TY - CONF A1 - Papaioannou, Savvina Maria T1 - XCT image analysis for characterizing 3D printed thermomagnetic materials in energy harvesting applications N2 - A critical amount of industrial energy input is lost as waste heat, and this amount peaks just above room temperature. The aim of this work is to develop a technology to convert this low-grade waste heat into electricity through a thermomagnetic generator based on Faraday's law of induction. To this end, water-flowable thermomagnetic elements are developed by the industrial partner to be used as heat exchanger components in the demonstrator. The 3D extrusion and post heat treatment process of the developed fine parts may introduce various defects that have an impact on their heat transfer efficiency, magnetic and mechanical properties. Here, the non-destructive characterisation technique of X-ray computed tomography (XCT) is used to evaluate the morphology of the developed components and to identify trends that contribute to the improvement of material performance in the demonstrator. In specific, XCT image analysis enables the 3D visualisation of the developed 3D-printed structures. Using DragonFly software, scalar quantities such as volume, total surface area and void fraction are estimated for each sample. More specifically, image segmentation using Otsu’s thresholding method, combined with morphological operations on the reconstructed 3D XCT volume, contributes to the estimation of the mean filament diameter, mean channel width and distribution of internal porosity along the printing direction. In addition, the repeatability and dimensional accuracy of the printing process are evaluated through slice analysis of each 3D-printed block, both along and perpendicular to the water-flow direction. T2 - Delft Days on Magnetocalorics (DDMC) CY - Delft, Netherlands DA - 20.11.2025 KW - X-ray computed tomography KW - Image analysis KW - Thermomagnetic KW - Heat exchangers PY - 2025 AN - OPUS4-65249 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė T1 - How experimental and computational methods allow us to design negative thermal expansion materials N2 - Combined experimental and computational methods allow comprehensive understanding, design, and tailoring of material properties. We focus on a well-known negative thermal expansion (NTE) material, zirconium vanadate (ZrV2O7), and address synthesis, characterisation and validation of results with computational simulations. Experimental and computational X-ray diffraction and Raman spectroscopy data highlighted differences between phase-pure and multiphase ceramics. These techniques allowed us to distinguish subtle differences in the structure of the material. Based on ab initio simulated phonon data, unaffected by impurities or instrumental errors, we could interpret the Raman spectra and visualise Raman active atom vibrations. These computational models allowed better insight and further experimental improvement while high-quality experimental data granted the validation and improvement of computational simulation strategy. T2 - Application of Neutrons and Synchrotron Radiation in Engineering Materials Science CY - Hamburg, Germany DA - 23.03.2025 KW - NTE KW - Sol-gel KW - Ab initio KW - Raman KW - XRD PY - 2025 AN - OPUS4-62832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hertwig, Andreas T1 - A multi-method study of femtosecond laser modification and ablation of amorphous hydrogenated carbon coatings N2 - We report here the optical constants of ECR (MW) and RF generated a-C:H layers before and after laser irradiation. The work is described in the following publication: https://doi.org/10.1007/s00339-024-07980-z The data uploaded are the optical constants (n and k) of the a-C:H layers before (base) and after (ROIx) laser irradiation. Please see the article for the nomenclature of the data and for the methods applied ot produce the layers, laser shots, and OK data. KW - Spectroscopic ellipsometry KW - Amorphous hydrogenated carbon layers KW - Laser materials processing KW - Correlative imaging spectroscopy PY - 2024 DO - https://doi.org/10.5281/zenodo.13928596 PB - Zenodo CY - Geneva AN - OPUS4-61855 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sachse, René T1 - Operando electrochemical spectroscopic ellipsometry: Material properties of highly active mesoporous IrOx films revealed under realistic OER conditions N2 - Hydrogen production via water electrolysis will be an essential cornerstone in development of sustainable, fossil-free fuel and chemical production on a global scale. The activity and stability of each catalyst is highly dependent on the properties of the coating, i.e., phase composition, crystallinity, accessible surface area, and many other factors. The key to developing improved catalysts is a better understanding of the relationships between their performance, stability, and physicochemical properties. However, these relationships can be complex and are also strongly influenced by the reaction environment. Therefore, operando analysis of the catalyst material during catalysis at realistic potentials and current densities is highly desirable. However, many analytical techniques cannot be applied in liquid environments at realistic potentials and current densities. We propose environmental ellipsometric analysis in a dedicated electrochemical flow cell as a method to evaluate gas evolution reactions operando under realistic working conditions. Figure 1 illustrates schematically the developed technique. Key factors to success are highly active model-type catalysts, a suitable sample environment, and a deep understanding of the appropriate model development, as well as concise cross validation with numerous other analytical techniques. The method was developed and validated by analyzing a calcination series (300 – 600 °C) of mesoporous templated IrOx films ex-situ and operando under oxygen evolution reaction (OER) conditions. The employed environmental electrochemical spectroscopic ellipsometric (ECSE) analysis revealed during OER the change of optical and electronic properties, i.e. the dielectric functions, resistivity and band-to-band transitions (p-d band transitions). Film thickness and porosity were validated by means of scanning electron microscopy (SEM), X-ray reflectometry (XRR) or ellipsometric porosimetry (EP), electrical and electronic properties by means of conductivity measurements, X-ray photoelectron spectroscopy (XPS) or UV-Vis-NIR absorption spectroscopy. The electronic structures of the catalysts from valence electron energy loss spectra (VEELS) derived from ε1 and ε2 from SE measurements reveal a direct correlation with electrochemical activities in OER. In the presentation reversible and irreversible potential-dependent changes of the catalyst properties during operation will be discussed along with the dynamics of gas formation, transport and dissolution at different potentials. T2 - 11th Workshop Ellipsometry (WSE 11) CY - Steyr, Austria DA - 06.09.2021 KW - Ectrocatalysis KW - Mesoporous iridium oxide films KW - Non-destructive operando analysis KW - Oxygen evolution reaction KW - Spectroscopic ellipsometry PY - 2021 AN - OPUS4-53915 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ren, L. A1 - Pollard, A. A1 - Hodoroaba, Vasile-Dan T1 - Measurement of Lateral Size of Graphene Oxide Flakes by SEM - An Update of the VAMAS TWA 41 Project P13 N2 - The progress of the VAMAS interlaboratory comparison Project P13 "Lateral size of graphene oxide flakes by SEM" within the Technical Working Area 41 "Graphene and Related 2D Materials" is presented. The challenges at sample preparation on substrates for accurate measurement and image analysis as well as two different image analysis approaches, containing exact guidance how to measure the main descriptors for the lateral size measurement of the imaged graphene oxide flakes with Scanning Electron Microscopy are described. Discrepancies are explained. The inclusion of the results into the corresponding ISO technical specification CD/TS 23879 is also discussed and planned, in relation with the AFM part. T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 50th Steering Committee Meeting CY - London, United Kingdom DA - 15.09.2025 KW - VAMAS KW - Interlaboratory comparison KW - Electron microscopy KW - Lateral size KW - Graphene oxide flakes PY - 2025 UR - https://www.vamas.org/twa41/documents/2023_vamas_twa41_project13_GO_SEM.pdf AN - OPUS4-64228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Hörenz, Christoph A1 - Pellegrino, F. A1 - Maurino, V. A1 - Durand, B. A1 - Taché, O. T1 - Nanoparticle size, shape, and concentration measurement at once – two VAMAS pre-standardization projects ready to start N2 - A case study on the TEM analysis of the size and shape distribution of TiO2 bipyramidal nanoparticles prepared on TEM grids was included in the recently published ISO standard ISO 21363. It was agreed to organize at a later stage a second inter-lab comparison with the nanoparticles distributed to the participants as a liquid suspension. Protocols for uniform nanoparticle deposition on suited supports developed and optimized within the EMPIR nPSize project are also prepared to be distributed. For this, we have chosen the VAMAS platform (www.vamas.org) which offers an excellent international infrastructure of laboratories with high competence in nanoparticle measurement. The VAMAS technical working area dedicated to nanoparticle measurement is TWA 34 ‘Nanoparticle populations’. For this type of nanoparticles, the size and shape distributions are the primary parameters to be reported. Due to the good deposition protocols developed, an automated image analysis is enabled (in contrast to the manual analysis of irregular TiO2 nanoparticles. In parallel with the TiO2 nanoparticle exercise, two spherical SiO2 nanoparticle samples with bi-modal size distributions (nominal relative number concentrations of 1:1 and 10:1) are prepared for a second VAMAS inter-lab comparison. Here, the nanoparticle concentration is the primary parameter to be measured. For the imaging methods it is targeted to measure the relative nanoparticle concentrations of the two modes. For the absolute nanoparticle concentration to be measured by imaging methods it is necessary to control the volume of the liquid suspension deposited on the substrate and to obtain such a homogeneous nanoparticle deposition on the substrate which allows to count (or extrapolate) all the deposited particles. KW - Electron microscopy KW - Inter-laboratory comparison KW - Nanoparticles KW - SiO2 KW - TiO2 KW - VAMAS PY - 2021 DO - https://doi.org/10.1017/S1431927621008126 VL - 27 IS - Suppl. 1 SP - 2250 EP - 2251 PB - Cambridge University Press AN - OPUS4-53124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - EMPIR nPSize Improved Traceability Chain of Nanoparticle Size Measurement - Outcomes for the Strategy/Metrology Groups of ISO/TC 229 Nanotechnologies N2 - The main outcomes of the EMPIR project nPSize are presented and the suitability of the new capabilities (e.g. reference materials, measurement procedures, VAMAS inter-laboratory comparisons) to be standardized and implemented in accredited analytical laboratories is discussed. Complementation and/or filling gaps of published and ongoing standardisation projects on size, shape and number concentration measurements under ISO/TC 229/JWG 2 are offered. T2 - Annual Meeting of ISO/TC 229 Nanotechnologies - Strategy and Metrology Groups CY - Online meeting DA - 06.11.2020 KW - Nanoparticles KW - Size KW - nPSize KW - Inter-laboratory comparison KW - ISO/TC 229 KW - VAMAS PY - 2020 AN - OPUS4-51544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Feltin, N. A1 - Crouzier, L. A1 - Delvallée, A. A1 - Pellegrino, F A1 - Maurino, V. A1 - Bartczak, D. A1 - Goenaga-Infante, H. A1 - Taché, O. A1 - Marguet, S. A1 - Testard, F. A1 - Artous, S. A1 - Saint-Antonin, F. A1 - Salzmann, Christoph A1 - Deumer, J. A1 - Gollwitzer, C. A1 - Koops, R. A1 - Sebaïhi, N. A1 - Fontanges, R. A1 - Neuwirth, M. A1 - Bergmann, D. A1 - Hüser, D. A1 - Klein, T. A1 - Hodoroaba, Vasile-Dan T1 - Metrological Protocols for Reaching Reliable and SI-Traceable Size Results for Multi-Modal and Complexly Shaped Reference Nanoparticles N2 - The study described in this paper was conducted in the framework of the European nPSize project (EMPIR program) with the main objective of proposing new reference certified nanomaterials for the market in order to improve the reliability and traceability of nanoparticle size measurements. For this purpose, bimodal populations as well as complexly shaped nanoparticles (bipyramids, cubes, and rods) were synthesized. An inter-laboratory comparison was organized for comparing the size measurements of the selected nanoparticle samples performed with electron microscopy (TEM, SEM, and TSEM), scanning probe microscopy (AFM), or small-angle X-ray scattering (SAXS). The results demonstrate good consistency of the measured size by the different techniques in cases where special care was taken for sample preparation, instrument calibration, and the clear definition of the measurand. For each characterization method, the calibration process is described and a semi-quantitative table grouping the main error sources is proposed for estimating the uncertainties associated with the measurements. Regarding microscopy-based techniques applied to complexly shaped nanoparticles, data dispersion can be observed when the size measurements are affected by the orientation of the nanoparticles on the substrate. For the most complex materials, hybrid approaches combining several complementary techniques were tested, with the outcome being that the reliability of the size results was improved. KW - Certified reference nanomaterials KW - Traceable nanoparticle size measurements; KW - Hybrid metrology KW - Scanning probe microscopy KW - Small-angle X-ray scattering KW - Electron microscopy PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571902 DO - https://doi.org/10.3390/nano13060993 SN - 2079-4991 VL - 13 IS - 6 - Special Issue "Identification and Quantification of Nanomaterials" SP - 1 EP - 25 PB - MDPI CY - Basel, CH AN - OPUS4-57190 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pu, Y. A1 - Celorrio, V. A1 - Stockmann, Jörg Manfred A1 - Sobol, Oded A1 - Sun, Z. A1 - Wang, W. A1 - Lawrence, M. J. A1 - Radnik, Jörg A1 - Russel, A. E. A1 - Hodoroaba, Vasile-Dan A1 - Huang, L. A1 - Rodriguez, P. T1 - Surface galvanic formation of Co-OH on Birnessite and its catalytic activity for the oxygen evolution reaction N2 - Low-cost, high-efficient catalysts for water splitting can be potentially fulfilled by developing earthabundant metal oxides. In this work, surface galvanic formation of Co-OH on K0.45MnO2 (KMO) was achieved via the redox reaction of hydrated Co2+ with crystalline Mn4+. The synthesis method takes place at ambient temperature without using any surfactant agent or organic solvent, providing a clean, green route for the design of highly efficient catalysts. The redox reaction resulted in the formation of ultrathin Co-OH nanoflakes with high electrochemical surface area. X-ray absorption spectroscopy (XAS) and X-ray photoelectron spectroscopy (XPS) analysis confirmed the changes in the oxidation state of the bulk and surface species on the Co-OH nanoflakes supported on the KMO. The effect of the anions, such as chloride, nitrate and sulfate, on the preparation of the catalyst was evaluated by electrochemical and spectrochemical means. XPS and Time of flight secondary ion mass spectrometry (ToF-SIMS) analysis demonstrated that the layer of CoOxHy deposited on the KMO and its electronic structure strongly depend on the anion of the precursor used during the synthesis of the catalyst. In particular, it was found that Cl- favors the formation of Co-OH, changing the rate-determining step of the reaction, which enhances the catalytic activity towards the OER, producing the most active OER catalyst in alkaline media. KW - Nanoparticles KW - Oxygen evolution reaction (OER) KW - Catalysis KW - ToF-SIMS KW - XPS KW - K-rich Birnessite (K0.45MnO2) PY - 2021 DO - https://doi.org/10.1016/j.jcat.2021.02.025 VL - 396 SP - 304 EP - 314 PB - Elsevier Inc. AN - OPUS4-52328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Terborg, R. A1 - Hodoroaba, Vasile-Dan T1 - Determination of Thin Film Thickness and Composition using Energy Dispersive EPMA N2 - Electron probe microanalysis (EPMA)is a non-destructive technique which assumes a sample of homogenous (bulk) chemical composition and can, therefore, not be used for thin film samples. However, in combination with one of the possible thin film software packages, STRATAGEM, the thickness as well as the composition of such films on a substrate can be determined. This has been demonstrated for FeNi on Si and SiGe on Al2O3 film systems. For both systems five samples with different elemental composition and a reference were produced and characterised by the Korean research institute KRISS using inductively coupled plasma mass spectrometry (ICP-MS), Rutherford backscattering (RBS), and transmission electron microscopy (TEM). In 2021, a new and open source thin film evaluation programme called BADGERFILM has been released. It can also be used to determine thin film composition and thickness from intensity ratios of the unknown sample and standards (k-ratios). In this contribution, we re-evaluated the data acquired for the FeNi and SiGe systems using the BADGERFILM software package and compared the resulting composition and thickness with the results of the established STRATAGEM software and other reference methods. With the current evaluation, the BADGERFILM software shows good agreement with the composition and thickness calculated by STRATAGEM and provided by the KRISS. These results between two well-known layered material systems analysed with available conventional EMPA approaches (STRATAGEM and direct thickness measurement by TEM) and a new one (BADGERFILM) proves that reliable non-destructive thin film analysis is possible. In this way, we validate the performance of the new software, which is not at all self-explanatory for such complex quantification algorithms lying behind the final quantified results. T2 - EMAS 2023 - 17th European Workshop on Modern Developments and Applications in Microbeam Analysis CY - Krakow, Poland DA - 07.05.2023 KW - Thin films KW - BADGER film KW - Electron probe microanallysis (EPMA) KW - FeNi thin film KW - Al2O3 thin films PY - 2023 UR - https://www.microbeamanalysis.eu/events/event/60-emas-2023-17th-european-workshop-on-modern-developments-and-applications-in-microbeam-analysis AN - OPUS4-57484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ciornii, Dmitri 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 - TY - JOUR A1 - Hülagü, Deniz A1 - Tobias, Charlie A1 - Climent Terol, Estela A1 - Gojani, Ardian A1 - Rurack, Knut A1 - Hodoroaba, Vasile-Dan T1 - Generalized Analysis Approach of the Profile Roughness by Electron Microscopy with the Example of Hierarchically Grown Polystyrene–Iron Oxide–Silica Core–Shell–Shell Particles N2 - The roughness as a property of core–shell (CS) microparticles plays a key role in their functionality. Quantitative evaluation of the roughness of CS microparticles is, however, a challenging task with approaches using electron microscopy images being scarce and showing pronounced differences in terms of methodology and results. This work presents a generalized method for the reliable roughness determination of nonplanar specimens such as CS particles from electron microscopic images, the method being robust and reproducible with a high accuracy. It involves a self-written software package (Python) that analyzes the recorded images, extracts corresponding data, and calculates the roughness based on the deviation of the identified contour. Images of single particles are taken by a dual mode scanning electron microscopy (SEM) setup which permits imaging of the same field-of-view of the sample with high resolution and surface sensitive in SE InLens mode as well as in transmission mode (TSEM). Herein, a new type of polystyrene core–iron oxide shell–silica shell particles is developed to serve as a set of lower micrometer-sized study objects with different surface roughness; the analysis of their images by the semiautomatic workflow is demonstrating that the particles’ profile roughness can be quantitatively obtained. KW - Core–shell particles KW - Image analysis KW - Nanoparticles KW - Roughness KW - SEM KW - transmission mode PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542576 DO - https://doi.org/10.1002/adem.202101344 SP - 1 EP - 9 PB - Wiley-VCH AN - OPUS4-54257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Towards automated electron microscopy image segmentation for nanoparticles of complex shape by convolutional neural networks N2 - In this contribution different ways are explored with the aim to generate suitable training data for ‘non-ideal’ samples using various approaches, e.g., computer-generated images or unsupervised learning algorithms such as generative adversarial networks (GANs). We used these data to train simple CNNs to produce segmentation masks of SEM images and tested the trained networks on real SEM images of complex nanoparticle samples. The novel use of CNN for the automated analysis of the size of nanoparticles of complex shape and with a high degree of agglomeration has proved to be a promising tool for the evaluation of particle size distribution on a large number of constituent particles. Further development and validation of the preliminary model, respectively larger training and validation data sets are necessary. T2 - Microscopy and Microanalysis 2020 CY - Online meeting DA - 03.08.2020 KW - Nanoparticles KW - Automatisation KW - Image segmentation KW - Convolutional neural networks KW - Electron microscopy PY - 2020 AN - OPUS4-51114 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Kim, K. J. A1 - Yu, H. A1 - Lee, S. M. A1 - Kwon, J. H. A1 - Ruh, H. A1 - Radnik, Jörg A1 - Archanjo, B. S. A1 - Annese, E. A1 - Damasceno, J. C. A1 - Achete, C. A. A1 - Yao, Y. A1 - Ren, L. A1 - Gao, H. A1 - Windover, D. A1 - Matsuzaki, H. A1 - Azuma, Y. A1 - Zhang, L. A1 - Fujimoto, T. A1 - Jordaan, W. A. A1 - Reed, B. A1 - Shard, A. G. A1 - Cibik, L. A1 - Gollwitzer, C. A1 - Krumrey, M. T1 - Final report of CCQM-K157 for the measurement of the amount of substance of HfO2 expressed as the thickness of nm films N2 - The key comparison CCQM-K157 for the thickness measurement of HfO2 films was performed by the Surface Analysis Working Group (SAWG) of the Consultative Committee for Amount of Substance (CCQM). The aim of CCQM-K157 is to establish the measurement traceability and to ensure the equivalency in the measurement capability of national metrology institutes for the thickness measurement of HfO2 films. In this key comparison, the thicknesses of six HfO2 films with the nominal thickness range from 0.7 nm to 6 nm were compared by x-ray photoelectron spectroscopy (XPS), x-ray reflectometry (XRR), transmission electron microscopy (TEM), spectroscopic ellipsometry (SE) and medium energy ion scattering spectrometry (MEIS). To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA). KW - CCQM KW - Thin Films KW - HfO2 KW - thickness KW - XPS PY - 2023 DO - https://doi.org/10.1088/0026-1394/60/1A/08010 VL - 60 SP - 08010 PB - IOP AN - OPUS4-63049 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan A1 - Jungnickel, H. A1 - Tentschert, J. A1 - Luch, A. A1 - Sogne, V. A1 - Maier, F. A1 - Burr, L. A1 - Schmid, D. A1 - Yoon, T.-H. A1 - Petters, R. A1 - Briffa, S.M. A1 - Valsami-Jones, E. T1 - Automation and Standardization—A Coupled Approach Towards Reproducible Sample Preparation Protocols for Nanomaterial Analysis N2 - Whereas the characterization of nanomaterials using different analytical techniques is often highly automated and standardized, the sample preparation that precedes it causes a bottleneck in nanomaterial analysis as it is performed manually. Usually, this pretreatment depends on the skills and experience of the analysts. Furthermore, adequate reporting of the sample preparation is often missing. In this overview, some solutions for techniques widely used in nano-analytics to overcome this problem are discussed. Two examples of sample preparation optimization by au-tomation are presented, which demonstrate that this approach is leading to increased analytical confidence. Our first example is motivated by the need to exclude human bias and focuses on the development of automation in sample introduction. To this end, a robotic system has been de-veloped, which can prepare stable and homogeneous nanomaterial suspensions amenable to a variety of well-established analytical methods, such as dynamic light scattering (DLS), small-angle X-ray scattering (SAXS), field-flow fractionation (FFF) or single-particle inductively coupled mass spectrometry (sp-ICP-MS). Our second example addresses biological samples, such as cells exposed to nanomaterials, which are still challenging for reliable analysis. An air–liquid interface has been developed for the exposure of biological samples to nanomaterial-containing aerosols. The system exposes transmission electron microscopy (TEM) grids under reproducible conditions, whilst also allowing characterization of aerosol composition with mass spectrometry. Such an approach enables correlative measurements combining biological with physicochemical analysis. These case studies demonstrate that standardization and automation of sample preparation setups, combined with appropriate measurement processes and data reduction are crucial steps towards more reliable and reproducible data. KW - Sample preparation KW - Automation KW - Nanomaterial analysis KW - Standardization PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543988 DO - https://doi.org/10.3390/molecules27030985 VL - 27 IS - 3 SP - 1 EP - 22 PB - MDPI AN - OPUS4-54398 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Hodoroaba, Vasile-Dan A1 - Fontanges, R. A1 - Delvallée, A. A1 - Deumer, J. A1 - Salzmann, C. A1 - Crouzier, L. A1 - Gollwitzer, C. A1 - Klein, T. A1 - Koops, R. A1 - Sebaihi, N. A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Artous, S. A1 - Taché, O. A1 - Feltin, N. T1 - Report on full algorithm sequences for nanoparticle detection and size measurement as developed on both a physical basis and by machine learning N2 - he main objective of the nPSize project is to improve the measurement capabilities for nanoparticle size based on both measurement methods traceable to SI units and new reference materials. Two basic approaches have been used in order to develop measurement procedures resulting in traceable results of the nanoparticle size distribution: physical modelling for the methods used in the project (TSEM, SEM, AFM and SAXS) and machine learning. Physical modelling: In this part, the physical models associated with different shape measurements for the techniques TSEM, SEM, AFM and SAXS have been collected and further developed with the aim to simulate the resulting signal as measured by the individual methods. Uncertainties and traceability associated with each model were investigated and evaluated. In the following, the progress on these physical models is reported for each individual method. Machine Learning modelling: The aim of this part is to use machine learning to enable automatic measurement of nanoparticle shape from expert a-priori information only. No physical model will be used as a-priori information in this task. The accuracy and traceability of the size results obtained by each technique will be analyzed and compared with the physical modelling. A machine learning database will then be used to create automatic detection algorithms. KW - Nanoparticles KW - Particle size distribution KW - SEM KW - TSEM KW - TEM KW - SAXS KW - AFM PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546531 DO - https://doi.org/10.5281/zenodo.5807864 SP - 1 EP - 20 PB - Zenodo CY - Geneva AN - OPUS4-54653 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Overview of CUSP and PlasticTrace N2 - The presentation summarises the work of CUSP and PlasticTrace EU joint research projects of the last year. T2 - Microplastics Scientific Workshop of PlasticsEurope CY - Amsterdam, The Netherlands DA - 08.05.2023 KW - Microplastics KW - Microplastics standardisation KW - Reference materials KW - Polymer 3R PY - 2023 AN - OPUS4-57460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Vladár, A. E. A1 - Hodoroaba, Vasile-Dan ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Characterization of nanoparticles by scanning electron microscopy N2 - In this chapter sample preparation, image acquisition, and nanoparticle size and shape characterization methods using the scanning electron microscope (SEM) in reflective and transmitted working modes are described. These help in obtaining reliable, highly repeatable results. The best solutions vary case-by-case and depend on the raw (powdered or suspension) nanoparticle material, the required measurement uncertainty and on the performance of the SEM. KW - Nanoparticles KW - Sample preparation KW - Electron microscopy KW - SEM KW - Size measurement KW - Shape KW - Threshold PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00002-X SP - 7 EP - 27 PB - Elsevier CY - Amsterdam AN - OPUS4-50120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arinchtein, A. A1 - Ye, M.-Y. A1 - Yang, Q. A1 - Kreyenschulte, C. A1 - Wagner, Andreas A1 - Frisch, M. A1 - Brückner, A. A1 - Kondratenko, E. A1 - Kraehnert, R. T1 - Dynamics of Reaction-Induced Changes of Model-Type Iron Oxide Phases in the CO2-Fischer-Tropsch-Synthesis N2 - Iron-based catalysts are employed in CO2-FTS due to their ability to convert CO2 into CO in a first step and their selectivity towards higher hydrocarbons in a second CO hydrogenation step. According to the literature, iron carbides represent the active phase for hydrocarbon formation and are claimed to emerge in the presence of CO. We propose nanostructured FeOx films as model systems to assess information about the complex phase transformations during CO2-FTS. Mesoporous hematite, ferrihydrite, maghemite, maghemite/magnetite films were exposed to CO2-FTS atmospheres at 20 bar and 300°C. Up to three distinct phases were observed depending on the timeon-stream (TOS): a sintered maghemite/magnetite phase, a carbidic core-shell structure, and a low-crystalline, needle-type oxide phase. Our findings indicate that the formation of an intermediary maghemite/magnetite phase, predominant after short TOS (30 h), precedes the evolution of the carbide phase. Yet, even after prolonged TOS (185 h), no full conversion into a bulk carbide is observed. KW - Nanostructured FeOx films KW - CO2 KW - Scanning Auger Spectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549709 DO - https://doi.org/10.1002/cctc.202200240 SN - 1867-3880 VL - 14 IS - 14 SP - 1 EP - 11 PB - Wiley-VCH AN - OPUS4-54970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmid, Thomas A1 - Hodoroaba, Vasile-Dan T1 - Correlative Analysis by Raman and other Micro & Nanospectroscopic Imaging Techniques N2 - In the present talk the basics of the Raman spectroscopy and particularly of Raman microscopy are explained. Advantages and disadvantages of the method are highlighted through selected case studies. In the second part of the lecture examples of correlative imaging with electron, X-ray, ion and optical microscopies from micro- to the nanoscale are highlighted. T2 - Charisma School on Raman Harmonisation CY - Turin, Italy DA - 19.10.2022 KW - Raman KW - Correlative Imaging KW - Microscopy KW - Hyperspectral imaging PY - 2022 UR - https://amdgroup.inrim.it/events/vamas-sc-meeting-47/program-sc47 AN - OPUS4-56094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -