TY - JOUR A1 - Kovacevic, E. A1 - Strunskus, T. A1 - Santhosh, N. M. A1 - Zavasnik, Z. A1 - Unger, Wolfgang A1 - Sauvage, T. A1 - Ammar, M.-R. A1 - Cvelbar, U. A1 - Berndt, J. T1 - Thermal stability studies of plasma deposited hydrogenated carbon nitride nanostructures JF - Carbon N2 - Thermally stable carbon nitride nanostructures have potential applications in surface coatings and automotive fields. In this work, hydrogenated nitrogen-rich carbon nitride nanoparticles have been synthesised via low-pressure low-power plasma vapour deposition technique from methane/Nitrogen gas mixture in a dry process. Thermal stability of the initially prepared hydrogenated carbon Nitride structures has been analysed by near-edge X-ray absorption fine-structure spectroscopy (NEXAFS, insitu), Raman spectroscopy, scanning and transmission electron microscopy and nuclear reaction Analysis (NRA). Thermal studies reveal the excellent stability of the material and nitrogen-rich characteristics (N/C ratio 0.5e0.2 ± 0.01). The obtained results suggest transformation of sp3-rich as-deposited carbon Nitride into sp2-carbon phase with more graphitic features upon thermal annealing. Such in-situ thermal studies of plasma deposited carbon nitrides confirm the conversion of sp3-rich phase to sp2-rich carbon phase at the critical temperature (about 450 K), without a huge loss in nitrogen content. The analysis revealed that the material is a stable plasma deposit after this critical temperature up to >1100 K. Additionally, super hydrophilic carbon nitride nanostructure transforms into a hydrophobic surface after thermal annealing. These thermally stable hydrophobic carbon nitride nanoparticles could be used as a promising material for the hydrophobic coatings for various applications, especially for harsh conditions. KW - Carbon nanoparticles KW - Hydrogenated nanostructures KW - Plasma deposition KW - NEXAFS KW - Thermal annealing PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-536163 DO - https://doi.org/10.1016/j.carbon.2021.08.008 SN - 0008-6223 VL - 184 SP - 82 EP - 90 PB - Elsevier Ltd. AN - OPUS4-53616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Senoner, M. A1 - Stockmann, Jörg M. A1 - Fernandez, V. A1 - Fairley, N. A1 - Passiu, C. A1 - Spencer, N. D. A1 - Rossi, A. T1 - Summary of ISO/TC 201 International Standard ISO 18516:2019 Surface chemical analysis - Determination of lateral resolution and sharpness in beam-based methods with a range from nanometres to micrometres and its implementation for imaging laboratory X-ray photoelectron spectrometers (XPS) JF - Surface and interface analysis N2 - ISO 18516:2019 Surface chemical analysis—Determination of lateral resolution and sharpness in beam-based methods with a range from nanometres to micrometres revises ISO 18516:2006 Surface chemical analysis—Auger electron spectroscopy and X-ray photoelectron spectroscopy—Determination of lateral resolution. It implements three different methods delivering parameters useful to express the lateral resolution: (1) the straight edge method, (2) the narrow line method and (3) the grating method. The theoretical background of these methods is introduced in ISO/TR 19319:2013 Surface chemical analysis—Fundamental approaches to determination of lateral resolution and sharpness in beam-based methods. The revised International Standard ISO 18516 delivers standardized procedures for the determination of the (1) effective lateral resolution by imaging of square-wave gratings, the (2) lateral resolution expressed as the parameter D12–88 characterizing the steepness of the sigmoidal edge spread function (ESF) determined by imaging a straight edge and (3) the lateral resolution expressed as the full width of half maximum of the line spread function (LSF), wLSF, determined by imaging a narrow line. The last method also delivers information on the shape of the LSF, which characterizes an individual imaging instrument. Finally, the implementation of all three standardized methods in the field of imaging laboratory X-ray photoelectron spectroscopy (XPS) is shortly presented. This part of the letter is based on the use of a new test sample developed at ETH Zurich, Switzerland. This test sample displays a micrometre scaled pattern motivated by the resolving power of recent imaging XPS instruments. KW - Grating method KW - Imaging AES KW - Imaging SIMS KW - Imaging XPS KW - Lateral resolution KW - Narrow line method KW - Noise in image KW - Resolution criterion KW - Straight edge method PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-536330 DO - https://doi.org/10.1002/sia.7025 SN - 1096-9918 VL - 54 IS - 4 SP - 320 EP - 327 PB - Wiley CY - Chichester AN - OPUS4-53633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Anja A1 - Krahl, T. A1 - Radnik, Jörg A1 - Wagner, Andreas A1 - Werner, W. S. M. A1 - Ritter, B. A1 - Kemnitz, E. A1 - Unger, Wolfgang T1 - Chemical in-depth analysis of (Ca/Sr)F2 core–shell like nanoparticles by X-ray photoelectron spectroscopy with tunable excitation energy JF - Surface and Interface Analysis N2 - The fluorolytic sol–gel synthesis is applied with the intention to obtain two different types of core–shell nanoparticles, namely, SrF2–CaF2 and CaF2–SrF2. In two separate fluorination steps for core and shell formation, the corresponding metal lactates are reacted with anhydrous HF in ethylene glycol. Scanning transmission electron microscopy (STEM) and dynamic light scattering (DLS) confirm the formation of particles with mean dimensions between 6.4 and 11.5 nm. The overall chemical composition of the particles during the different reaction steps is monitored by quantitative Al Kα excitation X-ray photoelectron spectroscopy (XPS). Here, the formation of stoichiometric metal fluorides (MF2) is confirmed, both for the core and the final core–shell particles. Furthermore, an in-depth analysis by synchrotron radiation XPS (SR-XPS) with tunable excitation energy is performed to confirm the core–Shell character of the nanoparticles. Additionally, Ca2p/Sr3d XPS intensity ratio in-Depth profiles are simulated using the software Simulation of Electron Spectra for Surface Analysis (SESSA). In principle, core–shell like particle morphologies are formed but without a sharp interface between calcium and strontium containing phases. Surprisingly, the in-depth chemical distribution of the two types of nanoparticles is equal within the error of the experiment. Both comprise a SrF2-rich core domain and CaF2-rich shell domain with an intermixing zone between them. Consequently, the internal morphology of the final nanoparticles seems to be independent from the synthesis chronology. KW - Metal fluorides KW - Sol-gel synthesis KW - Synchrotron radiation KW - X-ray photoelectron spectroscopy PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522284 DO - https://doi.org/10.1002/sia.6937 SN - 0142-2421 VL - 53 IS - 5 SP - 494 EP - 508 PB - Wiley VCH AN - OPUS4-52228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steiner, S. A1 - Heldt, J. A1 - Sobol, Oded A1 - Unger, Wolfgang A1 - Frömeling, T. T1 - Influence of oxygen vacancies on core-shell formation in solid solutions of (Na,Bi)TiO3 and SrTiO3 JF - Journal of the American Ceramic Society N2 - Solid solutions of (Na,Bi)TiO3 (NBT) and SrTiO3 (ST) are materials of interest for high-strain or high-energy density capacitor applications. Often, they exhibit chemical heterogeneity and develop core-shell structures during regular solid-state synthesis with an NBT-rich core. In this case, the NBT forms first so that the strontium needs to diffuse into the material to reach chemical homogeneity. Depending on the presence of core-shell structures, the electrical properties can vary drastically. In this work, we rationalize the effect of variations in oxygen vacancy concentration by Fe-acceptor and Nb-donor doping. It can be shown that a diffusion couple of strontium and oxygen is responsible for chemical homogenization and that the oxygen vacancy content can control the formation of a core-shell structure. KW - Lead-free ceramics KW - Bismuth titanates KW - Core-shell structures KW - Diffusion/diffusivity KW - Ferroelectricity/ferroelectric materials PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525988 DO - https://doi.org/10.1111/jace.17845 SP - 1 EP - 10 PB - Wiley Periodicals LLC, John Wiley & Sons, Inc. AN - OPUS4-52598 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kjaervik, Marit A1 - Ramstedt, M. A1 - Schwibbert, Karin A1 - Dietrich, P. M A1 - Unger, Wolfgang T1 - Comparative Study of NAP-XPS and Cryo-XPS for the Investigation of Surface Chemistry of the Bacterial Cell-Envelope JF - Frontiers in Chemistry N2 - Bacteria generally interact with the environment via processes involving their cell-envelope. Thus, techniques that may shed light on their surface chemistry are attractive tools for providing an understanding of bacterial interactions. One of these tools is Al Kα-excited photoelectron spectroscopy (XPS) with its estimated information depth of <10 nm. XPS-analyses of bacteria have been performed for several decades on freeze-dried specimens in order to be compatible with the vacuum in the analysis chamber of the spectrometer. A limitation of these studies has been that the freeze-drying method may collapse cell structure as well as introduce surface contaminants. However, recent developments in XPS allow for analysis of biological samples at near ambient pressure (NAP-XPS) or as frozen hydrated specimens (cryo-XPS) in vacuum. In this work, we have analyzed bacterial samples from a reference strain of the Gram-negative bacterium Pseudomonas fluorescens using both techniques. We compare the results obtained and, in general, observe good agreement between the two techniques. Furthermore, we discuss advantages and disadvantages with the two analysis approaches and the output data they provide. XPS reference data from the bacterial strain are provided, and we propose that planktonic cells of this strain (DSM 50090) are used as a reference material for surface chemical analysis of bacterial systems. KW - P. Fluorescens KW - Cryo XPS KW - NAP-XPS KW - DSM 5009 PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525640 DO - https://doi.org/10.3389/fchem.2021.666161 VL - 9 SP - Article 666161 PB - Frontiers CY - Switzerland AN - OPUS4-52564 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ehlert, Christopher A1 - Holzweber, Markus A1 - Lippitz, Andreas A1 - Unger, Wolfgang A1 - Saalfrank, Peter T1 - A detailed assignment of NEXAFS resonances of imidazolium based ionic liquids JF - Physical Chemistry Chemical Physics N2 - In Near Edge X-Ray Absorption Fine Structure (NEXAFS) spectroscopy X-Ray photons are used to excite tightly bound core electrons to low-lying unoccupied orbitals of the system. This technique offers insight into the electronic structure of the system as well as useful structural information. In this work, we apply NEXAFS to two kinds of imidazolium based ionic liquids ([CnC₁im]⁺[NTf₂]⁻ and [C₄C₁im]⁺[I]⁻). A combination of measurements and quantum chemical calculations of C K and N K NEXAFS resonances is presented. The simulations, based on the transition potential density functional theory method (TP-DFT), reproduce all characteristic features observed by the experiment. Furthermore, a detailed assignment of resonance features to excitation centers (carbon or nitrogen atoms) leads to a consistent interpretation of the spectra. KW - Ionic liquids KW - NEXAFS KW - DFT spectrum simulations PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-367223 DO - https://doi.org/10.1039/c5cp07434g SN - 1463-9076 SN - 1463-9084 VL - 18 IS - 12 SP - 8654 EP - 8661 PB - Royal Society of Chemistry CY - Cambridge, UK AN - OPUS4-36722 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neukammer, J. A1 - Hussels, M. A1 - Kummrow, A. A1 - Devonshire, A. A1 - Foy, C. A1 - Huggett, J. A1 - Parkes, H. A1 - Zel, J. A1 - Milavec, M. A1 - Schimmel, H. A1 - Unger, Wolfgang A1 - Akgoz, M. A1 - McHugh, V. A1 - Grunert, H.-P. A1 - Zeichhardt, H. T1 - Survey results on nucleic acid tests of infectious diseases: present status and need for rapid and patient near diagnostics JF - GMS Zeitschrift zur Förderung der Qualitätssicherung in medizinischen Laboratorien N2 - This survey will discuss current and emerging isothermal and rapid polymerase chain reaction (PCR) based nucleic acid amplification methods for patient near diagnostics. To assess the clinical need of rapid diagnostics for infectious diseases based on nucleic acid tests (NATs) we performed and analysed a questionnaire among laboratories participating in corresponding INSTAND ring trials for external quality assurance. The questions concerning new amplification technologies like isothermal nucleic acid amplification, potentially suited to significantly decrease turnaround times, were complemented by questions to evaluate the present status of NATs. Besides end-users, companies were also addressed by sending out a manufacturer specific questionnaire. Analysis of the answers from 48 laboratories in 14 European countries revealed that a much shorter turnaround time is requested for selected pathogens compared to about 2 h or longer when applying temperature cycling amplification, i.e. PCR. In this context, most frequently mentioned were MRSA, norovirus, influenza A and B viruses, cytomegalovirus (CMV) as well as hepatitis B virus (HBV) and hepatitis C virus (HCV). At present, 8% of the laboratories having participated in this survey apply isothermal amplification of nucleic acid to identify infectious pathogens. KW - Nucleic acid tests KW - Infectious diseases KW - Virus detection KW - Bacteria detection KW - Isothermal nucleic acid amplification KW - Status report KW - Questionnaire KW - NAT KW - PCR PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:0183-lab0000160 UR - http://www.egms.de/static/en/journals/lab/2015-6/lab000016.shtml DO - https://doi.org/10.3205/lab000016 SN - 1869-4241 VL - 6 SP - 1 EP - 11 PB - GMS CY - Düsseldorf AN - OPUS4-36133 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ehlert, Christopher A1 - Unger, Wolfgang A1 - Saalfrank, P. T1 - C K-edge NEXAFS spectra of graphene with physical and chemical defects: a study based on density functional theory JF - Physical chemistry, chemical physics N2 - Recently, C K-edge Near Edge X-ray Absorption Fine Structure (NEXAFS) spectra of graphite (HOPG) surfaces have been measured for the pristine material, and for HOPG treated with either bromine or krypton plasmas (Lippitz et al., Surf. Sci., 2013, 611, L1). Changes of the NEXAFS spectra characteristic for physical (krypton) and/or chemical/physical modifications of the surface (bromine) upon plasma treatment were observed. Their molecular origin, however, remained elusive. In this work we study by density functional theory, the effects of selected point and line defects as well as chemical modifications on NEXAFS carbon K-edge spectra of single graphene layers. For Br-treated surfaces, also Br 3d X-ray Photoelectron Spectra (XPS) are simulated by a cluster approach, to identify possible chemical modifications. We observe that some of the defects related to plasma treatment lead to characteristic changes of NEXAFS spectra, similar to those in experiment. Theory provides possible microscopic origins for these changes. KW - Graphene KW - NEXAFS KW - Spectrum simulation KW - Density functional theory PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-309658 DO - https://doi.org/10.1039/c4cp01106f SN - 1463-9076 SN - 1463-9084 VL - 16 IS - 27 SP - 14083 EP - 14095 PB - The Royal Soc. of Chemistry CY - Cambridge AN - OPUS4-30965 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mozetic, M. A1 - Ostrikov, K. A1 - Ruzic, D.N. A1 - Curreli, D. A1 - Cvelbar, U. A1 - Vesel, A. A1 - Primc, G. A1 - Leisch, M. A1 - Jousten, K. A1 - Malyshev, O.B. A1 - Hendricks, J.H. A1 - Kövér, L. A1 - Tagliaferro, A. A1 - Conde, O. A1 - Silvestre, A.J. A1 - Giapintzakis, J. A1 - Buljan, M. A1 - Radic, N. A1 - Drazic, G. A1 - Bernstorff, S. A1 - Biedermann, H. A1 - Kylián, O. A1 - Hanus, J. A1 - Milosevic, S. A1 - Galtayries, A. A1 - Dietrich, Paul A1 - Unger, Wolfgang A1 - Lehocky, M. A1 - Sedlarik, V. A1 - Stana-Kleinschek, K. A1 - Drmota-Petric, A. A1 - Pireaux, J.J. A1 - Rogers, J.W. A1 - Anderle, M. T1 - Recent advances in vacuum sciences and applications JF - Journal of physics D N2 - Recent advances in vacuum sciences and applications are reviewed. Novel optical interferometer cavity devices enable pressure measurements with ppm accuracy. The innovative dynamic vacuum standard allows for pressure measurements with temporal resolution of 2 ms. Vacuum issues in the construction of huge ultra-high vacuum devices worldwide are reviewed. Recent advances in surface science and thin films include new phenomena observed in electron transport near solid surfaces as well as novel results on the properties of carbon nanomaterials. Precise techniques for surface and thin-film characterization have been applied in the conservation technology of cultural heritage objects and recent advances in the characterization of biointerfaces are presented. The combination of various vacuum and atmospheric-pressure techniques enables an insight into the complex phenomena of protein and other biomolecule conformations on solid surfaces. Studying these phenomena at solid–liquid interfaces is regarded as the main issue in the development of alternative techniques for drug delivery, tissue engineering and thus the development of innovative techniques for curing cancer and cardiovascular diseases. A review on recent advances in plasma medicine is presented as well as novel hypotheses on cell apoptosis upon treatment with gaseous plasma. Finally, recent advances in plasma nanoscience are illustrated with several examples and a roadmap for future activities is presented. KW - Vacuum KW - Surface KW - Plasma KW - Interface KW - Nanoscience PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-304884 DO - https://doi.org/10.1088/0022-3727/47/15/153001 SN - 0022-3727 SN - 1361-6463 VL - 47 IS - 15 SP - 153001-1 EP - 153001-23 PB - IOP Publ. CY - Bristol AN - OPUS4-30488 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinrich, Thomas A1 - Traulsen, Christoph Hans-Henning A1 - Darlatt, Erik A1 - Richter, S. A1 - Poppenberg, J. A1 - Traulsen, N.L. A1 - Linder, I. A1 - Lippitz, Andreas A1 - Dietrich, Paul A1 - Dib, B. A1 - Unger, Wolfgang A1 - Schalley, C.A. T1 - The versatility of 'Click' reactions at surfaces: Molecular recognition at interfaces JF - RSC Advances N2 - In order to investigate molecular recognition on surfaces, an azide-functionalized monolayer was deposited on gold. The monolayer was characterized by X-ray photoelectron spectroscopy (XPS) and angle-resolved near-edge X-ray absorption fine structure (NEXAFS) experiments and the decomposition of the azide upon irradiation with X-ray beams was investigated. Subsequently, various alkyne-functionalized host and guest molecules were attached to the azide by 1,3-dipolar cycloaddition. These modified surfaces and their host–guest chemistry were analysed by XPS and angle-resolved NEXAFS. The reversibility of guest binding was shown for one example as a proof of principle. KW - 'Click' reaction KW - Azide-terminated surfaces KW - SAMs KW - Host guest molecules KW - Molecular recognition at interfaces PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-306463 DO - https://doi.org/10.1039/C4RA01730G SN - 2046-2069 VL - 4 IS - 34 SP - 17694 EP - 17702 PB - RSC Publishing CY - London AN - OPUS4-30646 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rades, Steffi A1 - Hodoroaba, Vasile-Dan A1 - Salge, T. A1 - Wirth, Thomas A1 - Lobera, M.P. A1 - Labrador, R.H. A1 - Natte, Kishore A1 - Behnke, Thomas A1 - Gross, Thomas A1 - Unger, Wolfgang T1 - High-resolution imaging with SEM/T-SEM, EDX and SAM as a combined methodical approach for morphological and elemental analyses of single engineered nanoparticles JF - RSC Advances N2 - The combination of complementary characterization techniques such as SEM (Scanning Electron Microscopy), T-SEM (Scanning Electron Microscopy in Transmission Mode), EDX (Energy Dispersive X-ray Spectroscopy) and SAM (Scanning Auger Microscopy) has been proven to be a powerful and relatively quick characterization strategy for comprehensive morphological and chemical characterization of individual silica and titania nanoparticles. The selected “real life” test materials, silica and titania, are listed in the OECD guidance manual as representative examples because they are often used as commercial nanomaterials. Imaging by high resolution SEM and in the transmission mode by T-SEM allows almost simultaneous surface and in-depth inspection of the same particle using the same instrument. EDX and SAM enable the chemical characterization of bulk and surface of individual nanoparticles. The core–shell properties of silica based materials are addressed as well. Titania nominally coated by silane purchased from an industrial source has been found to be inhomogeneous in terms of chemical composition. KW - surface and in-depth inspection KW - silica nanoparticles KW - titania nanoparticles PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-316296 DO - https://doi.org/10.1039/c4ra05092d SN - 2046-2069 VL - 4 IS - 91 SP - 49577 EP - 49587 PB - RSC Publishing CY - London AN - OPUS4-31629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guo, Y. A1 - Lippitz, Andreas A1 - Saftien, P. A1 - Unger, Wolfgang A1 - Kemnitz, E. T1 - Tuning the surface properties of novel ternary iron(III) fluoride-based catalysts using the template effect of the matrix JF - Dalton transactions N2 - Sol–gel prepared ternary FeF3–MgF2 materials have become promising heterogeneous catalysts due to their porosity and surface Lewis/Brønsted acidity (bi-acidity). Despite the good catalytic performance, nanoscopic characterisations of this type of material are still missing and the key factors controlling the surface properties have not yet been identified, impeding both a better understanding and further development of ternary fluoride catalysts. In this study, we characterised the interaction between the bi-acidic component (FeF3) and the matrix (MgF2) on the nano-scale. For the first time, the formation pathway of FeF3–MgF2 was profiled and the template effect of MgF2 during the synthesis process was discovered. Based on these new insights two novel materials, FeF3–CaF2 and FeF3–SrF2, were established, revealing that with decreasing the atomic numbers (from Sr to Mg), the ternary fluorides exhibited increasing surface acidity and surface area but decreasing pore size. These systematic changes gave rise to a panel of catalysts with tuneable surface and bulk properties either by changing the matrix alkaline earth metal fluoride or by adjusting their ratios to Fe or both. The template effect of the alkaline earth metal fluoride matrix was identified as the most probable key factor determining the surface properties and further influencing the catalytic performance in ternary fluoride based catalysts, and paves the way to targeted design of next-generation catalysts with tunable properties. KW - Catalysis KW - Surface analysis KW - XPS PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-327410 DO - https://doi.org/10.1039/c4dt03229b SN - 1477-9226 SN - 1477-9234 SN - 1364-5447 VL - 44 IS - 11 SP - 5076 EP - 5085 PB - RSC CY - Cambridge AN - OPUS4-32741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schwarz, F. A1 - Heinrich, Thomas A1 - Lippitz, Andreas A1 - Unger, Wolfgang A1 - Schalley, C. T1 - A photoswitchable rotaxane operating in monolayers on solid support JF - Chemical Communication N2 - A novel photoswitchable rotaxane was synthesised and its switching behaviour in solution was analysed with NMR and UV-Vis. A monolayer of rotaxanes was deposited on glass surfaces and the on-surface photoswitching was investigated. Angle-resolved NEXAFS spectra revealed a preferential orientation that reversibly changes upon switching. KW - XPS KW - NEXAFS KW - Photoswitchable rotaxane KW - Self assembly PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-386814 DO - https://doi.org/10.1039/c6cc08586e SN - 0022-4936 SN - 1364-548X SN - 0009-241x SN - 1359-7345 VL - 52 IS - 100 SP - 14458 EP - 14461 PB - Royal Society of Chemistry (RSC) AN - OPUS4-38681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Beiranvand, Z. A1 - Kakanejadifard, A. A1 - Donskyi, Ievgen A1 - Faghani, A. A1 - Tu, Z. A1 - Lippitz, Andreas A1 - Sasanpour, P. A1 - Maschietto, F. A1 - Paulus, B. A1 - Haag, R. A1 - Adeli, M. T1 - Functionalization of fullerene at room temperature: toward new carbon vectors with improved physicochemical properties JF - RSC Advances N2 - In this work, fullerene has been functionalized with cyanuric Chloride at room temperature by a nitrene mediated [2 + 1] cycloaddition reaction. The adduct after functionalization is inherently in the form of azafulleroid and shows broad UV absorption in the wavelength range of 200–800 nm, as well as photothermal conversion and fluorescence with a high quantum yield. KW - Functionalization of fullerenes KW - XPS KW - NEXAFS PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-387076 DO - https://doi.org/10.1039/c6ra23419d SN - 2046-2069 VL - 6 IS - 114 SP - 112771 EP - 112775 PB - Royal Society of Chemistry (RSC) AN - OPUS4-38707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Unger, Wolfgang T1 - Non-destructive surface measurements N2 - Materials and chemical producers require detailed knowledge of surface chemistry for research into new products. One way to understand a surface without damaging it is to bombard it with an electron beam, causing its atoms to emit characteristic X-rays enabling identification. The measurement of these must be precise as many elements emissions are close in energy – traceable reference materials will ensure instruments using this technique are stable and accurate. KW - Metrology KW - EDS KW - EDX PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-388647 UR - http://www.euramet.org/metrology-for-societys-challenges/metrology-for-industry/impact-case-studies-emrp-industry-theme/ SP - 1 EP - 2 CY - Teddington AN - OPUS4-38864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Unger, Wolfgang T1 - IND15 JRP SurfChem: Traceable quantitative surface chemical analysis for industrial applications N2 - The SurfChem project has made a significant contribution to traceable quantitative surface chemical analysis for industrial applications by delivering new certified reference materials and test samples for specific technical applications. Regular performance tests of instruments, metrological methodology for the detection of (bio)organic surface species, ambient and non-destructive surface chemical analysis for in-line process control and new in situ characterisation techniques of catalytically active surfaces have been achieved. KW - Surface analysis KW - Metrology KW - Euramet EMRP PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-388673 UR - http://www.euramet.org/research-innovation/search-research-projects/details/?eurametCtcp_project_show%5Bproject%5D=1115&eurametCtcp_project%5Bback%5D=893&cHash=5fd23fc7f759db18176584b5d8a5fe89 SP - 1 EP - 39 CY - Teddington AN - OPUS4-38867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kjaervik, Marit A1 - Schwibbert, Karin A1 - Dietrich, P. A1 - Thissen, A. A1 - Unger, Wolfgang T1 - Surface characterisation of Escherichia coli under various conditions by near-ambient pressure XPS JF - Surface and Interface Analysis N2 - Bacteria are inherently in a hydrated state and therefore not compatible to ultra-high vacuum techniques such as XPS without prior sample preparation involving freeze drying or fast freezing. This has changed with the development of near-ambient pressure (NAP)-XPS, which makes it possible to characterise the bacterial surface with minimal sample preparation. This paper presents NAP-XPS measurements of Escherichia coli under various NAP conditions: at 11 mbar in a humid environment, at 2 mbar after drying in the chamber, pre-dried at 4 mbar, and at 1 mbar after overnight pumping at 10^−4 mbar. The high-resolution spectra of carbon, nitrogen, and oxygen are presented and found to be in general agreement with XPS measurements from freeze-dried and fast-frozen bacteria. However, it was found that the amount of carbon components associated with polysaccharides increases relative to aliphatic carbon during drying and increases further after overnight pumping. This implies that drying has an impact on the bacterial surface. T2 - European conference on applications of surface and interface analysis (ECASIA'17) CY - Montpellier, France DA - 24.09.2018 KW - Bacteria KW - E. coli KW - NAP-XPS PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-454047 DO - https://doi.org/10.1002/sia.6480 SN - 0142-2421 SN - 1096-9918 VL - 50 IS - 11 SP - 996 EP - 1000 PB - John Wiley & Sons CY - Hoboken, New Jersey, USA AN - OPUS4-45404 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Anja A1 - Swaraj, S. A1 - Sparnacci, K. A1 - Unger, Wolfgang T1 - Shell thickness determination for PTFE‐PS core‐shell nanoparticles using scanning transmission X‐ray microscopy (STXM) JF - Surface and Interface Analysis N2 - A scanning transmission X‐ray microscopy (STXM)‐based methodology is introduced for determining the dimensions (shell thickness, core and total diameter) of core‐shell nanoparticles, which exhibit a strong X‐ray absorption contrast and a well‐defined interface between core and shell material. A low radiation dosage during data acquisition and, therefore, less X‐ray beam‐induced damage of the sample is achieved by recording STXM images only at 2 predetermined energies of maximum Absorption contrast, instead of recording a stack of images across the whole absorption edge. A model core‐shell nanoparticle, polytetrafluoroethylene (PTFE) cores with polystyrene (PS) shell, is used for demonstration. Near‐edge X‐ray absorption fine structure spectroscopy confirms the significant difference in X‐ray absorption behavior between PTFE and PS. Additionally, because of the insolubility of styrene in PTFE a well‐defined interface between particle core and shell is expected. To validate the STXM results, both the naked PTFE cores as well as the complete core‐shell nanoparticles are examined by scanning electron microscopy (SEM). The introduced STXM‐based methodology yields particle dimensions in agreement with the SEM results and provides additional information such as the position of the particle core, which cannot be extracted from a SEM micrograph. T2 - European conference on applications of surface and interface analysis (ECASIA'17) CY - Montpellier, France DA - 24.09.2017 KW - Core-shell nanoparticles KW - Polymers KW - PS KW - PTFE KW - SEM KW - STXM PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-449700 DO - https://doi.org/10.1002/sia.6464 SN - 1096-9918 SN - 0142-2421 VL - 50 IS - 11 SP - 1077 EP - 1082 PB - John Wiley & Sons CY - Hoboken, New Jersey, USA AN - OPUS4-44970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Anja A1 - Sparnacci, K. A1 - Unger, Wolfgang A1 - Tougaard, S. T1 - Determining nonuniformities of core-shell nanoparticle coatings by analysis of the inelastic background of X-ray photoelectron spectroscopy survey spectra JF - Surface and interface analysis N2 - Most real core-shell nanoparticle (CSNP) samples deviate from an ideal core-shell structure potentially having significant impact on the particle properties. An ideal structure displays a spherical core fully encapsulated by a shell of homogeneous thickness, and all particles in the sample exhibit the same shell thickness. Therefore, analytical techniques are required that can identify and characterize such deviations. This study demonstrates that by analysis of the inelastic background in X-ray photoelectron spectroscopy (XPS) survey spectra, the following types of deviations can be identified and quantified: the nonuniformity of the shell thickness within a nanoparticle sample and the incomplete encapsulation of the cores by the shell material. Furthermore, CSNP shell thicknesses and relative coverages can be obtained. These results allow for a quick and straightforward comparison between several batches of a specific CSNP, different coating approaches, and so forth. The presented XPS methodology requires a submonolayer distribution of CSNPs on a substrate. Poly(tetrafluoroethylene)-poly(methyl methacrylate) and poly(tetrafluoroethylene)-polystyrene polymer CSNPs serve as model systems to demonstrate the applicability of the approach. KW - Core-shell KW - Nanoparticles KW - Inelastic background KW - Polymers KW - QUASES KW - XPS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511315 DO - https://doi.org/10.1002/sia.6865 SN - 0142-2421 SN - 1096-9918 VL - 52 SP - 1 EP - 8 PB - Wiley CY - Chichester AN - OPUS4-51131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tu, Z. A1 - Donskyi, Ievgen A1 - Qiao, H. A1 - Zhu, Z. A1 - Unger, Wolfgang A1 - Hackenberger, C. P. R. A1 - Chen, W. A1 - Adeli, M. A1 - Haag, R. T1 - Graphene Oxide-Cyclic R10 Peptide Nuclear Translocation Nanoplatforms for the Surmounting of Multiple-Drug Resistance JF - Advanced Functional Materials N2 - Multidrug resistance resulting from a variety of defensive pathways in Cancer has become a global concern with a considerable impact on the mortality associated with the failure of traditional chemotherapy. Therefore, further research and new therapies are required to overcome this challenge. In this work, a cyclic R10 peptide (cR10) is conjugated to polyglycerol-covered nanographene oxide to engineer a nanoplatform for the surmounting of multidrug resistance. The nuclear translocation of the nanoplatform, facilitated by cR10 peptide, and subsequently, a laser-triggered release of the loaded doxorubicin result in efficient anticancer activity confirmed by both in vitro and in vivo experiments. The synthesized nanoplatform with a combination of different features, including active nucleus-targeting, highloading capacity, controlled release of cargo, and photothermal property, provides a new strategy for circumventing multidrug resistant cancers. KW - Graphen Oxide KW - Nanoplatform KW - Cancer PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510061 DO - https://doi.org/10.1002/adfm.202000933 VL - 30 IS - 35 SP - 2000933 PB - Wiley VCH AN - OPUS4-51006 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stockmann, Jörg M. A1 - Radnik, Jörg A1 - Bütefisch, S. A1 - Busch, I. A1 - Weimann, T. A1 - Passiu, C. A1 - Rossi, A. A1 - Unger, Wolfgang T1 - A new test specimen for the determination of the field of view of small-area X-ray photoelectron spectrometers JF - Surface and Interface Analysis N2 - Small-area/spot photoelectron spectroscopy (SAXPS) is a powerful tool for the investigation of small surface features like microstructures of electronic devices, sensors or other functional surfaces, and so forth. For evaluating the quality of such microstructures, it is often crucial to know whether a small signal in a spectrum is an unwanted contamination of the field of view (FoV), defined by the instrument settings, or it originated from outside. To address this issue, the d80/20 parameter of a line scan across a chemical edge is often used. However, the typical d80/20 parameter does not give information on contributions from the long tails of the X-ray beam intensity distribution or the electron-optical system as defined by apertures. In the VAMAS TWA2 A22 project “Applying planar, patterned, multi-metallic samples to assess the impact of analysis area in surface-chemical analysis,” new test specimen was developed and tested. The here presented testing material consists of a silicon wafer substrate with an Au-film and embedded Cr circular and square spots with decreasing dimensions from 200 μm down to 5 μm. The spot sizes are traceable to the length unit due to size measurements with a metrological SEM. For the evaluation of the FoV, we determined the Au4f intensities measured with the center of the FoV aligned with the center of the spot and normalized to the Au4f intensity determined on the Au-film. With this test specimen, it was possible to characterize, as an example, the FoV of a Kratos AXIS Ultra DLD XPS instrument. T2 - ECASIA 2019 CY - Dresden, Germany DA - 15.09.2019 KW - Field of view KW - Reference material KW - Selected area XPS KW - Small-area XPS KW - Small-spot XPS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509902 DO - https://doi.org/10.1002/sia.6831 SN - 1096-9918 VL - 52 IS - 12 SP - 890 EP - 894 PB - John Wiley & Sons Ltd AN - OPUS4-50990 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ahmed, R. A1 - Vaishampayan, A. A1 - Cuellar-Camacho, J. L. A1 - Wight, D. J. A1 - Donskyi, Ievgen A1 - Unger, Wolfgang A1 - Grohmann, E. A1 - Haag, R. A1 - Wagner, O. T1 - Multivalent Bacteria Binding by Flexible Polycationic Microsheets Matching Their Surface Charge Density JF - Advance Material Interfaces N2 - Aiming at the overall negative surface charge of bacteria, a new strategy of antibacterial agents based on large polymer-modified graphene oxide (GO) sheets is assessed. The presented flexible, polycationic Sheets match the size and charge density of the Escherichia coli surface charge density (2 × 1014 cm−2). These matching parameters create an unspecific but very strong bacteria adsorber by multivalent, electrostatic attraction. Their interaction with bacteria is visualized via atomic force and confocal microscopy and shows that they effectively bind and wrap around E. coli cells, and thereby immobilize them. The incubation of Gram-negative and -positive bacteria (E. coli and methicillin-resistant Staphylococcus aureus, MRSA) with these polycationic sheets leads to the inhibition of proliferation and a reduction of the colony forming bacteria over time. This new type of antibacterial agent acts in a different mode of Action than classical biocides and could potentially be employed in medicinal, technical, or agriculture applications. The presented microsheets and their unspecific binding of cell interfaces could further be employed as adsorber material for bacterial filtration or immobilization for imaging, analysis, or sensor technologies. KW - Surface charge KW - Bacteria KW - Graphene oxide KW - Escherichia coli KW - XPS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509651 DO - https://doi.org/10.1002/admi.201902066 VL - 7 IS - 15 SP - 1902066 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-50965 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sobol, Oded A1 - Straub, F. A1 - Wirth, Thomas A1 - Holzlechner, G. A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang T1 - Real Time Imaging of Deuterium in a Duplex Stainless Steel Microstructure by Time-of-Flight SIMS JF - Nature - Scientific Reports N2 - For more than one century, hydrogen assisted degradation of metallic microstructures has been identified as origin for severe technical component failures but the mechanisms behind have not yet been completely understood so far. Any in-situ observation of hydrogen transport phenomena in microstructures will provide more details for further elucidation of these degradation mechanisms. A novel experiment is presented which is designed to elucidate the permeation behaviour of deuterium in a microstructure of duplex stainless steel (DSS). A hydrogen permeation cell within a TOF-SIMS instrument enables electrochemical charging with deuterium through the inner surface of the cell made from DSS. The outer surface of the DSS permeation cell exposed to the vacuum has been imaged by TOF-SIMS vs. increasing time of charging with subsequent chemometric treatment of image data. This in-situ experiment showed evidently that deuterium is permeating much faster through the ferrite phase than through the austenite phase. Moreover, a direct proof for deuterium enrichment at the austenite-ferrite interface has been found. KW - Characterization and analytical techniques KW - Corrosion KW - Imaging technique KW - Mass spectrometry PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-353872 UR - http://www.nature.com/articles/srep19929 DO - https://doi.org/10.1038/srep19929 SN - 2045-2322 VL - 6 IS - 19929 SP - 1 EP - 7 PB - nature publishing group CY - London, United Kingdom AN - OPUS4-35387 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Afantitis, A. A1 - Melagraki, G. A1 - Isigonis, P. A1 - Tsoumanis, A. A1 - Varsou, D. D. A1 - Valsami-Jones, E. A1 - Papadiamantis, A. A1 - Ellis, L.-J. A. A1 - Sarimveis, H. A1 - Doganis, P. A1 - Karatzas, P. A1 - Tsiros, P. A1 - Liampa, I. A1 - Lobaskin, V. A1 - Greco, D. A1 - Serra, A. A1 - Kinaret, P. A. S. A1 - Saarimäki, L. A. A1 - Grafström, R. A1 - Kohonen, P. A1 - Nymark, P. A1 - Willighagen, E. A1 - Puzyn, T. A1 - Rybinska-Fryca, A. A1 - Lyubartsev, A. A1 - Jensen, K. A. A1 - Brandenburg, J. G. A1 - Lofts, S. A1 - Svendsen, C. A1 - Harrison, S. A1 - Maier, D. A1 - Tamm, K. A1 - Jänes, J. A1 - Sikk, L. A1 - Dusinska, M. A1 - Longhin, E. A1 - Rundén-Pran, E. A1 - Mariussen, E. A1 - El Yamani, N. A1 - Unger, Wolfgang A1 - Radnik, Jörg A1 - Tropsha, A. A1 - Cohen, Y. A1 - Lesczynski, J. A1 - Hendren, C. O. A1 - Wiesner, M. A1 - Winkler, D. A1 - Suzuki, N. A1 - Yoon, T. H. A1 - Choi, J.-S. A1 - Sanabria, N. A1 - Gulumian, M. A1 - Lynch, I. T1 - NanoSolveIT Project: Driving nanoinformatics research to develop innovative and integrated tools for in silico nanosafety assessment JF - Computational and Structural Biotechnology Journal N2 - Nanotechnology has enabled the discovery of a multitude of novel materials exhibiting unique physicochemical (PChem) properties compared to their bulk analogues. These properties have led to a rapidly increasing range of commercial applications; this, however, may come at a cost, if an association to long-term health and environmental risks is discovered or even just perceived. Many nanomaterials (NMs) have not yet had their potential adverse biological effects fully assessed, due to costs and time constraints associated with the experimental assessment, frequently involving animals. Here, the available NM libraries are analyzed for their suitability for integration with novel nanoinformatics approaches and for the development of NM specific Integrated Approaches to Testing and Assessment (IATA) for human and environmental risk assessment, all within the NanoSolveIT cloud-platform. These established and well-characterized NM libraries (e.g. NanoMILE, NanoSolutions, NANoREG, NanoFASE, caLIBRAte, NanoTEST and the Nanomaterial Registry (>2000 NMs)) contain physicochemical characterization data as well as data for several relevant biological endpoints, assessed in part using harmonized Organisation for Economic Co-operation and Development (OECD) methods and test guidelines. Integration of such extensive NM information sources with the latest nanoinformatics methods will allow NanoSolveIT to model the relationships between NM structure (morphology), properties and their adverse effects and to predict the effects of other NMs for which less data is available. The project specifically addresses the needs of regulatory agencies and industry to effectively and rapidly evaluate the exposure, NM hazard and risk from nanomaterials and nano-enabled products, enabling implementation of computational ‘safe-by-design’ approaches to facilitate NM commercialization. KW - Nanoinformatics KW - Hazard assessment KW - (Quantitative) Structure-Active Relationships KW - Safe-by-design KW - Predictive modelling PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505952 DO - https://doi.org/10.1016/j.csbj.2020.02.023 VL - 18 SP - 583 EP - 602 PB - Elsevier B.V. AN - OPUS4-50595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weigert, Florian A1 - Müller, A. A1 - Häusler, I. A1 - Geißler, Daniel A1 - Skroblin, D. A1 - Unger, Wolfgang A1 - Radnik, Jörg A1 - Resch-Genger, Ute T1 - Combining HR‑TEM and XPS to elucidate the core–shell structure of ultrabright CdSe/CdS semiconductor quantum dots JF - Scientific reports N2 - Controlling thickness and tightness of surface passivation shells is crucial for many applications of core–shell nanoparticles (NP). Usually, to determine shell thickness, core and core/shell particle are measured individually requiring the availability of both nanoobjects. This is often not fulfilled for functional nanomaterials such as many photoluminescent semiconductor quantum dots (QD) used for bioimaging, solid state lighting, and display technologies as the core does not show the applicationrelevant functionality like a high photoluminescence (PL) quantum yield, calling for a whole nanoobject approach. By combining high-resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS), a novel whole nanoobject approach is developed representatively for an ultrabright oleic acid-stabilized, thick shell CdSe/CdS QD with a PL quantum yield close to unity. The size of this spectroscopically assessed QD, is in the range of the information depth of usual laboratory XPS. Information on particle size and monodispersity were validated with dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) and compared to data derived from optical measurements. In addition to demonstrating the potential of this novel whole nanoobject approach for determining architectures of small nanoparticles, the presented results also highlight challenges faced by different sizing and structural analysis methods and method-inherent uncertainties. KW - Photoluminescence KW - Single particle KW - Microscopy KW - Particle architecture KW - Thickness KW - SAXS KW - Shell KW - XPS KW - TEM KW - Semiconductor KW - Quantum dot KW - Photophysics KW - Quantum yield PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517911 DO - https://doi.org/10.1038/s41598-020-77530-z VL - 10 IS - 1 SP - 20712 PB - Springer Nature AN - OPUS4-51791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Anja A1 - Heinrich, Thomas A1 - Tougaard, S. A1 - Werner, W. S. M. A1 - Hronek, M. A1 - Kunz, Valentin A1 - Radnik, Jörg A1 - Stockmann, Jörg M. A1 - Hodoroaba, Vasile-Dan A1 - Benemann, Sigrid A1 - Nirmalananthan-Budau, Nithiya A1 - Geißler, Daniel A1 - Sparnacci, K. A1 - Unger, Wolfgang T1 - Determining the thickness and completeness of the shell of polymer core-shell nanoparticles by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and transmission scanning electron microscopy JF - The journal of physical chemistry C N2 - Core–shell nanoparticles (CSNPs) have become indispensable in various industrial applications. However, their real internal structure usually deviates from an ideal core–shell structure. To control how the particles perform with regard to their specific applications, characterization techniques are required that can distinguish an ideal from a nonideal morphology. In this work, we investigated poly(tetrafluoroethylene)–poly(methyl methacrylate) (PTFE–PMMA) and poly(tetrafluoroethylene)–polystyrene (PTFE–PS) polymer CSNPs with a constant core diameter (45 nm) but varying shell thicknesses (4–50 nm). As confirmed by transmission scanning electron microscopy (T-SEM), the shell completely covers the core for the PTFE–PMMA nanoparticles, while the encapsulation of the core by the shell material is incomplete for the PTFE–PS nanoparticles. X-ray photoelectron spectroscopy (XPS) was applied to determine the shell thickness of the nanoparticles. The software SESSA v2.0 was used to analyze the intensities of the elastic peaks, and the QUASES software package was employed to evaluate the shape of the inelastic background in the XPS survey spectra. For the first time, nanoparticle shell thicknesses are presented, which are exclusively based on the analysis of the XPS inelastic background. Furthermore, principal component analysis (PCA)-assisted time-of-flight secondary-ion mass spectrometry (ToF-SIMS) of the PTFE–PS nanoparticle sample set revealed a systematic variation among the samples and, thus, confirmed the incomplete encapsulation of the core by the shell material. As opposed to that, no variation is observed in the PCA score plots of the PTFE–PMMA nanoparticle sample set. Consequently, the complete coverage of the core by the shell material is proved by ToF-SIMS with a certainty that cannot be achieved by XPS and T-SEM. KW - XPS KW - T-SEM KW - ToF-SIMS KW - Core-shell nanoparticles PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-499165 DO - https://doi.org/10.1021/acs.jpcc.9b09258 VL - 123 IS - 49 SP - 29765 EP - 29775 PB - American Chemical Society CY - Washington, DC AN - OPUS4-49916 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kaur, I. A1 - Ellis, L.-J. A1 - Romer, I. A1 - Tantra, R. A1 - Carriere, M. A1 - Allard, S. A1 - Mayne-L'Hermite, M. A1 - Minelli, C. A1 - Unger, Wolfgang A1 - Potthoff, A. A1 - Rades, Steffi A1 - Valsami-Jones, E. T1 - Dispersion of nanomaterials in aqueous media: Towards protocol optimization JF - Journal of Visualized Experiments N2 - The sonication process is commonly used for de-agglomerating and dispersing nanomaterials in aqueous based media, necessary to improve homogeneity and stability of the suspension. In this study, a systematic step-wise approach is carried out to identify optimal sonication conditions in order to achieve a stable dispersion. This approach has been adopted and shown to be suitable for several nanomaterials (cerium oxide, zinc oxide, and carbon nanotubes) dispersed in deionized (DI) water. However, with any change in either the nanomaterial type or dispersing medium, there needs to be optimization of the basic protocol by adjusting various factors such as sonication time, power, and sonicator type as well as temperature rise during the process. The approach records the dispersion process in detail. This is necessary to identify the time Points as well as other above-mentioned conditions during the sonication process in which there may be undesirable changes, such as damage to the particle surface thus affecting surface properties. Our goal is to offer a harmonized approach that can control the Quality of the final, produced dispersion. Such a guideline is instrumental in ensuring dispersion quality repeatability in the nanoscience community, particularly in the field of nanotoxicology. KW - Dispersion of nanomaterials KW - Aqueous media KW - Protocol development PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-435886 UR - https://www.jove.com/video/56074 DO - https://doi.org/10.3791/56074 SN - 1940-087X IS - 130 SP - e560741, 1 EP - e560741, 23 PB - MyJove Corp. CY - Cambridge, MA, USA AN - OPUS4-43588 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Swaraj, S. A1 - Dietrich, Paul A1 - Unger, Wolfgang T1 - Simultaneous surface and bulk sensitive XAS measurements of magnetic particle clusters JF - IOP Conf. Series: Journal of Physics: Conf. Series N2 - Magnetic iron oxide nanoparticle clusters (mnpc) coated with organic stabilizers were investigated using scanning transmission x-ray microscopy (STXM). Simultaneous surface and bulk sensitive Fe L3 edge absorption spectra, obtained using a photomultiplier tube and a channeltron, were used to detect subtle changes in the oxidation state in the surface and bulk of Iron Oxide mnpc. The effectiveness of this mode of STXM operation is demonstrated for These nanoparticle clusters. T2 - X-Ray Microscopy Conference 2016 (XRM 2016) CY - Oxford, UK DA - 15.08.2016 KW - Scanning transmission x-ray microscopy (STXM) KW - Magnetic nanoparticles KW - Fe L3 edge absorption spectra PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-435907 UR - http://iopscience.iop.org/article/10.1088/1742-6596/849/1/012014/meta DO - https://doi.org/10.1088/1742-6596/849/1/012014 VL - 849 SP - 012014, 1 EP - 012014, 4 PB - IOP Publishing AN - OPUS4-43590 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Dietrich, P. A1 - Thissen, A. A1 - Kulak, N. A1 - Kjaervik, Marit A1 - Unger, Wolfgang T1 - XPS surface chemical analysis of aqueous solutions with EnviroESCA T2 - SPECS Application Notes N2 - Water and aqueous reagents are essential in any biological process or system. But apart from a few special low vapor-pressure cases, liquids have not been accessible to any technique requiring UHV conditions. EnviroESCA opens up this exciting field of applications. In this paper first results from water based samples are presented as a proof of concept to demonstrate the special capabilities of EnviroESCA analyzing liquid samples. The following solutions were investigated under near ambient pressure conditions: i.) water, ii.) brine, iii.) an oil in water dispersion, iv.) aqueous iron(II) sulfate heptahydrate, and v.) a suspension of nano silver particles in water. KW - Surface Analysis KW - Near Ambient Pressure XPS KW - Aqueous Solutions PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-394603 UR - http://www.enviro.specs.de/cms/upload/bilder/EnviroESCA/Applications/Liquids/Application-Note_EnviroESCA_Aqueous_Solutions.pdf N1 - BAM Mitarbeiter Beitrag im Acknowledgement definiert. IS - #000394 SP - 1 PB - SPECS CY - Berlin AN - OPUS4-39460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abbas, F. A1 - Donskyi, Ievgen A1 - Gholami, M. A1 - Ziem, B. A1 - Lippitz, Andreas A1 - Unger, Wolfgang A1 - Böttcher, C. A1 - Rabe, J. A1 - Haag, R. A1 - Adeli, M. T1 - Controlled covalent functionalization of thermally reduced graphene oxide to generate defined bifunctional 2D nanomaterials JF - Angewandte Chemie International Edition N2 - A controlled, reproducible, gram-scale method is reported for the covalent functionalization of graphene Sheets by a one-pot nitrene [2+1] cycloaddition reaction under mild conditions. The reaction between commercially available 2,4,6-trichloro-1,3,5-triazine and sodium azide with thermally reduced graphene oxide (TRGO) results in defined dichlorotriazine-functionalized sheets. The different reactivities of the chlorine substituents on the functionalized graphene allow stepwise post-modification by manipulating the temperature. This new method provides unique access to defined bifunctional 2D nanomaterials, as exemplified by chiral surfaces and multifunctional hybrid architectures. KW - Graphene oxide KW - Bifunctional 2D nanomaterials KW - XPS KW - NEXAFS KW - AFM PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-394789 DO - https://doi.org/10.1002/ange.201612422 SN - 1433-7851 VL - 56 IS - 10 SP - 2675 EP - 2679 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-39478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Swaraj, S. A1 - Dietrich, Paul A1 - Unger, Wolfgang T1 - Simultaneous surface and bulk sensitive XAS measurements of magnetic particle clusters JF - Journal of Physics: Conference Series N2 - Magnetic iron oxide nanoparticle clusters (mnpc) coated with organic stabilizers were investigated using scanning transmission x-ray microscopy (STXM). Simultaneous surface and bulk sensitive Fe L₃ edge absorption spectra, obtained using a photomultiplier tube and a channeltron, were used to detect subtle changes in the oxidation state in the surface and bulk of Iron Oxide mnpc. The effectiveness of this mode of STXM operation is demonstrated for these nanoparticle clusters. T2 - X-Ray Microscopy Conference 2016 (XRM 2016) CY - Oxford, UK DA - 15.08. 2016 KW - Fe L3 edge absorption spectra KW - Scanning transmission x- ray microscopy KW - Magnetic iron oxide nanoparticle clusters KW - XAS PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-410576 UR - http://iopscience.iop.org/article/10.1088/1742-6596/849/1/012014/pdf DO - https://doi.org/10.1088/1742-6596/849/1/012014 SN - 1742-6588 VL - 849 SP - 012014, 1 EP - 012014, 5 PB - IOP Publishing AN - OPUS4-41057 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Röhsler, Andreas A1 - Sobol, Oded A1 - Unger, Wolfgang A1 - Böllinghaus, Thomas T1 - Comprehensive study of deuterium-induced effects in in austenitic stainless steel AISI 304L JF - International Journal for Hydrogen Energy N2 - The damaging impact of hydrogen on the austenitic stainless steel AISI 304 L was analysed. To this aim, samples were charged electrochemically with the hydrogen isotope deuterium (2H, D) and examined with time-of-flight secondary ion mass spectrometry (ToF-SIMS) and electron backscatter diffraction (EBSD). The fusion of the obtained chemical and structural information revealed local enrichment of deuterium in austenite, transformation into martensite, crack formation and severe roughening of the specimen surface. The results indicated that martensite was not only formed during charging but also during Desorption and ToF-SIMS examinations. Furthermore, cross-sections of deuterium-charged samples revealed that in preferred deformation bands a g/ε/a 0 evolution is taking place. By means of microscopic analyses and carrier gas hot extraction (CGHE), it was found that the use of NaAsO2 as recombination poison decreased the uptake of hydrogen significantly and resulted in severe precipitation on the specimen surfaces. This is in contrast to the popular presumption that NaAsO2 enhances the uptake of hydrogen (and deuterium) during electrochemical charging by hampering its recombination from Atoms to molecules. KW - AISI 304L KW - Hydrogen KW - ToF-SIMS KW - Deuterium KW - Martensite PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-477540 DO - https://doi.org/10.1016/j.ijhydene.2019.03.058 SN - 0360-3199 SN - 1879-3487 VL - 44 IS - 23 SP - 12228 EP - 12238 PB - Elsevier Ltd. AN - OPUS4-47754 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -