TY - CHAP A1 - Radnik, Jörg ED - Wandelt, K. T1 - X-ray photoelectron spectroscopy for investigation of heterogeneous catalytic process N2 - Heterogeneous catalysis is a key technology in modern industrial societies. The main steps of a catalytic process take place at the surfaces of complex materials. For the investigations of these surfaces X-ray photoelectron spectroscopy is widely used and fits ideally. At some suitable examples, it will be explained how XPS can help to understand such catalysts better. The focus is on selective oxidation catalysts, one of the main challenges of present research. Here it will illustrate, how changes in the near surface region influence the catalyst performance and, herewith the different stages (activation, maximum performance and deactivation) in the life of catalysts. Additionally, it will be stressed out how important information at different depth regions (surface, near-surface region, bulk) can be useful for comprehensive understanding of the material. Another important subject is nanostructured catalysts with molecular sieves as supports or defined complexes as precursors. Finally, the combination of XPS with other methods used in the analysis of catalysts, e.g. electron microscopy, X-ray absorption spectroscopy and low energy ion scattering will be discussed. KW - X-ray photoelectron spectroscopy KW - Depth information KW - Heterogeneous catalysis KW - Structure-properties relationships PY - 2018 SN - 978-0-12-809739-7 VL - 1 SP - 607 EP - 614 PB - Elsevier AN - OPUS4-44876 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hansen, B. A1 - Hodoroaba, Vasile-Dan T1 - Analysis of a certified copper alloy with Micro-XRF on SEM N2 - Copper alloys have found widespread application in various fields. The elemental composition determines the properties of the alloys and consequently their application. Therefore, knowing the composition of a copper alloy is very important. Metrological institutes like the BAM (German Federal Institute for Materials Research and Testing) offer reference materials that can be used to prove the accuracy of the applied analysis method. The aim of this application note is to demonstrate how Micro-X-ray fluorescence spectroscopy (Micro-XRF) expediently supplements the analysis of copper alloys by using Bruker’s micro-focus X-ray source XTrace attached to a scanning electron microscope (SEM) and operating with an energy dispersive spectrometer. KW - XRF KW - µ-XRF KW - SEM/EDX KW - Copper alloy PY - 2018 UR - https://www.bruker.com/fileadmin/user_upload/8-PDF-Docs/X-rayDiffraction_ElementalAnalysis/Microanalysis_EBSD/LabReports/App_mxrf_sem_03_analysis_Cu_alloy_lores.pdf SP - 1 EP - 4 PB - Bruker Nano GmbH CY - Berlin AN - OPUS4-44677 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Donėlienė, J. A1 - Rudzikas, M. A1 - Rades, Steffi A1 - Dörfel, Ilona A1 - Peplinski, Burkhard A1 - Sahre, Mario A1 - Pellegrino, F. A1 - Maurino, V. A1 - Ulbikas, J. A1 - Galdikas, A. A1 - Hodoroaba, Vasile-Dan T1 - Morphology and structure of TixOy nanoparticles generated by femtosecond laser ablation in water N2 - In this work femto-second pulsed laser ablation in liquid (PLAL) procedure for the generation of titanium oxide nanoparticles (NP) is reported with the purpose of understanding morphology and structure of the newly generated NPs. Ablation duration was varied for optimization of NP generation processes between 10 and 90 min. Surface morphology of NPs as well as their size and shape (distribution) were analysed by various complementary electron microscopy techniques, i.e. SEM, TSEM and TEM. The crystalline structure of titanium oxide particles was investigated byXRD(two instruments operated in different geometries) and HR-TEM. Concentration of generated titanium oxide NPs in liquid was analysed by ICP-MS. A mix of crystalline (mainly anatase), partly crystalline and amorphous spherical titanium oxide NPs can be reported having a mean size between 10 and 20 nm, which is rather independent of the laser ablation (LA) duration. A second component consisting of irregularly shaped, but crystalline titanium oxide nanostructures is co-generated in the LA water, with more pronounced occurrence at longer LA times. The provenance of this component is assigned to those spherical particles generated in suspension and passing through the converging laser beam, being hence subject to secondary irradiation effects, e. g. fragmentation. KW - Titanium oxide KW - Nanoparticles KW - Laser ablation in liquid KW - Particle morphology KW - Nanoparticle structure PY - 2018 DO - https://doi.org/10.1088/2053-1591/aaba56 SN - 2053-1591 VL - 5 IS - 4 SP - 045015-1 EP - 045015-12 PB - IOP Publishing CY - London, UK AN - OPUS4-44678 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit A1 - Dietrich, P. A1 - Thissen, A. A1 - Schwibbert, Karin A1 - Unger, Wolfgang T1 - Quantitative biocide profile measurements by calibrated NAP-XPS N2 - Progress update for the EMPIR-project MetVBadBugs- Quantitative measurement and imaging of drug-uptake by bacteria with antimicrobial resistance. T2 - MetVBadBugs 26 M project meeting CY - South Mimms, UK DA - 05.07.2018 KW - Biofilms KW - Alginate KW - Antibiotics KW - E. coli KW - XPS PY - 2018 AN - OPUS4-45402 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Salge, T. A1 - Wäsche, Rolf A1 - Hodoroaba, Vasile-Dan T1 - Advanced light element and low energy X-ray analysis of a TiB2 – TiC – SiC ceramic material using EDS spectrum imaging N2 - The accurate EDS microanalysis of light elements such as boron and carbon by spectrum imaging will be demonstrated using a sintered hard ceramic material composed of the three major phases titanium boride (TiB2), titanium carbide (TiC), silicon carbide (SiC) and minor phases, sub-μm in size. The combination of these three materials leads to improved mechanical and tribological properties. Silicon carbide is a material used for mechanical seals. It has the disadvantage of reduced failsafe running functions, causing increased wear when running dry. The added titanium components (TiC and TiB2) improve the failsafe running functions. This technology has already been transferred to industrial applications. KW - EDS KW - Spectrum imaging KW - Ceramic KW - Phase analysis KW - Light elements PY - 2018 UR - https://www.bruker.com/fileadmin/user_upload/8-PDF-Docs/X-rayDiffraction_ElementalAnalysis/Microanalysis_EBSD/LabReports/App_eds_10_LE_keramik_Rev1_1_lores.pdf SP - 1 EP - 5 CY - Berlin AN - OPUS4-44622 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Terborg, R. A1 - Hodoroaba, Vasile-Dan T1 - Analysis of the elemental composition and thickness of a Fe-Ni film on Si using Bruker ESPRIT and SAMx STRATAGem N2 - Quantitative analysis of a bulk sample requires that the composition of the sample is homogeneous over the analyzed volume. For inhomogenous samples the calculation of the matrix effects is not correct and this can lead to wrong results in the element concentrations. For samples containing a layer structure a different quantitative evaluation has to be applied. This can be provided with the standard-based analysis in ESPRIT in combination with the STRATAGem software. KW - Thin film analysis KW - SEM/EDX KW - EPMA KW - k-values PY - 2018 UR - https://www.bruker.com/products/x-ray-diffraction-and-elemental-analysis/eds-wds-ebsd-sem-micro-xrf-and-sem-micro-ct/quantax-eds-for-sem/applications/layer-analysis.html SP - 1 EP - 4 CY - Berlin AN - OPUS4-44594 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit A1 - Unger, Wolfgang T1 - New work item proposal for a technical report for ISO/TC 201 WG4 “Surface characterization of biomaterials”: Surface chemical analysis – Surface chemical analysis of cells and biofilms N2 - The proposed ISO Technical Report provides a description of a variety of physical methods of analytical chemistry by which bacteria and biofilms can be analysed. The state of the art, sample requirements and strengths associated with each method are identified. Presented at the DIN-meeting for NA 062-08-16 AA „Chemische Oberflächenanalyse und Rastersondenmikroskopie“ T2 - 18. Sitzung des DIN-meeting NA 062-08-16 AA "Chemische Oberflächenanalyse und Rastersondenmikroskopie“ CY - Berlin, Germany DA - 08.11.2018 KW - 3D nano SIMS KW - Fourier transform infrared spectroscopy KW - Raman-spectroscopy KW - Biofilms KW - XPS PY - 2018 AN - OPUS4-46548 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja A1 - Unger, Wolfgang A1 - Wirth, Thomas A1 - Kjaervik, Marit A1 - Cant, D. A1 - Shard, A. A1 - Clifford, C. T1 - Measurement of the thickness and nature of nanoparticle coatings - ISO/PWI TR 23173 N2 - This presentation explains the outline and scientific content of the ISO technical report 23173 "Measurement of the thickness and nature of nanoparticle coatings using electron spectroscopies". This technical report deals with those electron spectroscopy methods that are able to determine the coating thickness of nanoparticles. This specifically includes X-ray photoelectron spectroscopy (XPS), energy-resolved X-Ray photoelectron spectroscopy (ERXPS) using synchrotron radiation, near abient pressure photoelectron spectroscopy (NAPXPS) and Auger electron spectroscopy (AES). T2 - 18. Sitzung des DIN-Normenausschusses 062-08-16 AA CY - Berlin, Germany DA - 08.11.2018 KW - Core-shell nanoparticles KW - Electron spectroscopy KW - XPS KW - Synchrotron radiation KW - AES PY - 2018 AN - OPUS4-46550 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Nanoanalytik-Aktivitäten @ BAM N2 - In dieser Präsentation werden Aktivitäten im Bereich der 'nano'-Charakterisierung bei der BAM vorgestellt. Beispiele von F&E-Projekten und -Kooperationen im nano-Analytik-Bereich bei der BAM werden genannt. Thematische Kooperations-Möglichkeiten zwischen BAM und dem Netzwerk NanoAnalytik und -Messtechnik in der Produktion werden diskutiert. T2 - Treffen des Netzwerkes NanoAnalytik und -Messtechnik CY - Berlin, Germany DA - 06.11.2018 KW - Nanoanalytik KW - Nano-Projekte KW - Nano-Kompetenzzentrum KW - Nano-Charakterisierung PY - 2018 UR - https://www.nanoinitiative-bayern.de/nanoanalytik/ AN - OPUS4-46563 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja A1 - Saleh, Maysoon I. A1 - Unger, Wolfgang T1 - Investigation of core-shell nanoparticles using a combination of scanning Auger microscopy (SAM) and scanning electron microscopy (SEM) N2 - Products containing engineered nanoparticles already encounter us in most areas of our daily life including cosmetics, clothing, detergents, paints, batteries and displays. In most cases the particles exhibit a core-shell morphology either voluntarily or involuntarily. The properties of the nanoparticle shell determine the interaction with their environment and, thus, reliable control over these properties means reliable control over the particles performance and their toxicity. Therefore, sophisticated techniques to measure thickness and elemental composition of the nanoparticle shell are urgently required. Scanning Auger microscopy (SAM) is a powerful technique with a lateral resolution below 10 nm and a chemical contrast based on the characteristic kinetic energy of Auger electrons related to specific atomic levels and, thus, to a specific element. This work explores the potential of SAM for characterizing the core-shell structure of nanoparticles. A sample system of upconversion NaYF4:Yb,Er cores coated with SiO2 is investigated. Auger spectra, line scans and elemental maps of single nanoparticles will be presented. Challenges encountered will be highlighted, such as damage to the sample by electron beam irradiation. Scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) are performed on the same samples, in order to verify the SAM results. T2 - BAM PhD Retreat CY - Warnemünde, Germany DA - 28.09.2018 KW - Core-shell nanoparticles KW - SAM KW - SEM KW - Surface analysis PY - 2018 AN - OPUS4-46270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas A1 - Müller, Anja A1 - Unger, Wolfgang T1 - Chemical characterisation of (core-shell) nanoparticles using PCA assisted ToF-SIMS and XPS N2 - The analysis of nanomaterials is currently an important task - especially in case of risk assessment – as the properties of these material class are not well understood. The rather high surface area of these objects renders their interactions significantly different to their corresponding bulk. Thus, the surface’s chemical composition must be investigated to get a better understanding and prediction of the nanomaterials’ behavior. ToF-SIMS and XPS have proven to be powerful tools to determine the general chemical composition. The superior surface sensitivity of ToF-SIMS furthermore allows us to study mainly the utmost atomic layers and thus gives us an idea of the interactions involved. Here, we present initial data on the analysis of Hyflon®-polystyrene core-shell nanoparticles which can be used as a model system due to the known preparation and a rather good chemical as well as physical separation of core and shell. Furthermore, results on Au nanoparticles with and without an antibody shell are presented. Principle component analysis (PCA) will be used to detect the influence of sample preparation and for a better separation of different samples. ToF-SIMS imaging is desired to be implemented for single particle detection as well. T2 - 3rd NanoSafety Forum for Young Scientists CY - Valetta, Malta DA - 08.09.2018 KW - Nanoparticles KW - ToF-SIMS KW - XPS PY - 2018 AN - OPUS4-46248 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Overview on the most advanced and suitable NanoDefine measurement methods N2 - The EC Recommendation on the definition of nanomaterial, based solely on size of the constituent particles, foresees development of harmonised measurement methods ensuring ‘consistent results across materials and over time’. The EU/FP7 research project NanoDefine has been exclusively dedicated to support the implementation of this EC Recommendation for the European Union’s legislation. For the first time, measurement techniques able to determine the size of nanoparticles have been evaluated systematically on a well-defined set of quality control materials (spherical, monodisperse) as well as industrial materials of complex shapes and considerable polydispersity. Particularly based on the analytical performance of the measurement techniques as tested on the challenging real-world particulate materials, it was possible to formulate recommendations for use of a new tiered approach consisting of screening and confirmatory techniques. Thus, a consistent framework of guidance for nanomaterial identification according to the EC Definition has been issued in form of the NanoDefiner e-tool, with a transparent decision flow scheme and an extensive user manual. Selected examples of analysis and classification as nano-/non-nanomaterials will be given, highlighting the limits of applicability of the available measurement techniques in dependence on sample properties. On some recent relevant developments in sample preparation – as a crucial part for an accurate analysis - will be also reported. T2 - VCI-NanoDefine Follow-up Meeting CY - VCI, Frankfurt am Main, Germany DA - 25.09.2018 KW - Nanoparticles KW - Nanomaterial KW - EC definition of nanomaterial KW - Nanoparticle size distribution PY - 2018 AN - OPUS4-46251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - EMPIR nPSize - improved traceability chain of nanoparticle size measurements - Is a liaison to CEN/TC 352 nanotechnologies useful? N2 - The main objectives of the new EMPIR project nPSize are to establish EU capability of traceable measurement of NP size and shape, lower uncertainties of NP size measurement by developement of new nano-CRMs, new models (physical and machine learning), 3D method combination, and also by new ISO and CEN standards on accurate NP size measurement and guidance and knowledge transfer. The envisaged outcomes of the project will be presented and their suitability will be discussed to be taken over as pertinent contributions to normative projects within CEN/TC 352 Nanotechnologies. T2 - Joint Working Groups and 24th CEN/TC 352 Nanotechnologies Meetings CY - DIN, Berlin, Germany DA - 09.10.2018 KW - Nanoparticles KW - Size KW - Particle size distribution KW - Particle shape KW - Traceability KW - Standardisation KW - CEN/TC 352 Nanotechnologies PY - 2018 AN - OPUS4-46252 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Procop, Mathias T1 - Check of the energy-dispersive X-ray spectrometers (EDS) performance with the BAM test material EDS-TM001/2 and BAM software EDS spectrometer test N2 - The test material EDS-TM001 together with an accompanying software package, “EDX spectrometer check”, have been made available in 2009 by BAM to be employed by EDS (energy dispersive spectrometer) users to check the performance of an EDS attached to the SEM. Particularly for test laboratories operating under accreditation schemes like ISO/IEC 17025, a periodical control of the critical instrumental parameters in end-user laboratories is required. With EDS-TM001 or EDS-TM002 (second generation) test material, this periodical check is reduced to the acquisition of only one 10 kV spectrum. The software “EDX spectrometer check” is destined to evaluate automatically this spectrum and determine the performance of the EDS in terms of energy resolution and calibration as well as possible alteration of low-energy efficiency due to detector contamination. Energy resolution can be compared with the specified values according to the international ISO standard ISO 15632:2012. EDS-TM is a synthetic material consisting of a thick layer of C, Al, Mn, Cu and Zr in a well-defined composition, deposited on a steel (in case of EDS-TM001) or silicon (in case of EDS-TM002) substrate. Meanwhile, more than one hundred laboratories (most of them located in Germany) use the EDS-TM001 or EDS-TM002 test material for the periodical check of their EDS. A detailed description of the test material and software together with examples of application was published recently. New results and gained experiences will be presented as well. T2 - BERM-15: International Symposium on Biological and Environmental Reference Materials CY - Berlin, Germany DA - 24.09.2018 KW - EDS KW - SEM/EDX KW - Test material KW - EDS-TM001 KW - EDS-TM002 KW - EDS Spectrometer Test KW - X-rays PY - 2018 AN - OPUS4-46253 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mino, L. A1 - Pellegrino, F. A1 - Rades, Steffi A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan A1 - Spotto, G. A1 - Maurino, V. A1 - Martra, G. T1 - Beyond shape engineering of TiO2 nanoparticles: Post-synthesis treatment dependence of surface hydration, hydroxylation, Lewis acidity and photocatalytic activity of TiO2 anatase nanoparticles with dominant {001} or {101} facets N2 - TiO2 anatase nanoparticles are among the relevant players in the field of light-responsive semiconductor nanomaterials used to face environmental and energy issues. In particular, shape-engineered TiO2 anatase nanosheets with dominant {001} basal facets gained momentum because of the possibility to exploit different and/or improved functional behaviors with respect to usual bipyramidal TiO2 anatase nanoparticles, mainly exposing {101} facets. Nevertheless, such behavior depends in a significant extent on the physicochemical features of surfaces exposed by nanosheets. They can vary in dependence on the presence or removal degree of capping agents, namely, fluorides, used for shape-engineering, and experimental investigations in this respect are still a few. Here we report on the evolution of interfacial/ surface features of TiO2 anatase nanosheets with dominant {001} facets from pristine nanoparticles fluorinated both in the bulk and at their surface to nanoparticles with F− free surfaces by treatment in a basic solution and to totally F− free nanoparticles by calcination at 873 K. The nanoparticles fluorine content and its subsequent evolution is determined by complementary techniques (ion chromatography, TOF-SIMS, XPS, AES, SEM-EDX), probing different depths. In parallel, the evolution of the electronic properties and the Ti valence state is monitored by UV−vis spectroscopy and XPS. The calcination treatment results in {001} facets poorly hydroxylated, hydrated, and hydrophilic, which appear as surface features consequent to the expected (1 × 4) reconstruction. Moreover, IR spectroscopy of CO adsorbed as probe molecule indicates that the Lewis acidity of Ti4+ sites exposed on (1 × 4) reconstructed {001} facets of calcined TiO2 nanosheets is weaker than that of cationic centers on {101} facets of bipyramidal TiO2 anatase nanoparticles. The samples have also been tested in phenol photodegradation highlighting that differences in surface hydration, hydroxylation, and Lewis acidity between TiO2 nanoparticles with nanosheet (freed by F− by calcination at 873 K) and bipyramidal shape have a strong impact on the photocatalytic activity that is found to be quite limited for the nanoparticles mainly exposing (1 × 4) reconstructed {001} facets. KW - Nanoparticles KW - TiO2 KW - F- doping KW - Shape-controlled nanoparticles KW - Nanosheets PY - 2018 DO - https://doi.org/10.1021/acsanm.8b01477 SN - 2574-0970 VL - 1 IS - 9 SP - 5355 EP - 5365 PB - ACS Publications CY - Washington, DC, U.S.A. AN - OPUS4-46157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - Hydrogen assisted cracking phenomena in duplex stainless steels elucidated by in- and ex-situ ToF-SIMS experiments N2 - In the presented research, the high potential and abilities of secondary ion mass spectrometry (ToF-SIMS) to detect and locally map the hydrogen distribution in two types of duplex stainless steels are shown. The research validates certain proposed mechanisms by combining ToF-SIMS with high-resolution scanning electron microscopy and electron-backscattered diffraction. The combination of data from several techniques on the same region was conducted in this field for the first time by applying data treatment of the ToF-SIMS raw data and data fusion approach. This powerful combination of methods allows reviewing of the occurring processes related to hydrogen assisted cracking. The step beyond the state of the art in this field was gained here by developing permeation and mechanical loading experiments within the ToF-SIMS during chemometric imaging of the hydrogen distribution in the microstructure. The research presents the necessary correlation between the hydrogen distribution and the resulted structural changes, the diffusion behavior in a duplex microstructure and stress induced diffusion of hydrogen by applying external load at the microscale. T2 - 6th WMRIF Early Career Scientist Summit CY - NPL Teddington UK DA - 18.06.2018 KW - ToF-SIMS KW - Duplex stainless steel KW - LDX KW - EBSD KW - Data-fusion PY - 2018 AN - OPUS4-46865 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded A1 - Böllinghaus, Thomas T1 - BAM’s role in materials science and hydrogen in metals: TOF-SIMS imaging N2 - Due to its low mass and high diffusivity in presence of compositional, thermal and mechanical gradients, hydrogen within a metallic microstructure can result in severe loss in ductility even at low concentrations and might lead eventually to a catastrophic and unpredictable failure of structural components during service. In this context, hydrogen mapping at the microscale is still considered among the most important challenges on the pathway towards a better understanding of the hydrogen transport and assisted cracking phenomena in metals, specifically in structural components, e.g. steels. Among the very few available techniques to localize hydrogen at the microscale, Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was proven to be a reliable tool. Based on the assumption that deuterium influence the microstructure similarly to hydrogen, in the following contribution ToF-SIMS was applied as the main technique to detect and locally map the deuterium distribution in several alloys: lean 2101 and standard 2205 duplex stainless steel (DSS), AISI 304L austenitic stainless steel and titanium 6Al-4V alloy. These alloys were selected as case studies in this work due to the wide use of them in many applications and environments which frequently provide critical conditions for hydrogen absorption and assisted degradation. The innovative design of in-situ and ex-situ experiments enabled us to elucidate the permeation, transport and trapping of deuterium in the microstructure in sub-micron resolution for the first time. In addition to the novel experimental setups, further progress was gained by applying computational multivariate data analysis (MVA) on the raw data and data fusion with high resolution structural characterization methods (scanning electron microscopy and electron back-scattered diffraction – SEM/EBSD). This combination allowed us to correlate the deuterium distribution and the influence on the microstructure. T2 - 4th Symposium on Innovative Measurement and Analysis for Structural Materials CY - Tokyo, Japan DA - 13.11.2018 KW - ToF-SIMS KW - Duplex stainless steel KW - Austenitic stainless steel KW - Principal Component Analysis KW - Data-fusion PY - 2018 UR - https://unit.aist.go.jp/tia-co/project/SIP-IMASM/sympo/2018/index.html AN - OPUS4-46867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas T1 - BAM and Division 6.1 N2 - This is a short overview of BAM and Division 6.1. We have insight into BAM's roles and responsibilities and the work we are doing in Division 6.1. T2 - Visit at CSEM Landquart CY - Landquart, Switzerland DA - 13.08.2018 KW - ToF-SIMS KW - AES KW - XPS KW - SEM PY - 2018 AN - OPUS4-46765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit A1 - Dietrich, P. A1 - Thissen, A. A1 - Schwibbert, Karin T1 - Surface characterisation of biological samples by near-ambient pressure XPS N2 - A presentation held for the seminar "Ausgewählte analytische Methoden der Physik" hosted by Prof. Birgit Kanngießer at TU Berlin. The first part focus on depth-dependent XPS-measurements (XPS, synchrotron HAXPES) to obtain a concentration profile of iodine in an artificial biofilm. In the second part, NAP-XPS measurements of various bacterial samples are presented. T2 - Forschungsseminar "Ausgewählte analytische Methoden der Physik", TU Berlin CY - Berlin, Germany DA - 17.07.2018 KW - Biofilms KW - Alginate KW - Agarose KW - HAXPES KW - NAP-XPS PY - 2018 AN - OPUS4-45505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Huang, M.-D. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Lippitz, Andreas A1 - Hodoroaba, Vasile-Dan A1 - Schmid, Thomas A1 - Heinrich, Hans-Joachim A1 - Recknagel, Sebastian A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Zirconium permanent modifiers for graphite furnaces used in absorption spectrometry: understanding their structure and mechanism of action N2 - The mechanism of action of zirconium permanent modifiers on graphite surfaces was investigated in order to understand its influence on the analytical signal in atomic and molecular absorption spectrometry (AAS/MAS). For this, the molecule formation of CaF was studied, which is used for the indirect analytical determination of fluorine in high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). The kinetics of this reaction was established by monitoring its molecular spectrum at different atomisation temperatures. An Arrhenius plot showed a pseudo-first order reaction with respect to fluorine (n = 1). An intermediate state was isolated, and its structure was elucidated by spectroscopic methods: scanning electron microscopy with energy dispersive X-ray spectroscopy (SEMEDX), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XANES and EXAFS), and Raman microspectroscopy. We propose here a mechanism, where ZrO2 acts as a heterogeneous catalyst: after a pyrolytic step, an intermediate state of ZrO(OCaF) is activated, and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface. No evidence of the formation of zirconium carbide was found. Consequently, as the CaF formation is catalysed by a heterogeneous catalyst, surface modifications with ZrO2 nanoparticles and ZrO xerogels were investigated in order to increase the surface area. Their influence was evaluated in the molecule formation of CaF, CaCl, CaBr, and CaI. Graphite furnace modification with zirconium oxide nanoparticles proves to be the best choice for fluorine analysis with a signal enhancement of more than eleven times with respect a non-coated graphite furnace. However, the influence of zirconium modifications in the analytical signals of Cl, and I is lower than the F signals or even negative in case of the Br. Understanding zirconium modifiers as heterogeneous catalysts offers a new perspective to AAS and MAS, and reveals the potential of surface analytical methods for development of improved permanent modifiers and graphite furnace coatings. KW - Zirconium KW - HR-CS-MAS KW - Graphite furnace KW - Nanoparticles KW - Xerogel KW - Calcium monofluoride KW - Absorption spectrometry PY - 2018 UR - https://pubs.rsc.org/en/content/articlelanding/2018/ja/c8ja00190a DO - https://doi.org/10.1039/C8JA00190A SN - 0267-9477 VL - 33 IS - 12 SP - 2034 EP - 2042 PB - Royal Society of Chemistry AN - OPUS4-46775 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -