finer starting powders up to nanopowders can also be observed in the field of ceramics. Their advantages consist, for example, in their lower activation energy, an increase in strength or unique optical properties. However, handling and characterization of the powders are much more difficult. The main reason for this is the very high adhesive forces between the particles and between particles and other surfaces, too. Therefore, submicron and even more so nanoparticles tend to agglomerate and their separation into primary particles during sample preparation prior to particle sizing is of particular challenge. A representative measurement sample is only obtained when it no longer contains agglomerates. The evaluation of the dispersion process and a decision on whether it was successful thus increases in importance for the reliability of the measurement results of particle sizing. The presentation uses examples to show possible approaches and provides information on possible sources of error. It is shown that successful granulometric characterisation of fine powders requires both an improved dispersion technique and very often an effective combination of two or more measurement methods. KW - Agglomerates KW - Nano-powder KW - Dispersion process PY - 2021 SN - 0173-9913 VL - 98 IS - 2 SP - 47 EP - 54 PB - Göller Verlag GmbH CY - Baden-Baden AN - OPUS4-52504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ciornii, Dmitri A1 - Drobne, D. A1 - Novak, S. A1 - Kranjc, E. A1 - Bohmer, N. A1 - Hodoroaba, Vasile-Dan A1 - Reuther, R. T1 - Knowledge, Information and Data Readiness Levels (KaRL) approach for Nanorisk Governance N2 - Nanomaterials may have brought many beneficial innovations with them in our daily lives and and have become indispensable for the society. However, one needs to be concerned of the risks which are still unknown and not sufficietly studied and therefore there is a need for a nanorisk governance. At the core of nanorisk governance is gathering, processing and analysing reliable data which will be used for decision making. The challenge is to assure data reliability and transform it into knowledge. To address this challenge, we used analogy to technology readiness level (TRL) approach (developed by NASA), and elaborated knowledge readiness level (KaRL). KaRL is a nine-scale system to categorize data and knowledge (documents) into levels of readiness for particular purposes and to enhance readiness level by using quality and completeness filters, compliance requirements, nanorisk-related tools, stakeholders’ input. By our approach we addressed key issues in nanotechnology such as societal and ethical concerns, circular economy and sustainability, traceability of data, knowledge and decisions. T2 - EC - HORIZON EUROPE NMBP-13 Joint Conference Risk Governance of nanotechnology CY - Online meeting DA - 12.04.2021 KW - Knowledge Readiness Level KW - Nanorisk KW - Nanomaterials KW - Data PY - 2021 AN - OPUS4-52471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -