TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Organic Surface Modification and Analysis of Titania Nanoparticles for Self-Assembly in Multiple Layers N2 - The characteristics of TiO2 coatings can greatly influence their final performance in large-scale applications. In the present study self-assembly of TiO2 nanoparticles (NPs) in multiple layers was selected as a deposition procedure on various substrates. For this, the main prerequisite constitutes the surface modification of both NPs and substrate with e.g. silane coupling agents. A set of functionalized TiO2 NPs has been produced by reaction with either (3- aminopropyl)triethoxysilane (APTES) or (3-aminopropyl)phosphonic acid (APPA) to functionalize the NP surface with free amino-groups. Then, the complementary functionalized NP set can be obtained from an aliquot of the first one, through the conversion of free surface amino-groups to aldehydes by reaction with glutaraldehyde (GA). Several types of TiO2 NPs differing in size, shape and specific surface area have been functionalized. FTIR, TGA, SEM/EDS, XPS, Auger electron spectroscopy (AES) and ToF-SIMS analyses have been carried out to evaluate the degree of functionalization, all the analytical methods employed demonstrating successful functionalization of TiO2 NP surface with APTES or APPA and GA. T2 - European Conference on Applications of Surface and Interface Analysis ECASIA 2019 CY - Dresden, Germany DA - 15.09.2019 KW - TiO2 KW - Layer-by-layer deposition KW - Surface functionalization KW - P25 KW - Surface characterization PY - 2019 AN - OPUS4-49279 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fernandez-Poulussen, D. A1 - Hodoroaba, Vasile-Dan T1 - Holistic, reliable and practical Characterization Framework for Graphene Family Materials, a correlated approach including Imaging based techniques N2 - ACCORDs is an Horizon Europe project working in the development of an imaging-based characterization framework (ACCORDs framework) for the holistic correlative assessment of Graphene Family Materials (GFMs) as a representative of 2D nanomaterials (NMs) to assess and predict 2D NMs health and environmental risks. The ACCORDs framework will operationalise safe and sustainable by design (SSbD) strategies proposed in past or ongoing H2020 projects or within OECD by correlating low-, medium-, and high-resolution physico-chemical-biological imaging-based methods with non-imaging methods in a tiered approach. ACCORDs will deliver the ACCORDs framework and user guidance, new imaging-based characterisation methods, reference in vitro tests, new reference 2D NMs for different matrices, a new minimum information reporting guideline for FAIR data sharing and reuse of images as well as an atlas with reference images for diagnostics of compromised safety of GFMs/GFM products. The new guidelines and standard proposals will be submitted to standardisation bodies to allow creation of regulatory ready products. The novelty of ACCORDs is in translating the principles of medical imaging-based diagnostics to 2D material hazard diagnostics. ACCORDs will accelerate industrial sectors in the area of aviation, marine construction, drone production, flexible electronics, photovoltaics, photocatalytics and print inks-based sensors. The value ACCORDs proposes to the graphene industry are practical, easy, imaging-based tools for GFM quality monitoring next to the production line with a possibility to be correlated with advanced highresolution imaging characterization methods in case hazard i.e. deviation from controls (benchmark values) are diagnosed. The ACCORDs framework and tools will contribute to the European Green Deal by addressing the topic: “Graphene: Europe in the lead” and to a new European strategy on standardization, released on 2nd February, 2022 T2 - Joint Regulatory Risk Assessors Summit – Advancing Safety & Sustainability Assessments of Advanced Materials CY - Paris, France DA - 19.06.2025 KW - Graphene-related 2D materials (GR2M) KW - Imaging KW - SSbD KW - ACCORDs PY - 2025 UR - https://macrame-project.eu/macrame-meetings-workshops/jointrras/#Agenda AN - OPUS4-63660 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Madbouly, Loay Akmal A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - Raman Spectroscopy and X-ray Photoelectron Spectroscopy of Commercial Functionalized Graphene N2 - Graphene has found widespread commercial use, particularly in flexible electronics and coatings for substrates such as paper and textiles, in the form of suspensions and inks (Zhang et al., 2017). Functionalization of graphene allows fine-tuning of properties like electrical conductivity. Structural and chemical features of graphene materials are typically analyzed by Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). While Raman spectroscopy plays a critical role in identifying the presence of graphene and characterizing its structural defects (Pollard et al., 2017), XPS examines the chemistry of graphene. This study investigates three types of graphene materials — graphene (unfunctionalized, G-graphene), fluorine-functionalized graphene (F-graphene), and nitrogen-functionalized graphene (N-graphene) — across three physical forms: powders, suspensions, and embedded in inks. Functionalization was performed via plasma treatment of G-graphene with fluorine or ammonia gases. Suspensions were obtained by dispersing powders in distilled water, while inks were formulated using diacetone alcohol, carbon black, and graphene. Raman spectroscopy analysis confirmed the graphitic nature of all materials and revealed differences in defect density across different forms. The characteristic D, G, and D’ bands varied in relative intensity, offering insight into structural integrity and functionalization effects. XPS measurements examined core-level spectra (C 1s, F 1s, N 1s), revealing chemical bonding environments and hybridization states, including the sp² and sp³ states. A notable decline in fluorine content in F-graphene suspensions and inks, relative to powders, was observed. Existence of organic fluorine and total absence of metallic fluorine were observed. Raman spectroscopy and XPS data provided a correlated view of structural and chemical evolution through the graphene production chain. T2 - Joint Regulatory Risk Assessors Summit – Advancing Safety & Sustainability Assessments of Advanced Materials CY - Paris, France DA - 19.06.2025 KW - Graphene-related 2D materials (GR2M) KW - Inks KW - Raman Spectroscopy KW - XPS KW - Functionalized graphene PY - 2025 UR - https://macrame-project.eu/macrame-meetings-workshops/jointrras/#Agenda AN - OPUS4-63661 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Morpho-Chemical Characterisation of Me-TiO2 Nanoparticles for Enhanced Photocatalytical Activity N2 - The conversion of solar energy into electricity and solar fuels is of crucial importance for a green and sustainable future. Water splitting using semiconductor photo-catalysts is considered a sustainable method to produce clean hydrogen (H2) fuel. Nevertheless, H2 photo-production efficiency remains still low, although extensive research works to understand better the mechanisms of the Hydrogen Evolution Reaction (HER) and the Oxygen Evolution Reaction (OER) are being carried out. In this respect, TiO2 is a key photoactive material, usually employed with a co-catalyst deposited onto the surface to enhance charge carriers’ separation and catalyze surface charge transfer reactions. The deposition of a co-catalyst on the TiO2 nanoparticle surface represents one successful way to enhance the activity of the photocatalyst through a modification of its surface and redox properties. In this context, high-resolution scanning electron microscopy coupled with elemental analysis by energy-dispersive X-ray spectroscopy (EDS) is fundamental for studying and understanding the effect of the nanoparticle morphology on the functional properties of shape-controlled TiO2 crystals (bipyramides, platelets, and elongated particles). Different types of metal-semiconductor combinations, TiO2 shapes and dopant metals (Ag, Pt, etc) and metal concentrations will be discussed. T2 - ECASIA 2022 CY - Limerick, Ireland DA - 29.05.2022 KW - Titania nanoparticles KW - Photocatalysis KW - Scanning electron microscopy KW - Energy dispersive X-ray spectroscopy PY - 2022 AN - OPUS4-54977 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pellegrino, F. A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - Unveiling Order in Graphene Oxide Synthesis Through A Design of Experiment and Chemometric Strategy Based on Tour’s Method N2 - Graphene oxide (GO), a derivative of graphene containing oxygen functional groups, shows significant potential for a wide range of applications due to its unique electrical, mechanical, and chemical properties. Traditional synthesis methods, such as Tour's method, often rely on trial-and-error, leading to variations in product quality and yield. To address these challenges, we applied Design of Experiments (DoE) to systematically investigate the effects of key synthesis parameters, including reaction temperature, reaction time, and oxidant concentration. We identified the most significant factors influencing GO characteristics using a Plackett-Burman design and chemometric analysis. Our results highlight that the oxidation level is the most critical factor, impacting outcomes observed through various characterization techniques, such as UV-Vis spectroscopy and X-Ray Diffraction. Principal Component Analysis (PCA) and Multiple Linear Regression (MLR) provided insights into the synthetic parameters most strongly affecting material properties. While some findings aligned with expectations, others were counterintuitive. For instance, oxidation temperature had a minimal effect on the final material characteristics and may not need to be prioritized in the synthesis process. On the other hand, stirring was found to enhance the homogeneity of the material and promote more uniform oxidation. This study demonstrates the effectiveness of DoE in the controlled production of graphene oxide, offering a reliable framework for manufacturing high-quality GO tailored to specific applications. By minimizing time and resource consumption, this approach is increasingly relevant in the context of materials science, which demands higher quality, safety and sustainability standards. T2 - Joint Regulatory Risk Assessors Summit – Advancing Safety & Sustainability Assessments of Advanced Materials CY - Paris, France DA - 19.06.2025 KW - Graphene oxide KW - Chemometry KW - UV-Vis KW - XRD KW - XPS KW - EDX PY - 2025 UR - https://macrame-project.eu/macrame-meetings-workshops/jointrras/#Agenda AN - OPUS4-63676 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Terborg, R. A1 - Boehm, S. T1 - Analysis of elemental composition of Fe1-xNix and Si1-xGex alloy thin films by EPMA and µ-XRF N2 - The present study reports on measurements on thin Fe-Ni films on silicon and first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide Substrate by electron probe microanalysis (EPMA). Standard-based and standardless EPMA (with EDS) results were used in combination with the thin film analysis software Stratagem for the quantification. Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results. Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex alloy films obtained by different surface Analysis techniques, such as X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and secondary ion mass spectrometry (SIMS) applied in the depth-profiling operation mode. Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. An excellent agreement has been obtained between the atomic fractions determined by EPMA and µ-XRF with the KRISS certified values. T2 - Microscopy & Microanalysis 2019 CY - Portland, OR, USA DA - 03.08.2019 KW - Thin films KW - EPMA KW - µ-XRF KW - Elemental composition KW - Atomic fraction KW - Fe-Ni KW - Si-Ge PY - 2019 AN - OPUS4-48709 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cios, Grzegorz A1 - Hodoroaba, Vasile-Dan T1 - High throughput nanoparticle analysis using transmission Kikuchi diffraction N2 - In the present paper we show an approach of measuring large numbers of nanoparticles in a single scan TKD. TiO2 anatase nanoparticles (NP) of bipyramidal shape were deposited on standard carbon grid used for TEM. The procedure used promoted formation of NP ‘monolayer’ islands with uniform distribution of NPs on the carbon surface which allowed mapping of large number of nanoparticles in the single island. Collection of whole map covering ~2800 nanoparticles took nearly 20 minutes. Inverse pole figure color coded map indicates that the NPs are either lying on a {101} facet (within 10° range around perfect {101} parallel to the carbon surface orientation) on the carbon film or are lying on a {100} facet (within 10° range around the perfect {100} parallel to the carbon surface orientation). Very unlikely was the NP orientation standing on a {001} face. The NPs size distribution described as equivalent circle diameter (ECD) has been also evaluated and the mean NP ECD was 59 nm with standard deviation of 15 nm, i.e. in good agreement with electron microscopy or AFM results. This study shows high potential of the technique for crystalline NPs analysis with respect to geometrical orientation of the particles on the substrate. With known orientation, the 3D dimensional characterisation of such non-spherical NPs becomes possible from 2D projection electron micrographs. Moreover, the NP size distribution can be easily extracted. Superior accuracies down to 1-2 nm are achievable. The approach is applicable also on thin lamellae extracted from particulate (or mesoporous) layers. T2 - EMAS 2023 - 17th European Workshop on Modern Developmennts and Applications in Microbeam Analysis CY - Krakow, Poland DA - 07.05.2023 KW - Nanoparticles KW - TKD KW - Electron microscopy KW - TiO2 KW - Orientation PY - 2023 UR - https://www.microbeamanalysis.eu/events/event/60-emas-2023-17th-european-workshop-on-modern-developments-and-applications-in-microbeam-analysis AN - OPUS4-57519 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul A1 - Hodoroaba, Vasile-Dan T1 - Understanding Correlative Electron Microscopy Imaging with SEM, STEM in SEM and TEM for the Accurate Characterization of Size and Shape of FeOx Nanoparticles N2 - The recently certified reference material (CRM) BAM-N012 as cubical iron oxide FeOx nanoparticles (NPs) of 8 nm area equivalent square edge length (ESL) and the RM candidate BAM-N013 as nearly spherical NPs of 22 nm size were analyzed in detail by electron microscopy (EM). For the metrological characterization with SEM, STEM in SEM and TEM, the understanding of the imaging contrasts and sensitivities, and the correct interpretation of the (art)effects which are inherent to each detection mode is necessary. The same sample areas with NPs deposited on a TEM grid were analyzed by two SEM acquisition modes, i. e. SE InLens and STEM in SEM using a dedicated transmission sample holder, and further, correlatively, analyzed with TEM. With increasing kV, SE InLens shows increasing particle size (unless overcharging at the particle boundaries is filtered), as a known effect. For STEM-in-SEM the particle size decreases significantly and individual particles are identified easier (at 2 kV only a few single particles can be detected automatically). ❑ Documentation of the sample preparation and measurement conditions (including optimization process) is important for reproducibility. ❑ Plasma cleaning, analysis in the transmission mode at SEM is recommended for FeOx NPs. ❑ Selection of the threshold algorithm can significantly alter the reported ECD. T2 - Microscopy and Microanalysis 2024 CY - Cleveland, OH, USA DA - 28.07.2024 KW - Nanoparticles KW - Electron microscopy KW - Iron oxide KW - Reference materials KW - Correlative microscopy KW - Size and shape distribution PY - 2024 AN - OPUS4-60806 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Analysis of Particle Size Distribution for Bimodal Model Nanoparticles by Scanning Electron Microscopy N2 - The present study addresses the capability of measurement of relative particle number concentration by scanning electron microscopy for model bimodal silica and gold samples prepared in the frame of the European research project “nPSize - Improved traceability chain of nanoparticle size measurements” as candidate reference nanoparticles. T2 - Microscopy and Microanalysis 2020 CY - Online meeting DA - 03.08.2020 KW - Nanoparticles KW - Silica KW - Gold KW - Electron microscopy KW - Particle size distribution PY - 2020 AN - OPUS4-51112 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) provides a non-destructive approach in the dedicated thin film analysis mode with the commercial StrataGem software. Recently, the open-source programme BadgerFilm by Moy and Fournelle became available. Similarly to StrataGem, it is based on the algorithm of Pouchou and Pichoir and needs intensity ratios of the unknown sample and standards (k-values). We have evaluated the k-values measured for the FeNi and SiGe film systems using the BadgerFilm software package and compared the thickness and composition with the results obtained with the established StrataGem software and other reference methods. The thicknesses of the SiGe films obtained by the BadgerFilm software agree within 20% with the StrataGem and TEM results; the elemental compositions BadgerFilm-StrataGEM agree within 2% with one exception (9%). T2 - Microscopy and Microanalysis 2022 CY - Portland, OR, USA DA - 31.07.2022 KW - Thin films KW - Thickness KW - Elemental composition KW - FeNi KW - SiGe KW - BadgerFilm KW - Electron Probe Microanalysis (EPMA) PY - 2022 AN - OPUS4-55522 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Morphological Characterization and Chemical Identification of TiO2 Nanoparticles Doped with Ultrafine Metal Particles for Enhanced Photocatalytical Activity N2 - Water splitting using semiconductor photo-catalysts is considered a sustainable method to produce clean hydrogen fuel. Nevertheless, H2 photo-production efficiency remains still low, although extensive research works to understand better the mechanisms of the Hydrogen Evolution Reaction (HER) and the Oxygen Evolution Reaction (OER) are being carried out. In this respect, TiO2 is a key photoactive material, usually employed with a co-catalyst deposited onto the surface to enhance charge carriers’ separation and catalyze surface charge transfer reactions. The deposition of a co-catalyst on the TiO2 nanoparticle surface represents one successful way to enhance the activity of the photocatalyst through a modification of its surface and redox properties. In this context, high-resolution scanning electron microscopy (SEM) coupled with elemental analysis by energy-dispersive X-ray spectroscopy (EDS) is fundamental for studying and understanding the effect of the nanoparticle morphology on the functional properties of shape-controlled TiO2 crystals (bipyramides, platelets, and elongated particles). Different types of metal-semiconductor combinations, TiO2 shapes and dopant metals (Ag, Pt, Au, Rh, Pd) and metal concentrations are discussed. T2 - Microscopy and Microanalysis 2022 CY - Portland, OR, USA DA - 31.07.2022 KW - Nanoparticles KW - Me-TiO2 KW - Photocatalysis KW - Morpho-chemical characterization KW - Shape KW - SEM/EDS PY - 2022 AN - OPUS4-55541 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Towards 3D understanding of non spherical nanoparticles by Transmission Kikuchi Diffraction (TKD) for improved particle size distribution by electron microscopy N2 - In this paper one refined approach is applied to determine the exact orientation of bipyramidal TiO2 nanoparticles prepared with good dispersion as almost isolated particles on a carbon TEM grid. The advantages of the recently developed high-throughput Transmission Kikuchi Diffraction (TKD) are used to identify quickly and reliably the geometrical orientation of the crystalline TiO2 nanoparticle bipyramids (anatase) on a statistically relevant number of particles. T2 - Microscopy and Microanalysis 2020 CY - Online meeting DA - 03.08.2020 KW - Nanoparticles KW - Transmission Kikuchi Diffraction (TKD) KW - TiO2 KW - 3D KW - Electron microscopy PY - 2020 AN - OPUS4-51113 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 - 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 - CONF A1 - Mrkwitschka, Paul A1 - Hodoroaba, Vasile-Dan T1 - Wire-Print as a Novel Sample Preparation Approach for Accurate Morphological Characterization of Constituent Particles of Graphene-Related 2D-Materials N2 - Graphene and graphene-oxide (GO) are used for instance in catalysis, biomedical applications, in inks and as composite materials. To ensure product quality and safe-by-design principles within the various application fields, the commercial material must be characterized and specified through well-known and standardized procedures. The accurate morphological characterization of 2D materials is a challenging task, requiring careful sample preparation on a substrate either as a powder or from liquid suspension. These must be isolated, homogeneously distributed, with good statistics of the counted particles. Various sample preparation approaches have been reported in the literature, e.g. electrospray, substrate surface treatment, embedding the particulate material and polishing the cross-section, or addition of ligands to the suspended nanostructures. In this study, a novel deposition procedure for graphene-related 2D materials (GR2Ms) was systematically tested for its efficacy. The quantitative analysis of the size and shape distribution of the materials was conducted using electron microscopy and was successfully tested in XPS and EDS experiments. The technique is an extension of the conventional drop-casting method and has been designated "wire-print" deposition. The result of such a wire-print deposition for a graphene-based suspension is shown in Figure, where various treatment conditions have been tested with a repetition of up to 10 times per condition, all together 86 spots on a silicon wafer of 10 mm². T2 - Graphene Week 2025 CY - Vicenza, Italy DA - 22.09.2025 KW - Graphene-related 2D materials (GR2M) KW - Sample peparation KW - Imaging KW - Electron Microscopy KW - Wire-print deposition method PY - 2025 AN - OPUS4-64248 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Correlative chemical imaging to reveal the nature of different commercial graphene materials N2 - Different synthesis techniques were developed which led to other graphene-related materials such as graphene oxide (GO) or elemental-doped graphene. Further chemical functionalization can enhance but also alter or reduce specific properties of the graphene. To reveal the nature of these materials a proper physico‑chemical characterization with different analytical techniques is crucial. Single-layer GO flakes provided by Graphenea (Spain) were prepared for systematic image analysis. These flakes were disposed on an alignment-marked SiO2 substrate and correlatively imaged by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Raman spectroscopy. The high lateral resolution and/ or extreme surface sensitivity of the mentioned techniques is necessary to explore monolayers. The ToF-SIMS images match well with the SEM and AFM images and provide information about the chemistry. With 2D Raman spectroscopy it is possible to differentiate between the number of stacked single-layer flakes. This is visualized in a 3D image. Well-defined GO flakes could be used as a reference material for imaging of graphene-like structures but also of other types of 2D materials. In addition to these monolayer GO flakes, commercial graphene-containing inks (Haydale) with a more complex morphology were also correlatively imaged. ToF-SIMS and SEM images were merged to identify the origin of different chemical fragments. The findings correlate closely with the expectation that the specific functionalizations (with fluorine and nitrogen as marker elements) are present only on the graphene flakes as presumed from the SEM images. Energy-dispersive X-ray spectroscopy (EDX) supports these results, yet with a much lower sensitivity compared to ToF-SIMS. T2 - Joint Regulatory Risk Assessors Summit – Advancing Safety & Sustainability Assessments of Advanced Materials CY - Paris, France DA - 19.06.2025 KW - ToF-SIMS KW - Imaging KW - Graphene-related 2D materials KW - SEM/EDX KW - Auger electron spectroscopy KW - Raman spectroscopy PY - 2025 UR - https://macrame-project.eu/macrame-meetings-workshops/jointrras/#Agenda AN - OPUS4-63656 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - Knowledge Infrastructure supporting image-based characterisation of 2D graphene materials N2 - To better understand the relationship between image features and biological effects such as toxicity,we have developed a method combining image thresholding and pixel-wise segmentation to create annotated datasets. These datasets are used to train machine learning models and establish human–AI learning loops for material classification and structure detection. We employ deep learning architectures such as ResNet, EfficientNet, and U-Net to automate the classification and segmentation of SEM/TEM images of 2D nanomaterials, with targeted manual annotation focusing on key structures (graphene flakes, agglomerates, contaminants, etc.). This approach ensures reproducible, large-scale analysis, which is essential for studying the links between structure and biological response. Finally, our methodology aligns with OECD requirements and contributes to the Safe and Sustainable by Design (SSbD) framework, aiming to enhance product reliability and sustainability. T2 - Joint Regulatory Risk Assessors Summit – Advancing Safety & Sustainability Assessments of Advanced Materials CY - Paris, France DA - 19.06.2025 KW - Graphene KW - 2D materials KW - Knowledge infrastructure KW - Imaging KW - Machine learning PY - 2025 UR - https://macrame-project.eu/macrame-meetings-workshops/jointrras/#Agenda AN - OPUS4-63682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fernandez-Poulussen, D. A1 - Hodoroaba, Vasile-Dan T1 - Holistic, reliable and practical Characterization Framework for Graphene Family Materials, a correlated approach including Imaging based techniques N2 - ACCORDs is an Horizon Europe project working in the development of an imaging-based characterization framework (ACCORDs framework) for the holistic correlative assessment of Graphene Family Materials (GFMs) as a representative of 2D nanomaterials (NMs) to assess and predict 2D NMs health and environmental risks. The ACCORDs framework will operationalise safe and sustainable by design (SSbD) strategies proposed in past or ongoing H2020 projects or within OECD by correlating low-, medium-, and high-resolution physico-chemical-biological imaging-based methods with non-imaging methods in a tiered approach. ACCORDs will deliver the ACCORDs framework and user guidance, new imaging-based characterisation methods, reference in vitro tests, new reference 2D NMs for different matrices, a new minimum information reporting guideline for FAIR data sharing and reuse of images as well as an atlas with reference images for diagnostics of compromised safety of GFMs/GFM products. The new guidelines and standard proposals will be submitted to standardisation bodies to allow creation of regulatory ready products. The novelty of ACCORDs is in translating the principles of medical imaging-based diagnostics to 2D material hazard diagnostics. ACCORDs will accelerate industrial sectors in the area of aviation, marine construction, drone production, flexible electronics, photovoltaics, photocatalytics and print inks-based sensors. The value ACCORDs proposes to the graphene industry are practical, easy, imaging-based tools for GFM quality monitoring next to the production line with a possibility to be correlated with advanced highresolution imaging characterization methods in case hazard i.e. deviation from controls (benchmark values) are diagnosed. The ACCORDs framework and tools will contribute to the European Green Deal by addressing the topic: “Graphene: Europe in the lead” and to a new European strategy on standardization, released on 2nd February, 2022. T2 - MaterialsWeek 2024 CY - Limassol, Cyprus DA - 17.06.2024 KW - Graphene KW - Graphene-related 2D materials KW - SSbD KW - Imaging KW - ACCORDs PY - 2024 AN - OPUS4-60573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Towards Standardised Procedures for Morphology Measurement of 2D-Materials by Imaging N2 - The industry uptake of graphene-related 2D materials (GR2M) material increases, and international standardization is critical to enable commercialization. Reliable, accurate, and reproducible measurements are important due to the multiple production routes and producers of the material to maintain quality in manufacture. Several standards are under development within ISO/TC 229 ‘Nanotechnologies’, i.e. ISO/AWI TS 23879 “Structural characterization of graphene oxide flakes: thickness and lateral size measurement using AFM and SEM” or ISO DTS 23359 “Chemical characterization of graphene in powders and suspensions”, which focus on determining the dimensional and chemical properties of GR2M. Interlaboratory comparisons are required to develop best practice and understand the associated measurement uncertainties. In this contribution challenges and solutions for the accurate measurement of the lateral size of GR2M will be discussed based on the results of a recently completed interlaboratory comparison organized under the pre-standardisation platform of VAMAS (www.vamas.org/twa41/documents/2023_vamas_twa41_project13_GO_SEM.pdf). Aspects related to sample preparation, measurement conditions, and image analysis with different approaches to extract the corresponding size and shape descriptors will be presented. A discussion on the measurement uncertainty budget associated to the final result will be also included. T2 - Graphene Week 2025 CY - Vicenza, Italy DA - 22.09.2025 KW - Graphene-related 2D materials (GR2M) KW - Interlaboratory comparison KW - VAMAS KW - Lateral size KW - ISO/TC 229 Nanotechnologies PY - 2025 AN - OPUS4-64250 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -