TY - CONF A1 - Radnik, Jörg T1 - Analytical and Characterisation Excellence in nanomaterial risk assessment: A tiered approach Task2.5 N2 - The final results of Task 2.5 "Optimization of sample preparation for characterization of ENPs using TOF-SIMS under real-life conditions (a.) UfZ: polymer template; b.) BAM: pressing of pellets)" were presented. T2 - ACEnano General Meeting CY - Amsterdam, The Netherlands DA - 05.03.2020 KW - Nanoparticles KW - ToF-SIMS KW - Preparation PY - 2020 AN - OPUS4-50572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Standardized Measurements of Surface - Functionalities on Nanoparticles N2 - Engineered nanoparticles (NPs) with various chemical compositions and surface functionalities are routinely fabricated for industrial applications such as medical diagnostics, drug delivery, sensing, catalysis, energy conversion and storage, optoelectronics, and information storage. NP function, interaction with biological species, and environmental fate are largely determined by surface functionalities. Reliable, reproducible, and standardized surface characterization methods are therefore vital for quality control of NPs, and mandatory to meet increasing concerns regarding their safety. Also, industry, international standardization organizations, regulatory agencies, and policymakers need validated and standardized measurement methods and reference materials. However, methodologies for determining NP surface properties, including the amount, chemical composition, and homogeneity of surface functionalities and coatings are largely non-standardized. Suitable methods for determining surface functionalities on ligand-stabilized core and core/shell NPs include advanced techniques such as traceable quantitative nuclear magnetic resonance (qNMR) as well as X-ray electron spectroscopy (XPS) and time of flight secondary ion mass spectrometry (ToF-SIMS), and simpler optical and electrochemical methods. The latter less costly methods are often used by SMEs, e.g., for quality control. To validate methods, establish measurement uncertainties, test reference materials, and produce reference data, international interlaboratory comparisons (ILC) on NP surface functionalization measurements are required and well characterized test and reference nanomaterials providing benchmark values.[1] These needs are addressed by the recently started European metrology project SMURFnano involving 12 partners from different National Metrology Institutes, designated institutes, and research institutes, two university groups as well as one large company and one SME producing NPs. This project as well as first results derived from the development of test and reference materials with a well characterized surface chemistry and ongoing interlaboratory comparisons will be presented. T2 - eMRS CY - Strasbourg, France DA - 27.05.2025 KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Synthesis KW - Silica KW - Upconversion nanoparticles KW - Optical assay KW - qNMR KW - Surface analysis KW - Ligand KW - Quantification KW - Functional group KW - XPS KW - ToF-SIMS KW - Polymer particle KW - Surface modification KW - Potentiometry KW - Metrology KW - Method KW - Validation KW - ILC PY - 2025 AN - OPUS4-63339 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - ToF-SIMS at advanced materials - from nano to energy N2 - The basic principles of ToF-SIMS will be explained. Examples of the use of ToF-SIMS for the investigation of titania and core-shell nanoplastic will be given. Furhtermore, 3d reconstruction is explained for nanoparticle research and energy-related materials. T2 - BUA Summer School Mass Spectrometry CY - Berlin, Germany DA - 04.10.2022 KW - ToF-SIMS KW - Nanomaterials KW - Imaging PY - 2022 AN - OPUS4-55897 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 - Bonse, Jörn T1 - Chemical and structural changes at the surface of titanium materials upon irradiation with near-infrared ultrashort laser pulses N2 - Due to its large strength-to-weight ratio and excellent biocompatibility, titanium materials are of paramount importance for medical applications, e.g. as implant material for protheses. In this work, the evolution of various types of laser-induced micro- and nanostructures emerging on titanium or titanium alloys upon irradiation by near-infrared ultrashort laser pulses (925 fs, 1030 nm) in air environment is studied for various laser fluence levels, effective number of pulses and at different pulse repetition rates (1 – 400 kHz). The morphologies of the processed surfaces were systematically characterized by optical and scanning electron microscopy (OM, SEM). Complementary white-light interference microscopy (WLIM) revealed the corresponding surface topographies. Chemical and structural changes were analysed through depth-profiling time-of-flight secondary ion mass spectrometry (TOF-SIMS) and X-ray diffraction (XRD) analyses. The results point towards a remarkable influence of the laser processing parameters on the surface topography, while simultaneously altering the near-surface chemistry via laser-induced oxidation effects. Consequences for medical applications are outlined. T2 - E-MRS Spring Meeting 2022 CY - Online meeting DA - 30.05.2022 KW - Laser-induced periodic surface structures (LIPSS) KW - Surface functionalization KW - ToF-SIMS KW - Chemical analysis KW - Titanium PY - 2022 AN - OPUS4-54931 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 - CONF A1 - Schusterbauer, Robert T1 - Correlative chemical imaging to reveal the nature of different commercial graphene materials N2 - Since the original report in 2004 by Novoselov and Geim, Graphene gained incredible attention due to its fascinating properties. In the past 20 years, the synthesis and functionalization of graphene has evolved significantly[3]. Different synthesis techniques were developed which led to other graphenerelated 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 kindly 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 (Figure b). 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 - MaterialsWeek 2024 CY - Limassol, Cyprus DA - 17.06.2024 KW - Graphene oxide flakes KW - ToF-SIMS KW - SEM KW - Raman KW - Correlative imaging PY - 2024 AN - OPUS4-60681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Habibimarkani, Heydar T1 - Time-of-flight secondary ion mass spectrometry (ToF-SIMS) for in situ investigation on FeNi nanoparticles N2 - The modern economy is dependent on catalysis, which is main efforts to create environmentally and energy-friendly technologies. The storage of excess electrical energy into chemical energy by splitting water into hydrogen and oxygen is a feasible solution to this energy demand. Due to their abundance on Earth and inherent stability in alkaline solution, transition-metal oxides have become one of several viable alternatives to noble-metal catalysts. Since NiFe oxide is one of the most active oxygen evolution reaction (OER) electrocatalysts for alkaline water electrolysis, it has been the subject of extensive research. In this work, NiFe2O4 nanoparticles (NPs) of various sizes, specific stoichiometric and non-stoichiometric Fe:Ni surface ratios are synthesized. we will use a combination of ultra-high vacuum surface analysis techniques, such as time-of-flight secondary ion mass spectrometry (TOF-SIMS) and X-ray photoelectron spectroscopy (XPS), to obtain the detailed characterization of the OER electrocatalysts top-surface layer, which is required to identify the rate-limiting step intermediates, and surface morphological changes at the electrolyte/catalyst. T2 - SALSA Make&Measure 2022 CY - Berlin, Germany DA - 15.09.2022 KW - ToF-SIMS KW - FeNi nanoparticles PY - 2022 AN - OPUS4-56157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schusterbauer, Robert T1 - Correlative chemical imaging to reveal the nature of different commercial graphene materials N2 - Since the original report in 2004 by Novoselov and Geim, Graphene gained incredible attention due to its fascinating properties. In the past 20 years, the synthesis and functionalization of graphene has evolved significantly[3]. Different synthesis techniques were developed which led to other graphenerelated 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 kindly 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 (Figure b). 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 - ECASIA 2024 CY - Gothenburg, Sweden DA - 09.06.2024 KW - Correlative imaging KW - ToF-SIMS KW - SEM KW - Graphene oxide flakes KW - Raman PY - 2024 AN - OPUS4-60680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - John, Elisabeth T1 - Exploring the SIMS Matrix Effect in High-Entropy Alloy Thin-Films N2 - Compared with traditional alloys, which typically consist of one or two main elements and small amounts of secondary elements, High Entropy Alloys (HEA) are characterized by the presence of multiple principal elements in almost equal proportions. This unique composition results in a high degree of disorder at the atomic level, leading to exceptional mechanical, physical, and often unexpected properties. HEAs have garnered significant attention in materials science and engineering due to their potential applications in a wide range of industries, from aerospace and automotive to electronics and renewable energy. Analyzing materials composed of multiple elements with spectroscopic techniques such as X-ray Photoelectron Spectroscopy (XPS), Auger-Electron Spectroscopy (AES) or Electron Probe Microanalysis (EPMA), can be challenging due to spectral overlap. This challenge reaches its peak if neighboring 3d elements are present, as it is the case for the famous Cantor alloy which is composed of Cr, Mn, Fe, Co and Ni. Moreover, each analytical method introduces its own set of challenges, e.g., the strong secondary fluorescence effect for neighbor elements in EPMA, thus, making the accurate elemental quantification in such materials difficult. If the material is available as thin film, additional constraints are inherently present. To provide a reference material for these analytical challenges HEAs are excellent candidates. Currently, there is no thin film reference available containing more than two elements. Our goal is to prepare thin films with a homogeneous thickness and defined, homogenous chemical composition to be analyzed by various methods dedicated to surface analysis. ToF-SIMS is an excellent method for the (3D) analysis of thin films, however due to the dependence of element ion yield on the surrounding chemical state i.e., the matrix effect, it is considered a non-quantitative method. In HEAs the elements are each present in a homogenous matrix which makes these materials interesting for investigation of the matrix effect. Moreover, we evaluate methods to minimize the disturbances of oxygen enhancement during the beginning of the sputter analysis and the effect of recoil mixing at the film/substrate interface with the aim to measure accurate depth profiles. T2 - SIMS 24 CY - La Rochelle, France DA - 09.09.2024 KW - High-entropy alloy KW - ToF-SIMS KW - Matrix Effect PY - 2024 AN - OPUS4-62511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -