TY - JOUR A1 - Schmack, R. A1 - Eckhardt, B. A1 - Koch, G. A1 - Ortel, Erik A1 - Kraehnert, R. T1 - ZnO coatings with controlled pore size, crystallinity and electrical conductivity N2 - Zinc oxide is a wide bandgap semiconductor with unique optical, electrical and catalytic properties. Many of its practical applications rely on the materials pore structure, crystallinity and electrical conductivity. We report a synthesis method for ZnO films with ordered mesopore structure and tuneable crystallinity and electrical conductivity. The synthesis relies on dip-coating of solutions containing micelles of an amphiphilic block copolymer and complexes of Zn2+ ions with aliphatic ligands. A subsequent calcination at 400 °C removes the template and induces crystallization of the pore walls. The pore structure is controlled by the template polymer, whereas the aliphatic ligands control the crystallinity of the pore walls. Complexes with a higher thermal stability result in ZnO films with a higher content of residual carbon, smaller ZnO crystals and therefore lower electrical conductivity. The paper discusses the ability of different types of ligands to assist in the synthesis of mesoporous ZnO and relates the structure and thermal stability of the precursor complexes to the crystallinity and electrical conductivity of the zinc oxide. KW - conductivity KW - EISA KW - pore templating KW - pore size control KW - ligands KW - zinc oxide PY - 2016 DO - https://doi.org/10.5755/j01.ms.22.1.8634 SN - 1392–1320 VL - 22 IS - 1 SP - 74 EP - 81 PB - Kaunas University of Technology, Lithuania AN - OPUS4-35550 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ortel, Erik A1 - Bernicke, M. A1 - Eckhardt, B. A1 - Bernsmeier, D. A1 - Schmack, R. A1 - Kraehnert, R. A1 - Lippitz, Andreas T1 - Synthesis and OER activity of NiO coatings with N2 - Catalysts based on nickel oxide are some of the most active catalysts for the oxygen evolution reaction (OER) in alkaline media. However, preparing catalytic coatings with high surface area and good accessibility of the active sites remains challenging. We present a new approach for the synthesis of homogeneous and binder-free nickel oxide coatings comprising a highly accessible ordered mesopore structure. The synthesis is achieved via evaporation induced self assembly utilizing PEOPB-PEO triblock copolymers as pore template and a chemical complex of Ni2+ and citric acid as precursor. Excessive crystallization behaviour of NiO is avoided by thermal conversion of the precursor into an amorphous Ni carbonate intermediate, followed by transition of the carbonate into the metal oxide. We present a comprehensive analysis of the obtained materials in terms of morphology, crystallinity, surface area, composition, and OER activity of differently calcined catalysts. Retaining a low crystallinity and high surface area during the Synthesis proofs to be the most important factor in obtaining a highly active OER catalyst. KW - XPS KW - nanoparticle KW - catalysis PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/slct.201600110/abstract DO - https://doi.org/10.1002/slct.201600110 VL - 2016 IS - 3/2016 SP - 482 EP - 489 PB - Wiley Online Library CY - Weinheim AN - OPUS4-35725 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bernicke, M. A1 - Ortel, Erik A1 - Reier, T. A1 - Bergmann, A. A1 - De Araujo, J.F. A1 - Strasser, P. A1 - Kraehnert, R. T1 - Iridium oxide coatings with templated porosity as highly active oxygen evolution catalysts: Structure-activity relationships N2 - Iridium oxide is the catalytic material with the highest stability in the oxygen evolution reaction (OER) performed under acidic conditions. However, its high cost and limited availability demand that IrO2 is utilized as efficiently as possible. We report the synthesis and OER performance of highly active mesoporous IrO2 catalysts with optimized surface area, intrinsic activity, and pore accessibility. Catalytic layers with controlled pore size were obtained by soft-templating with micelles formed from amphiphilic block copolymers poly(ethylene oxide)-b-poly(butadiene)-b-poly(ethylene oxide). A systematic study on the influence of the calcination temperature and film thickness on the morphology, phase composition, accessible surface area, and OER activity reveals that the catalytic performance is controlled by at least two independent factors, that is, accessible surface area and intrinsic activity per accessible site. Catalysts with lower crystallinity show higher intrinsic activity. The catalyst surface area increases linearly with film thickness. As a result of the templated mesopores, the pore surface remains fully active and accessible even for thick IrO2 films. Even the most active multilayer catalyst does not show signs of transport limitations at current densities as high as 75 mA cm-2. KW - Electrochemistry KW - Iridium KW - Structure–activity relationships KW - Template synthesis KW - Water splitting PY - 2015 DO - https://doi.org/10.1002/cssc.201402988 SN - 1864-5631 SN - 1864-564X VL - 8 IS - 11 SP - 1908 EP - 1915 PB - Wiley-VCH CY - Weinheim AN - OPUS4-33503 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bernsmeier, D. A1 - Bernicke, M. A1 - Ortel, Erik A1 - Bergmann, A. A1 - Lippitz, Andreas A1 - Nissen, J. A1 - Schmack, R. A1 - Strasser, P. A1 - Polte, J. A1 - Kraehnert, R. T1 - Nafion-free carbon-supported electrocatalysts with superior hydrogen evolution reaction performance by soft templating N2 - Efficient water electrolysis requires electrode coatings with high catalytic activity. Platinum efficiently catalyzes the hydrogen evolution reaction in acidic environments, but is a rare and expensive metal. The activity achieved per metal atom can be increased if small Pt particles are dispersed onto electrically conductive, highly accessible and stable support materials. However, the addition of Nafion, a typical binder material used in the manufacture of electrode coatings, can decrease catalytic activity by the blocking of pores and active surface sites. A new approach is reported for the direct synthesis of highly active Nafion-free Pt/C catalyst films consisting of small Pt nanoparticles supported in size-controlled mesopores of a conductive carbon film. The synthesis relies on the co-deposition of suitable Pt and C precursors in the presence of polymer micelles, which act as pore templates. Subsequent carbonization in an inert atmosphere produces porous catalyst films with controlled film thickness, pore size and particle size. The catalysts clearly outperform all Nafion-based Pt/C catalysts reported in the literature, particularly at high current densities. KW - XPS KW - SEM KW - TEM KW - SAXS KW - Catalysis KW - Electrochemistry PY - 2017 DO - https://doi.org/10.1002/celc.201600444 SN - 2196-0216 VL - 4 IS - 1 SP - 221 EP - 229 PB - Wiley Online Library CY - Weinheim AN - OPUS4-39733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ortel, Erik A1 - Fischer, A. A1 - Chuenchom, L. A1 - Polte, Jörg A1 - Smarsly, B. A1 - Krähnert, R. T1 - Mesoporous metal oxide films with controlled pore size, wall thickness and pore hierarchy templated by PEO-b-PB-b-PEO triblock copolymers T2 - 24. Deutsche Zeolith- Tagung CY - Magdeburg, Germany DA - 2012-03-07 PY - 2012 AN - OPUS4-25122 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ortel, Erik T1 - Mesopoous metal oxide films with controlled pore size, wall thickness and pore hierarchy templated by PEO-b-PEO triblock copolymers T2 - 24. Deutsche Zeolith -Tagung CY - Magdeburg, Germany DA - 2012-03-07 PY - 2012 AN - OPUS4-25717 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ortel, Erik T1 - Determination of Thin Film Porosity by SEM/EDX: Application to mesoporous TiO2 layers T2 - International summer workshop "Nanoscience meets Metrology" CY - Erice (Sicily) Italy DA - 2015-07-27 PY - 2015 AN - OPUS4-34703 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ortel, Erik T1 - Thin Film Porosity Determined by X-Rays at SEM: Application to mesoporous T2 - Bruker Seminartage zur Mikroanalyse CY - Berlin DA - 2015-10-14 PY - 2015 AN - OPUS4-34740 LA - deu 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 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 - CONF A1 - Ortel, Erik T1 - Improved Spatial Resolution of EDX/SEM for the Elemental Analysis of Nanoparticles T2 - Microscopy & Microanalysis 2015 CY - Portland, Oregon, USA DA - 2015-08-02 PY - 2015 AN - OPUS4-33870 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ortel, Erik T1 - Charakterisierung von TiO2-Nanopartikeln mit kontrollierter Form mittels Rasterelektronenmikroskopie (SEM und TSEM) T2 - Methoden zur Präparation von Partikeln auf Substraten und Strategien zur Messung mit Elektronenmikroskopie (SEM) und Rasterkraftmikroskopie (AFM) CY - Berlin, Germany DA - 2014-07-07 PY - 2014 AN - OPUS4-31065 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ortel, Erik T1 - Imaging of shape-engineered TiO2 nanoparticles by high-resolution SEM/EDX T2 - EMAS 2015 - 14th European Workshop on Modern Developments and applications in microbeam analysis CY - Portoroz, Slovenia DA - 2015-05-03 PY - 2015 AN - OPUS4-33242 LA - deu 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 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 - Hodoroaba, Vasile-Dan A1 - Cios, G. A1 - Tokarski, T. A1 - Mansfeld, Ulrich A1 - Ortel, Erik A1 - Mielke, Johannes A1 - Pellegrino, F. A1 - Maurino, V. T1 - Towards 3D Understanding of Non-spherical Nanoparticles by Transmission Kikuchi Diffraction (TKD) for Improved Particle Size Distribution by Electron Microscopy N2 - In this paper one refined approach is applied to determine the exact orientation of bipyramidal TiO2 nanoparticles prepared with good dispersion as almost isolated particles on a carbon TEM grid. The advantages of the recently developed high-throughput Transmission Kikuchi Diffraction (TKD) are used to identify quickly and reliably the geometrical orientation of the crystalline TiO2 nanoparticle bipyramids (anatase) on a statistically relevant number of particles. KW - Nanoparticles KW - Transmission Kikuchi Diffraction (TKD) KW - Electron microscopy KW - TiO2 KW - 3D PY - 2020 DO - https://doi.org/10.1017/S1431927620013999 VL - 26 IS - S2 SP - 260 EP - 261 PB - Cambridge University Press CY - Cambridge, UK AN - OPUS4-51772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ortel, Erik T1 - SEM/EDX for the Determination of Thin Film Porosity: Application to mesoporous TiO2 layers T2 - MC2015 CY - Göttingen DA - 2015-09-06 PY - 2015 AN - OPUS4-34707 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ortel, Erik T1 - Determination of porosity of highly porous thin films by combined SEM-EDS analysis T2 - EMAS 2015 - 14th European Workshop on Modern Developments and applications in microbeam analysis CY - Portoroz, Slovenia DA - 2015-05-03 PY - 2015 AN - OPUS4-33244 LA - deu 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 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 - 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 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 - CONF A1 - Ortel, Erik T1 - Accurate Shape and Size Determination of Engineered NPs by Electron Microscopy (SEM, T-SEM, TEM, SAED) T2 - MC2015 CY - Göttingen DA - 2015-09-06 PY - 2015 AN - OPUS4-34706 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wollschläger, Nicole A1 - Palasse, L. A1 - Häusler, Ines A1 - Dirscherl, K. A1 - Oswald, F. A1 - Narbey, S. A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan T1 - Characterization of the inner structure of porous TiO2 nanoparticle films in dye sensitive solar cells (DSSC) by focused ion beam (FIB) tomography and transmission Kikuchi diffraction (TKD) in the scanning electron microscope (SEM) N2 - A combined methodical approach is tested for the first time with respect to the characterization of the inner structure of porous TiO2 layers infiltrated with ruthenium molecular sensitizer as typically used in modern dye sensitized solar cells (DSSC). Their performance is directly linked to the surface area ‘offered’ by the pore Network to the dye. The micrometer thick layer employed was manufactured by screen-printing of a starting TiO2 powder constituted of shape-controlled, bipyramidal anatase nanoparticles (NPs) on FTO/glass substrates. The analytical methods exploited in our study are Focused Ion Beam (FIB) slicing followed by 3D reconstruction as well as the new approach transmission Kikuchi diffraction (TKD) technology in the scanning electron microscope (SEM). While the first method results in the visualization of the 3D pore network within the TiO2 layer, the second one can be successfully applied to analyze the crystal orientation of grains (i.e. NPs in our case) in nanometer resolution. Moreover, size and shape distribution of the TiO2 NPs within the layer can be extracted. SEM in transmission mode and atomic force microscopy (AFM) have been used to verify the dimensional data obtained by the new combined methodical approach. Its analytical benefits but also the challenges and limitations are highlighted. KW - Transmission Kikuchi diffraction KW - Focused ion beam tomography KW - Titanium dioxide KW - Nanoparticles KW - Porosity KW - Particle size KW - DSSC PY - 2017 DO - https://doi.org/10.1016/j.matchar.2017.06.030 SN - 1044-5803 SN - 1873-4189 VL - 131 SP - 39 EP - 48 PB - Elsevier AN - OPUS4-40875 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 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 - CONF A1 - Maurino, V. A1 - Pellutiè, L. A1 - Pellegrino, F. A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan A1 - Isopescu, R. T1 - Synthesis of size and shape controlled TiO2 nanoparticles: possible CRM’s candidates for size, shape and functional properties N2 - Titanium dioxide is one of the most studied metal oxides due to its chemical, surface, electronic and (photo)catalytic properties, providing this material of multisectorial applications ranging from healthcare, photocatalysis, smart materials with self cleaning and self sterilizing properties and solar energy harvesting. However it is difficult to correlate the functional properties of TiO2 nanomaterials to the properties at single nanoparticle level due to the high polydispersity in shape, size and surface features of the currently available TiO2 nanoparticles (NPs). Although intensive experimental and theoretical studies have been conducted on the reactivity of different surfaces of metal oxides such as TiO2 much less attention is paid on the dependence of functional properties, like photocatalytic activity, dye adsorption, open circuit potential and fill factor in dye sensitized solar cells, on crystal facets in different orientations. One of the goal of SETNanoMetro project was the development of design rules to tune crystal facets of TiO2 NPs in order to optimize and control functional properties. In the present work we have developed a series of design rules in order to obtain sets of anatase TiO2 NPs with low polydispersity and to tune their shape and size by hydrothermal processing of Ti(IV)- Triethanolamine complex in presence of different shape controllers. Through a careful experimental design, a predictive soft model was developed. The model is able to predict the synthesis outcome allowing to tune the shape factor from 5 (prisms) to 1.5 (bipyramids) to 0.2 (platelets). This allows to control the main crystal facets exposed ranging from (100) to (001). Due to the dependence of functional properties of nanomaterials on shape distribution and not only size, the availability of NPs sets with uniform and well defined and tunable shapes can be of paramount relevance in order to produce reference nanomaterials for shape measurement. T2 - NanoWorkshop 2018: Workshop on Reference Nanomaterials CY - Berlin, Germany DA - 14.05.2018 KW - Anatase KW - shape control KW - Hydrothermal synthesis PY - 2019 SN - 978-3-95606-440-1 SN - 0179-0609 VL - F-61 SP - 146 EP - 162 PB - Physikalisch-Technische Bundesanstalt CY - Braunschweig und Berlin AN - OPUS4-49993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pellegrino, F. A1 - Isopescu, R. A1 - Pellutiè, L. A1 - Sordello, F. A1 - Rossi, A. M. A1 - Ortel, Erik A1 - Martra, G. A1 - Hodoroaba, Vasile-Dan A1 - Maurino, V. T1 - Machine learning approach for elucidating and predicting the role of synthesis parameters on the shape and size of TiO2 nanoparticles N2 - In the present work a series of design rules are developed in order to tune the morphology of TiO2 nanoparticles through hydrothermal process. Through a careful experimental design, the influence of relevant process parameters on the synthesis outcome are studied, reaching to the develop predictive models by using Machine Learning methods. The models, after the validation and training, are able to predict with high accuracy the synthesis outcome in terms of nanoparticle size, polydispersity and aspect ratio. Furthermore, they are implemented by reverse engineering approach to do the inverse process, i.e. obtain the optimal synthesis parameters given a specific product characteristic. For the first time, it is presented a synthesis method that allows continuous and precise control of NPs morphology with the possibility to tune the aspect ratio over a large range from 1.4 (perfect truncated bipyramids) to 6 (elongated nanoparticles) and the length from 20 to 140 nm. KW - Machine learning KW - Nanoparticles KW - Titanium dioxide KW - Size KW - Shape KW - Synthesis PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515084 DO - https://doi.org/10.1038/s41598-020-75967-w VL - 10 IS - 1 SP - 18910 PB - Springer Nature AN - OPUS4-51508 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wollschläger, Nicole A1 - Häusler, Ines A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan A1 - Palasse, L. A1 - Dirscherl, K. T1 - Characterization of porous, TiO2 nanoparticle films using on-axis TKD in SEM – a new nano-analysis tool for a large-scale application N2 - A combined methodical approach is tested with respect to the characterization of the inner structure of porous TiO2 layers as typically used in modern dye sensitized solar cells (DSSC). Their performance is directly linked to the surface area of the pore network. The micrometer thick layer employed was manufactured by screen-printing of a starting TiO2 powder constituted of shape-controlled, bipyramidal anatase nanoparticles on FTO/glass substrates. The analytical methods exploited in our study are Focused Ion Beam (FIB) slicing followed by 3D reconstruction as well as the new approach transmission Kikuchi diffraction (TKD) technology in the scanning electron microscope (SEM). Size and shape distribution of the TiO2 NPs within the layer can be extracted. SEM in transmission mode and atomic force microscopy (AFM) have been used to verify the dimensional data obtained by the new combined methodical approach. Its analytical benefits but also the challenges and limitations are highlighted. KW - TiO2 KW - TKD KW - Particle size distribution KW - Nanoparticles KW - Porous film PY - 2017 UR - https://www.cambridge.org/core/services/aop-cambridge-core/content/view/8A8B29335A2F4D0CB6922F6F5A19C5DC/S1431927617003397a.pdf/characterization_of_porous_tio2_nanoparticle_films_using_onaxis_tkd_in_sem_a_new_nanoanalysis_tool_for_a_largescale_application.pdf DO - https://doi.org/10.1017/S1431927617003397 VL - 23 IS - S1 (July) SP - 542 EP - 543 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-41924 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ortel, Erik A1 - Häusler, Ines A1 - Österle, Werner A1 - Narbey, S. A1 - Oswald, F. A1 - Andersen, I. H. A1 - Holzweber, Markus A1 - Unger, Wolfgang A1 - Hodoroaba, Vasile-Dan T1 - In-depth structural and chemical characterization of engineered TiO2 films N2 - Analytical routines for a comprehensive in-depth morphological, structural, and chemical characterization of functionalized TiO2 films by using different state-of-the-art analytical techniques are presented and discussed with the main objective to identify potential reference TiO2 coating parameters able to be certified at a later stage. TiO2 films fabricated by two different synthetic procedures as representative for two main large-scale applications were selected: (i) pulsed d.c. magnetron sputtering for photocatalytic applications and (ii) screen printing from preformed anatase nanoparticles. The screen-printed films were further loaded with a sensitizing dye for application as a dye-sensitized solar cell. Film properties such as microstructure and crystallographic texture of pulsed d.c. magnetron sputtering synthesized films were systematically studied by means of scanning nanobeam electron diffraction in a transmission electron microscope and the surface and inner morphology by scanning electron microscopy. The dye distribution over the depth of screen-printed TiO2 layers was analyzed before and after dye-loading by means of energy dispersive X-ray spectroscopy at scanning electronmicroscope, Auger electron spectroscopy and time-of-flight secondary ion mass spectrometry. The long-term goal of the present study is the improvement of quality of the TiO2 film parameters as measured by using different types of reference TiO2 coatings having specific parameters certified. T2 - 16th European Conference on Applications of Surface and Interface Analysis ECASIA'15 CY - Granada, Spain DA - 28.09.2015 KW - Mapping KW - Line scan KW - Depth profiling KW - TiO2 films KW - Crystallinity KW - Ru dye sensitizer PY - 2016 DO - https://doi.org/10.1002/sia.5966 SN - 0142-2421 SN - 1096-9918 VL - 48 SP - 664 EP - 669 PB - John Wiley & Sons, Ltd. AN - OPUS4-36791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pellegrino, Francesco A1 - Ortel, Erik A1 - Mielke, Johannes A1 - Schmidt, R. A1 - Maurino, V. A1 - Hodoroaba, Vasile-Dan T1 - Customizing New Titanium Dioxide Nanoparticles with Controlled Particle Size and Shape Distribution: A Feasibility Study Toward Reference Materials for Quality Assurance of Nonspherical Nanoparticle Characterization N2 - An overview is given on the synthesis of TiO2 nanoparticles with well-defined nonspherical shapes (platelet like, bipyramidal, and elongated), with the focus on controlled, reproducible synthesis, as a key requirement for the production of reference materials with homogeneous and stable properties. Particularly with regard to the nanoparticle shapes, there is a high need of certified materials, solely one material of this type being commercially available since a few months (elongated TiO2). Further, measurement approaches with electron microscopy as the golden method to tackle the nanoparticle shape are developed to determine accurately the size and shape distribution for such nonspherical particles. A prerequisite for accurate and easy (i.e., automated) image analysis is the sample preparation, which ideally must ensure a deposition of the nanoparticles from liquid suspension onto a substrate such that the particles do not overlap, are solvent-free, and have a high deposition density. Challenges in the Synthesis of perfectly monodispersed and solvent-free TiO2 nanoparticles of platelet and acicular shapes are highlighted as well as successful measurement approaches on how to extract from 2D projection electron micrographs the most accurate spatial information, that is, true 3D size, for example, of the bipyramidal nanoparticles with different geometrical orientations on a substrate. KW - Nanoparticles KW - Titanium dioxide KW - Reference materials KW - Standardisation KW - Particle size and shape distribution PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538849 DO - https://doi.org/10.1002/adem.202101347 VL - 24 IS - 6 SP - 1 EP - 10 PB - Wiley-VCH AN - OPUS4-53884 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ortel, Erik T1 - Determination of porosity of highly porous thin films by combined SEM-EDS analysis T2 - EMAS 2015 - 14th European Workshop on Modern Developments and applications in microbeam analysis CY - Portoroz, Slovenia DA - 2015-05-03 PY - 2015 AN - OPUS4-33245 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Iannarelli, L. A1 - Giovannozzi, A. M. A1 - Morelli, F. A1 - Viscotti, F. A1 - Bigini, P. A1 - Maurino, V. A1 - Spotto, G. A1 - Martra, G. A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan A1 - Rossi, A. M. A1 - Diomede, L. T1 - Shape engineered TiO2 nanoparticles in Caenorhabditis elegans: a Raman imaging based approach to assist tissue-specific toxicological studies N2 - Titanium dioxide (TiO₂) nanoparticles (NPs) are one of the main sources of the nanoparticulate matter to which humans are directly exposed and several studies have demonstrated their potential toxic effects. The in vivo detailed spatial distribution of TiO₂ NPs is investigated herein for the first time, using a 2D chemical imaging analysis based on confocal Raman spectroscopy. The invertebrate nematode C. elegans was employed as a prototypical model of living organisms. Rod, bipyramidal and quasispherical engineered TiO₂ NPs with different primary particle sizes and agglomeration states were prepared, characterized and then administered to nematodes. Exploiting the typical fingerprint of TiO₂ in the Raman spectrum, we monitored the biodistribution of NPs inside the worm using a non-invasive, label-free method. The high spatial resolution chemical imaging and the specificity of the Raman technique in the localization of TiO₂ NPs helped in the design of behavioral C. elegans studies aimed at elucidating the relationship among the size, shape, and agglomeration state of NPs and their ability to induce specific toxic effects. Rod-shaped NPs were the most toxic, greatly impairing pharyngeal function, reproduction and larval growth; this indicates that the rod shape, more than the bipyramidal and spherical shapes, enables NPs to interact with biological systems. These findings indicate that this Raman-nematode combined approach represents a step forward in the field of detection of NPs in living organisms, and being rapid and inexpensive enough, it can be applied as the first screening for the ability of NPs to biodistribute and exert toxicological properties in vivo. KW - Titanium dioxide KW - Nanoparticles KW - Caenorhabdtis elegans KW - Micro-Raman imaging KW - Nanotoxicology PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-369695 UR - http://pubs.rsc.org/en/content/articlelanding/2016/ra/c6ra09686g#!divAbstract DO - https://doi.org/10.1039/c6ra09686g SN - 2046-2069 VL - 6 SP - 70501 EP - 70509 PB - Royal Society of Chemistry CY - Thomas Graham House, Cambridge AN - OPUS4-36969 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lavric, V. A1 - Isopescu, R. A1 - Maurino, V. A1 - Pellegrino, F. A1 - Pellutiè, L. A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan T1 - A new model for nano-TiO2 crystal birth and growth in hydrothermal treatment using an oriented attachment approach N2 - The synthesis of TiO2 was studied in an original hydrothermal process that uses triethanolamine titanium complex Ti(TeoaH)2 as a Ti precursor and triethanolamine (TeoaH3) as a shape controller to obtain bipyramidal anatase nanoparticles. Backed-up by experimental evidence, i.e., time profiles for Ti(IV) species concentrations together with crystal shape and particle size distributions measured by dynamic light scattering and electron microscopy, a mathematical model was built. The model includes chemical reactions responsible for TiO2 generation in solution and the subsequent anatase nucleation and crystal growth. The oriented attachment mechanism was adopted to explain the build-up of crystals with equilibrium anatase structure (Wulff structure) and time-varying shape factor. This complex mathematical model was solved writing and validating an in-house software using the Matlab (Natick, MA, USA) environment. The process was simulated for a batch time of 50 h, and the results, in terms of main species concentration and crystal size distributions, are in rather good agreement with the experimental measurements. KW - Nanoparticles KW - TiO2 KW - SEM/EDX KW - Modelling KW - Crystal growth PY - 2017 UR - http://pubs.acs.org/doi/pdf/10.1021/acs.cgd.7b00302 DO - https://doi.org/10.1021/acs.cgd.7b00302 SN - 1528-7483 SN - 1528-7505 VL - 17 IS - 11 SP - 5640 EP - 5651 PB - ACS Publications AN - OPUS4-42724 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grulke, E. A. A1 - Yamamoto, K. A1 - Kumagai, K. A1 - Häusler, Ines A1 - Österle, Werner A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan A1 - Brown, S. C. A1 - Chan, C. A1 - Zheng, J. A1 - Yamamoto, K. A1 - Yashiki, K. A1 - Song, N. W. A1 - Kim, Y. H. A1 - Stefaniak, A. B. A1 - Schwegler-Berry, D. A1 - Coleman, V. A. A1 - Jämting, Å. K. A1 - Herrmann, J. A1 - Arakawa, T. A1 - Burchett, W. W. A1 - Lambert, J. W. A1 - Stromberg, A. J. T1 - Size and shape distributions of primary crystallites in titania aggregates N2 - The primary crystallite size of titania powder relates to its properties in a number of applications. Transmission electron microscopy was used in this interlaboratory comparison (ILC) to measure primary crystallite size and shape distributions for a commercial aggregated titania powder. Data of four size descriptors and two shape descriptors were evaluated across nine laboratories. Data repeatability and reproducibility was evaluated by analysis of variance. One-third of the laboratory pairs had similar size descriptor data, but 83% of the pairs had similar aspect ratio data. Scale descriptor distributions were generally unimodal and were well-described by lognormal reference models. Shape descriptor distributions were multi-modal but data visualization plots demonstrated that the Weibull distribution was preferred to the normal distribution. For the equivalent circular diameter size descriptor, measurement uncertainties of the lognormal distribution scale and width parameters were 9.5% and 22%, respectively. For the aspect ratio shape descriptor, the measurement uncertainties of the Weibull distribution scale and width parameters were 7.0% and 26%, respectively. Both measurement uncertainty estimates and data visualizations should be used to analyze size and shape distributions of particles on the nanoscale. KW - Measurement uncertainty KW - Size distribution KW - Shape distribution KW - TEM KW - Titania PY - 2017 DO - https://doi.org/10.1016/j.apt.2017.03.027 SN - 0921-8831 VL - 28 IS - 7 SP - 1647 EP - 1659 PB - Elsevier B.V. AN - OPUS4-40478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ortel, Erik A1 - Hertwig, Andreas A1 - Berger, D. A1 - Esposito, P. A1 - Rossi, A. M. A1 - Kraehnert, R. A1 - Hodoroaba, Vasile-Dan T1 - New approach on quantification of porosity of thin films via electron-excited X‑ray spectra N2 - One of the crucial characteristics of functionalized thin films is their porosity (i.e., the ratio between the pore volume and the volume of the whole film). Due to the very low amount of material per coated area corresponding to thin films, it is a challenge for analytics to measure the film porosity. In this work, we present an Approach to determine the porosity of thin films by means of electron probe microanalysis (EPMA) either by wavelength-dispersive X-ray spectrometry (WDX) or by energy-dispersive X-ray spectrometry (EDX) with a scanning electron microscope (SEM). The procedure is based on the calculation of the film mass deposition from electron-excited X-ray spectra. The mass deposition is converted into film density by division of measured film thickness. Finally, the film porosity is calculated from the measured film density and the density of bulk, nonporous film material. The general applicability of the procedure to determine the porosity is demonstrated on thin templated mesoporous TiO₂ films, dip-coated on silicon wafer, with controlled porosity in the range of 15 to 50%. The high accuracy of the mass deposition as determined from X-ray spectra was validated with independent methods (ICP-OES and weighing). Furthermore, for the validation of the porosity results, ellipsometry, interference fringes method (IFM), and focused ion beam (FIB) cross sectioning were employed as independent techniques. Hence, the approach proposed in the present study is proven to be suited as a new analytical tool for accurate and relatively fast determination of the porosity of thin films. KW - Porosity KW - X-rays KW - EDX KW - Thin film KW - TiO2 KW - Density KW - Mass deposition KW - STRATAGem PY - 2016 UR - http://pubs.acs.org/doi/abs/10.1021/acs.analchem.6b00847 DO - https://doi.org/10.1021/acs.analchem.6b00847 VL - 88 IS - 14 SP - 7083 EP - 7090 PB - ACS Publications CY - 1155 Sixteenth Street N.W., Washington, DC 20036 AN - OPUS4-36911 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pellegrino, F. A1 - Pellutiè, L. A1 - Sordello, F. A1 - Minero, C. A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan A1 - Maurino, V. T1 - Influence of agglomeration and aggregation on the photocatalytic activity of TiO2 nanoparticles N2 - Particle aggregation and agglomeration influence the optical properties of materials and therefore theirability to absorb and scatter the incoming radiation, also affecting their photocatalytic activity. Wehave studied the correlation between aggregation and photocatalytic activity for titanium dioxide bymeans of experimental measurements of extinction and photocatalytic activity and calculations of theiroptical properties (extinction, absorption and scattering cross-sections). This approach can be adoptedto quantitatively assess the quantum yields of the heterogeneous photocatalytic systems. The study wasperformed on TiO2PC105 Cristal ACTiVTM, made of aggregated (and agglomerated) primary particles of anatase. The size of the aggregates has been reduced with ultra-sonication. Aqueous suspensions of the obtained materials were characterized by measuring the optical properties (UV–vis extinction), the sizing properties (DLS) and the photocatalytic activity (degradation of phenol under standard con-ditions). The extinction and absorption spectra of the suspensions were derived from the calculatedcoefficients, considering also the size distributions measured with DLS, and revealed that light absorptionis maximized when particle aggregation and agglomeration are avoided, while diffusion of the incomingradiation dominates when large aggregates and agglomerates are present. The present paper represents a valuable approach to the accurate and reproducible measurement of the photocatalytic activity ofTiO2nanoparticles suspensions, thus allowing a more reliable comparison of the properties of different materials. KW - Titanium dioxide KW - Nanoparticles KW - Agglomeration/aggregation KW - Photocatalysis KW - Quantum yield PY - 2017 DO - https://doi.org/10.1016/j.apcatb.2017.05.046 SN - 0926-3373 SN - 1873-3883 VL - 216 SP - 80 EP - 87 PB - Elsevier B.V. AN - OPUS4-40477 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 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 - Ortel, Erik A1 - Kraehnert, R. A1 - Galbert, F. A1 - Hodoroaba, Vasile-Dan T1 - Thin film porosity determined by X-rays at SEM N2 - Various applications such as automotive catalysts, photocatalysis and sensors rely on thin coatings with high active surface area. The development of new and improved coatings requires in-depth understanding of the film morphology and texture. Especially the film porosity is a key parameter to identify structure-property relationships in applications. However, an accurate porosity determination of thin porous coatings is a challenging. In this contribution we present and discuss a new approach for determining the porosity of films by x-rays at SEM. KW - Thin film KW - Porosity KW - EDX KW - SEM KW - Stratagem KW - WDX PY - 2015 DO - https://doi.org/10.1017/S1431927615009319 SN - 1431-9276 SN - 1435-8115 VL - 21 IS - Suppl. 3 SP - Paper 0852, 1707 EP - 1708 PB - Cambridge University Press CY - New York, NY AN - OPUS4-34162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ortel, Erik T1 - Thin Film Porosity Determined by X-Rays at SEM T2 - Microscopy & Microanalysis 2015 Meeting CY - Portland, USA DA - 2015-08-02 PY - 2015 AN - OPUS4-34708 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosu, Dana-Maria A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan A1 - Kraehnert, R. A1 - Hertwig, Andreas ED - Hertwig, Andreas ED - Hinrichs, K. ED - Beck, Uwe ED - Esser, N. T1 - Ellipsometric porosimetry on pore-controlled TiO2 layers N2 - The practical performance of surface coatings in applications like catalysis, water splitting or batteries depends critically on the coating materials’ porosity. Determining the porosity in a fast and nondestructive way is still an unsolved problem for industrial thin-films technology. As a contribution to calibrated, non-destructive, optical layer characterisation, we present a multi-method comparison study on porous TiO2 films deposited by sol-gel synthesis on Si wafers. The ellipsometric data were collected on a range of samples with different TiO2 layer thickness and different porosity values. These samples were produced by templated sol-gel synthesis resulting in layers with a well-defined pore size and pore density. The ellipsometry measurement data were analysed by means of a Bruggeman effective medium approximation (BEMA), with the aim to determine the mixture ratio of void and matrix material by a multi-sample analysis strategy. This analysis yielded porosities and layer thicknesses for all samples as well as the dielectric function for the matrix material. Following the idea of multi-method techniques in metrology, the data was referenced to imaging by electron microscopy (SEM) and to a new EPMA (electron probe microanalysis) porosity approach for thin film analysis. This work might lead to a better metrological understanding of optical porosimetry and also to better-qualified characterisation methods for nano-porous layer systems. 1. IntroductionPorous materials, especially porous thin films play an importantrole in chemical and physical technology in every case where thecontact area between two media has to be maximised. From cataly-sis to photochemistry and photovoltaics, the applications of porouslayer materials are diverse and numerous [1–6].The accurate and non-destructive characterisation of porousfilms for layered systems poses a challenge. This applies especiallyfor the key parameter of porous films, their porosity, i.e. the mix-ing ratio between the Matrix of the film (host material) and thepore volume which is empty or filled with a fluid medium (inclu-sions). This parameter influences most of the physical and chemicalproperties of a porous thin film and is therefore essential for theunderstanding as well as the optimisation of this class of materials. T2 - International Conference on Spectroscopic Ellipsometry (ICSE-7) CY - Berlin, Germany DA - 06.06.2016 KW - Spectroscopic ellipsometry KW - Porous materials KW - Porosimetry KW - Multi-sample analysis KW - Thin film metrology PY - 2017 DO - https://doi.org/10.1016/j.apsusc.2016.11.055 SN - 0169-4332 SN - 1873-5584 VL - 421 IS - Part B SP - 487 EP - 493 PB - Elsevier B.V. AN - OPUS4-42517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ortel, Erik T1 - Shape recognition of nanoparticles by high-resolution SEM and TSEM T2 - Microscopy & Microanalysis 2015 Meeting CY - Portland, USA DA - 2015-08-02 PY - 2015 AN - OPUS4-34709 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ortel, Erik T1 - Shape recognition of nanoparticles by high-resolution SEM and TSEM T2 - International summer workshop Nanoscience meets Metrology CY - Erice, Italy DA - 2015-07-27 PY - 2015 AN - OPUS4-34705 LA - deu 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 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 - CONF A1 - Ortel, Erik T1 - Structural Characterization of Shape-engineered TiO2 Nanoparticles by XRD and SAED T2 - International summer workshop Nanoscience meets Metrology CY - Erice, Italy DA - 2015-07-27 PY - 2015 AN - OPUS4-34704 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kraehnert, R. A1 - Ortel, Erik A1 - Paul, B. A1 - Eckhardt, B. A1 - Kanis, M. A1 - Liu, R. A1 - Antoniou, A. T1 - Electrochemically dealloyed platinum with hierarchical pore structure as highly active catalytic coating N2 - Micro structured reactors are attractive candidates for further process intensification in heterogeneous catalysis. However, they require catalytic coatings with significantly improved space-time yields compared to traditional supported catalysts. We report the facile synthesis of homogeneous nanocrystalline Pt coatings with hierarchical pore structure by electrochemical dealloying of amorphous sputter-deposited platinum silicide layers. Thickness, porosity and surface composition of the catalysts can be controlled by the dealloying procedure. XPS analysis indicates that the catalyst surface is primarily composed of metallic Pt. Catalytic tests in gas-phase hydrogenation of butadiene reveal the typical activity, selectivity and activation energy of nanocrystalline platinum. However, space time yields are about 13 to 200 times higher than values reported for Pt-based catalysts in literature. The highly open metallic pore structure prevents heat and mass transport limitations allowing for very fast reactions and reasonable stability at elevated temperatures. KW - Pt catalysts KW - Pt–Si layers KW - Scanning Electron Microscopy (SEM) KW - Transmission Electron Microscopy (TEM) KW - pore structure KW - electrochemical dealloying PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-351393 DO - https://doi.org/10.1039/C4CY00851K SN - 2044-4753 SN - 2044-4761 VL - 5 IS - 1 SP - 206 EP - 216 PB - RSC Publ. CY - Cambridge AN - OPUS4-35139 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ortel, Erik A1 - Polte, J. A1 - Bernsmeier, D. A1 - Eckhardt, B. A1 - Paul, B. A1 - Bergmann, A. A1 - Strasser, P. A1 - Emmerling, Franziska A1 - Kraehnert, R. T1 - Pd/TiO2 coatings with template-controlled mesopore structure as highly active hydrogenation catalyst N2 - Micro-structured reactors offer excellent mass and heat transport capabilities and can therefore sustain very high reaction rates and space–time-yields also for highly exothermic catalytic reactions. However, such high rates cannot be reached when the reactors are coated or filled with conventional catalysts powders. We present a strategy for the direct synthesis of highly active wall-coated supported catalysts via co-deposition of a pore template (here micelles formed from PEO-b-PPO-b-PEO) and a precursors for the metal oxide (TiCl4) along with a compatible precursor for the active metal (PdCl2). The obtained catalytic coatings possess a template-controlled open pore structure and excellent mechanical stability. Moreover, the active metal is highly dispersed and well-distributed across the coating also at high Pd loadings. The corresponding high activity along with rapid mass transfer enabled by the open pore system results in the best space–time-yields in the gas-phase hydrogenation of butadiene reported so far in literature for a supported catalyst. KW - Titanium oxide films KW - Palladium nanoparticle KW - Wall-coated supported catalysts KW - Template-controlled mesoporous materials KW - Hydrogenation of 1,3-butadiene PY - 2015 DO - https://doi.org/10.1016/j.apcata.2014.12.044 SN - 0926-860X SN - 1873-3875 VL - 493 SP - 25 EP - 32 PB - Elsevier CY - Amsterdam AN - OPUS4-32465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eckhardt, B. A1 - Ortel, Erik A1 - Bernsmeier, D. A1 - Polte, J. A1 - Strasser, P. A1 - Vainio, U. A1 - Emmerling, Franziska A1 - Kraehnert, R. T1 - Micelle-templated oxides and carbonates of zinc, cobalt, and aluminium and a generalized strategy for their synthesis N2 - Catalysis, energy storage, and light harvesting require functional materials with tailored porosity and nanostructure. However, common synthesis methods that employ polymer micelles as structure-directing agents fail for zinc oxide, for cobalt oxide, and for metal carbonates in general. We report the synthesis of the oxides and carbonates of zinc, cobalt, and aluminum with micelle-templated structure. The synthesis relies on poly(ethylene oxide)-block-poly(butadiene)-block-poly(ethylene oxide) triblock copolymers and a new type of precursor formed by chemical complexation of a metal nitrate with citric acid. A general synthesis mechanism is deduced. Mechanistic insights allow for the prediction of optimal processing conditions for different oxides and carbonates based on simple thermogravimetric analysis. Employing this synthesis, films of ZnO and Co3O4 with micelle-controlled mesoporosity become accessible for the first time. It is the only soft-templating method reported so far that also yields mesoporous metal carbonates. The developed synthesis is generic in nature and can be applied to many other metal oxides and carbonates. KW - EISA KW - Pore templating KW - Metal oxide KW - Metal carbonate KW - Zinc oxide KW - Cobalt oxide PY - 2013 DO - https://doi.org/10.1021/cm400535d SN - 0897-4756 SN - 1520-5002 VL - 25 IS - 14 SP - 2749 EP - 2758 PB - American Chemical Society CY - Washington, DC AN - OPUS4-29113 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ortel, Erik A1 - Fischer, A. A1 - Chuenchom, L. A1 - Polte, Jörg A1 - Emmerling, Franziska A1 - Smarsly, B.M. A1 - Kraehnert, R. T1 - New triblock copolymer templates, PEO-PB-PEO, for the synthesis of titania films with controlles mesopore size, wall thickness, and bimodal porosity N2 - The synthesis and properties of a series of new structure-directing triblock copolymers with PEO-PB-PEO structure (PEO = poly(ethylene oxide) and PB = polybutadiene) and their application as superior pore-templates for the preparation of mesoporous titania coatings are reported. Starting from either TiCl4 or from preformed TiO2 nanocrystalline building blocks, mesoporous crystalline titanium oxide films with a significant degree of mesoscopic ordered pores are derived, and the pore size can be controlled by the molecular mass of the template polymer. Moreover, the triblock copolymers form stable micelles already at very low concentration, i.e., prior to solvent evaporation during the evaporation-induced self-assembly process (EISA). Consequently, the thickness of pore walls can be controlled independently of pore size by changing the polymer-to-precursor ratio. Thus, unprecedented control of wall thickness in the structure of mesoporous oxide coatings is achieved. In addition, the micelle formation of the new template polymers is sufficiently distinct from that of typical commercial PPO-PEO-PPO polymers (Pluronics; PPO = poly(propylene oxide)), so that a combination of both polymers facilitates bimodal porosity via dual micelle templating. KW - Mesoporous materials KW - Titanium oxide films KW - Anatase nanoparticles KW - PEO-PB-PEO KW - Dual templating PY - 2012 DO - https://doi.org/10.1002/smll.201101520 SN - 1613-6810 SN - 1613-6829 VL - 8 IS - 2 SP - 298 EP - 309 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-26277 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -