TY - INPR A1 - Devi, Sarita A1 - Riedel, Soraya A1 - Döring, Sarah A1 - Hiller, Lukas A1 - Flemig, Sabine A1 - Singh, Chandan A1 - Konthur, Zoltán A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf T1 - Antibodies Functionalized Magnetic Fe-Metal-Organic Framework Based Biosensor for Electrochemical Detection of Tetanus NeuroToxin N2 - This work presents a MOF-integrated microfluidic flow-cell based immunodetection of the tetanus toxoid (TT) using electrochemical technique for the first time. Metal-organic frameworks (MOFs) are coordination polymers, and composed of a metal center and organic linkers. Several synthesis methods have been reported to achieve the desired properties in MOFs. In this work, we report the hydrothermal synthesis of a magnetic and conductive iron-based MOF (Fe-MOF) which was utilized to develop a biosensor in conjugation with the human monoclonal antibody SA13 against TT (anti-TT mAb) for the detection of the tetanus neurotoxin (TeNT). The one-pot synthesis of this magnetic and conductive Fe-MOF was performed in a hydrothermal reactor (108℃) using the Fe3+/Fe2+ precursors as 1.2/1 mmol and dual ligands, i.e., tetrahydroxy-1,4-benzoquinone and 2-aminobenzene-1,4-dicarboxylic acid. The Fe-MOF was characterized using XRD, DLS, FTIR, and electron microscopy. The Fe-MOF was further conjugated with L-phenylalanine (pH 8.6) to increase the electric conductivity of the Fe-MOF (Fe-MOF/Phe) on the screen-printed gold electrode as studied by cyclic voltammetry (CV). The anti-TT mAb was conjugated on the Fe-MOF/Phe surface with the help of ethylenediamine (Fe-MOF/Phe/EDA/anti-TT mAb) delivered good binding affinity for the TT antigen revealing the applicability of this biosensor for TT detection by CV. The limit of detection of the Fe-MOF/Phe/EDA/anti-TT mAb-based biosensor for TT was 9.4 ng/ml in spiked buffer. There is negligible cross-reactivity in the presence of bovine serum albumin. This study shows the applicability of magnetic MOFs in the detection of various other microbial toxins or other biomolecules. KW - Magnetic Metal-Organic Framework KW - Tetanus toxoid KW - L-phenylalanine KW - Antibody KW - Label-free detection KW - Electrochemical immunosensor PY - 2024 DO - https://doi.org/10.2139/ssrn.4935745 SP - 1 EP - 48 PB - Elsevier Inc. AN - OPUS4-62196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Challenges in Correlative imaging of Advanced Materials N2 - Newly developed methodical approaches with an emphasis on correlative imaging analysis of morphology and chemistry of nanomaterials will be presented. Correlative imaging by high-resolution SEM with STEM-in-SEM as well as with EDS, and further with AFM, or with the new technique TKD (Transmission Kikuchi Diffraction) will be explained on various examples of nanostructures, both as starting materials and as embedded/functionalized nanoparticles in products. The unique analytical benefits of the Auger electron probe as a veritable nano-tool for the local surface chemistry will be highlighted. Examples of hybrid analysis of the bulk of nanomaterials by X-ray Spectroscopy and the highest surface-sensitive methods XPS and ToF-SIMS as advanced surface characterization methods available in the Competence Centre nano@BAM will be showed. Particularly for the spatially resolved analysis of the chemistry of nanostructures, such in-depth and lateral gradients of chemistry within mesoporous thin layers, or the completeness of the shells of core-shell nanoparticles, the latter methods are inherent. Other dedicated developments like approaches for the quantitative determination of the porosity of thin mesoporous layers by electron probe microanalysis (EPMA) with SEM or the quantitative determination of the roughness of particle surface by high-resolution imaging with electron microscopy will be also presented. T2 - Workshop: Harmonisation & Standardisation of Test Methods for Nano- and Advanced Materials CY - Online meeting DA - 18.11.2024 KW - Imaging KW - Advanced materials KW - Correlative imaging KW - Nanomaterials KW - Electron microscopy KW - ToF-SIMS PY - 2024 UR - https://macrame-project.eu/macrame-meetings-workshops/2nd-joint-online-workshop-harmonisation-standardisation-of-test-methods-for-nano-and-advanced-materials/ AN - OPUS4-61858 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Rossi, Andrea A1 - Alladio, Eugenio A1 - Drobne, Damjana A1 - Hodoroaba, Vasile-Dan A1 - Jurkschat, Kerstin A1 - Kononenko, Veno A1 - Madbouly, Loay Akmal A1 - Mrkwitschka, Paul A1 - Novak, Sara A1 - Radnik, Jörg A1 - Saje, Špela A1 - Santalucia, Rosangela A1 - Sordello, Fabrizio A1 - Pellegrino, Francesco T1 - Publisher correction: Development of a one-pot synthesis of rGO in water by optimizing Tour’s method parameters N2 - This is a publisher's correction to the original article "Development of a one-pot synthesis of rGO in water by optimizing Tour’s method parameters" that was published online on 27th September 2024 in "Scientific reports" (DOI: 10.1038/s41598-024-73606-2). PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-617590 DO - https://doi.org/10.1038/s41598-024-77468-6 SN - 2045-2322 VL - 14 IS - 1 SP - 1 PB - Springer Nature CY - London AN - OPUS4-61759 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stockmann, Jörg Manfred A1 - Radnik, Jörg A1 - Bütefisch, Sebastian A1 - Weimann, Thomas A1 - Hodoroaba, Vasile-Dan T1 - A New XPS Test Material for More Reliable Analysis of Microstructures N2 - A reference material is required for small‐area XPS because it has been used more frequently for surface control in recent years and many operators use incorrect field of views. To address this problem, we developed a test material starting in 2019. We optimised this XPS test material dedicated to the control of analysis position on the sample, with respect to the following factors: type of XPS instruments available on the market, the manufacturing process and sample handling. Test structures are now aligned along lines instead of on a circle radius, so that the individual structures can be accessed more quickly and easily. In addition, a larger test structure of 300 μm and another one in an intermediate size of 18 μm were added. Smaller test structures under 50 μm have been annotated with finder grids/arrows around them so that they are easier to find. Further, the manufacturing process was changed from e‐beam lithography to a mask process to be able to offer the test material at a favourable price. The use of masks also had to be adapted for the new manufacturing process so that the smallest square structures are also realised as such and do not show any distortion of the structure boundaries. The quality control using a metrological SEM confirmed a very reproducible manufacturing process. It is demonstrated that the test material can be successfully employed to find the most suitable beam size of the XPS system used for the analysis of small (μm range) surface features. KW - Small-area measurements KW - Test material KW - XPS KW - XPS imaging PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-616577 DO - https://doi.org/10.1002/sia.7367 SP - 1 EP - 6 PB - Wiley AN - OPUS4-61657 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Liaison between ISO/TC 202 Microbeam Analysis and VAMAS/TWA 37 Quantitative Microstructural Analysis N2 - The liaison between ISO/TC 202 Microbeam Analysis and VAMAS/TWA 37 Quantitative Microstructural Analysis and other TWAs 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. T2 - 31st Plenary Meeting of ISO/TC202 Microbeam Analysis CY - Tokio, Japan DA - 29.10.2024 KW - ISO TC 202 KW - Microbeam Analysis KW - Interlaboratory comparison KW - VAMAS KW - Standardisation PY - 2024 AN - OPUS4-61513 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Liaison Report ISO/TC 229 for ISO/TC 202 and vice-versa N2 - The liaison between the two ISO technical committees TC 229 Nanotechnologies and TC 202 Microbeam analysis, in both directions, is described in detail with highlight on the projects under developement since 2023 and which involve input/knowledge from ISO/TC 202. T2 - 31st Plenary Meeting of ISO/TC202 Microbeam Analysis CY - Tokio, Japan DA - 29.10.2024 KW - ISO TC 202 KW - ISO TC 229 KW - Standardisation KW - Nanotechnologies KW - Microbeam analysis PY - 2024 AN - OPUS4-61511 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. The implementation of the results into the corresponding ISO technical specification AWI/TS 23879 is also discussed and planned, in relation with the AFM part. T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 49th Steering Committee Meeting CY - Rio de Janeiro, Brazil DA - 23.09.2024 KW - VAMAS KW - Graphene oxide KW - SEM KW - Lateral size KW - Interlaboratory comparison PY - 2024 UR - http://www.vamas.org/twa41/documents/2023_vamas_twa41_project13_GO_SEM.pdf AN - OPUS4-61434 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fagan, Jeffrey A1 - Hodoroaba, Vasile-Dan T1 - VAMAS TWA Nanoparticle Populations Projects 15 and 16 N2 - The progress in the VAMAS Project #15 "Measurement of particle size and shape distribution of bipyramidal titania including deposition from liquid suspension" within TWA 34 Nanoparticle Populations is presented with highlight of the following points: - Determine and compare particle size and shape distribution by means of electron microscopy (SEM, TEM, STEM-in-SEM), atomic force microscopy (AFM) and small angle X-ray scattering (SAXS). - Determine uncertainty induced by deposition protocol from liquid suspension with comparison to known values from a prior ILC with already deposited nanoparticles on TEM grids. - Provide comparative validation of protocols for the techniques other than TEM. Further, the VAMAS/TWA 34 Project #16 "Measurement of (relative) number concentration of bimodal silica nanoparticles including deposition from liquid suspension" is presented. Follwowing points are discusssed: - Validate the performance of imaging methods to measure the relative number concentration by electron microscopy (SEM, TEM) and atomic force microscopy (AFM) and two modes of bimodal (30 and 60 nm) silica nanoparticles - Validate the performance of small angle X-ray scattering (SAXS) for the traceable measurement of the number concentration of the two modes. T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 49th Steering Committee Meeting CY - Rio de Janeiro, Brazil DA - 23.09.2024 KW - VAMAS KW - Nanoparticles KW - Nanoparticle size and shape distribution KW - Particle number concentration KW - Interlaboratory comparison KW - Standardisation PY - 2024 UR - http://www.vamas.org/twa34/index.html AN - OPUS4-61422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - VAMAS Regional Report Germany 2024 N2 - Regional standardisation activities and how VAMAS can help in any way to promote activities are reported. Activities related to organisational updates, government initiatives/priorities (especially related to Advanced Materials), details of any strategy documents publicly available, networks within Germany and how we engage are presented. T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 49th Steering Committee Meeting CY - Rio de Janeiro, Brazil DA - 23.09.2024 KW - VAMAS KW - Advanced materials KW - Standardisation PY - 2024 UR - http://www.vamas.org/ AN - OPUS4-61405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Correlative physic-chemical analysis of advanced materials and BAM’s green and zero-related advanced materials activities – Benefits and challenges by examples N2 - Following points are presented: - Nanomaterials BAM, as research materials & CRMs, incl pre-standardization, automated analysis & automated synthesis - 2D-materials BAM HEurope ACCORDs approach Green Deal inspired correlative imaging based characterisation for safety profiling of 2D materials - Sample preparation @BAM , inclusion to standards - Thin Films @BAM as Reference Material Candidates, i) mesoporous, ii) HEA - Substitutional,Transition Me oxides as electrocatalysts a project @BAM - Sustainable mechanochemical reaction engineering projects @BAM. T2 - VAMAS Workshop Advanced Materials Challenges and Standardization Needs for a Greener World CY - Rio de Janeiro, Brazil DA - 25.09.2024 KW - Nanomaterials KW - Advanced materials KW - 2D materials KW - Sample preparation KW - Thin films KW - Reference materials KW - Safety KW - Automation PY - 2024 AN - OPUS4-61404 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Report VAMAS/TWA 37 "Quantitative Microstructural Analysis" & Liaison with ISO/TC 202 "Microbeam Analysis" N2 - The progress in activities on Quantitative MicroStructural Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 Microbeam Analysis is presented and discussed with respect to the identification and launching corresponding VAMAS projects. The ongoing projects "Development of guidelines for reproducible TEM specimen preparation by FIB processing", "Measurement of dislocation density in metallic materials by Transmission Electron Microscope (TEM)", "Repeatability of high angular resolution electron backscatter diffraction (HR-EBSD) analysis for elastic strain measurements", and "Measurement of grain size and distribution of nanocrystalline nickel by using Transmission Kikuchi Diffraction (TKD) in SEM" are presented in detail. T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 49th Steering Committee Meeting CY - Rio de Janeiro, Brazil DA - 23.09.2024 KW - VAMAS KW - Interlaboratory comparison KW - Microbeam Analysis KW - FIB KW - SEM KW - TEM KW - Sample preparation PY - 2024 UR - www.vamas.org/twa37/index.html AN - OPUS4-61388 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sachse, René A1 - Kotil, Leyla A1 - Matjacic, Lidija A1 - McMahon, Greg A1 - Bernicke, Michael A1 - Bernsmeier, Denis A1 - Kraehnert, Ralph A1 - Hertwig, Andreas A1 - Hodoroaba, Vasile-Dan T1 - Morphological and Chemical Nanoscale Analysis of Mesoporous Mixed IrOx-TiOy Thin Films as Electrode Materials N2 - orous films play an important role particularly in energy applications like photovoltaics, electrolysis or batteries. Thin film properties such as thickness, chemical composition, crystallinity of the framework, and porosity define the activity of the porous films. The accurate morpho-chemical characterisation of mesoporous thin films is a challenging analytical task which requires the consideration of new analytical approaches based on the combination of data of different methods able to address the structure and chemical composition at the nanoscale. In this contribution we characterise thin mesoporous iridium-titanium mixed oxide film properties by Electron Probe Microanalysis (EPMA) with Energy-Dispersive X-ray Spectroscopy (EDS) at an SEM applied in a dedicated “thin film analysis” approach (1). Thus, the film mass deposition, film thickness and the film density can be determined. Further, by dividing the measured film density to an assumed (theoretical) metal oxide framework (skeletal) density, the thin film porosity can be extracted, too. In order to assess the homogeneity of the thin film properties like the chemical composition, Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) and Auger Electron Spectrometry are applied in the depth profiling mode, so that possible in-depth gradients are detected. Lateral inhomogeneities in the chemical composition and structure of the thin mesoporous films are also identified by applying the same methods in the line-scan or mapping mode, which can be further combined with in-depth sputtering for 3D information. The role of the spatial resolution of the analytical methods considered, which can go down well below 100 nm, will be highlighted. KW - Mesoporous thin films KW - Imaging KW - TiO2 KW - Ir oxid KW - Auger electron spectroscopy KW - ToF-SIMS KW - SEM/EDX PY - 2024 DO - https://doi.org/10.1093/mam/ozae044.252 VL - 30 IS - Supplement 1 SP - 541 EP - 542 PB - Oxford University Press (OUP) AN - OPUS4-61185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Salzmann, Christoph A1 - Heilmann, Maria A1 - Pellegrino, Francesco A1 - Durand, Bénédicte A1 - Taché, Olivier A1 - Zurutuza, Amaia A1 - Hodoroaba, Vasile-Dan T1 - Ongoing International Interlaboratory Comparisons on Size, Shape and (Relative) Concentration of Complex Nanoparticles under the Pre-Standardization Platform of VAMAS N2 - An overview with the basics of size and shape measurement of particles and 2D structures according to established methodologies (and popular imaging processing software packages) with imaging techniques is given. Main descriptors are explained based on case studies with ongoing interlaboratory comparisons under the pre-standardisation platform of VAMAS. KW - VAMAS KW - Interlaboratory comparison KW - Imaging KW - Size distribution KW - Particle concentration KW - 2D materials PY - 2024 DO - https://doi.org/10.1093/mam/ozae044.319 VL - 30 IS - Supplement 1 SP - 669 EP - 670 PB - Oxford University Press (OUP) AN - OPUS4-61183 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rossi, Andrea A1 - Alladio, Eugenio A1 - Drobne, Damjana A1 - Hodoroaba, Vasile-Dan A1 - Jurkschat, Kerstin A1 - Kononenko, Veno A1 - Madbouly, Loay Akmal A1 - Mrkwitschka, Paul A1 - Novak, Sara A1 - Radnik, Jörg A1 - Saje, Špela A1 - Santalucia, Rosangela A1 - Sordello, Fabrizio A1 - Pellegrino, Francesco T1 - Development of a one-pot synthesis of rGO in water by optimizing Tour’s method parameters N2 - Since its first synthesis in 2004, graphene has been widely studied and several different synthesis methods has been developed. Solvent exfoliation of graphite and the reduction of graphene oxide previously obtained through graphite oxidation are the most employed. In this work, we exploited synthesis conditions of a method usually employed for obtaining graphene oxide (the Tour’s method) for directly obtaining a very poorly oxidised material with characteristics like reduced graphene oxide. For the first time, a one-pot synthesis of reduced graphene oxide (rGO) is reported avoiding the use of a post-synthesis chemical or thermal reduction of the graphene oxide that requires further reagents, heat and time. KW - Graphene KW - 2D-materials KW - Tour's method KW - rGO KW - One-pot synthesis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611827 DO - https://doi.org/10.1038/s41598-024-73606-2 SN - 2045-2322 VL - 14 SP - 1 EP - 10 PB - Springer Nature CY - London AN - OPUS4-61182 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Salzmann, Christoph A1 - Pellegrino, Francesco A1 - Hodoroaba, Vasile-Dan T1 - STEM-in-SEM versus SE-InLens-type-SEM as a Reliable Analytical Pair-Tool for Measurement of Nanoparticle Size and Shape Distribution N2 - Following points are addressed in this contribution: Advantages of correlative analysis in electron microscopy; Measurement principle of the different electron microscopy modes used; Presentation of the nanomaterials used for this study; Role of sample preparation; and, with particular description, the Sequence kV-variation with InLens SE & transmission SEM detection of the same field-of-view. KW - Nanoparticles KW - Electron microscopy KW - Metrology KW - Particle size distribution PY - 2024 DO - https://doi.org/10.1093/mam/ozae044.308 VL - 30 IS - Supplement_1 SP - 650 EP - 651 PB - Oxford University Press (OUP) AN - OPUS4-61042 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ankli, P.P. A1 - Ali, A. A1 - Hodzic, S. A1 - Logachov, A. A1 - Maciejczuk, K. A1 - Milochiv, A. A1 - Hardy, S. A1 - Hardy, B. A1 - Novak, S. A1 - Kranjc, E. A1 - Kononenko, V. A1 - Saje, S. A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg A1 - Akmal, Loay A1 - Mrkwitschka, Paul A1 - Pellegrino, F. A1 - Rossi, A. A1 - Alladio, E. A1 - Sordello, F. A1 - Gulumian, M. A1 - Valsami-Jones, E. A1 - Andraos, C. A1 - Wepener, V. A1 - Jurkschat, K. A1 - Jones, E. A1 - Singh, D. A1 - Ibrahim, B. A1 - van der Zande, M. A1 - Fernandez-Poulussen, D. A1 - Queipo, P. A1 - Drobne, D. T1 - Data management for image-based characterisation of 2D nano-materials N2 - The ACCORDs project, funded through Horizon Europe, is pioneering a novel approach to investigate Graphene Family Materials (GFMs) through image analysis. Our aim is to unveil how these materials might influence health and the environment. To achieve this, we are developing a platform designed for the easy retrieval, access, sharing, and utilisation of GFM data and the coordination between biological and physico-chemical data formats. Integral to this platform is an OMERO-based library for image storage, alongside data collection forms and image analysis tools. Efforts are underway to streamline the process for researchers to upload and disseminate their findings, manage information within a database and navigate the data with ease. Adhering to REMBI guidelines, which set the standard for annotating biological images with metadata, we ensure our data collection is comprehensive and adheres to established best practices. Initially, we are employing thresholding and basic machine learning techniques for image segmentation, laying the groundwork for advanced analysis through deep learning to gain more profound insights. Upon completion, the project will deliver a comprehensive platform facilitating efficient data and image management concerning GFMs. This platform will enable the straightforward discovery and use of protocols and results, all organised in accordance with the FAIR principles – Findable, Accessible, Interoperable, and Reusable. This initiative is poised to significantly impact materials science, enhancing our comprehension of the safety and environmental implications of 2D materials. KW - Graphene KW - Image analysis KW - Data management PY - 2024 DO - https://doi.org/10.1016/j.toxlet.2024.07.655 VL - 399 SP - S271 PB - Elsevier B.V. AN - OPUS4-61011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mrkwitschka, Paul A1 - Abram, Sarah-Luise A1 - Rühle, Bastian 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 Iron Oxide 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. KW - Nanoparticles KW - Iron oxide KW - Electron microscopy KW - Reference materials KW - Particle size distribution KW - Imaging PY - 2024 DO - https://doi.org/10.1093/mam/ozae044.339 VL - 30 IS - Supplement_1 SP - 710 EP - 711 PB - Oxford University Press (OUP) AN - OPUS4-61007 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Ongoing International Interlaboratory Comparisons on Size, Shape and (Relative) Concentration of Complex Nanoparticles under the Pre-Standardization Platform of VAMAS N2 - Traceable morphological and chemical characterization of nanomaterials with respect to the various possible sizes, size distributions, shapes, and concentrations of real-world nanoparticles (NPs) is a challenging task. Particularly for the nonspherical, non-monodisperse nanoparticles – as typically for most of the commercial particles, including their strong tendency to agglomerate, there is a lack of standard operation procedures providing accurate nanoparticle characterisation. In the framework of the pre-standardisation framework of VAMAS (Versailles Project on Advanced Materials and Standards, www.vamas.org) two interlaboratory comparison (ILC) studies are being carried out under the Technical Working Area (TWA) 34 “Nanoparticle Populations”:i) Project #15 addresses the analysis of the size and shape distribution of TiO2 bipyramidal NPs by traceable imaging methods such as TEM, SEM, STEM-in-SEM, AFM as well as with SAXS as an ensemble method. This ILC is thought as the next level development of the case studies exemplified in the published ISO standards ISO 21363 and ISO 19749. It was agreed to complete the first ILC with the NPs already prepared according to the same procedure on a TEM grid, and, at a later stage, to carry out second ILCs with the same NPs distributed to the participants as liquid suspensions together with protocols for the uniform NP deposition on suited substrates - as developed and optimized within the European project nPSize. Once having good deposition protocols available, the door for automated image analysis gets opened. Corresponding image analysis protocols and reporting templates have been distributed to the ILC participants, too. ii) Project #16: two spherical SiO2 NP samples with bi-modal size distributions in two nominal relative number concentrations were prepared and distributed also as liquid suspensions accompanied by sample preparation, measurement, and image analysis protocols and reporting templates. Here, the NP concentration is the primary parameter to be measured. For the imaging methods it is targeted to measure the relative nanoparticle concentrations (relative populations of the two modes). The results of all the participating laboratories, in both ILCs, compiled in comparative representations will be shown and discussed for the first time. The reduction of the measurement uncertainties associated to the size, shape and number-concentration results induced by the significant improvement of the sample preparation on substrates (as single particles with a high-density coverage), combined with well-defined image analysis procedures will be highlighted. Finally, a very recent 3rd ILC an the determination of lateral size of Graphene Oxide flakes by SEM is presented as project P13 under VAMAS TWA41 Graphene and Related 2D. T2 - Microscopy and Microanalysis 2024 CY - Cleveland, OH, USA DA - 28.07.2024 KW - VAMAS KW - Interlaboratory comparison KW - Imaging KW - Nanoparticles KW - Electron microscopy KW - Graphene oxide KW - Particle size distribution PY - 2024 AN - OPUS4-60875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hülagü, Deniz A1 - Tobias, Charlie A1 - Dao, R. A1 - Komarow, P. A1 - Rurack, Knut A1 - Hodoroaba, Vasile-Dan T1 - Dataset accompanying the publication "Towards 3D determination of the surface roughness of core-shell microparticles as a routine quality control procedure by scanning electron microscopy" N2 - This dataset accompanies the following publication: Hülagü, D., Tobias, C., Dao, R., Komarov, P., Rurack, K., Hodoroaba, V.-D., Towards 3D determination of the surface roughness of core-shell microparticles as a routine quality control procedure by scanning electron microscopy. Sci.Rep, 14, 17936 (2024), https://doi.org/10.1038/s41598-024-68797-7. It contains SEM and AFM-in-SEM images of polystyrene (PS) core particles, polystyrene-iron oxide (PS/Fe3O4) core-shell particles, and polystyrene-iron oxide-silica (PS/Fe3O4/SiO2) core-shell-shell particles. Please refer to the publication and its supporting information for more details on the acquisition and contents of the dataset, as well as the GitHub repository at https://github.Com/denizhulagu/roughness-analysis-by-electron-microscopy. The investigated particles were produced at BAM laboratories as previously described in: Hülagü, D. et al. Generalized analysis approach of the profile roughness by electron microscopy with the example of hierarchically grown polystyrene–iron oxide–silica core–shell–shell particles. Adv. Eng. Mater. 24, 2101344, https://doi.org/10.1002/adem.202101344 (2022). Tobias, C., Climent, E., Gawlitza, K. & Rurack, K. Polystyrene microparticles with convergently grown mesoporous silica shells as a promising tool for multiplexed bioanalytical assays. ACS Appl. Mater. Interfaces 13, 207, https://dx.doi.org/10.1021/acsami.0c17940 (2020). KW - Core–shell particles KW - Image analysis KW - Roughness KW - Scanning electron microscopy KW - Atomic force microscopy KW - Tilting KW - Batch analysis PY - 2024 UR - https://zenodo.org/records/11108726 DO - https://doi.org/10.5281/zenodo.11108725 PB - Zenodo CY - Geneva AN - OPUS4-60760 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 -