TY - JOUR A1 - Obenlüneschloß, Jorit A1 - Boysen, Nils A1 - Rönnby, Karl A1 - Muriqi, Arbresha A1 - Hoffmann, Volker A1 - Abad Andrade, Carlos Enrique A1 - Rogalla, Detlef A1 - Brokmann, Ulrike A1 - Rädlein, Edda A1 - Nolan, Michael A1 - Devi, Anjana T1 - Rare Mononuclear Lithium-Carbene Complex for Atomic Layer Deposition of Lithium Containing Thin Films N2 - Lithium is the core material of modern battery technologies and fabricating the lithium‐containing materials with atomic layer deposition (ALD) confers significant benefits in control of film composition and thickness. In this work, a new mononuclear N‐heterocyclic carbene (NHC) stabilized lithium complex, [Li(tBuNHC)(hmds)], is introduced as a promising precursor for ALD of lithium‐containing thin films. Structural characterization is performed, comparing density functional theory (DFT) and single‐crystal X‐ray diffraction (SC‐XRD), confirming a rare mononuclear structure. Favorable thermal properties for ALD applications are evidenced by thermogravimetric analysis (TGA). The compound exhibits a low melting point, clean evaporation, and its volatility parameters are encouraging compared to other lithium precursors. ALD trials using [Li(tBuNHC)(hmds)] with ozone demonstrate its effectiveness in depositing LiSixOy films. The ALD process exhibits a saturated growth per cycle (GPC) of 0.95 Å. Compositional analysis using Rutherford backscattering spectrometry/nuclear reaction analysis (RBS/NRA), X‐ray photoelectron spectrometry (XPS), and glow discharge optical emission spectrometry (GD‐OES), confirms the presence of lithium and silicon in the expected ratios. This work not only presents a new ALD precursor but also contributes to the understanding of lithium chemistry, offering insights into the intriguing coordination chemistry and thermal behavior of lithium complexes stabilized by NHC ligands. KW - Atomic layer deposition (ALD) KW - N-heterocyclic carbene (NHC) ligands KW - Lithium ALD precursor chemistry KW - Mononuclear Li–carbene complex [Li(tBuNHC)(hmds)] KW - Li-silicate thin films (LiSixOy) KW - Thermal properties & TGA/volatility KW - Compositional analysis (RBS/NRA, XPS, GD-OES) PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643790 DO - https://doi.org/10.1002/anie.202513066 SN - 1433-7851 N1 - Es gibt eine parallele Sprachausgabe (deutsch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (German), a link is in the field related identifier SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim AN - OPUS4-64379 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Campos de Oliveira, Paula T1 - Advancing microstructural characterisation of ceramic cores for aerospace: from state-of-the-art to in-situ synchrotron X-ray computed tomography N2 - Ceramic cores are crucial for manufacturing turbine blades in aircraft engines, creating intricate cooling channels that improve engine efficiency and reduce emissions. During high-temperature casting, the cores undergo significant microstructural changes, including phase transitions, particle rearrangements, and porosity transformations, which can affect their properties and must be carefully controlled. State-of-the-art characterisation techniques for ceramic cores mostly rely on 2D methods, such as scanning and transmission electron microscopy. While valuable, these methods are limited in capturing the 3D complexity of the material. Advances in X-ray computed tomography (XCT) offer a more comprehensive perspective on 3D microstructures, but conventional XCT often lacks the resolution and in-situ capabilities to study microstructural evolution under casting conditions. Synchrotron XCT (SXCT) addresses these limitations, offering high spatial and temporal resolution with features down to 1 µm, enabling in-situ investigations. This study highlights the potential of SXCT, revealing previously unseen 3D microstructural features in ceramic cores, such as agglomeration, porosity evolution, surface reactions, microcracking, and particle orientation. These findings provide a more realistic view of dynamic changes during casting, advancing the understanding of core behaviour. Despite its advantages, SXCT is still rarely used in the field due to challenges such as limited access to synchrotron facilities and sample movement artifacts. Future developments, including high-temperature and vacuum compatible CT setups, could enhance this technique, leading to a better optimisation of ceramics performance. T2 - XIXth Conference of the European Ceramic Society (ECERS 2025) CY - Dresden, Germany DA - 31.08.2025 KW - Synchrotron KW - X-ray Computed Tomography KW - Ceramic core KW - Aerospace KW - Microstructure PY - 2025 AN - OPUS4-64050 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Morphological Analysis of Graphene Oxide by SEM and Correlative Field-Flow Fractionation Coupled with Multi-Angle Light Scattering N2 - Since the first free-standing monolayer graphene sheet was successfully prepared in 2004 [1], graphene and graphene oxide materials achieved the necessary technical readiness level to be considered for use in commercial products. Moreover, the focus has shifted from fundamental research towards expanding the applicability of graphene-related 2D materials (GR2M) and to improve their competitiveness with established materials [2]. Significant advances have been made especially in applications regarding optoelectronics, energy storage materials, chemical additives, sensor applications etc. [3]. Composite products containing graphene and functionalized graphene such as inks and dyes have shown enhanced performance regarding longevity, wettability, and can be tailored for specific purposes through dedicated functionalization. For accurate physico-chemical characterization, GR2M products in their raw form or as part of composites present challenges in terms of sample preparation, choice of analytical method and evaluation of data. For instance, in the context of imaging, these challenges encompass: (a) the selection of images magnifications being representative for all the flakes ranging in size from hundreds of nanometers to micrometers; (b) the selection of representative flakes for adequate statistics, which may involve the separation of overlapping/agglomerating flakes by segmentation; and (c) the classification of diverse morphologies such as irregularly shaped/crumpled flakes, porous flakes and particulate features present in the sample. The complexity of the analytical task has needed the introduction of specific ontology for 2D materials to identify the proper descriptors characterizing confidently the morphological features of interest. Regarding light scattering techniques such as Dynamic Light Scattering (DLS) and Multi-Angle Light Scattering (MALS) commonly used for process control in industry as a first measure, an alternative approach would be necessary. This is in part due to the use of the standard sphere-model for 2D materials as appearing to be inappropriate, whilst a disc-shape model potentially yields more suitable results. Standardization efforts are underway to establish a baseline for accurate characterization of aimed measurands with sufficient statistics. To date, the measurement methods recommended by standardization bodies for the morphological-structural characterization of GR2M’s are AFM, Raman Spectroscopy and SEM and/or TEM. The acquisition of statistically relevant numbers of flakes for a thorough characterization using TEM and AFM is particularly time-consuming. The size distribution of graphene oxide- and graphene-containing inks was investigated by using a correlative approach coupling Centrifugal Field-Flow Fractionation (CF3) [4] with MALS. Up to now, promising results for Field-Flow Fractionation have been achieved only with respect to the separation into size classes of GO samples as well as of graphene oxide mixed with graphene by Asymmetrical Field-Flow Fractionation (AF4) [5], [6]. Besides the online characterization by MALS, the eluting size fractions obtained by CF3 were also collected and subsequently measured by SEM. Successful separation into size fractions allows us to apply ensemble techniques such as MALS to samples that were previously not measurable according to best-practices. In this study, the following material sub-classes have been observed with SEM: (i) nano-graphite mixed with graphene flakes, (ii) graphene oxide few- and multi-layer flakes with diverse and highly complex morphology, and (iii) graphene oxide of well-defined size and shape with >95% single- and bilayer content were investigated. Data on the class size ranges was obtained by MALS after separation with CF3 and consideration of a disc-shape model. Significant effort was invested into the sample preparation for CF3 measurements to achieve a recovery rate of >80%, well above the recommended 70% by ISO/TS 21362:2018 for validation purposes. The material fractions collected after the CF3 measurement were separately deposited on a silicon wafer and the size results of the SEM analysis were correlated with the corresponding mean sizes obtained with MALS. T2 - Microscopy and Microanalysis 2025 CY - Salt Lake City, UTAH, USA DA - 27.07.2025 KW - Advanced Material KW - CF3 KW - SEM KW - Morphology PY - 2025 AN - OPUS4-64084 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Correlative chemical imaging to reveal the nature of different commercial graphene materials N2 - Different synthesis techniques were developed which led to other graphene-related materials such as graphene oxide (GO) or elemental-doped graphene. Further chemical functionalization can enhance but also alter or reduce specific properties of the graphene. To reveal the nature of these materials a proper physico‑chemical characterization with different analytical techniques is crucial. Single-layer GO flakes provided by Graphenea (Spain) were prepared for systematic image analysis. These flakes were disposed on an alignment-marked SiO2 substrate and correlatively imaged by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Raman spectroscopy. The high lateral resolution and/ or extreme surface sensitivity of the mentioned techniques is necessary to explore monolayers. The ToF-SIMS images match well with the SEM and AFM images and provide information about the chemistry. With 2D Raman spectroscopy it is possible to differentiate between the number of stacked single-layer flakes. This is visualized in a 3D image. Well-defined GO flakes could be used as a reference material for imaging of graphene-like structures but also of other types of 2D materials. In addition to these monolayer GO flakes, commercial graphene-containing inks (Haydale) with a more complex morphology were also correlatively imaged. ToF-SIMS and SEM images were merged to identify the origin of different chemical fragments. The findings correlate closely with the expectation that the specific functionalizations (with fluorine and nitrogen as marker elements) are present only on the graphene flakes as presumed from the SEM images. Energy-dispersive X-ray spectroscopy (EDX) supports these results, yet with a much lower sensitivity compared to ToF-SIMS. T2 - Joint Regulatory Risk Assessors Summit – Advancing Safety & Sustainability Assessments of Advanced Materials CY - Paris, France DA - 19.06.2025 KW - ToF-SIMS KW - Imaging KW - Graphene-related 2D materials KW - SEM/EDX KW - Auger electron spectroscopy KW - Raman spectroscopy PY - 2025 UR - https://macrame-project.eu/macrame-meetings-workshops/jointrras/#Agenda AN - OPUS4-63656 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Reliable analysis of the elemental composition of graphene oxide flakes with energy dispersive spectroscopy (SEM/EDS) and x-ray photoelectron spectroscopy (XPS) N2 - Suspensions of graphene-related 2D materials (GR2M) are broadly used for further applications like printable electronics. The reliable quantification of the composition of graphene-related 2D materials as liquid suspensions is still a challenging task, which can hinder the commercialisation of the products. Specific parameters to be measured are defined, e.g. the oxygen-to-carbon (O/C) concentration ratio, the trace metal impurities, or the functional groups present [1], but reference protocols are still missing. One of the central methods for the quantification is X-ray photoelectron spectroscopy (XPS) as a rather expensive method. Therefore, the development of cheaper alternatives is highly desired. One attractive alternative of XPS is energy-dispersive spectroscopy (EDS) which is usually coupled with scanning electron microscopy (SEM). This combination is one of the most widely used methods in analytical laboratories. In this contribution the results of a systematic study on the capability of SEM/EDS to reliably quantify the O/C ratio in a well-defined and well-characterized graphene oxide material [2] are presented. The robustness of the SEM/EDS results obtained at various measurement conditions (various excitation energies) is tested by comparing the results to the established XPS analysis [3], which has been carried out on the same samples. It is demonstrated that for samples prepared by drop-casting on a substrate, both surface-sensitive XPS analysis and bulk-characterising EDS result in very similar elemental composition of oxygen and carbon for thick spots. Further, the effect of untight deposited material enabling co-analysis of the (silicon) substrate, is evaluated for both methods, XPS and EDS. The last results clearly show the influence of the substrate on the analysis of the results and stressed out the importance of the sample preparation. T2 - E-MRS Spring Meeting CY - Strasbourg, France DA - 26.05.2025 KW - Graphene oxide KW - Reliable Analysis KW - Ionic Liquid KW - Reference Material PY - 2025 AN - OPUS4-63336 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Liaison report from VAMAS/TWA 37 Quantitative Microstructural Analysis to ISO/TC 202 Microbeam Analysis N2 - The liaison between VAMAS/TWA 37 Quantitative Microstructural Analysis and other TWAs to ISO/TC 202 Microbeam Analysis since the last Annual Meeting of ISO/TC 202 is reported. The VAMAS/TWA 37 projects initiated in the last year and the new ones in the planing phase are highlighted with technical and organisational details. Also need for more participants in 2 projects is discussed. T2 - 32nd Plenary Meeting of ISO/TC 202 Microbeam Analysis CY - London, United Kingdom DA - 28.10.2025 KW - VAMAS KW - Quantitative microstructural analysis KW - ISO KW - Standardisation KW - Interlaboratory comparisons PY - 2025 AN - OPUS4-64552 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - Knowledge Infrastructure supporting image-based characterisation of 2D graphene materials N2 - To better understand the relationship between image features and biological effects such as toxicity,we have developed a method combining image thresholding and pixel-wise segmentation to create annotated datasets. These datasets are used to train machine learning models and establish human–AI learning loops for material classification and structure detection. We employ deep learning architectures such as ResNet, EfficientNet, and U-Net to automate the classification and segmentation of SEM/TEM images of 2D nanomaterials, with targeted manual annotation focusing on key structures (graphene flakes, agglomerates, contaminants, etc.). This approach ensures reproducible, large-scale analysis, which is essential for studying the links between structure and biological response. Finally, our methodology aligns with OECD requirements and contributes to the Safe and Sustainable by Design (SSbD) framework, aiming to enhance product reliability and sustainability. T2 - Joint Regulatory Risk Assessors Summit – Advancing Safety & Sustainability Assessments of Advanced Materials CY - Paris, France DA - 19.06.2025 KW - Graphene KW - 2D materials KW - Knowledge infrastructure KW - Imaging KW - Machine learning PY - 2025 UR - https://macrame-project.eu/macrame-meetings-workshops/jointrras/#Agenda AN - OPUS4-63682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - In depth analysis of commercial functionalized graphene nanoplateles towards structure-activity relationships N2 - The analysis of commercial graphene related products from the raw material to inks is discussed and the input to structure-activity relationships. Different approaches to obtain structure-activity relationships like operando or using data mining are presented. Challenges and recommendation to obtain structure-activity relationships are given. T2 - Joint Regulator Risk Summit: Advancing Safety & Sustainability Assessments of Advanced Materials CY - Paris, France DA - 19.06.2025 KW - Functionalized graphene KW - Structure activity relationsships KW - Commercialisation PY - 2025 AN - OPUS4-63565 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chemello, Giovanni A1 - Despotelis, Konstantinos A1 - Paton, Keith A1 - Clifford, Charles A A1 - Pollard, Andrew A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Approaches for the measurement of lateral dimensions of graphene oxide flakes using scanning electron microscopy N2 - There is a practical need, especially from the industrial community, to accurately measure the size and shape of graphene oxide (GO) flakes of commercial origin, in a reliable, simple, and unambiguous way. The sample preparation is a decisive step to obtain a homogeneous distribution of flakes on a substrate, which is suitable for image analysis. A certain level of inhomogeneity was still found but could be accepted for the purpose of this lateral size measurement study. A measurement procedure for Scanning Electron Microscopy (SEM) including sample preparation, measurement, image analysis and reporting was developed and validated to be applied for the lateral size analysis of “real-world” 2D flakes. Samples were produced for analysis by drop casting GO dispersions onto Si/SiO2 substrates. After SEM imaging, the images were analysed using two approaches to derive size and shape parameters. The influence of different operators has been evaluated. A maximum difference of 10% for the size descriptor and 2% for shape descriptor was found for both image analysis approaches when different samples of the same source material are measured and analysed by the same operator, hence indicating variability caused by sample preparation and analysing different sample areas. When different laboratories/operators perform the image analysis on exactly the same images and same flakes, the deviation found for the size descriptor is 2% and 4.6% corresponding to the two approaches applied, while no difference in the shape descriptor is observed. KW - Graphene oxide KW - SEM KW - Lateral dimension KW - Standardisation KW - Imaging PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625070 DO - https://doi.org/10.1088/2632-959X/adae28 VL - 6 IS - 1 SP - 1 EP - 11 PB - IOP Publishing AN - OPUS4-62507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madbouly, Loay Akmal A1 - Mrkwitschka, Paul A1 - Stockmann, Jörg Manfred A1 - Jones, Elliot A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Comparative Elemental Analysis of Commercial Functionalized Graphene Nanoplatelets Along the Production Chain With X‐Ray Photoelectron and Energy‐Dispersive X‐Ray Spectroscopy N2 - Graphene has been commercialized for over a decade, primarily in the form of suspensions and inks. In this study, we investigate the properties of graphene nanoplatelets (GNPs) and their functionalized derivatives, incorporating fluorine or nitrogen as functional groups (FG). The analysis was conducted on three forms, that is, powders, suspensions, and inks, using X‐ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) with energy‐dispersive X‐ray spectroscopy (EDX). The objective of this work is to establish a rapid and comprehensive systematic approach for elemental analysis of commercial functionalized graphene, which can be used for quality control. Functionalization is employed to tailor the material's physical and chemical properties. In our study, graphene samples, functionalized with fluorine or ammonia in a plasma reactor, were investigated. Both XPS and EDX were applicable for all three forms and showed, in general, similar trends between the three forms, so that both XPS and EDX can be used for quality control of GNPs along the production chain. KW - Commercial graphene KW - Functionalized graphene KW - Graphene inks KW - SEM/EDS KW - XPS PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625752 DO - https://doi.org/10.1002/sia.7386 SN - 1096-9918 SP - 1 EP - 7 PB - Wiley AN - OPUS4-62575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - John, Elisabeth A1 - Weise, Matthias A1 - Radnik, Jörg A1 - Stockmann, Jörg Manfred A1 - Lange, Thorid A1 - Sahre, Mario A1 - Hodoroaba, Vasile-Dan T1 - Towards a New Reference Material—Analytical Challenges in Examining High-Entropy Alloy Thin Films N2 - A new high-entropy alloy (HEA) consisting of titanium, chromium, manganese, iron, and nickel was deposited as a thin-film on silicon substrates using magnetron sputtering from a novel segmented target composed of metal stripes. This material was explored with the goal to create a new reference material for surface analysis and evaluation of complex composite materials. The film's morphology was initially characterized by scanning electron microscopy (SEM), followed by crystallographic analysis using X-ray diffraction (XRD) and selected area electron diffraction (SAED). The two-dimensional compositional homogeneity was assessed using a combination of scanning and transmission electron microscopy (TEM) with energy-dispersive spectroscopy (EDS), X-ray fluorescence (XRF), time-of-flight secondary ion mass spectrometry (ToF-SIMS), and X-ray photoelectron spectroscopy (XPS). The in-depth chemical composition was further analysed using ToF-SIMS and Auger electron spectroscopy (AES). Our findings demonstrate that it is possible to produce thin HEA films with a homogeneous in-depth composition from a segmented target. Notably, despite the fixed composition of the target, we were able to vary the HEA's composition by exploiting inhomogeneities within the magnetrons sputter plasma. Additionally, we successfully created HEA films with significant compositional gradients. T2 - ECASIA CY - Gothenburg, Sweden DA - 10.06.2024 KW - Reference material KW - High-entropy alloy KW - Thin-films PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625777 DO - https://doi.org/10.1002/sia.7387 SN - 1096-9918 SP - 1 EP - 8 PB - Wiley AN - OPUS4-62577 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dumit, Verónica I. A1 - Furxhi, Irini A1 - Nymark, Penny A1 - Afantitis, Antreas A1 - Ammar, Ammar A1 - Amorim, Monica J. B. A1 - Antunes, Dalila A1 - Avramova, Svetlana A1 - Battistelli, Chiara L. A1 - Basei, Gianpietro A1 - Bossa, Cecilia A1 - Cimpan, Emil A1 - Cimpan, Mihaela Roxana A1 - Ciornii, Dmitri A1 - Costa, Anna A1 - Delpivo, Camilla A1 - Dusinska, Maria A1 - Fonseca, Ana Sofia A1 - Friedrichs, Steffi A1 - Hodoroaba, Vasile-Dan A1 - Hristozov, Danail A1 - Isigonis, Panagiotis A1 - Jeliazkova, Nina A1 - Kochev, Nikolay A1 - Kranjc, Eva A1 - Maier, Dieter A1 - Melagraki, Georgia A1 - Papadiamantis, Anastasios G. A1 - Puzyn, Tomasz A1 - Rauscher, Hubert A1 - Reilly, Katie A1 - Jiménez, Araceli Sánchez A1 - Scott‐Fordsmand, Janeck J. A1 - Shandilya, Neeraj A1 - Shin, Hyun Kil A1 - Tancheva, Gergana A1 - van Rijn, Jeaphianne P. M. A1 - Willighagen, Egon L. A1 - Wyrzykowska, Ewelina A1 - Bakker, Martine I. A1 - Drobne, Damjana A1 - Exner, Thomas E. A1 - Himly, Martin A1 - Lynch, Iseult T1 - Challenges and Future Directions in Assessing the Quality and Completeness of Advanced Materials Safety Data for Re‐Usability: A Position Paper From the Nanosafety Community N2 - Ensuring data quality, completeness, and interoperability is crucial for progressing safety research, Safe‐and‐Sustainable‐by‐Design approaches, and regulatory approval of nanoscale and advanced materials. While the FAIR (Findable, Accessible, Interoperable, and Re‐usable) principles aim to promote data re‐use, they do not address data quality, essential for data re‐use for advancing sustainable and safe innovation. Effective quality assurance procedures require (meta)data to conform to community‐agreed standards. Nanosafety data offer a key reference point for developing best practices in data management for advanced materials, as their large‐scale generation coincided with the emergence of dedicated data quality criteria and concepts such as FAIR data. This work highlights frameworks, methodologies, and tools that address the challenges associated with the multidisciplinary nature of nanomaterial safety data. Existing approaches to evaluating the reliability, relevance, and completeness of data are considered in light of their potential for integration into harmonized standards and adaptation to advance material requirements. The goal here is to emphasize the importance of automated tools to reduce manual labor in making (meta)data FAIR, enabling trusted data re‐use and fostering safer, more sustainable innovation of advanced materials. Awareness and prioritization of these challenges are critical for building robust data infrastructures. KW - Advanced materials KW - Safety data KW - Re-usability KW - Nanosafety KW - SSbD KW - FAIR KW - Standardisation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652918 DO - https://doi.org/10.1002/adsu.202500567 SN - 2366-7486 SP - 1 EP - 18 PB - Wiley-VCH CY - Weinheim AN - OPUS4-65291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Towards Standardised Procedures for Morphology Measurement of 2D-Materials by Imaging N2 - The industry uptake of graphene-related 2D materials (GR2M) material increases, and international standardization is critical to enable commercialization. Reliable, accurate, and reproducible measurements are important due to the multiple production routes and producers of the material to maintain quality in manufacture. Several standards are under development within ISO/TC 229 ‘Nanotechnologies’, i.e. ISO/AWI TS 23879 “Structural characterization of graphene oxide flakes: thickness and lateral size measurement using AFM and SEM” or ISO DTS 23359 “Chemical characterization of graphene in powders and suspensions”, which focus on determining the dimensional and chemical properties of GR2M. Interlaboratory comparisons are required to develop best practice and understand the associated measurement uncertainties. In this contribution challenges and solutions for the accurate measurement of the lateral size of GR2M will be discussed based on the results of a recently completed interlaboratory comparison organized under the pre-standardisation platform of VAMAS (www.vamas.org/twa41/documents/2023_vamas_twa41_project13_GO_SEM.pdf). Aspects related to sample preparation, measurement conditions, and image analysis with different approaches to extract the corresponding size and shape descriptors will be presented. A discussion on the measurement uncertainty budget associated to the final result will be also included. T2 - Graphene Week 2025 CY - Vicenza, Italy DA - 22.09.2025 KW - Graphene-related 2D materials (GR2M) KW - Interlaboratory comparison KW - VAMAS KW - Lateral size KW - ISO/TC 229 Nanotechnologies PY - 2025 AN - OPUS4-64250 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eggert, Claudia A1 - Hodoroaba, Vasile-Dan T1 - Welcome and Introduction N2 - Nanotechnology has emerged over the past decade as a key field involving the design, characterization, production, and application of materials, structures, devices, and systems at the nanometer scale. Due to their large specific surface area and significant surface chemistry, nanomaterials offer enhanced material properties and product functionalities. However, alongside these advancements comes the potential risk to humans and the environment. The development of nanomaterials has provided new opportunities to understand matter at the nanoscale, accelerating the creation of innovative advanced materials and devices. The expertise gained in the standardization and regulation of nanomaterials, particularly in characterizing nanoparticulate matter, should be applied to other innovative advanced materials, such as (nano)composites, 2D structures, additive manufactured materials, gels, and foams. Initial guidance for the safe-and-sustainable-by-design (SSbD) development of advanced materials during the early innovation phase has been introduced by various groups and projects. Additionally, digital material passports (DMP) and digital product passports (DPP) need to be defined and implemented uniformly across Europe. In 2024, the Innovative Advanced Materials Initiative (IAM-I) was launched by European stakeholders to contribute to a "Research and Innovation ecosystem that will significantly accelerate the time-to-market of sustainable innovative advanced materials (IAMs) and associated technologies designed for a digital circular economy." Knowledge transfer is a crucial pillar of this ecosystem, and a future IAM-I Academy could be a valuable tool. Initially, it is essential to define "education & training needs to boost Europe’s competitiveness and sovereignty within the area of IAM." T2 - Nano and Beyond - What can we learn from Nano for other Innovative Advanced Materials? CY - Online meeting DA - 04.07.2025 KW - Advance Materials KW - Nanomaterials KW - IAM-I KW - SSbD KW - DMP KW - DPP PY - 2025 UR - https://www.bam-akademie.de/kursangebot/kurs/webinar-nano-and-beyond-55.html?lang=en AN - OPUS4-63690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Advanced physico-chemical Characterisation & Correlation of Results with different Methods for GFMs N2 - An accurate characterisation of the morphological, structural, and chemical properties of nano and advanced materials is key for the understanding of the material functionality and constitutes the basis for future optimisation or even prediction of the product performance. Further, the correlation of the physical-chemical properties with results from biological testing leads to an understanding of the potential toxicological effects so that a minimisation of the materials risks becomes possible. The presentation will highlight with examples the importance of the selection of the relevant parameters/descriptors and particularly their measurement for the reliable characterisation of the morphology, structure, and chemistry of graphene-related 2D-materials (GR2M’s) [1-3]. One crucial aspect is also one of most challenging ones in the characterisation chain: the proper sample preparation, which shall be tailored to the accurate measurement of the defined analytical parameter. Practical examples of measurement of morphological descriptors of GR2M’s, such as equivalent circular diameter (ECD), minimum and maximum Feret, and aspect ratio with electron microscopy, or of the thickness with atomic force microscopy (AFM) will be showed, together with quantitative chemical characterisation with X-ray photoelectron spectroscopy (XPS) and, newly, with energy-dispersive X-ray spectroscopy with a scanning electron microscope (SEM/EDX) [4] by evaluating accurately the elemental content as the ratio of O/C and the composition of impurities. Another relevant, but challenging part of the characterisation of GR2M’s, particularly as the final products containing mostly low amounts of GR2M’s, is the analysis of homogeneity of the chemical composition by sensitive imaging methods. Examples of successful analysis with secondary ion mass spectrometry (SIMS), even if not quantitative, will be presented. T2 - Joint online Workshop: Harmonisation & Standardisation of Test Methods for Nano- and Advanced Materials CY - Paris, France DA - 19.06.2025 KW - Physico-chemical characterisation KW - Graphene-related 2D materials KW - OECD KW - Standardisation KW - GO flakes PY - 2025 UR - https://macrame-project.eu/macrame-meetings-workshops/ws_hamonisation_standardisation_2023/ AN - OPUS4-63557 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Measurement of the Lateral Size of Graphene Oxide Flakes by SEM N2 - The progress of the VAMAS interlaboratory comparison Project P13 "Lateral size of graphene oxide flakes by SEM" within the Technical Working Area 41 "Graphene and Related 2D Materials" is presented. The challenges at sample preparation on substrates for accurate measurement and image analysis as well as two different analysis approaches, containing exact guidance how to measure the main descriptors for the lateral size measurement of the imaged graphene oxide flakes with Scanning Electron Microscopy are highlighted. The size and shape distributions as measured by 17 laboratories are showed expressed in size and shape descriptors extracted from SEM images by using two proposed measurement approaches. The implementation of the results into the corresponding ISO technical specification AWI/TS 23879 is discussed and planned, in relation with the AFM part. T2 - ISO/TC 229 Nanotechnologies Meeting Week CY - Stockholm, Sweden DA - 19.05.2025 KW - Graphene oxide KW - Interlaboratory comparison KW - SEM KW - Lateral size KW - VAMAS KW - ISO/TC 229 Nanotechnologies PY - 2025 AN - OPUS4-63189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - The next steps in the standardisation of graphene-related and other 2D materials (GR2M) N2 - The first products with graphene-related 2D material (GR2M) are on the market. In this phase trust is essential for the commercial success of these products, between the individual partners of the product value chain, and between the manufacturer and the consumer. Standards are an important tool for building this trust. The first steps have been taken in standardisation, e.g. in terminology and the characterization of raw materials. But there are still some challenges to overcome such as bringing the standards to the factory floor and real-world products. For the validation of new protocols and methods there is a need of reference data and materials. But not only the measurement should be reproducible, the whole analytical workflow from sample storage and preparation to data analysis should be reproducible. Another important issue is the establishment of credible structure-activity relationships which allows the prediction of the properties of the GR2M, but also of the biological activity including the safety for the human health and the environment. Such relationships can be used for read-across and grouping and can facilitate the regulation of the advanced materials. In addition, 2D materials beyond graphene should also be considered and can benefit from the experience from the standardisation of graphene and graphene oxide. T2 - Nanomaterials Standardization Strategy Forum - Europe - Republic of Korea CY - Online meeting DA - 08.07.2025 KW - Commercialisation KW - Product-value chain KW - Confidence building PY - 2025 AN - OPUS4-63731 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Standardized Chemical Composition Analysis of Graphene Oxide Flakes with SEM/EDS and XPS Works Reliably N2 - Reliable quantification of the chemical composition of graphene-related 2D materials as powders and liquid suspensions is a challenging task. Analytical methods such as XPS, ICP-MS, TGA and FTIR are recommended to be used in ongoing projects at standardization bodies. The specific parameters to be measured are also defined, e.g. the oxygen-to-carbon (O/C) concentration ratio, the trace metal impurities, or the functional groups present [1]. In this contribution, for the first time, the results of a systematic study on the capability of SEM/EDS to reliably quantify the O/C ratio in a well-defined and well-characterized graphene oxide material [2] are presented. It is expected that the quantitative EDS analysis of light elements emitting characteristic X-ray lines below 1 keV to be provided with significantly larger measurement uncertainties than the analysis of elements with an atomic number of 11 (Na) or above [3]. The robustness of the SEM/EDS results obtained at various measurement conditions (various excitation energies) is tested by comparing the results to the established XPS analysis [4], which has been carried out on the same samples. A crucial step in sample preparation from liquid suspension with graphene oxides flakes onto a substrate for analysis with both XPS and EDS. It is demonstrated that if a closed and enough thick drop-cast deposited spot is succeeded to be deposited on a substrate, both surface-sensitive XPS analysis and bulk-characterizing EDS result in very similar elemental composition of oxygen and carbon. Hence, theoretical, expected O/C atomic ratio values for pure graphene oxide of ~0.5 [1] are achieved (with both methods), see Figure 1. Further, the effect of untight deposited material enabling co-analysis of the (silicon) substrate, is evaluated for both methods, XPS and EDS. To note that all the EDS results in this study have been quantified standardless. The effect of the variation of beam voltage on the result of the quantification of the O/C ratio is shown in Figure 2. No clear tendency is visible by varying the kV, which is a confirmation of the quality of the standardless analysis at the used EDS spectrometer. The results of this study demonstrate the reliability of the reference measurement protocol for SEM/EDS to be introduced into ISO/DTS 23359, including the dedicated sample preparation, particularly for the cases when the concentration of the GO flakes in stock liquid suspension is low. Further, also the consideration of this GO material as one of the very few available as a commercial material on the market as the very first GO reference material with regard to its morphology as well as chemical composition. Both the standard measurement procedure and the candidate reference material will immensely contribute to characterise reliably the chemical composition of graphene-related 2D materials with SEM/EDS as one of the most widely used methods in analytical laboratories. T2 - Microscopy and Microanalysis 2025 CY - Salt Lake City, UTAH, USA DA - 27.07.2025 KW - Graphene oxide flakes KW - SEM/EDS KW - XPS KW - O/C ratio KW - Impurities PY - 2025 AN - OPUS4-64085 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Physical-chemical Characterization of Graphene-Related 2D Materials: Development of Approaches for Reliable Quantification N2 - An accurate characterisation of the morphological, structural, and chemical properties of nano and advanced materials is key for the understanding of the material functionality and constitutes the basis for future optimisation or even prediction of the product performance. Further, the correlation of the physical-chemical properties with results from biological testing leads to an understanding of the potential toxicological effects so that a minimisation of the materials risks becomes possible. The presentation will highlight with examples the importance of the selection of the relevant parameters/descriptors and particularly their measurement for the reliable characterisation of the morphology, structure, and chemistry of graphene-related 2D-materials (GR2M’s) [1-3]. One crucial aspect is also one of most challenging ones in the characterisation chain: the proper sample preparation, which shall be tailored to the accurate measurement of the defined analytical parameter. Practical examples of measurement of morphological descriptors of GR2M’s, such as equivalent circular diameter (ECD), minimum and maximum Feret, and aspect ratio with electron microscopy, or of the thickness with atomic force microscopy (AFM) will be showed, together with quantitative chemical characterisation with X-ray photoelectron spectroscopy (XPS) and, newly, with energy-dispersive X-ray spectroscopy with a scanning electron microscope (SEM/EDX) [4] by evaluating accurately the elemental content as the ratio of O/C and the composition of impurities. Another relevant, but challenging part of the characterisation of GR2M’s, particularly as the final products containing mostly low amounts of GR2M’s, is the analysis of homogeneity of the chemical composition by sensitive imaging methods. Examples of successful analysis with secondary ion mass spectrometry (SIMS), even if not quantitative, will be showed. T2 - SaferWorldbyDesign Webinars CY - Online meeting DA - 25.03.2025 KW - Graphene-related 2D materials KW - Standardisation KW - Interlaboratory comparison KW - Physico-chemical characterisation PY - 2025 UR - https://saferworldbydesign.com/webinars/ AN - OPUS4-62791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Quantitative EDS analysis on graphene related 2D materials N2 - The elemental analysis of solid matter by means of the Energy-Dispersive X-Ray Spectrometry (EDS) is meanwhile posible as a quick (seconds!) and more and more accurate analysis via standardsless (instantaneous) quantification. The sensitivity & quantification accuracy for light elements (C, O,..) has significantly increased in the recent years. The availability via table-top SEMs with incorporated EDS is also enhanced. Further, the EDS analysis at an SEM is well-standardized, see ISO/TC 202 Microbeam Analysis & VAMAS/ TWA 37 Quantitative Microstructural Analysis in good liaisonships with ISO/TC 229 Nanotechnologies. It is demostrated that key parameters such as oxygen-to-carbon atomic-% ratio and impurities can be realibly measured, with XPS as a reference method. Various EDS spectrometers and analysis conditions are tested and the validity of the EDS quantification of an ionic liquid of well-defined chemical composition is demonstrated. Next steps are to launch a corresponding VAMAS interlaboratory comparison and to discuss within ISO/TC 229 towards inclusion of EDS as a routine method for the elemental analysis of GR2M into the ISO/TS 23359 Nanotechnologies — Chemical characterization of GR2Ms in powders and suspensions. T2 - Annual Microscopy Community Meeting for the National Research Council in Canada CY - Online meeting DA - 18.11.2025 KW - Graphene-related 2D materials (GR2M) KW - Elemental analysis KW - Light elements KW - SEM/EDS KW - Standardisation PY - 2025 AN - OPUS4-64766 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -