TY - JOUR A1 - Schusterbauer, Robert A1 - Mrkwitschka, Paul A1 - Sahre, Mario A1 - Corrao, Elena A1 - Zurutuza, Amaia A1 - Doolin, Alexander A1 - Pellegrino, Francesco A1 - Radnik, Jörg A1 - Donskyi, Ievgen S. A1 - Hodoroaba, Vasile-Dan T1 - Correlative Chemical Imaging to Reveal the Nature of Different Commercial Graphene Materials N2 - Proper physicochemical characterization of advanced materials and complex industrial composites remains a significant challenge, particularly for nanomaterials, whose nanoscale dimensions and mostly complex chemistry challenge the analysis. In this work, we employed a correlative analytical approach that integrates atomic force microscopy (AFM), scanning electron microscopy (SEM) coupled with energy‐dispersive X‐ray spectroscopy (EDS), time‐of‐flight secondary ion mass spectrometry (ToF‐SIMS), Auger electron spectroscopy (AES), and Raman spectroscopy. This combination enables detailed chemical and structural characterization with sub‐micrometer spatial resolution. Three commercial graphene‐based materials of varying complexity were selected and investigated to test the analytical performance of this approach. Furthermore, one of the commercial graphene oxide samples was chemically functionalized via amination and fluorination. This allowed us to assess how surface modifications influence both the material properties and the limits of the applied analytical techniques. KW - Analytical methods KW - Commercial products KW - Correlative analysis KW - Graphene KW - Surface imaging PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654765 DO - https://doi.org/10.1002/smtd.202502344 SN - 2366-9608 SP - 1 EP - 10 PB - Wiley VHC-Verlag AN - OPUS4-65476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rossi, Andrea A1 - Corrao, Elena A1 - Alladio, Eugenio A1 - Drobne, Damjana A1 - Hodoroaba, Vasile-Dan A1 - Jurkschat, Kerstin A1 - Kononenko, Veno A1 - Madbouly, Loay Akmal A1 - Mrkwitschka, Paul A1 - Yasamin, Nakhli A1 - Novak, Sara A1 - Radnik, Jörg A1 - Saje, Špela A1 - Santalucia, Rosangela A1 - Sordello, Fabrizio A1 - Pellegrino, Francesco T1 - Multivariate optimization and characterization of graphene oxide via design of experiments and chemometric analysis N2 - Controlling the structure and properties of graphene oxide (GO) remains a challenge due to the poor reproducibility of conventional synthetic protocols and limited understanding of parameter-property relationships. In this study, we present an integrated analytical framework that combines Design of Experiments (DoE) with chemometric modelling to systematically assess the effects of eight synthesis variables on GO’s physicochemical and functional features. A Plackett–Burman experimental design enabled efficient screening of synthesis conditions, while comprehensive characterization (spanning UV–Vis spectroscopy, XPS, SEM–EDX, TEM–EDX, and XRD) was coupled with multivariate tools (Principal Component Analysis and Multiple Linear Regression) to identify statistically significant correlations between synthetic inputs and material responses. Notably, we demonstrate that UV–Vis spectra can serve as a robust proxy for oxidation state, offering a rapid and accessible alternative to surface-sensitive methods. The approach yields a predictive analytical toolkit for guiding GO synthesis and highlights a generalizable strategy for the rational design of flat nanomaterials. This work supports reproducible, resource-efficient material development aligned with Safe and Sustainable by Design (SSbD) principles. KW - Graphene oxide KW - 2D-materials KW - Design of Experiment KW - Synthesis KW - Chemometric analysis PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652576 DO - https://doi.org/10.1016/j.flatc.2025.100988 SN - 2452-2627 VL - 55 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-65257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mrkwitschka, Paul A1 - Sahre, Mario A1 - Corrao, Elena A1 - Pellegrino, Francesco A1 - Alonso, Beatriz A1 - Zurutuza, Amaia A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Standardized Elemental Composition Analysis of Graphene‐Related 2D Materials (GR2M) With SEM/EDS and XPS Works Reliably N2 - Reliable quantification of the chemical composition of graphene‐related 2D materials (GR2M) as powders and liquid suspensions is a challenging task. Analytical methods such as X‐ray photoelectron spectroscopy (XPS), inductively coupled plasma mass spectrometry (ICP‐MS), thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy (FTIR) are recommended by standardization bodies. The specific parameters to be measured are also defined, e.g., the oxygen‐to‐carbon (O/C) atomic ratio, the trace metal impurities, or the functional groups. In this contribution, for the first time, results of a systematic study on the capability of energy‐dispersive X‐ray spectroscopy (EDS) at a scanning electron microscope (SEM) to reliably quantify the O/C ratio and impurities remained from the synthesis of selected GR2M are reported. The robustness of SEM/EDS analysis is verified for various measurement conditions (different excitations and EDS detectors) and the validity of the results is tested by comparison to the established XPS analysis. Moreover, an ionic liquid is used as a reference material for the quantification of the light elements such as C, N, O and F. The study clearly demonstrates the reliability of the fast and widely available SEM/EDS as a standard method for the quantification of the elemental composition of GR2M and generally of light materials. KW - Graphene oxide flakes KW - Impurities KW - O/C ratio KW - SEM/EDS KW - Standard KW - XPS PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-656748 DO - https://doi.org/10.1002/smll.202511283 SN - 1613-6810 SP - 1 EP - 10 PB - Wiley-VHC GmbH AN - OPUS4-65674 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hickel, Tilmann A1 - Waske, Anja A1 - Tehranchi, Ali A1 - Bhattacharya, Biswajit A1 - Stawski, Tomasz M. A1 - Fellinger, Tim-Patrick A1 - Mehmood, Asad A1 - Witt, Julia A1 - Ozcan, Ozlem A1 - Guilherme Buzanich, Ana A1 - Kumar, Sourabh A1 - Mishra, Rajesh Kumar A1 - Holzer, Marco A1 - Stucchi de Camargo, Andrea Simone A1 - Agudo Jácome, Leonardo A1 - Manzoni, Anna A1 - Fantin, Andrea A1 - John, Elisabeth A1 - Hodoroaba, Vasile-Dan A1 - Bührig, Sophia A1 - Murugan, Jegatheesan A1 - Marschall, Niklas A1 - George, Janine A1 - Darvishi Kamachali, Reza A1 - Maaß, Robert A1 - Emmerling, Franziska T1 - Chemically complex materials enable sustainable high-performance materials N2 - Chemically complex materials (CCMats) 􀀀 including high-entropy alloys, oxides, and related multi-principal element systems 􀀀 offer a paradigm shift in materials design by leveraging chemical diversity to simultaneously optimize functional, structural, and sustainability criteria. The vastness of the compositional and structural space in CCMats propels the field into an expanding exploratory state. To reconcile functional and structural performance across this immense parameter space remains an open challenge. This Perspective evaluates the opportunities and challenges associated with harnessing chemical complexity across a broad spectrum of applications, such as hydrogen storage, ionic conductors, catalysis, magnetics, dielectrics, semiconductors, optical materials, and multifunctional structural systems. It is delineated how three central design strategies: targeted substitution (SUB), defect engineering (DEF), and diversity management (DIV) enable the reconciliation of high functional performance with long-term structural stability and environmental responsibility. Advances in computational thermodynamics, microstructure simulations, machine learning, and multimodal characterization are accelerating the exploration and optimization of CCMats, while robust data infrastructures and automated synthesis workflows are emerging as essential tools for navigating their complex compositional space. By fostering cross-disciplinary knowledge transfer and embracing data-driven design, CCMats are poised to deliver next-generation materials solutions that address urgent technological, energy, and environmental demands. KW - Chemically complex materials KW - Structural stability KW - Functional performance KW - Design strategies KW - Sustainability PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655598 UR - https://www.sciencedirect.com/science/article/pii/S1359028626000033?via%3Dihub DO - https://doi.org/10.1016/j.cossms.2026.101256 SN - 1359-0286 VL - 42 SP - 1 EP - 26 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-65559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Habibimarkani, Heydar A1 - Abram, Sarah-Luise A1 - de Oliveira Guilherme Buzanich, Ana A1 - Prinz, Carsten A1 - Sahre, Mario A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - In-depth analysis of FeNi-based nanoparticles for the oxygen evolution reaction N2 - This study investigates the effect of varying iron-to-nickel ratios on the catalytic performance of Fe-Ni oxide nanoparticles (NPs) for the oxygen evolution reaction (OER). Addressing the issue of high energy wastage due to large overpotentials in OER, we synthesized and characterized different NP catalysts with different Fe: Ni oxide ratios. Transmission Electron Microscopy (TEM), Energy Dispersive X-ray Spectroscopy (EDS), and X-ray Diffraction (XRD) were employed to determine the morphology, elemental and phase composition of the NPs. Furthermore, in-depth profiling with X-ray Photoelectron Spectroscopy (XPS) and Hard X-ray Photoelectron Spectroscopy (HAXPES) revealed that iron predominantly exists as oxide, while nickel exhibits both metallic and oxidic forms depending on the Fe content. XPS indicated an enrichment of iron at the NP surface, whereas HAXPES and EDS data agreed on the bulk stoichiometry. The assessment of the catalytic activity via cyclic voltammetry (CV) showed that the Fe: Ni ratio of 2:3 exhibited superior performance, characterized by lower overpotential and a smaller Tafel slope. KW - Fe-Ni oxide KW - Nanoparticles KW - OER KW - Catalytic performance KW - Cyclic voltammetry PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626932 UR - https://www.nature.com/articles/s41598-025-92720-3 DO - https://doi.org/10.1038/s41598-025-92720-3 VL - 15 IS - 1 SP - 1 EP - 17 PB - Springer Nature AN - OPUS4-62693 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madbouly, Loay Akmal A1 - Sturm, Heinz A1 - Doolin, Alexander A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - Chemical Analysis of Commercial Functionalized Graphene Nanoplatelets along the Production Process with Raman Spectroscopy and X-ray Photoelectron Spectroscopy N2 - Commercial applications increasingly rely on functionalized graphene nanoplatelets (GNPs) supplied as powders, aqueous suspensions, and printable inks, yet their process−structure−property relationships across the production chain remain to be fully mapped. Here we apply a correlative Raman spectroscopy (Raman) and X-ray photoelectron spectroscopy (XPS) workflow to nine independent industrial graphene batches spanning three surface chemistries, raw (R), fluorinated (F), and nitrogen-functionalized (N), in all three physical forms which are powders, suspensions, and inks. Raman mapping (with a 532 nm excitation laser) showed that I2D/IG is highest for N samples and lowest for R-ink. A 2D-vs-G correlation places all samples on a trajectory parallel to the pure-doping vector, which can correlate to holes in the graphene lattice. The mean point-defect spacing is LD = 8.4−10.0 nm. High-resolution XPS resolves the accompanying chemical changes: F-powder exhibits distinct C−F (289 eV), C−F2 (292 eV), and C−F3 (293 eV) components and loses roughly half its F content upon dispersion in deionized water or ink formulation; inks of all chemistries show a pronounced O−C=O peak near 289−290 eV originated from the ink compounds. N-functionalized samples showed a prominent C−N (285.5 eV) only for the ink formulated N-functionalized sample. This study establishes a process-aware blueprint linking the functionalization route and formulation step to lattice disorder and surface chemistry, offering transferable quality-control metrics for graphene supply chains in industrial products/applications such as coatings, storage devices, and printed electronics. KW - Functionalized graphene KW - Raman Spectroscopy KW - XPS KW - Chemical analysis PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652548 DO - https://doi.org/10.1021/acs.jpcc.5c06820 SN - 1932-7447 VL - 129 IS - 50 SP - 22033 EP - 22040 PB - American Chemical Society (ACS) AN - OPUS4-65254 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Reliable physico–chemical characterisation of graphene-related and other 2D materials: present and future N2 - In the path of commercialisation of graphene-related and other 2D materials the consolidation has begun. In this phase, it is important to build trust between the individual partners in the product value chain. This requires trustworthy statements based on reliable and reproducible material characterisation. The first steps have been taken to measure graphene and other related 2D materials (GR2Ms) under well-defined conditions. Measurands and protocols for key methods were made available for this purpose. But there are still some challenges to overcome such as (i) reference materials, (ii) reference data, (iii) reproducibility throughout the workflow, (iv) credible structure-activity relationships, bringing the standards to (v) the factory floor and to (vi) real-word products. In addition, 2D materials beyond graphene should also be considered exploiting the knowledge gained from the characterisation of GR2M. KW - 2D Materials KW - Commercialisation KW - Standardisation KW - Trust PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638122 DO - https://doi.org/10.1088/2053-1583/aded9d SN - 2053-1583 VL - 12 IS - 4 SP - 1 EP - 8 PB - IOP Publishing AN - OPUS4-63812 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chemello, Giovanni A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - XPS–SEM/EDS Tandem Analysis for the Elemental Composition of Functionalized Graphene Nanoplatelets N2 - Over the past decade, energy-dispersive X-ray spectrometry (EDS) with scanning electron microscopy (SEM) has advanced to enable the accurate analysis of light elements such as C, N, or O. For this reason, EDS is becoming increasingly interesting as an analytical method for the elemental analysis of functionalized graphene and could be an attractive alternative to Xray photoelectron spectroscopy (XPS), which is considered the most important method for elemental analysis. In this study, comparative XPS and EDS investigations under different excitation conditions are carried out on commercially available powders containing graphene particles with different morphologies. The slightly different XPS/HAXPES and EDS results can be explained by the different information depths of the methods and the functionalization of the particle surfaces. For the material with smaller graphene particles and higher O/C ratios, all methods reported a lower O/C ratio in pellets compared with the unpressed powder samples. This clearly shows that sample preparation has a significant influence on the quantification results, especially for such a type of morphology. Overall, the study demonstrates that EDS is a reliable and fast alternative to XPS for the elemental quantification of functionalized graphene particles, provided that differences in the information depth are taken into account. Particle morphology can be examined in parallel with quantitative element analysis, since EDS spectrometers are typically coupled with SEM, which are available in a huge number of analytical laboratories. KW - Graphene oxide KW - SEM/EDS KW - XPS/HAXPES KW - Elemental composition KW - Functionalization PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647294 DO - https://doi.org/10.1021/acsomega.5c07830 SN - 2470-1343 SP - 1 EP - 7 PB - American Chemical Society (ACS) AN - OPUS4-64729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Devi, Sarita A1 - Riedel, Soraya A1 - Döring, Sarah A1 - Hiller, Lukas A1 - Kaliyaraj Selva Kumar, Archana 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 metal-organic framework (MOF)-integrated microfluidic flow-cell (MFC) based immunodetection of the tetanus toxoid (TT) using electrochemical technique for the first time. The magnetic property of Fe-MOF helped to hold them on the working electrode at detection zone of MFC surpassing the requirement of additional conjugation chemistry, whereas the conductive property was utilized to observe the change in signal efficiency in the presence of TT. The one-pot hydrothermal synthesis of a magnetic and conductive iron-based MOF (Fe-MOF) was performed 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 conjugated with L-phenylalanine (Fe-MOF/Phe) to increase its electric conductivity owing to the enhanced electron flow rate. The human monoclonal antibody SA13 against TT (anti-TT mAb) was conjugated on the Fe-MOF/Phe surface with the help of ethylenediamine (Fe-MOF/Phe/EDA/anti-TT mAb). The binding affinity of Fe-MOF/Phe/EDA/anti-TT mAb for the TT antigen was evaluated using cyclic voltammetry technique. 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. This study shows the applicability of these Fe-MOFs in the detection of various other microbial toxins or other biomolecules. KW - Antikörper KW - Elektrochemischer Immunoassay KW - Molecular Organic Framework (MOF) KW - Microfluidics KW - Rekombinant PY - 2025 DO - https://doi.org/10.1016/j.snb.2025.137381 SN - 0925-4005 VL - 431 SP - 1 EP - 12 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-62673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Habibimarkani, Heydar A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan A1 - John, Elisabeth T1 - Probing Surface Changes in Fe–Ni Oxide Nanocatalysts with a ToF-SIMS-Coupled Electrochemistry Setup and Principal Component Analysis N2 - Understanding catalyst surface dynamics under operating conditions is essential for improving electrocatalytic performance. Here, we present a novel approach combining electrochemical treatment with contamination-free transfer to Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS), followed by principal component analysis (PCA), to probe surface and interfacial changes in Ni–Fe oxide nanoparticles stabilized by polyvinylpyrrolidone (PVP) during the oxygen evolution reaction (OER). The surface analysis at three distinct treatment stages revealed distinct chemical fingerprints across pristine nanoparticles, after exposure to 1 M KOH electrolyte, and after cyclic voltammetry treatment. The results highlight a progressive transition from ligand-rich to ligand-depleted interfaces, with PVP-related fragments dominant in the early stages and metal- and electrolyte-derived species emerging after activation. Complementary ToF-SIMS analysis of electrolyte deposited on Si wafers after each treatment step confirms the concurrent leaching of PVP and Fe–Ni-based fragments during OER. These findings underscore the dynamic nature of catalyst–electrolyte interfaces and demonstrate a robust strategy for monitoring surface-sensitive chemical changes associated with the nanoparticles, especially during the initial cycles of the OER. KW - Fe-Ni oxide KW - Nanocatalysts KW - ToF-SIMS KW - Electrochemistry KW - PCA (principal component analysis) KW - OER PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652667 DO - https://doi.org/10.1021/acs.analchem.5c03894 SN - 0003-2700 SP - 1 EP - 8 PB - American Chemical Society (ACS) AN - OPUS4-65266 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 - JOUR A1 - Putzu, Mara A1 - Wiesner, Yosri A1 - Weimann, Christiane A1 - Hodoroaba, Vasile-Dan A1 - Muniategui Lorenzo, Soledad A1 - Fernández-Gonzáles, Verónica A1 - Booth, Andy M. A1 - Igartua, Amaia A1 - Benismail, Nizar A1 - Coïc, Laureen A1 - Chivas-Joly, Carine A1 - Fenoglio, Ivana A1 - Rossi, Andrea Mario A1 - Giovannozzi, Andrea Mario A1 - Altmann, Korinna T1 - Optimization of tablet processing as a reference material for microplastic detection methods N2 - Reference materials (RMs) are essential and highly demanded tools for the development and validation of methods for microplastic (MP) quantification in complex matrices, to ensure comparable and harmonized approaches aligned with EU commission criteria for monitoring MPs (e.g., Drinking Water Directive and Urban Wastewater Treatment Directive). This study investigates different approaches for optimizing the production of polypropylene (PP) RMs in the form of water-soluble tablets, which were carefully evaluated for their homogeneity and stability according to ISO Guide 30, ISO 33401, and ISO 33405. PP particles (1–100 μm) were produced by cryomilling and embedded in a lactose/PEG matrix, then pressed into tablets (18 µg theoretical PP mass). The production process was optimized by varying (i) the size distribution of the matrix components and (ii) the mixer instrument. The materials obtained were characterized by thermogravimetric analysis to assess the homogeneity distribution of MPs with respect to PP mass in the individual tablets and their stability over a 4-month period. The most promising approach, with a homogenous mass of 19 μg (standard deviation of 4 μg), relative standard deviation of 19%, was further investigated for homogeneity by comparison with thermo-analytical mass determination methods, such as TED-GC/MS (thermal extraction desorption-gas chromatography/mass spectrometry) and Py-GC/MS (pyrolysis-gas chromatography-mass spectrometry), and for number-based characterization using micro-Raman spectroscopy. Material characterization was also examined using laser diffraction, scanning electron microscopy, and ATR-FTIR. Based on the results, the optimized processing protocol yields a PP RM suitable for quality control and method performance studies supporting standardization. KW - Microplastics KW - TED-GC/MS KW - Reference materials KW - Polypropylene PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653290 DO - https://doi.org/10.1007/s00216-025-06271-7 SN - 1618-2642 SP - 1 EP - 14 PB - Springer Science and Business Media LLC AN - OPUS4-65329 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ciornii, Dmitri A1 - Hodoroaba, Vasile-Dan A1 - Wachtendorf, Volker A1 - Fengler, Petra A1 - Altmann, Korinna T1 - Interlaboratory Comparison Reveals State of the Art in Microplastic Detection and Quantification Methods N2 - In this study, we investigate the current accuracy of widely used microplastic (MP) detection methods through an interlaboratory comparison (ILC) involving ISO-approved techniques. The ILC was organized under the prestandardization platform of VAMAS (Versailles Project on Advanced Materials and Standards) and gathered a large number (84) of analytical laboratories across the globe. The aim of this ILC was (i) to test and to compare two thermo-analytical and three spectroscopical methods with respect to their suitability to identify and quantify microplastics in a water-soluble matrix and (ii) to test the suitability of the microplastic test materials to be used in ILCs. Two reference materials (RMs), polyethylene terephthalate (PET) and polyethylene (PE) as powders with rough size ranges between 10 and 200 μm, were used to press tablets for the ILC. The following parameters had to be assessed: polymer identity, mass fraction, particle number concentration, and particle size distribution. The reproducibility, SR, in thermo-analytical experiments ranged from 62%−117% (for PE) and 45.9%−62% (for PET). In spectroscopical experiments, the SR varied between 121% and 129% (for PE) and 64% and 70% (for PET). Tablet dissolution turned out to be a very challenging step and should be optimized. Based on the knowledge gained, development of guidance for improved tablet filtration is in progress. Further, in this study, we discuss the main sources of uncertainties that need to be considered and minimized for preparation of standardized protocols for future measurements with higher accuracy. KW - Microplastics KW - Interlaboratory comparison KW - PlasticsFatE KW - PET KW - PE KW - Reference materials KW - VAMAS KW - Thermo-analytical methods KW - Spectroscopical methods PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630462 DO - https://doi.org/10.1021/acs.analchem.4c05403 SN - 1520-6882 VL - 97 SP - 8719 EP - 8728 PB - ACS Publications AN - OPUS4-63046 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 - Hülagü, Deniz A1 - Tobias, Charlie A1 - Dao, Radek A1 - Komarov, Pavel A1 - Rurack, Knut A1 - Hodoroaba, Vasile-Dan T1 - Towards 3D determination of the surface roughness of core–shell microparticles as a routine quality control procedure by scanning electron microscopy N2 - AbstractRecently, we have developed an algorithm to quantitatively evaluate the roughness of spherical microparticles using scanning electron microscopy (SEM) images. The algorithm calculates the root-mean-squared profile roughness (RMS-RQ) of a single particle by analyzing the particle’s boundary. The information extracted from a single SEM image yields however only two-dimensional (2D) profile roughness data from the horizontal plane of a particle. The present study offers a practical procedure and the necessary software tools to gain quasi three-dimensional (3D) information from 2D particle contours recorded at different particle inclinations by tilting the sample (stage). This new approach was tested on a set of polystyrene core-iron oxide shell-silica shell particles as few micrometer-sized beads with different (tailored) surface roughness, providing the proof of principle that validates the applicability of the proposed method. SEM images of these particles were analyzed by the latest version of the developed algorithm, which allows to determine the analysis of particles in terms of roughness both within a batch and across the batches as a routine quality control procedure. A separate set of particles has been analyzed by atomic force microscopy (AFM) as a powerful complementary surface analysis technique integrated into SEM, and the roughness results have been compared. 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://nbn-resolving.org/urn:nbn:de:kobv:b43-607590 DO - https://doi.org/10.1038/s41598-024-68797-7 SN - 2045-2322 VL - 14 IS - 1 SP - 1 EP - 13 PB - Springer Science and Business Media LLC AN - OPUS4-60759 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 - JOUR A1 - Voss, Heike A1 - Knigge, Xenia A1 - Knapic, D. A1 - Weise, Matthias A1 - Sahre, Mario A1 - Hertwig, Andreas A1 - Sacco, A. A1 - Rossi, A. M. A1 - Radnik, Jörg A1 - Müller, Kai A1 - Wasmuth, Karsten A1 - Krüger, Jörg A1 - Hassel, A. W. A1 - Hodoroaba, Vasile-Dan A1 - Bonse, Jörn T1 - Picosecond laser processing of hierarchical micro–nanostructures on titanium alloy upon pre- and postanodization: morphological, structural, and chemical effects N2 - Recent publications indicate that the order of electrochemical anodization (before or after the laser processing step) plays an important role for the response of bone-forming osteoblasts—an effect that can be utilized for improving permanent dental or removable bone implants. For exploring these different surface functionalities, multimethod morphological, structural, and chemical characterizations are performed in combination with electrochemical pre- and postanodization for two different characteristic microspikes covered by nanometric laser-induced periodic surface structures on Ti–6Al–4V upon irradiation with near-infrared ps-laser pulses (1030 nm wavelength, ≈1 ps pulse duration, 67 and 80 kHz pulse repetition frequency) at two distinct sets of laser fluence and beam scanning parameters. This work involves morphological and topographical investigations by scanning electron microscopy and white light interference microscopy, structural material examinations via X-ray diffraction, and micro-Raman spectroscopy, as well as near-surface chemical analyses by X-ray photoelectron spectroscopy and hard X-ray photoelectron spectroscopy. The results allow to qualify the mean laser ablation depth, assess the spike geometry and surface roughness parameters, and provide new detailed insights into the near-surface oxidation that may affect the different cell growth behavior for pre- or postanodized medical implants. T2 - 2023 E-MRS Spring Meeting, Symposium L "Making light matter: lasers in material sciences and photonics" CY - Strasbourg, France DA - 29.05.2023 KW - Hierarchical micro-nanostructures KW - Laser-induced periodic surface structures (LIPSS) KW - Ultrashort laser pulses KW - Ti-6Al-4V alloy KW - X-ray photoelectron spectroscopy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601962 DO - https://doi.org/10.1002/pssa.202300920 SN - 1862-6319 SP - 1 EP - 11 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-60196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -