TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Rades, Steffi A1 - Borghetti, P. A1 - Ortel, Erik A1 - Wirth, Thomas A1 - Garcia, S. A1 - Gómez, E. A1 - Blanco, M. A1 - Alberto, G. A1 - Martra, G. T1 - Organic surface modification and analysis of titania nanoparticles for self‐assembly in multiple layers JF - Surface and Interface Analysis N2 - The characteristics of TiO2 coatings can greatly influence their final performance in large‐scale applications. In the present study, self‐assembly of TiO2 nanoparticles (NPs) in multiple layers was selected as a deposition procedure on various substrates. For this, the main prerequisite constitutes the surface modification of both NPs and substrate with, for example, silane coupling agents. A set of functionalized TiO2 NPs has been produced by reaction with either (3‐aminopropyl)triethoxysilane (APTES) or (3‐aminopropyl)phosphonic acid (APPA) to functionalize the NP surface with free amino‐groups. Then, the complementary functionalized NP set can be obtained from an aliquot of the first one, through the conversion of free surface amino groups to aldehydes by reaction with glutaraldehyde (GA). Several types of TiO2 NPs differing in size, shape, and specific surface area have been functionalized. Fourier‐transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), SEM/ energy‐dispersive X‐ray spectroscopy (EDS), XPS, Auger electron spectroscopy (AES), and Time‐of‐Flight (ToF)‐SIMS analyses have been carried out to evaluate the degree of functionalization, all the analytical methods employed demonstrating successful functionalization of TiO2 NP surface with APTES or APPA and GA. KW - TiO2 KW - Nanoparticles KW - Surface functionalization KW - Layer-by-layer deposition KW - Surface chemical analysis PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508601 DO - https://doi.org/10.1002/sia.6842 SN - 1096-9918 VL - 52 IS - 12 SP - 829 EP - 834 PB - John Wiley & Sons Ltd AN - OPUS4-50860 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rades, Steffi A1 - Borghetti, P. A1 - Ortel, Erik A1 - Wirth, Thomas A1 - Blanco, M. A1 - Gómez, E. A1 - Martinez, A. A1 - Jupille, J. A1 - Martra, G. A1 - Hodoroaba, Vasile-Dan T1 - Control of functionalization of supports for subsequent assembly of titania nanoparticle films JF - Surface and Interface Analysis N2 - For self‐assembling of TiO2 nanoparticles in multiple layers by layer‐by‐layer deposition to be applied to TiO2 thin films with defined and homogeneous thickness for large‐scale applications, the proper functionalization of substrate surface is a prerequisite to guarantee sufficient adhesion. The substrates selected and tested in the present paper were conductive, fluorine‐doped tin oxide (FTO) glass, nonconductive silica glass, and titanium alloy. The current study focusses on the analytical control of the stepwise functionalization of the substrates with 3‐aminopropyltriethoxysilane and glutaraldehyde (GA) for both the FTO glass and silica glass and with 3‐aminepropyl phosphonic acid and GA for Ti alloy. The analyses have been conducted by means of surface sensitive methods, X‐ray photoelectron spectroscopy, Auger electron spectroscopy, and time‐of‐flight secondary ions mass spectrometry. Chemical composition of surface of functionalized substrates shows differences in the degree and type of modification in dependence on substrate. It could be demonstrated that the best functionalized substrates were the conductive FTO glasses. The analysis of the functionalized Ti substrates has revealed that the surface coverage with 3‐aminepropyl phosphonic acid and GA molecules is an inhomogeneous one, and further optimization of the two‐step functionalization on the Ti alloy substrate is necessary. KW - Nanoparticles KW - Surface functionalization KW - TiO2 KW - SEM/EDX KW - Auger Electron Spectroscopy KW - ToF-SIMS KW - Thin films PY - 2018 DO - https://doi.org/10.1002/sia.6398 SN - 0142-2421 SN - 1096-9918 VL - 50 IS - 11 SP - 1200 EP - 1206 PB - John Wiley & Sons, Ltd. AN - OPUS4-46406 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rades, Steffi A1 - Oswald, F. A1 - Narbey, S. A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Analytical approach for characterization of morphology and chemistry of a CH3NH3PbI3/TiO2 solar cell layered system JF - Surface and Interface Analysis N2 - Manufacturing of new perovskite layered solar cells with constant high light conversion Efficiency over time may be hampered by the loss of efficiency caused by structural and/or chemical alterations of the complex layered system. SEM/EDX combined with XPS were chosen as an appropriate methodical approach to characterize perovskite laboratory cells in depth and at surface, before and after light exposure. The layered perovskite system investigated here is based on glass covered with fluorine doped tin oxide, followed by thin films of TiO2, ZrO2, and a thick monolithic carbon. TiO2 film is subdivided into a dense layer covered by porous one constituted of nanoparticles of truncated bipyramidal shape. This layered system serves as the matrix for the perovskite. EDX spectral maps on cross sections of specimen have shown that Pb and I are distributed homogeneously throughout the porous layers C, ZrO2, and TiO2. SEM/EDX data show that 20 weeks of ambient daylight did not change significantly the in‐depth distribution of the elemental composition of Pb and I throughout the entire solar cell system. It was confirmed with EDX that nanoparticles identified in high‐resolution SEM micrographs contain mainly Pb and I, indicating these to be the perovskite crystals. However, a compositional and chemical altering began in the near‐surface region of the outermost ~10 nm after 2 months of illumination which was observed with XPS. T2 - ECASIA 2017 CY - Montpellier, France DA - 24.09.2017 KW - Solar Cell KW - SEM KW - EDX KW - XPS KW - layered system PY - 2018 DO - https://doi.org/10.1002/sia.6410 SN - 0142-2421 SN - 1096-9918 VL - 50 IS - 11 SP - 1234 EP - 1238 PB - John Wiley & Sons, Ltd. AN - OPUS4-46394 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 JF - ACS Applied Nano Materials 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 - 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 JF - Materials Research Express 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 - 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 - Electron Microscopy and X-Ray Diffraction Analysis of Titanium Oxide Nanoparticles Synthesized by Pulsed Laser Ablation in Liquid JF - Microscopy and Microanalysis N2 - A 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 by XRD(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 - Laser ablation in liquid KW - Nanoparticles KW - Titanium oxide KW - Particle morphology PY - 2018 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/electron-microscopy-and-xray-diffraction-analysis-of-titanium-oxide-nanoparticles-synthesized-by-pulsed-laser-ablation-in-liquid/AE368446FAC70E08C514F9AEABFD131B DO - https://doi.org/10.1017/S1431927618009030 VL - 24 IS - S1 (August) SP - 1710 EP - 1711 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-45949 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rades, Steffi A1 - Oswald, F. A1 - Narbey, S. A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Complementary methodical approach for the analysis of a perovskite solar cell layered system JF - Microscopy and Microanalysis N2 - Loss in efficiency of perovskite solar cells may be caused by structural and/or chemical alterations of the complex layered system. SEM/EDX combined with XPS were chosen as appropriate methodical approach to characterise perovskite laboratory cells in depth and complementary on top, before and after light exposure. The layered perovskite system investigated here is based on glass covered with fluorine doped tin oxide (FTO), followed by three porous thin films of TiO2, ZrO2 and a thick monolithic carbon. This layered system serves as the matrix for the perovskite. After infiltration of perovskite solution and annealing, EDX spectral maps on cross-sections of the specimen have been measured. The distribution of relevant elements – Si, Sn, Ti, Zr and C – correlates conclusively with layers visible in the acquired SEM images. Lead and iodine are distributed throughout the porous layers C, ZrO2 and TiO2. By EDX it was found that several weeks of ambient daylight did not change significantly the qualitative elemental composition of lead and iodine throughout the solar cell system. It was confirmed with EDX that nanoparticles identified in high-resolution SEM micrographs contain mainly Pb and I, indicating these to be the perovskite crystals. However, a time-dependent compositional and chemical altering was observed with XPS for the near-surface region of the outermost ~10 nm after two months of illumination. KW - Pervskite solar cells KW - TiO2 KW - Porous layer KW - SEM/EDX KW - XPS PY - 2017 UR - https://www.cambridge.org/core/services/aop-cambridge-core/content/view/0E9E937542BC8B5535900B53B7F667E9/S1431927617010558a.pdf/complementary_methodical_approach_for_the_analysis_of_a_perovskite_solar_cell_layered_system.pdf DO - https://doi.org/10.1017/S1431927617010558 VL - 23 IS - S1 (July) SP - 1978 EP - 1979 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-41925 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rades, Steffi A1 - Ortel, Erik A1 - Wirth, Thomas A1 - Holzweber, Markus A1 - Pellegrino, F. A1 - Martra, G. A1 - Hodoroaba, Vasile-Dan T1 - Analysis of fluorine traces in TiO2 nanoplatelets by SEM/EDX, AES and TOF-SIMS JF - Microscopy and Microanalysis N2 - Hydrothermal synthesis of anatase TiO2 nanosheets with a high fraction of exposed {001} facets and related high photocatalytic activity - as an alternative to bipyramidal anatase TiO2 nanoparticles mainly exposing the {101} facets. The scope of the material preparation work is the thermal reduction of residual fluorides from HF (capping agent) induced during the synthesis of TiO2 nanosheets by calcination at 873K. The analytical task consists of detection and localization of fluorine present at the surface and/or in the bulk of TiO2 nanosheets before and after calcination by SEM/EDX, Auger electron spectroscopy and ToF-SIMS. KW - Fluorine KW - SEM/EDX KW - TiO2 nanoplatelets KW - Auger electron spectroscopy KW - TOF-SIMS PY - 2017 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/analysis-of-fluorine-traces-in-tio2-nanoplatelets-by-semedx-aes-and-tofsims/91EA2C0666B7927FCA57D2AD114910F6 DO - https://doi.org/10.1017/S1431927617010200 SN - 1435-8115 SN - 1431-9276 VL - 23 IS - S1 (July) SP - 1908 EP - 1909 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-42455 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rades, Steffi A1 - Hodoroaba, Vasile-Dan A1 - Ortel, Erik A1 - Wirth, Thomas A1 - Borghetti, P. A1 - Garcia, S. A1 - Gómez, E. A1 - Blanco, M. A1 - Alberto, Gabriele A1 - Martra, G. T1 - Organic surface modification and analysis of titania nanoparticles for self-assembly in multiple layers JF - Microscopy and Microanalysis N2 - Parameters of TiO2 coatings can greatly influence their final performance in largescale applications such as photocatalytic measurements, orthopedic and/or dental prostheses, cell cultures, and dye-sensitized solar cells. From different film deposition procedures, self-assembly of TiO2 NPs in multiple layers was selected for systematic characterization. EDX, AES and ToF-SIMS analysis have been carried out in order to evaluate the functionalization of several types of TiO2 NPs differing in size, shape and surface area. KW - TiO2 KW - Nanoparticles KW - Surface modification KW - Functionalization PY - 2017 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/organic-surface-modification-and-analysis-of-titania-nanoparticles-for-selfassembly-in-multiple-layers/66776A4CA7FD059CE39041A99A922D90 DO - https://doi.org/10.1017/S1431927617010029 SN - 1431-9276 SN - 1435-8115 VL - 23 IS - S1 (July) SP - 1872 EP - 1873 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-42457 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Rades, Steffi A1 - Salge, T. A1 - Mielke, Johannes A1 - Ortel, Erik A1 - Schmidt, R. T1 - Characterisation of nanoparticles by means of high-resolution SEM/EDS in transmission mode JF - IOP Conf. Series: Materials Science and Engineering N2 - Advances in scanning electron microscopy (SEM) enable the high-resolution imaging of single nanoparticles (NPs) with sizes well below 10 nm. The SEM analysis in transmission mode (T-SEM) of NPs on thin film supports has many benefits when compared to the analysis of NPs on bulk substrates. The enhanced material (mass – thickness) contrast of the T-SEM imaging mode is well suited for in-depth and, particularly valuable, to very accurate, traceable, lateral dimensional measurements of NPs. Compared to samples prepared on bulk substrates, T-SEM with energy dispersive X-ray spectroscopy (EDS) achieves a drastically improved spatial resolution of the emitted X-rays. The poor signal-to-noise ratio of the X-ray spectra emitted by a single nanoparticle (NP) can be improved by the use of high-sensitivity (high collection solid angle) silicon drift (SDD), energy-dispersive X-ray spectrometers (EDS). The EDS spectral imaging of a single NP with a spatial resolution below 10 nm has become possible. This is demonstrated by means of various examples of nanostructures. Advanced data processing of T-SEM/EDS results sets the stage for the automated classification of NPs by feature analysis. This method combines the detection of morphological structures of interest by image processing of T-SEM micrographs with the chemical classification by EDS. T2 - European Microbeam Analysis Society’s 14th European Workshop on Modern Developments and Applications in Microbeam Analysis (EMAS 2015) CY - Portorož, Slovenia DA - 03.05.2015 KW - High-resolution KW - SEM KW - T-SEM KW - EDX KW - Nanoparticles PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355628 UR - http://iopscience.iop.org/article/10.1088/1757-899X/109/1/012006 DO - https://doi.org/10.1088/1757-899X/109/1/012006 SN - 1757-899X VL - 109 SP - 012006-1 EP - 012006-12 PB - IOP Publishing Ltd CY - Bristol, UK AN - OPUS4-35562 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mielke, Johannes A1 - Rades, Steffi A1 - Ortel, Erik A1 - Salge, T. A1 - Hodoroaba, Vasile-Dan T1 - Improved spatial resolution of EDX/SEM for the elemental analysis of nanoparticles JF - Microscopy and microanalysis N2 - The interest in nanoparticles remains at a high level in fundamental research since many years and increasingly, nanoparticles are incorporated into consumer products to enhance their performance. Consequently, the accurate and rapid characterization of nanoparticles is more and more demanded. Electron microscopy (SEM, TSEM and TEM) is one of the few techniques which are able to image individual nanoparticles. It was demonstrated recently that the transmission electron microscopy at a SEM can successfully be applied as a standard method to characterize accurately the size (distribution) and shape of nanoparticles down to less than 10 nm. PY - 2015 DO - https://doi.org/10.1017/S1431927615009344 SN - 1431-9276 SN - 1435-8115 VL - 21 IS - Suppl. 3 SP - Paper 0855, 1713 EP - 1714 PB - Cambridge University Press CY - New York, NY AN - OPUS4-34923 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Senoner, Mathias A1 - Maaßdorf, A. A1 - Rooch, Heidemarie A1 - Österle, Werner A1 - Malcher, M. A1 - Schmidt, M. A1 - Kollmer, F. A1 - Paul, D. A1 - Hodoroaba, Vasile-Dan A1 - Rades, Steffi A1 - Unger, Wolfgang T1 - Lateral resolution of nanoscaled images delivered by surface-analytical instruments: application of the BAM-L200 certified reference material and related ISO standards JF - Analytical and bioanalytical chemistry N2 - The certified reference material BAM-L200, a nanoscale stripe pattern for length calibration and specification of lateral resolution, is described. BAM-L200 is prepared from a cross-sectioned epitaxially grown layer stack of AlxGa1–xAs and InxGa1–xAs on a GaAs substrate. The surface of BAM-L200 provides a flat pattern with stripe widths ranging down to 1 nm. Calibration distances, grating periods and stripe widths have been certified by TEM with traceability to the length unit. The combination of gratings, isolated narrow stripes and sharp edges of wide stripes offers plenty of options for the determination of lateral resolution, sharpness and calibration of length scale at selected settings of imaging surface-analytical instruments. The feasibility of the reference material for an analysis of the lateral resolution is demonstrated in detail by evaluation of ToF-SIMS, AES and EDX images. Other applications developed in the community are summarized, too. BAM-L200 fully supports the implementation of the revised International Standard ISO 18516 (in preparation) which is based on knowledge outlined in the Technical Report ISO/TR 19319:2013. KW - AES KW - BAM-L200 KW - CRM KW - EDX KW - Imaging KW - Lateral resolution KW - Sharpness KW - Standardisation KW - STXM KW - ToF-SIMS KW - XPEEM KW - XPS KW - Certified reference material KW - Imaging surface analysis PY - 2015 DO - https://doi.org/10.1007/s00216-014-8135-7 SN - 1618-2642 SN - 1618-2650 VL - 407 IS - 11 SP - 3211 EP - 3217 PB - Springer CY - Berlin AN - OPUS4-33033 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Rades, Steffi A1 - Salge, T. A1 - Mielke, Johannes A1 - Ortel, Erik A1 - Schmidt, R. T1 - Characterisation of nanoparticles by means of high-resolution SEM/EDS T2 - EMAS 2015 - 14th European workshop on modern developments and applications in microbeam analysis N2 - Advances in scanning electron microscopy (SEM) enable the high-resolution imaging of single nanoparticles (NPs) with sizes well below 10 nm. The SEM analysis in transmission mode (T-SEM) of NPs on thin film supports has many benefits when compared to the analysis of NPs on bulk substrates. The enhanced material (mass - thickness) contrast of the T-SEM imaging mode is well suited for in-depth and, particularly valuable, to very accurate, traceable, lateral dimensional measurements of NPs. Compared to samples prepared on bulk substrates, T-SEM with energy dispersive X-ray spectroscopy (EDS) achieves a drastically improved spatial resolution of the emitted X-rays. The poor signal-to-noise ratio of the X-ray spectra emitted by a single nanoparticle (NP) can be improved by the use of high-sensitivity (high collection solid angle) silicon drift (SDD), energy-dispersive X-ray spectrometers (EDS). The EDS spectral imaging of a single NP with a spatial resolution below 10 nm has become possible. This is demonstrated by means of various examples of nanostructures. Advanced data processing of T-SEM/EDS results sets the stage for the automated classification of NPs by feature analysis. This method combines the detection of morphological structures of interest by image processing of T-SEM micrographs with the chemical classification by EDS. T2 - EMAS 2015 - 14th European workshop on modern developments and applications in microbeam analysis CY - Portoroz, Slovenia DA - 03.05.2015 KW - SEM KW - T-SEM KW - EDX KW - Nanoparticles KW - High-resolution PY - 2015 SN - 978-90-8227-691-6 DO - https://doi.org/10.1088/1757-899X/109/1/012006 SP - NUR code:972 - Materials Science, 187-199 AN - OPUS4-33258 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rades, Steffi A1 - Salge, T. A1 - Schmidt, R. A1 - Hodoroaba, Vasile-Dan T1 - Need for large-area EDS detectors for imaging nanoparticles in a SEM operating in transmission mode JF - Microscopy and microanalysis KW - EDS KW - EDX KW - Nanoparticles KW - High-resolution KW - SEM KW - T-SEM KW - Large-area EDS PY - 2014 DO - https://doi.org/10.1017/S1431927614005030 SN - 1431-9276 SN - 1435-8115 VL - 20 IS - Suppl. S 3 SP - 662 EP - 663 PB - Cambridge University Press CY - New York, NY AN - OPUS4-31389 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Salge, T. A1 - Terborg, R. A1 - Ball, A. D. A1 - Broad, G.R. A1 - Kearsley, A.T. A1 - Jones, C.G. A1 - Smith, C. A1 - Rades, Steffi A1 - Hodoroaba, Vasile-Dan ED - Hozak, P. T1 - Advanced SEM/EDS analysis using an annular silicon drift detector (SDD): Applications in nano, life, earth and planetary sciences below micrometer scale T2 - IMC 2014 - 18th International microscopy congress (Proceedings) T2 - IMC 2014 - 18th International microscopy congress CY - Prague, Czech Republic DA - 2014-09-07 PY - 2014 SN - 978-80-260-6720-7 SP - IT-5-P-1842, 1-2 AN - OPUS4-31944 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Rades, Steffi A1 - Unger, Wolfgang T1 - Inspection of morphology and elemental imaging of single nanoparticles by high-resolution SEM/EDX in transmission mode JF - Surface and interface analysis N2 - In the frame of the European project NanoValid, potential candidates of reference nanomaterials are manufactured and systematically characterized in particular with respect to their morphology (shape, size and size distribution). In this study, by exploiting the transmission operation mode in a high-resolution SEM, known as transmission SEM, the potential of this methodical approach is demonstrated by means of representative examples of nanoparticles. The method enables quick and accurate morphological inspection and systematic characterization. Energy dispersive X-ray spectroscopy imaging of single nanoparticles by using the transmission mode is demonstrated as feasible, too. KW - Single nanoparticles KW - SEM KW - TEM KW - T-SEM KW - EDX KW - Imaging KW - Transmission KW - NanoValid KW - Scanning electron microscopy (SEM) KW - High-resolution KW - Transmission in SEM KW - Energy dispersive KW - X-ray spectroscopy KW - Nanoparticles KW - Characterization PY - 2014 DO - https://doi.org/10.1002/sia.5426 SN - 0142-2421 SN - 1096-9918 VL - 46 IS - 10-11 SP - 945 EP - 948 PB - Wiley CY - Chichester AN - OPUS4-31577 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 - Hodoroaba, Vasile-Dan A1 - Rades, Steffi A1 - Natte, Kishore A1 - Orts Gil, Guillermo A1 - Unger, Wolfgang T1 - Morphology of nanoparticles - A characterization using high-resolution SEM JF - GIT Imaging & Microscopy N2 - Potential candidates of reference nano-materials are manufactured and systematically characterized in particular with respect to their morphology (shape, size and size distribution) in the frame of the running large European project NanoValid. By exploiting the transmission operation mode in a SEM, known as T-SEM, it is demonstrated by means of three representative examples of nanoparticles how a quick morphological inspection up to a complete, metrological characterization is feasible. KW - Nanoparticles KW - SEM KW - TEM KW - T-SEM KW - NanoValid PY - 2013 SN - 1439-4243 SN - 1863-7809 VL - 15 IS - 1 SP - 54 EP - 56 PB - GIT-Verl. CY - Darmstadt AN - OPUS4-27925 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -