TY - CONF A1 - Omar, Hassan A1 - Szymoniak, Paulina A1 - Hertwig, Andreas A1 - Schönhals, Andreas T1 - Growth Kinetics and Molecular Mobility of the Adsorbed Layer of Poly(bisphenol-A Carbonate) (PBAC), Polysulfone (PSU), and Poly (2-Vinyl Pyridine) (P2VP) N2 - Interactions between a polymer and a substrate interface play a vital role in understanding the improvement in thin film material properties as well as serving as a model for nanocomposites. For any non-repulsive polymer-substrate interactions, polymer segments form an irreversibly adsorbed layer and show a slowdown in the glassy dynamics and thus an increase in the thermal glass transition temperature compared to the bulk-like values. The growth kinetics of the adsorbed layer showed a deviation for both poly (bisphenol-A carbonate) (PBAC) and polysulfone (PSU), two bulky polymers containing a functional group (phenyl ring) in the backbone, compared to conventional polymers previously studied like poly-2-vinyl pyridine (P2VP). This deviation was attributed to the bulkiness of the phenyl rings. . Further investigations into the influence of the adsorbed layer on glassy dynamics were conducted. The molecular mobility and glass transition for thin films of PBAC and PSU were compared to bulk samples of each polymer. Broadband dielectric spectroscopy, atomic force microscopy, and ellipsometry were primarily used and additionally supported by sum frequency generation spectroscopy. T2 - Deutsche Physikalische Gesellschaft (DPG) Tagung CY - Berlin, Germany DA - 17.03.2024 KW - Thin films KW - Adsorbed Layer KW - Atomic Force Microscopy KW - Ellipsometry KW - Dielectric Spectroscopy PY - 2024 AN - OPUS4-59821 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Sachse, René A1 - Kotil, L. A1 - Matjacic, L. A1 - McMahon, G. A1 - Bernicke, M. A1 - Bernsmeier, D. A1 - Kraehnert, R. A1 - Hertwig, Andreas T1 - Morphological and chemical analysis of mesoporous mixed IrOx-TiOy thin films as electrode materials N2 - Porous films play an important role particularly in energy applications like photovoltaics, electrolysis or batteries. Thin film properties such as thickness, chemical composition, crystallinity of the framework, and porosity define the activity of the porous films. The accurate morpho-chemical characterisation of mesoporous thin films is a challenging analytical task which requires the consideration of new analytical approaches based on the combination of data of different methods able to address the structure and chemical composition at the nanoscale. In this contribution we characterise thin mesoporous iridium-titanium mixed oxide film properties by Electron Probe Microanalysis (EPMA) with Energy-Dispersive X-ray Spectroscopy (EDS) at an SEM applied in a dedicated “thin film analysis” approach (1). Thus, the film mass deposition, film thickness and the film density can be determined. Further, by dividing the measured film density to an assumed (theoretical) metal oxide framework (skeletal) density, the thin film porosity can be extracted, too. In order to assess the homogeneity of the thin film properties like the chemical composition, Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) and Auger Electron Spectrometry are applied in the depth profiling mode, so that possible in-depth gradients are detected. Lateral inhomogeneities in the chemical composition and structure of the thin mesoporous films are also identified by applying the same methods in the line-scan or mapping mode, which can be further combined with in-depth sputtering for 3D information. The role of the spatial resolution of the analytical methods considered, which can go down well below 100 nm, will be highlighted. T2 - 2024 Spring Meeting of the European Materials Research Society (E-MRS) CY - Strasbourg, France DA - 27.05.2024 KW - Mesoporous KW - Thin films KW - Iridium oxide KW - Titanium oxide KW - Thin film analysis KW - Porosity KW - SIMS KW - Auger electron spectroscopy PY - 2024 AN - OPUS4-60185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Krüger, Jörg T1 - Structuring of thin films by ultrashort laser pulses JF - Applied physics A N2 - Modern life and global communication would not be possible without technologically tailored thin films; they are omnipresent in daily life applications. In most cases, the films are deposited entirely at the carrying substrates in a specific processing step of the device or sample. In some cases, however, removal or modification must be performed locally, i.e., site-controlled and material selective through an additional laser processing step. For that ultrashort laser pulses with durations in the femtosecond and picosecond range can provide unique advantages and capabilities in industrially scalable schemes. This article reviews the current state of the research and corresponding industrial transfer related to the structuring of thin films by ultrashort pulsed lasers. It focuses on the pertinent historic developments, reveals the relevant physical and chemical effects, explores the ultimate limits, and discusses selected industrial and scientific applications. KW - Thin films KW - Laser processing KW - Ultrashort lasers KW - Laser damage KW - Femtosecond laser ablation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565732 DO - https://doi.org/10.1007/s00339-022-06229-x SN - 0947-8396 SN - 1432-0630 VL - 129 IS - 1 SP - 1 EP - 38 PB - Springer CY - Berlin AN - OPUS4-56573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Terborg, R. A1 - Kim, K. J. A1 - Hodoroaba, Vasile-Dan T1 - Elemental composition and thickness determination of thin films by electron probe microanalysis JF - Surface and Interface Analysis N2 - Electron probe microanalysis (EPMA) applies to solid samples of homogenous (bulk) chemical composition and can usually not be applied to structures which are inhomogeneous in the micrometer range such as thin film systems down to a few nm. However, in combination with the established thin film software Stratagem, the thickness as well as the elemental composition of thin films on a substrate can be determined. This has been recently successfully demonstrated for Fe-Ni on Si and Si-Ge on Al2O3 thin film systems. For both systems five samples of different elemental composition and a reference were produced and characterised by inductively coupled plasma mass spectrometry (ICP-MS), Rutherford backscattering (RBS), and transmission electron microscopy (TEM) as reference values. Last year, a new and open-source thin film evaluation programme called BadgerFilm has been released. It can also be used to determine thin film composition and thickness from intensity ratios of the unknown sample and standards (k-ratios). In this contribution, we reevaluated the data acquired for the Fe-Ni and Si-Ge systems using the BadgerFilm software package and compared the obtained elemental compositions and thickness values with the results of the Stratagem software and the reference methods. The conclusion is that the BadgerFilm software shows good agreement with the elemental composition and thickness calculated by Stratagem (mostly <2% for both composition and thickness) and with the reference values for two representative thin film systems (<1%–2% for composition and <10%–20% for thickness). KW - Elemental composition KW - EPMA KW - Film thickness KW - Thin films PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576368 DO - https://doi.org/10.1002/sia.7183 SN - 0142-2421 VL - 55 SP - 496 EP - 500 PB - Wiley AN - OPUS4-57636 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Omar, Hassan A1 - Szymoniak, Paulina A1 - Hertwig, Andreas A1 - Schönhals, Andreas T1 - Growth Kinetics and Molecular Mobility of the adsorbed Layer of Poly(bisphenol-A Carbonate) (PBAC), Polysulfone (PSU), and Poly (2-Vinyl Pyridine) (P2VP) N2 - Interactions between a polymer and a substrate interface play a vital role in understanding the improvement in thin film material properties as well as serving as a model for nanocomposites. For any non-repulsive polymer-substrate interactions, polymer segments form an irreversibly adsorbed layer and show a slowdown in the glassy dynamics and thus an increase in the thermal glass transition temperature compared to the bulk-like values. The growth kinetics of the adsorbed layer obey a two-step mechanism: formation of immobilized layer with flat segmental conformations and a loosely bound layer with stretched chains pinned to the surface. Here the adsorbed layer was studied for: poly (bisphenol-A carbonate) (PBAC) and polysulfone (PSU), two bulky polymers containing a functional group (phenyl ring) in the backbone and compared to poly (2-vinyl pyridine) (P2VP), where the backbone is a vinyl-derivative and the functional group (pyridine) is in the side chain. The growth kinetics for PBAC and PSU were found to deviate from the well-known mechanism, observed for polymers such as P2VP. Atomic force microscopy and ellipsometry were used for this investigation and was additionally supported by broadband dielectric spectroscopy. T2 - Deutschen Physikalische Gesellschaft (DPG) Tagung CY - Dresden, Germany DA - 26.03.2023 KW - Thin films KW - Adsorbed Layer KW - Broadband dielectric spectroscopy KW - Atomic force microscopy KW - Growth Kinetics PY - 2023 AN - OPUS4-57282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Terborg, R. A1 - Hodoroaba, Vasile-Dan A1 - Kim, K.J. T1 - Determination of Thin Film Thickness and Composition using Energy Dispersive EPMA N2 - Electron probe microanalysis (EPMA)is a non-destructive technique which assumes a sample of homogenous (bulk) chemical composition and can, therefore, not be used for thin film samples. However, in combination with one of the possible thin film software packages, STRATAGEM, the thickness as well as the composition of such films on a substrate can be determined. This has been demonstrated for FeNi on Si and SiGe on Al2O3 film systems. For both systems five samples with different elemental composition and a reference were produced and characterised by the Korean research institute KRISS using inductively coupled plasma mass spectrometry (ICP-MS), Rutherford backscattering (RBS), and transmission electron microscopy (TEM). In 2021, a new and open source thin film evaluation programme called BADGERFILM has been released. It can also be used to determine thin film composition and thickness from intensity ratios of the unknown sample and standards (k-ratios). In this contribution, we re-evaluated the data acquired for the FeNi and SiGe systems using the BADGERFILM software package and compared the resulting composition and thickness with the results of the established STRATAGEM software and other reference methods. With the current evaluation, the BADGERFILM software shows good agreement with the composition and thickness calculated by STRATAGEM and provided by the KRISS. These results between two well-known layered material systems analysed with available conventional EMPA approaches (STRATAGEM and direct thickness measurement by TEM) and a new one (BADGERFILM) proves that reliable non-destructive thin film analysis is possible. In this way, we validate the performance of the new software, which is not at all self-explanatory for such complex quantification algorithms lying behind the final quantified results. T2 - EMAS 2023 - 17th European Workshop on Modern Developments and Applications in Microbeam Analysis CY - Krakow, Poland DA - 07.05.2023 KW - Thin films KW - BADGER film KW - Electron probe microanallysis (EPMA) KW - FeNi thin film KW - Al2O3 thin films PY - 2023 UR - https://www.microbeamanalysis.eu/events/event/60-emas-2023-17th-european-workshop-on-modern-developments-and-applications-in-microbeam-analysis AN - OPUS4-57484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Omar, Hassan A1 - Szymoniak, Paulina A1 - Hertwig, Andreas A1 - Schönhals, Andreas T1 - Probing Nanoscale Relaxation Behavior in Thin Polymer Films N2 - The investigations into the complicated effects of film thickness on bulk properties of thin polymer films has yielded conflicting results. The reduction in molecular mobility, and with it an increase in the glass transition temperature, for thin films of poly (bisphenol A carbonate) (PBAC) was assigned to the formation of an adsorbed layer. The adsorbed layer was obtained by washing away the loosely bounded chains using a good solvent. Next, using atomic force microscopy (AFM), the thickness of each sample was measured after annealing for various times at three different annealing temperatures. The growth of this adsorbed layer was shown to deviate from the previously reported 2-step mechanism seen for other polymers. For PBAC, after very long annealing times at high temperatures the thin films were dewetted, where segments of the adsorbed layer were removed from the substrate. T2 - Royal Society of Chemistry (RSC) Poster CY - Online meeting DA - 28.02.2023 KW - Thin films KW - Adsorbed Layer KW - Broadband dielectric spectroscopy KW - Atomic force microscopy KW - Growth Kinetics PY - 2023 AN - OPUS4-57196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Advanced Characterization of the Surface Morphology and Chemistry within nano@BAM N2 - Both essential aspects of the surface of solid matter, its morphology and chemistry, are studied traditionally at BAM starting in the 60’s with different cyclical research focus areas, mostly related either to applicative research or method development. In the recent years, the focus has shifted almost exclusively to the nano-analytics of advanced materials such as complex nanoparticles, (ultra)thin films/coatings, nanocomposites, 2D materials, energy materials, etc. This is also the reason why BAM has established recently the new Competence Center nano@BAM (www.bam.de/Navigation/DE/Themen/Material/Nanotechnologie/sichere-nanomaterialien.html) with the five sub-fields nanoCharacterisation, nanoMaterial, nanoSafety, nanoData and nanoTechnology. The link to the BAM central guidelines to the safety in technology and chemistry is given by the development of reference products such as reference measurement procedures, reference (nano)materials, and newly reference data sets. Thus, an internationally well-networked group in surface analysis has been established @BAM, with regular contributions to integral analytical characterization with metrological and standardization background. Examples of newly developed methodical approaches will be given with an emphasis on correlative nano-analysis of morphology and chemistry of nanomaterials. Correlative imaging by STEM-in-SEM with high-resolution SEM and EDX, and further with AFM or the new technique TKD (Transmission Kikuchi Diffraction) will be explained on various examples of nanostructures, both as starting materials and embedded/functionalized nanoparticles in products. The unique analytical benefits of the Auger electron probe as a veritable nano-tool for surface chemistry will be highlighted. The panoply of advanced surface characterization methods @BAM is completed by discussing examples of hybrid analysis of the bulk of nanomaterials by X-ray Spectroscopy with the highest surface-sensitive methods X-ray Photoelectron Spectroscopy (XPS) and Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS). Particularly for the analysis of the surface chemistry of nanostructures, such as the completeness of the shells of core-shell nanoparticles or in-depth and lateral gradients of chemistry within mesoporous thin layers, the latter methods are inherent. Other special developments like approaches for the quantitative determination of the roughness of particle surface by electron microscopy or for the quantitative determination of the porosity of thin mesoporous layers by electron probe microanalysis (EPMA) with SEM will be presented. T2 - Seminar of the Academic Centre for Materials and Nanotechnology CY - Online meeting DA - 12.05.2022 KW - Nanoparticles KW - Thin films KW - Nano Characterisation KW - Nanomaterials KW - Surface morphology KW - Surface chemistry PY - 2022 UR - https://www.agh.edu.pl/en/info/article/seminar-advanced-characterization-of-the-surface-morphology-and-chemistry-within-nanobam/ AN - OPUS4-54820 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Liaison report from VAMAS with ISO/TC 202 Microbeam Analysis N2 - The progress in the activities on Microbeam Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 is presented and discussed with respect to the possibility of identifying and launching related VAMAS projects/inter-laboratory comparisons. The recently started project FIB sample processing for TEM is presented. Next projects in the pipeline involving EBSD and TKD are shortly announced. The need of more promotion for the engagement of more experts from industry and academia at national, European and international level is highlighted. Also, the competition with the other technical working areas (on 'nano' or materials-related) is critically discussed. T2 - 29th Annual Meeting of ISO/TC 202 Microbeam Analysis CY - Online meeting DA - 28.11.2022 KW - VAMAS KW - ISO/TC 202 KW - Microbeam Analysis KW - EBSD KW - Electron microscopy KW - Thin films PY - 2022 AN - OPUS4-56424 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Terborg, R. A1 - Hodoroaba, Vasile-Dan A1 - Kim, K. J. T1 - Determination of Thin Film Thickness and Composition using Energy Dispersive EPMA N2 - Electron Probe Microanalysis (EPMA) provides a non-destructive approach in the dedicated thin film analysis mode with the commercial StrataGem software. Recently, the open-source programme BadgerFilm by Moy and Fournelle became available. Similarly to StrataGem, it is based on the algorithm of Pouchou and Pichoir and needs intensity ratios of the unknown sample and standards (k-values). We have evaluated the k-values measured for the FeNi and SiGe film systems using the BadgerFilm software package and compared the thickness and composition with the results obtained with the established StrataGem software and other reference methods. The thicknesses of the SiGe films obtained by the BadgerFilm software agree within 20% with the StrataGem and TEM results; the elemental compositions BadgerFilm-StrataGEM agree within 2% with one exception (9%). T2 - Microscopy and Microanalysis 2022 CY - Portland, OR, USA DA - 31.07.2022 KW - Thin films KW - Thickness KW - Elemental composition KW - FeNi KW - SiGe KW - BadgerFilm KW - Electron Probe Microanalysis (EPMA) PY - 2022 AN - OPUS4-55522 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Omar, Hassan A1 - Szymoniak, Paulina A1 - Hertwig, Andreas A1 - Schönhals, Andreas T1 - Invesitgation of Thin Film Interactions with Inorganic Surfaces N2 - Thin polymer films are of vital importance due to their low production costs and wide range of applications in sensors, electronics, and coatings. Their geometry is ideal for the study of confinement effects, specifically one-dimensional confinement, on the thermodynamic properties and segmental dynamics of polymers. For this investigation, films of PC are prepared on both glass and silica substrates to measure the dielectric and calorimetric behavior as a function of film thickness. The methodology consists of broadband dielectric spectroscopy (BDS), ellipsometry, and atomic force microscopy (AFM). Using ellipsometry, the glass transition shows an increase with decreasing film thickness. Compared to a previous investigation of PC where dilatometry was used, an increase in PC was seen, but now only at thicknesses below 20 nm. Therefore, the critical thickness of PC, where the bulk-like layer no longer percolates through the film, is dependent on the method probing the glass transition. The dielectric behavior shows a deviation from bulk behavior with decreasing film thickness, although still showing a Vogel-Fulcher-Tammann (VFT) temperature dependence for all films. The influence of the adsorbed layer on the molecular mobility was also addressed. T2 - Deutschen Physikalische Gesellschaft (DPG) Tagung CY - Regensburg, Germany DA - 04.09.2022 KW - Thin films KW - Adsorbed Layer KW - Broadband dielectric spectroscopy PY - 2022 AN - OPUS4-55706 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt-Grund, R. A1 - Sturm, C. A1 - Hertwig, Andreas T1 - Ellipsometry and polarimetry - Classical measurement techniques with always new developments, concepts, and applications JF - Advanced optical technologies N2 - Ellipsometry is a matured experimental method, whose roots reach back into the early phase of modern optics itself. It is often attributed to be invented by Paul Drude in the last decade of the 19th century, but similar techniques had already been applied for years before Drude started his work. With this Special Issue about ellipsometry and related techniques, we hope to bring more attention to this method and advance and propagate it to be used by a broader community. We have collected a good mixture of articles: some texts are more in the line of users’ tutorial and best practice guides; others are intended to show recent developments of the method. With this collection, we also hope to show the generally rapidly expanding possibilities of ellipsometry and polarimetry to draw attention of new users and previously unrelated communities to this valuable tool. KW - Ellipsometry KW - Polarimetry KW - Surfaces KW - Thin films KW - Optical analysis PY - 2022 DO - https://doi.org/10.1515/aot-2022-0025 SN - 2192-8584 SN - 2192-8576 VL - 11 IS - 3-4 (Topical issue: Ellipsometry) SP - 57 EP - 58 PB - De Gruyter CY - Berlin AN - OPUS4-55467 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR ED - Schmidt-Grund, R. ED - Sturm, C. ED - Hertwig, Andreas T1 - Topical issue: Ellipsometry T2 - Advanced optical technologies N2 - Ellipsometry is a matured experimental method, whose roots reach back into the early phase of modern optics itself. It is often attributed to be invented by Paul Drude in the last decade of the 19th century, but similar techniques had already been applied for years before Drude started his work. With this Special Issue about ellipsometry and related techniques, we hope to bring more attention to this method and advance and propagate it to be used by a broader community. KW - Spectroscopy KW - Ellipsometry KW - Surfaces KW - Thin films KW - Advanced optics KW - Optical measurement technology PY - 2022 UR - https://www.degruyter.com/journal/key/aot/11/3-4/html#contents SN - 2192-8584 SN - 2192-8576 VL - 11 IS - 3-4 SP - 47 EP - 147 PB - De Gruyter CY - Berlin AN - OPUS4-55468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Terborg, R. A1 - Kim, K. J. A1 - Hodoroaba, Vasile-Dan T1 - Determination of Thin Film Thickness and Composition using Energy Dispersive EPMA JF - Microscopy and Microanalysis N2 - The thickness of thin films can be measured by various methods, e.g., profilometry, ellipsometry, atomic force microscopy (AFM), or X-ray reflectometry. For the additional determination of thin film composition, techniques like X-ray photoelectron spectroscopy (XPS) or mass spectrometry-based techniques can be used. An alternative non-destructive technique is electron probe microanalysis (EPMA). This method assumes a sample of homogenous (bulk) chemical composition, so that it cannot be usually applied to thin film samples. However, in combination with the thin film software StrataGEM, the thickness as well as the composition of such films on a substrate can be determined. This has been demonstrated for FeNi on Si and SiGe on Al2O3 film systems. For both systems five samples with different elemental composition and a reference were produced and characterised by Korean research institute KRISS using inductively coupled plasma mass spectrometry (ICP-MS), Rutherford backscattering (RBS), and transmission electron microscopy (TEM). These samples were used for an international round robin test. In 2021, a new and open-source thin film evaluation programme called BadgerFilm has been released. It can also be used to determine thin film composition and thickness from intensity ratios of the unknown sample and standards (k-ratios). In this contribution, we re-evaluated the data acquired for the FeNi and SiGe systems using the BadgerFilm software package and compared the resulting composition and thickness with the results of the established StrataGEM software and other reference methods. With the current evaluation, the BadgerFilm software shows good agreement with the composition and thickness calculated by StrataGEM and as the reference values provided by the KRISS. KW - Thin films KW - Elemental composition KW - Film thickness KW - EPMA (Electron Probe Microanalysis) PY - 2022 DO - https://doi.org/10.1017/S143192762200318X VL - 28 IS - Suppl. 1 SP - 672 EP - 673 PB - Cambridge University Press AN - OPUS4-55437 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan A1 - Terborg, R. A1 - Kim, K.J. T1 - Elemental Composition and Thickness Determination of Thin Films by Electron Probe Microanalysis (EPMA) N2 - microscopy (AFM), or X-ray reflectometry. For the additional determination of thin film composition, techniques like X-ray photoelectron spectroscopy (XPS) or mass spectrometry-based techniques can be used. An alternative non-destructive technique is electron probe microanalysis (EPMA). This method assumes a sample of homogenous (bulk) chemical composition, so that it cannot be usually applied to thin film samples. However, in combination with the thin film software StrataGEM, the thickness as well as the composition of such films on a substrate can be determined. This has been demonstrated for FeNi on Si and SiGe on Al2O3 film systems. For both systems five samples with different elemental composition and a reference were produced and characterised by Korean research institute KRISS using inductively coupled plasma mass spectrometry (ICP-MS), Rutherford backscattering (RBS), and transmission electron microscopy (TEM). These samples were used for an international round robin test. In 2021, a new and open-source thin film evaluation programme called BadgerFilm has been released. It can also be used to determine thin film composition and thickness from intensity ratios of the unknown sample and standards (k-ratios). In this contribution, we re-evaluated the data acquired for the FeNi and SiGe systems using the BadgerFilm software package and compared the resulting composition and thickness with the results of the established StrataGEM software and other reference methods. With the current evaluation, the BadgerFilm software shows good agreement with the composition and thickness calculated by StrataGEM and as the reference values provided by the KRISS. T2 - ECASIA 2022 CY - Limerick, Ireland DA - 29.05.2022 KW - Thin films KW - Electron Probe Microanalysis KW - Interlaboratory Comparisons PY - 2022 AN - OPUS4-54963 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hudson, A.D. A1 - Jamieson, O. A1 - Crapnell, R.D. A1 - Rurack, Knut A1 - Soares, T.C.C. A1 - Mecozzi, F. A1 - Laude, A. A1 - Gruber, J. A1 - Novakovic, K. A1 - Peeters, M. T1 - Dual detection of nafcillin using a molecularly imprinted polymer-based platform coupled to thermal and fluorescence read-out JF - Materials Advances N2 - Reported here is the production of molecularly imprinted polymer (MIP) films, integrating a fluorescent moiety that serves as both an element for template interaction and signalling, for the thermal and optical detection of the beta-lactam antibiotic nafcillin. Fluorescein methacrylate (FluMa) was synthesized and introduced during the molecular imprinting process as the sole monomer and in a 1 : 1 mixture with methacrylic acid (MAA), allowing to draw first conclusions on the MIP formation potential of such a rather large and rigid monomer. At first, MIP microparticles containing FluMa were prepared by free radical polymerisation. Optical batch rebinding experiments revealed that FluMa can act as a functional monomer for selective detection of nafcillin; however, the addition of MAA as co-monomer significantly improved performance. Subsequently, thin MIP films containing FluMa were deposited onto functionalised glass slides and the influence of porogen, drying time, and monomer composition was studied. These MIP-functionalised glass electrodes were mounted into a customised 3D-printed flow cell, where changes in the liquid were either evaluated with a thermal device or using fluorescence bright field microscopy. Thermal analysis demonstrated that multiple MIP layers enhanced sensor specificity, with detection in the environmentally relevant range. The fluorescence bright field microscope investigations validated these results, showing an increase in the fluorescence intensity upon exposure of the MIP-functionalised glass slides to nafcillin solutions. These are promising results for developing a portable sensor device that can be deployed for antibiotics outside of a dedicated laboratory environment, especially if sensor design and fluorophore architecture are optimised. KW - Molecularly Imprinted Polymers KW - Fluorescence KW - Antibiotics KW - Heat-transfer Measurements KW - Thin films PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-540044 DO - https://doi.org/10.1039/D1MA00192B VL - 2 IS - 15 SP - 5105 EP - 5115 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-54004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abboud, M. A1 - Motallebzadeh, A. A1 - Duygulu, O. A1 - Maaß, Robert A1 - Özerinc, S. T1 - Microstructure and nanomechanical behavior of sputtered CuNb thin films JF - Intermetallics N2 - We report on the mechanical properties of Cu–Nb alloys produced by combinatorial magnetron sputtering. Depending on the composition, the microstructure is either fully amorphous (~30–65 at.% Cu), a dispersion of Cu crystallites in an amorphous matrix (~70 at.%), or a dominant crystalline phase with separated nanoscale amorphous zones (~80 at.% Cu). Nanomechanical probing of the different microstructures reveals that the hardness of the fully amorphous alloy is much higher than a rule of mixture would predict. We further demonstrate a remarkable tunability of the resistance to plastic flow, ranging from ca. 9 GPa in the amorphous regime to ca. 2 GPa in the fully crystalline regime. We rationalize these findings based on fundamental structural considerations, thereby highlighting the vast structure-property design space that this otherwise immiscible binary alloy provides. KW - Deposition microstructure KW - Metallic glasses KW - Thin films KW - Mechanical properties KW - Nanocrystalline structure PY - 2021 DO - https://doi.org/10.1016/j.intermet.2021.107249 SN - 0966-9795 VL - 136 SP - 1 EP - 7 PB - Elsevier CY - Amsterdam AN - OPUS4-52777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gawek, Marcel A1 - Madkour, Sherif A1 - Szymoniak, Paulina A1 - Radnik, Jörg A1 - Schönhals, Andreas T1 - Energy Dependent XPS Measurements on Thin Films of a Poly(vinyl methyl ether)/Polystyrene Blend in Dependence on Film Thickness – Concentration Profile on a Nanometer Resolution to Understand the Behavior of Nanofilms JF - Soft Matter N2 - The composition of the surface layer in dependence from the distance of the polymer/air interface in thin films with thicknesses below 100 nm of miscible polymer blends in a spatial region of a few nanometers is not investigated completely. Here, thin films of the blend poly vinyl methyl ether) (PVME)/polystyrene (PS) with a composition of 25/75 wt% are investigated by Energy Resolved X-ray Photoelectron Spectroscopy (ER-XPS) at a synchrotron storage ring using excitation energies lower than 1 keV. By changing the energy of the photons the information depth is varied in the range from ca. 1 nm to 10 nm. Therefore, the PVME concentration could be estimated in dependence from the distance of the polymer/air interface for film thicknesses below 100 nm. Firstly, as expected for increasing information depth the PVME concentration decreases. Secondly, it was found that the PVME concentration at the surface has a complicated dependence on the film thickness. It increases with decreasing film thickness until 30 nm where a maximum is reached. For smaller film thicknesses the PVME concentration decreases. A simplified layer model is used to calculate the effective PVME concentration in the different spatial regions of the surface layer. KW - Energy dependent XPS KW - Soft X-ray KW - Thin films PY - 2021 DO - https://doi.org/10.1039/d1sm00656h VL - 17 IS - 29 SP - 6985 EP - 6994 PB - The Royal Chemical Society AN - OPUS4-53039 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Terborg, R. A1 - Boehm, S. A1 - Kim, K. J. T1 - Analysis of elemental composition of Fe1-xNix and Si1-xGex alloy thin films by electron probe microanalysis and micro-focus X-ray fluorescence JF - Surface and Interface Analysis N2 - The present study reports on results of analysis of the elemental composition of thin films by electron probe microanalysis with energy dispersive (ED-EPMA) X-ray spectrometry in conjunction with the dedicated thin-film analysis software package Stratagem and by X-ray fluorescence in its version with a micro-focus X-ray fluorescence (μ-XRF) source attached to a scanning electron microscope (SEM). Two thin-film systems have been analyzed: Fe1-xNix on silicon wafer and Si1-xGex on Al2O3 substrate, in both cases the layers being grown to a thickness of about 200 nm by ion beam sputter deposition. Samples of five different atomic fractions have been produced and analyzed for each thin-film system. Moreover, reference samples with certified elemental composition and thickness have been also available. This study is part of an interlaboratory comparison organized in the frame of standardization technical committee ISO/TC 201 “Surface chemical analysis.” Two laboratories have been analyzed by ED-EPMA (one laboratory standardless and one laboratory using both standardless and with standards variants) and one laboratory by μ-XRF (standardless and with standards). All the elemental compositions obtained with different methods are in very good agreement for the complete two sets of five samples each. KW - Thin films KW - Elemental composition KW - FeNi KW - SiGe KW - Electron probe microanalysis KW - X-ray Fluorescence PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509262 DO - https://doi.org/10.1002/sia.6834 SN - 0142-2421 VL - 52 IS - 12 SP - 929 EP - 932 PB - John Wiley & Sons Ltd AN - OPUS4-50926 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fahmy, Alaa A1 - El Sabbagh, M. A1 - Bedair, M. A1 - Gangan, A. A1 - El-Sabbah, M. A1 - El-Bahy, S. A1 - Friedrich, J. T1 - One-step plasma deposited thin SiOxCy films for corrosion resistance of low carbon steel JF - Journal of Adhesion Science and Technology N2 - Tetraethyl orthosilicate (TEOS) was used as a chemical precursor to deposit ultra-thin SiO x C y plasma polymer films onto mild steel surfaces for preventing the corrosion process. The structure–property relationships of the coatings were evaluated by X-ray Photo Spectroscopy (XPS), X-Ray Diffraction (XRD), Fourier Transform InfraRed spectroscopy (ATR-FTIR) and Energy Dispersive X-ray spectroscopy (EDX) completed with Scanning Electron Microscopy (SEM). The SEM micrographs confirmed a pinhole-free surface morphology of the low-pressure deposited plasma polymer films. The TEOS molecules become fragmented in the plasma by numerous collisions with energy-rich electrons and heavier particles. Recombination of fragments and condensation onto the steel substrate is responsible for the formation of organic SiO containing plasma polymer layers. Such thin layers consist of predominantly SiO x structures. Their properties are determined largely by the gap distance between the two samples used as electrodes in the plasma. The efficiency of the corrosion-protecting coating was compared with uncoated samples. The corrosion protection was determined by exposure of samples to 3.5% NaCl aqueous solutions. For this purpose, polarization and Electrochemical Impedance Spectroscopy (EIS) were used to monitor the corrosion. The optimal gap distance between the electrodes was determined for corrosion protection. The best protective efficiency reached more than 97% of the total protection as measured at room temperature. KW - Thin films KW - Corrosion resistance KW - Mild steel KW - Plasma treatments KW - Tetraethyl orthosilicate PY - 2020 DO - https://doi.org/10.1080/01694243.2020.1856539 VL - 35 IS - 16 SP - 1734 EP - 1751 PB - Taylor & Francis AN - OPUS4-52303 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Sachse, René A1 - Hertwig, Andreas A1 - Kraehnert, R. T1 - Analysis of elemental composition and porosity of mesoporous IrOx-TiOx thin films by SEM/EDS N2 - Porous materials play an important role in several fields of technology, especially for energy applications like photovoltaics, electrolysis or batteries. The activity of porous films is affected by properties like porosity, film thickness, chemical composition of the material, as well as the crystallinity of the framework. The complex morphology of such porous films constitutes a challenge even for modern analytical techniques and requires new approaches employing the combination/complementation of data of different analytical methods. In this contribution, we characterise thin mesoporous iridium-titanium mixed oxide film properties by electron probe microanalysis (EPMA) with energy-dispersive X-ray spectroscopy (EDS) at an SEM. Mesoporous iridium oxide - titanium oxide (IrOx-TiOx) films were prepared via dip-coating of a solution containing a triblock-copolymer as structure-directing agent, an iridium precursor as well as a titanium precursor in ethanol. IrOx-TiOx films were synthesized with different amounts of iridium and calcined in air. The SEM micrographs reveal for all films the achievement of a well-ordered mesoporous structure and homogeneous films with thicknesses between 67 nm and 152 nm. For the determination of film elemental composition and porosity, EPMA can be used as part of a combined SEM/EDS/STRATAGem analysis. Elemental compositions and mass depositions (in μg cm-2) of IrOx-TiOx films were calculated with the thin film analysis Software STRATAGem via k-values measured with SEM/EDS. Pure bulk Ir, TiO2 and Si were measured as references. The average density of the films was obtained from the mass Deposition and the film thickness as measured by cross-section SEM. The porosity was then extracted from the measured average film density divided by a theoretical bulk density. The latter is calculated from the weight fractions of IrOx and TiOx as determined with STRATAGem and the bulk mass densities of IrO2 and TiO2 (rutil) from literature. The fitting results of the k-values from the STRATAGem software, which are in fair agreement with the measured k-values. The application of the SEM/EDS/STRATAGem approach for accurate porosity determination on pure mesoporous TiOx films and pure porous IrOx films has been recently demonstrated. The porosities of pure IrOx, TiOx and mixed IrOx-TiOx films in this study have been determined. The contribution will assess in detail the advantages and limitations of the combined SEM/EDS/STRATAGem analysis for the morphology and porosity of thin metal oxide films. Moreover, the comparison with other measurement techniques and the combination of datasets from multiple measurements will be discussed. T2 - EMAS 2019 - 16th European Workshop on MODERN DEVELOPMENTS AND APPLICATIONS IN MICROBEAM ANALYSIS CY - Trondheim, Norway DA - 19.05.2019 KW - Thin films KW - Porous layers KW - Electron probe microanalysis (EPMA) KW - Porosity PY - 2019 AN - OPUS4-48107 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duwe, M. A1 - Quast, J.-H. A1 - Schneider, S. A1 - Fischer, Daniel A1 - Beck, Uwe T1 - Thin-film metrology of tilted and curved surfaces by imaging Mueller-matrix ellipsometry JF - Journal of Vacuum Science & Technology B N2 - For the vast majority of ellipsometric measurements, the application of planar substrates is mandatory and requires a proper sample alignment prior to the measurement. Here, the authors present a generalized approach of how to extract the isotropic ellipsometric sample parameters from an imaging Mueller-matrix measurement even if the sample is significantly misaligned. They validate the method by layer-thickness calculations based on imaging Mueller-matrix measurements of flat crystalline silicon samples that were misaligned on purpose. Furthermore, they also exploit this method’s capabilities to perform spatially resolved layer-thickness measurements of a single-layer indium-tin-oxide coating on a fused-silica microlens without the need of realignment or repositioning of the sample during the measurement. T2 - 8th International conference on spectroscopic ellipsometry (ICSE-8) CY - Barcelona, Spain DA - 26.05.2019 KW - Metrology KW - Thin films KW - Polarization spectroscopy KW - Spectroskopic Imaging KW - Mueller-Matrix imaging ellipsometry PY - 2019 DO - https://doi.org/10.1116/1.5122757 SN - 2166-2746 SN - 2327-9877 VL - 37 IS - 6 SP - 062908 PB - AIP CY - New York, NY AN - OPUS4-50209 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Terborg, R. A1 - Boehm, S. A1 - Kim, K. J. T1 - Measurement of Elemental Composition of and SiGe Alloy Thin Films by EPMA and µ-XRF N2 - The present study reports on measurements on thin Fe-Ni films on silicon and first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide Substrate by electron probe microanalysis (EPMA). Standard-based and standardless EPMA (with EDS) results were used in combination with the thin film analysis software Stratagem for the quantification. Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results. Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex alloy films obtained by different surface Analysis techniques, such as X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and secondary ion mass spectrometry (SIMS) applied in the depth-profiling operation mode. Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. An excellent agreement has been obtained between the atomic fractions determined by EPMA and µ-XRF with the KRISS certified values. T2 - European Conference on Applications of Surface and Interface Analysis ECASIA 2019 CY - Dresden, Germany DA - 15.09.2019 KW - Thin films KW - EPMA KW - XRF KW - FeNi KW - SiGe PY - 2019 AN - OPUS4-49278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Terborg, R. A1 - Boehm, S. A1 - Kim, K. J. T1 - Analysis of elemental composition of Fe1-xNix and Si1-xGex alloy thin films by EPMA and µ-XRF N2 - The present study reports on measurements on thin Fe-Ni films on silicon and first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide Substrate by electron probe microanalysis (EPMA). Standard-based and standardless EPMA (with EDS) results were used in combination with the thin film analysis software Stratagem for the quantification. Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results. Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex alloy films obtained by different surface Analysis techniques, such as X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and secondary ion mass spectrometry (SIMS) applied in the depth-profiling operation mode. Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. An excellent agreement has been obtained between the atomic fractions determined by EPMA and µ-XRF with the KRISS certified values. T2 - Microscopy & Microanalysis 2019 CY - Portland, OR, USA DA - 03.08.2019 KW - Thin films KW - EPMA KW - µ-XRF KW - Elemental composition KW - Atomic fraction KW - Fe-Ni KW - Si-Ge PY - 2019 AN - OPUS4-48709 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sachse, René A1 - Kotil, L. A1 - Hodoroaba, Vasile-Dan A1 - Bernsmeier, Denis A1 - Kraehnert, R. A1 - Hertwig, Andreas T1 - Spectroscopic ellipsometric analysis of elemental composition and porosity of mesoporous iridium-titanium mixed oxide thin films for electrocatalytic splitting of water N2 - Porous materials play an important role in several fields of technology, especially for energy applications like photovoltaics, electrolysis or batteries. The activity of porous films is affected by properties like porosity, film thickness, chemical composition of the material as well as the crystallinity of the framework. The complex morphology of such porous films constitutes a challenge for modern analytical techniques and requires approaches employing the combination/complementation of data of different analytical methods. In this contribution we characterize thin mesoporous iridium-titanium mixed oxide film properties by spectroscopic ellipsometry (SE). Mesoporous iridium oxide - titanium oxide (IrOx-TiOx) films were prepared via dip-coating of a solution containing a triblock-copolymer as structure-directing agent, an iridium precursor as well as a titanium precursor in ethanol. Deposited films with different amounts of iridium (0 wt%Ir to 100 wt%Ir) were synthesized and calcined in air. The thin films were analyzed with SE using the Bruggeman effective medium approximation (BEMA) for modelling. The results were compared with electron probe microanalysis (EPMA) as part of a combined SEM/EDS/STRATAGem Analysis. T2 - 8th International conference on spectroscopic ellipsometry (ICSE-8) CY - Barcelona, Spain DA - 26.05.2019 KW - Mesoporous iridium-titanium mixed oxides KW - Thin films KW - Spectroscopic ellipsometry KW - Oxygen evolution reaction KW - EPMA KW - Ellipsometric porosimetry PY - 2019 AN - OPUS4-48387 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Szymoniak, Paulina T1 - Glass transition and glassy dynamics of thin polymer films and polymer nanocomposites N2 - Polymers at interfaces play a major role in a broad variety of applications ranging from engineering purposes (for instance polymer based nanocomposites) to high tech implications (for instance light emitting diodes). Here the glass transition and glassy dynamics is considered for epoxy-based nanocomposite with Layered Double Hydroxide nanofiller and for thin films of a misicble polymer blend of PVME/PS with thicknesses down to 7 nm. The materials are investigated by spectroscopic techniques (broadband and specific heat spectroscopy), as well as by fast scanning calorimetry and small- and wide-angle X-ray scattering. T2 - Seminarvortrag Columbia University CY - New York, USA DA - 11.03.2019 KW - Nanocomposites KW - Rigid amorphous fraction KW - Thin films KW - Interfaces PY - 2019 AN - OPUS4-47565 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 - CONF A1 - Rades, Steffi A1 - Ortel, Erik A1 - Wirth, Thomas A1 - García, Sarai A1 - Gómez, Estibaliz A1 - Blanco, Miren A1 - Alberto, Gabriele A1 - Martra, Gianmario A1 - Hodoroaba, Vasile-Dan T1 - Surface and in-depth analysis of functionalization of TiO2 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. T2 - EMAS 2017 - 15th European Workshop on MODERN DEVELOPMENTS AND APPLICATIONS IN MICROBEAM ANALYSIS and IUMAS-7 Meeting CY - Constance, Germany DA - 07.05.2017 KW - Functionalization KW - Surface analysis KW - Nanoparticles KW - Thin films PY - 2017 AN - OPUS4-40266 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Daniel A1 - Hertwig, Andreas A1 - Beck, Uwe A1 - Lohse, V. A1 - Negendank, D. A1 - Kormunda, M. A1 - Esser, N. T1 - Thin SnOx films for surface plasmon resonance enhanced ellipsometric gas sensing (SPREE) JF - Beilstein Journal of Nanotechnology N2 - Background: Gas sensors are very important in several fields like gas monitoring, safety and environmental applications. In this approach, a new gas sensing concept is investigated which combines the powerful adsorption probability of metal oxide conductive sensors (MOS) with an optical ellipsometric readout. This concept Shows promising results to solve the problems of cross sensitivity of the MOS concept. Results: Undoped tin oxide (SnOx) and iron doped tin oxide (Fe:SnOx) thin add-on films were prepared by magnetron sputtering on the top of the actual surface plasmon resonance (SPR) sensing gold layer. The films were tested for their sensitivity to several gas species in the surface plasmon resonance enhanced (SPREE) gas measurement. It was found that the undoped tin oxide (SnOx) shows higher sensitivities to propane (C3H8) then to carbon monoxide (CO). By using Fe:SnOx, this relation is inverted. This behavior was explained by a change of the amount of binding sites for CO in the layer due to this iron doping. For hydrogen (H2) no such relation was found but the sensing ability was identical for both layer materials. This observation was related to a different sensing mechanism for H2 which is driven by the Diffusion into the layer instead of adsorption on the surface. Conclusion: The gas sensing selectivity can be enhanced by tuning the properties of the thin film overcoating. A relation of the binding sites in the doped and undoped SnOx films and the gas sensing abilities for CO and C3H8 was found. This could open the path for optimized gas sensing devices with different coated SPREE sensors. KW - Doped tin oxide KW - Ellipsometry KW - Gas sensing KW - Surface plasmon KW - Resonance KW - Thin films KW - Transparent conductive oxides PY - 2017 DO - https://doi.org/10.3762/bjnano.8.56 SN - 2190-4286 VL - 8 SP - 522 EP - 529 AN - OPUS4-39391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madkour, Sherif A1 - Szymoniak, Paulina A1 - Heídari, M. A1 - von Klitzing, R. A1 - Schönhals, Andreas T1 - Unveiling the dynamics of self-assembled layers of thin films of poly(vinyl methyl ether) (PVME) by nanosized relaxation spectroscopy JF - ACS Applied Materials and Interfaces N2 - A combination of nanosized dielectric relaxation (BDS) and thermal spectroscopy (SHS) was utilized to characterize the dynamics of thin films of Poly(vinyl methyl ether) (PVME) (thicknesses: 7 nm – 160 nm). For the BDS measurements, a recently designed nano-structured electrode system is employed. A thin film is spin-coated on an ultra-flat highly conductive silicon wafer serving as the bottom electrode. As top electrode, a highly conductive wafer with non-conducting nanostructured SiO2 nano-spacers with heights of 35 nm or 70 nm is assembled on the bottom electrode. This procedure results in thin supported films with a free polymer/air interface. The BDS measurements show two relaxation processes, which are analyzed unambiguously for thicknesses smaller than 50 nm. The relaxation rates of both processes have different temperature dependencies. One process coincidences in its position and temperature dependence with the glassy dynamics of bulk PVME and is ascribed to the dynamic glass transition of a bulk-like layer in the middle of the film. The relaxation rates were found to be thickness independent as confirmed by SHS. Unexpectedly, the relaxation rates of the second process obey an Arrhenius-like temperature dependence. This process was not observed by SHS and was related to the constrained fluctuations in a layer, which is irreversibly adsorbed at the substrate with a heterogeneous structure. Its molecular fluctuations undergo a confinement effect resulting in the localization of the segmental dynamics. To our knowledge, this is the first report on the molecular dynamics of an adsorbed layer in thin films. KW - Broadband dielectric spectroscopy KW - AC-nanochip calorimetry KW - Nanostructured capacitors KW - Thin films PY - 2017 UR - http://pubs.acs.org/doi/pdf/10.1021/acsami.6b14404 DO - https://doi.org/10.1021/acsami.6b14404 SN - 1944-8244 VL - 9 IS - 8 SP - 7535 EP - 7546 PB - ACS Publications CY - Washington DC AN - OPUS4-39291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Madkour, Sherif A1 - Szymoniak, Paulina A1 - Schönhals, Andreas T1 - In-situ probing of the dynamics of irreversibly adsorbed layers in PVME thin films N2 - For many years now, the so-called three layer model (free-surface, bulk-like, and adsorbed layers) has been commonly used, along with other parameters, to explain the deviations seen in glass transition and glassy dynamics for polymers confined into thin films, compared to their bulk value. Nevertheless, due to the hard accessibility of the adsorbed layers in supported films, little is known about the nature of their dynamics and how they really influences the overall dynamics of the thin films. Here, the irreversibly self-assembled adsorbed layer of a low MW Poly (vinyl methyl ether) (PVME) is solvent-leached from a 200 nm film. The thickness and topography of this layer is checked with Atomic Force Microscopy (AFM), to insure no dewetting and low roughness. Further, the dynamics of the adsorbed layer is then in-situ probed with Broadband Dielectric Spectroscopy (BDS). A recently developed nano-structured capacitor arrangement was employed; where a silicon wafer with nanostructured SiO2 nano-spacers, with heights of 35 nm, is placed on top of a thin film spin coated on an ultra-flat highly conductive silicon wafer. All results will be discussed in detail and quantitatively compared to our recent work on the glassy dynamics of PVME thin films (50 nm- 7nm), where BDS measurements showed two thickness-independent relaxation processes. The first process was assigned to the -relaxation of a bulk-like layer. Whereas the second process showed a different temperature dependence and was ascribed to the relaxation of polymer segments adsorbed at the substrate. To our knowledge, this is the first in-situ study of the dynamics of an irreversibly adsorbed layer. T2 - 8th International Discussion Meeting Relaxation in Complex Systems CY - Wisla, Poland DA - 23.07.2017 KW - Thin films PY - 2017 AN - OPUS4-41190 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Rades, Steffi A1 - Oswald, F. A1 - Narbey, S. A1 - Radnik, Jörg T1 - Complementary methodical approach for the analysis of a perovskite solar cell layered system N2 - Loss in efficiency of perovskite solar cells may be caused by structural and/or chemical alterations of the complex layered system. As these changes might take place either in the bulk and/or on the surface of the stratified material, analytical tools addressing both key issues are selected and combined. 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. The TiO2 film is subdivided into a dense layer covered by a porous one constituted of nanoparticles with a truncated bipyramidal shape. 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. In a SEM micrograph taken of the cross-section of a sample after illumination, the glass substrate and all layers FTO, TiO2, ZrO2 as well as C are clearly identified. 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. T2 - Microscopy & Microanalysis 2017 Meeting CY - St. Louis, MO, USA DA - 06.08.2017 KW - Thin films KW - EDX KW - XPS KW - SEM KW - Nanoparticles KW - Perovskite KW - TiO2 PY - 2017 AN - OPUS4-41664 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg A1 - Madkour, Sherif A1 - Lippitz, Andreas A1 - Schönhals, Andreas A1 - Unger, Wolfgang T1 - Anomalous surface composition in thin films of a poly(vinyl methyl ether) / polystyrene blend N2 - Highly surface-sensitive X-ray photoelectron spectroscopy at HE-SGM beamline revealed in the outermost region (< 2nm) of thin films (15 -65 nm) of PVME/PS blends a relative high amount of PS, whereas in slightly deeper regions PVME was enriched. Such enrichment of PVME in the whole near-surface region was proposed in former investigations based on conventional XPS studies. T2 - Bessy User Meeting 2017 CY - Berlin, Germany DA - 13.12.2017 KW - Energy resolved XPS KW - Depth profiling KW - Thin films KW - Polymer blends PY - 2017 AN - OPUS4-43443 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stockmann, Jörg M. A1 - Hertwig, Andreas A1 - Beck, Uwe T1 - Visualization of low-contrast surface modifications: thin films, printed pattern, laser-induced changes, imperfections, impurities, and degradation N2 - Industrial quality control (QC) nowadays requires the visualization of surface modifications from the macro-scopic to the microscopic or even nanoscopic scale. This is a prerequisite to the evaluation of functionality and reliability, the detection of defects and their separation of artefacts. The diversity of applications ranges from low-E glazings and solar panels, micro- and optoelectronics, micro- and smart devices to sensor-on-chip and lab-on-chip systems [1]. Optical microcopy (light, confocal laser scanning, white light interference) as established QC-tool is operated at normal incidence, i.e. p- and s-polarization are undistinguishable. Either light-intensity in terms of grey scale and colour or intensity-correlated effects of phase shifts are used. In case of ellipsometry, operated at oblique incidence, p- and s-polarization matter, and amplitude ratios and phase shifts upon reflection are measured. Hence, information content must be much higher. The visualization of surface modifications may be very challenging for coating/substrate systems of either al-most identical optical constants, e.g. transparent films on substrates of the same material, or minor film thick-ness, substance quantity and affected area, e.g. ultra-thin or island films. Ellipsometry gives access to the con-trast of intensity (I), amplitude ratio (Ψ), and phase shift (Δ) with nanometer-scaled vertical and micrometer-scaled lateral sensitivity, one is able to identify tiny changes within an unmodified surface. As both mapping ellipsometry (ME) and imaging ellipsometry (IE) are operated in the optical far-field, surface inspection is also possible on the macroscopic scale. Near the Brewster-angle of the bare, undamaged, clean, and fresh substrate, the contrast to add-on and sub-off features is superior. Fig. 1 shows three examples of ellipsometric imaging, i.e. a thin SnO:Ni film on SiO2/Si (Fig. 1a), a dried stain of an anti-body solution on cyclo-olefin-polymer (COP) shown in Fig. 1b, and a polyimide film residue on SiO2/Si (Fig. 1c). For all of these examples, ellipsometry provides much better contrast between substrate and surface modification than optical microscopy, sometimes primarily caused by the oblique incidence (Figs. 1a and 1c), in other cases related to the phase sensitivity of ellipsometry (Fig. 1b). Other examples are laser surface modifications and the corrosion of glass. In these cases, optical microscopy and IE yield to similar results, how-ever only ellipsometry gives access to modelling. Further investigated coating/substrate systems are 100Cr6 steel, native oxide on silicon, borosilicate glass, and the polymer polycarbonate with deposited films of graphene and ta-C:H, printed and dried pattern of liquids such as water, cleaning agents, and dissolved silicone. Besides imaging ellipsometry, referenced spectral ellipsometry (RSE) has been applied, combining the advantages of both optical microscopy (fast measurement) and ellipsometry (high sensitivity to tiny modifications). T2 - International Conference on Spectroscopic Ellipsometry (ICSE-7) CY - Berlin, Germany DA - 06.06.2016 KW - Ellipsometry KW - Thin films KW - Impurities KW - Degradation PY - 2016 AN - OPUS4-37068 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Nanoparticles and films characterization: Electron microscopy and related techniques N2 - Scanning Electron Microscopy (SEM) represents the mostly widespread method available in analytical laboratories dedicated to the characterization of physical properties such as morphology of various solid materials from ‘micro-’ down to the nanometre scale. The use of secondary electrons excited by a sharply, nm-focussed primary electron beam enables at any modern SEM to image objects with high in-depth and lateral sensitivity, i.e. with high spatial resolution. Hence, e. g. nanoparticles (NPs) are able to be easily characterized with respect to their individual size and shape, but also to the morphology of their surface. By preparing the nano-objects on thin membranes as electron transparent samples it is possible to perform electron microscopy in the transmission mode (TEM and TSEM). The corresponding transmission (i.e. mass-thickness) contrast reveals in-depth information, but is also well suited for dimensional measurements in the 2D projection image. Both the surface sensitive mode and the transmission one are meanwhile available at any modern SEM. If an X-ray spectrometer is attached to an electron microscope, it is possible to analyse the characteristic X-rays induced by electron bombardment. Most electron microscopes have attached an energy dispersive X-ray spectrometer (EDX) so that EDX elemental maps can be carried out. Recent technological developments of high throughput EDS detectors and their advantages regarding high-resolution X-ray analysis down to the nm range are reviewed. High-resolution micrographs (SEM, TSEM, TEM) and corresponding X-ray elemental maps on various representative nanoparticles, but also layered samples prepared in cross-section, will be presented and discussed. The importance of selecting the best suited analysis conditions will be highlighted. Also other, often challenging, topics such as sample preparation and image data processing will be critically addressed by practical examples. Further analytical techniques able to be employed at an electron microscope, like cathodoluminescence (CL) or micro-X-ray fluorescence (µXRF) will be briefly surveyed. T2 - Nanoscience Meets Metrology - Synthesis, Characterization, Testing and Applications of Validated Nanoparticles - International Summer School CY - Turin, Italy DA - 04.09.2016 KW - Nanoparticles KW - Electron microscopy KW - High-resolution KW - Thin films KW - X-ray spectroscopy PY - 2016 UR - http://www.setnanometro.eu/events/ AN - OPUS4-37325 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosu, Dana-Maria A1 - Hertwig, Andreas A1 - Beck, Uwe T1 - The accuracy and reproducibility in thickness determination of thin films using SE N2 - Maintaining a consistent product quality is critical for the thin film industry. Therefore, the development of highly accurate protocols able to detect variations and nonidealities in manufactured thin film devices is essential and helps improve production quality and decrease manufacturing costs. The present work will discuss the accuracy and reproducibility in the determination of the thickness of thin films relevant for optoelectronic industry using spectroscopic ellipsometry, starting with the importance of set-up calibration, the need for very well defined calibration standards suitable for real devices and not least, the importance of accurate data analysis. As ellipsometry is an indirect method and theoretical modelling is needed to obtain the desired information regarding the investigated samples (e.g. thickness, roughness, optical constants), the model uncertainty has to be discussed and taken into account. If for ideal samples consisting of single layers with well-known optical constants the determination of thickness and roughness is straight forward and pretty accurate, for real samples, more complex theoretical models are needed and extracting accurate information regarding the samples can be very challenging. With careful calibration and a multidisciplinary approach, a combined measurement methodology can be developed enabling reliability, comparability, and accuracy. For production-relevant operation, maintaining the ease of use and scalability of ellipsometry as a technique can also be retained. T2 - EOSAM (European Optical Society Annual Meeting) CY - Berlin, Germany DA - 26.09.2016 KW - Spectroscopic ellipsometry KW - Thin films KW - Film thickness determination KW - Uncertainty PY - 2016 AN - OPUS4-38109 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rades, Steffi A1 - Ortel, Erik A1 - Wirth, Thomas A1 - Garcia, Sarai A1 - Gomez, Estibaliz A1 - Blanco, Miren A1 - Alberto, Gabriele A1 - Martra, Gianmario A1 - Hodoroaba, Vasile-Dan T1 - Analysis of functionalization of TiO2 nanoparticles and various substrates by means of SEM-EDX, AES and ToF-SIMS N2 - The physico-chemical characteristics of TiO2 coatings can greatly influence their final performance. In SETNanoMetro, different deposition procedures are being set for applying films of TiO2 NPs with defined and homogenous thickness on supports of interest for the applications studied in the project. The selected substrates are the following: (i) Silica glasses for photocatalytic measurements, (ii) Ti-alloys for orthopedic and/or dental prostheses, and for cell cultures, and (iii) Conductive glasses (e.g. Fluorine doped Tin Oxide, FTO) for dye-sensitized solar cells. From the different film deposition procedures studied within the project Self-assembly of TiO2 NPs in multiple layers was selected. For this, surface modification of the substrate and of TiO2 nanoparticles (NPs) with e.g. silane coupling agents is a prerequisite. First attempts to prepare the self-assembled coating on the functionalized glass substrates seem to indicate that the functionalized NPs adhere to the substrates, even if the final coatings were not homogenous and presented agglomerates. ToF-SIMS results support this outcome. In order to use the layer-by-layer deposition technique for the formation of TiO2 films by controlled self-assembly of the TiO2 NPs, the proper complementary moieties for the functionalization of the NPs were chosen. A first set of NPs has been produced by reaction with (3-aminopropyl)phosphonic acid (APPA) in order to functionalize the surface with free amino-groups. Then, the complementary 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. A proper approach for the functionalization of two types of TiO2, commercial P25 (Evonik) and SETNanoMetro-sample labelled UT001, with APPA was developed. A second set of NPs consisting of three types of TiO2 NPs, P25 and SETNanoMetro NPs (TiO2 NPs with high specific surface area > 150 m2/g and TiO2 NPs with low size < 20 nm) was functionalized with (3-aminopropyl)triethoxysilane (APTS). As for the previous set of NPs, the complementary NP set was obtained through the conversion of free surface amino-groups to aldehydes by reaction with glutaraldehyde. EDX, AES and ToF-SIMS spectra were collected and analyzed to demonstrate the presence of the surface functionalization of the different types of TiO2 NPs. T2 - Nanoscience meets Metrology - Synthesis, Characterization, Testing and Applications of Validated Nanoparticles - International Summer School CY - Turin, Italy DA - 04.09.2016 KW - Time-of-flight secondary-ion mass spectrometry KW - X-ray spectroscopy KW - Auger electron spectroscopy KW - Electron microscopy KW - Nanoparticles KW - Thin films PY - 2016 UR - http://www.setnanometro.eu/events/ AN - OPUS4-38064 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Derrien, Thibault J.-Y. A1 - Krüger, Jörg A1 - Bulgakova, N. M. A1 - Bonse, Jörn T1 - Multi-wavelength, multi-material prediction tools for the LIPSS community N2 - This talk presents multi-wavelength, multi-material prediction tools serving as useful models for researchers working in the field of laser-induced periodic surface structures (LIPSS). These models explain the role of surface plasmon polaritons (SPPs) in the formation of LIPSS. They particularly consider the cases of (i) “lossy” materials (where the imaginary part of the dielectric permittivity should not be neglected) and (ii) the excitation of SPPs in a thin film configuration (where two film interfaces become plasmonically active and couple to each other). T2 - 6th International LIPSS Workshop CY - Heraklion (Crete), Greece DA - 24.11.2016 KW - Surface plasmon polaritons KW - Laser-induced periodic surface structures (LIPSS) KW - Lossy materials KW - Thin films PY - 2016 AN - OPUS4-38512 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stockmann, Jörg M. A1 - Hertwig, Andreas A1 - Beck, Uwe T1 - Visualization of low-contrast surface modifications: Thin films, printed pattern, laser-induced changes, imperfections, impurities, and degradation JF - Applied Surface Science N2 - Visualization of surface modifications may be very challenging for coating/substrate systems of either almost identical optical constants, e.g. transparent films on substrates of the same material, or minor film thickness, substance quantity and affected area, e.g. ultra-thin or island films. Methods for visualization are optical microscopy (OM), imaging ellipsometry (IE), and referenced spectroscopic ellipsometry (RSE). Imaging ellipsometry operates at oblique incidence near Brewster angle of the bare, clean or unmodified substrate. In this configuration, reflected intensities are rather weak. However, the contrast to add-on and sub-off features may be superior. Referenced spectroscopic ellipsometry operates in a two-sample configuration but with much higher intensities. In many cases, both ellipsometric techniques reveal and visualize thin films, printed-pattern, laser-induced changes, and impurities better than optical microscopy. In particular for stratified homogeneous modifications, ellipsometric techniques give access to modelling and hence thickness determination. Modifications under investigation are polymer foil residue on silicon, laser-induced changes of ta-C:H coatings on 100Cr6 steel, imperfections of ta-C:H on thermal silicon oxide, degradation of glass, thin film tin oxide pattern on silicon, printed and dried pattern of liquids such as deionized water, cleaning agents, and dissolved silicone. © 2016 Elsevier B.V. All rights reserved. T2 - International Conference on Spectroscopic Ellipsometry (ICSE-7) CY - Berlin, Germany DA - 06.06.2016 KW - Optical microscopy (OM) KW - Imaging ellipsometry (IE) KW - Referenced spectroscopic ellipsometry (RSE) KW - Thin films KW - Impurities KW - Degradation PY - 2016 DO - https://doi.org/10.1016/j.apsusc.2016.10.145 SN - 0196-4332 VL - 2017 IS - 421 SP - 807 EP - 812 PB - Elsevier B.V. AN - OPUS4-42136 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schott, M. A1 - Szczerba, Wojciech A1 - Kurth, D.G. T1 - Detailed study of layer-by-layer self-assembled and dip-coated electrochromic thin films based on metallo-supramolecular polymers JF - Langmuir N2 - Electrochromic thin films of metallo-supramolecular polyelectrolytes based on Fe(OAc)2 and 1,4-bis(2,2':6',2''-terpyridin-4'-yl)benzene are readily prepared by layer-by-layer (LbL) deposition or dip-coating on transparent conducting electrode surfaces. By applying a potential, we can switch the color of the films from blue to colorless. Because of the strong absorption and the fast switching speed, the color change can be observed with the eye. The devices show reversible switching and cycle stability. KW - Layer-by-layer self assembly KW - Dip coating KW - Thin films KW - Metallo-supramolecular polyelectrolytes KW - Electrochromism PY - 2014 DO - https://doi.org/10.1021/la501590a SN - 0743-7463 SN - 1520-5827 VL - 30 IS - 35 SP - 10721 EP - 10727 PB - American Chemical Society CY - Washington, DC AN - OPUS4-31734 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schade, U. A1 - Ritter, E. A1 - Bawagan, A.D.O. A1 - Beckmann, Jörg A1 - Aziz, E. F. T1 - Far-infrared absorption measurements on thin polymer films T2 - IRMMW-THz 2014 - 39th International conference on infrared, millimeter, and terahertz waves N2 - Interference fringes in the far-infrared spectra of thin films are the result of the coherent adding up of waves and can influence the spectral interpretation by concealing smaller features. A number of methods have been developed in order to eliminate such oscillating features from the transmittance spectrum. The paper critically evaluates the total transmission-reflection technique and applies the method to quantify the spectra of different polymer films. T2 - IRMMW-THz 2014 - 39th International conference on infrared, millimeter, and terahertz waves CY - Tucson, Arizona, USA DA - 14.09.2014 KW - Far-infrared spectra KW - Thin films KW - Total transmission reflection technique KW - Infrared spectroscopy KW - Light absorption KW - Light reflection KW - Polymer films KW - Far-infrared absorption measurements KW - Thin polymer films KW - Interference fringes KW - Spectral interpretation KW - Transmittance spectrum KW - Oscillating features KW - Total transmission-reflection technique KW - Interference KW - Absorption KW - Finite impulse response filters KW - Optical films KW - Optical reflection PY - 2014 UR - http://ieeexplore.ieee.org/stamp/stamp.jsp?tp=&arnumber=6956145&isnumber=6955975 SN - 978-1-4799-3877-3 DO - https://doi.org/10.1109/IRMMW-THz.2014.6956145 IS - IEEE Catalog No.: CFP14IMM-ART SP - 1 EP - 2 AN - OPUS4-32700 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fahmy, A. A1 - Friedrich, Jörg Florian T1 - Degradation behavior of thin polystyrene films on exposure to Ar plasma and its emitted radiation JF - Journal of adhesion science and technology N2 - Spin-coated films of amorphous polystyrene (PS) were exposed to argon plasma for a few seconds to several minutes. The PS film was either in direct contact with the plasma or was shielded from the direct plasma contact by filters with different cutoff wavelengths in the vacuum UV region or by a Faraday cage (FC) made from metal mesh to prevent the impinging of charged species. Only energy-rich neutrals and plasma radiation may be operative in presence of the FC. lithium fluoride (LiF) filter protects the sample from direct contact with the plasma. Wavelengths of plasma radiation shorter than c. 105 nm (≈ 11.8 eV) were cut off. Glass filters made of fused SiO2 have a cutoff at λ ≈175?nm completely the vacuum UV radiation of plasma (ca. 175 nm ≈ 7.0 eV). These energies are sufficient to produce C–C, C–H bond scissions in case of direct Ar plasma exposure and Ar plasma exposure with use of the LiF filter. Only quartz glass shielding did not produce significant effects on the polymer surface in comparison to the reference PS, either in surface energy or O/C ratio or in IR spectra. Oxygen plasma has worked most aggressive and had etched the PS film, thus establishing a steady state between introduction of new oxygen functionalities and polymer etching. Ar plasma exposure produces also oxidation and etching of the polymer films as the oxygen plasma. Using of a FC during Ar plasma exposure or the LiF filter a slightly weaker oxidation was observed. KW - Polystyrene KW - Plasma treatment KW - Plasma emitted radiation KW - Degradation KW - Thin films PY - 2013 DO - https://doi.org/10.1080/01694243.2012.705528 SN - 0169-4243 SN - 1568-5616 VL - 27 IS - 3 SP - 324 EP - 338 PB - VNU Science Press CY - Utrecht AN - OPUS4-26315 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hertwig, Andreas A1 - De Castro, F.A. T1 - Newsletter - Metrology for the manufacturing of thin films KW - Metrology KW - Thin films KW - Optoelectronics KW - Photovoltaics KW - Coatings technology KW - Traceability PY - 2012 UR - http://projects.npl.co.uk/optoelectronic_films/documents/EMRP%20ThinFilms_Newsletter%20Feb%202012.pdf IS - February SP - 1 EP - 4 AN - OPUS4-25505 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Kim, K.J. A1 - Unger, Wolfgang T1 - Energy dispersive electron probe microanalysis (ED-EPMA) of elemental composition and thickness of Fe-Ni alloy films JF - Surface and interface analysis N2 - The elemental composition of thin Fe-Ni alloy films deposited on silicon substrates were determined by electron probe microanalysis with an energy dispersive spectrometer using the STRATAGem software. The work was part of ample inter-laboratory comparisons organized in the frame of CCQM/SAWG (Consultative Committee for Amount of Substance/Surface Analysis Working Group). Therefore, the evaluation of the measurement uncertainties is treated in detail. By having the mass coverage and estimating a layer density, the layer thickness could be derived. KW - Thin films KW - Fe-Ni KW - Energy dispersive electron probe microanalysis (ED-EPMA) KW - STRATAGem KW - k-values KW - Mass coverage KW - Elemental composition KW - Thickness KW - CCQM PY - 2012 DO - https://doi.org/10.1002/sia.4975 SN - 0142-2421 SN - 1096-9918 VL - 44 IS - 11-12 SP - 1459 EP - 1461 PB - Wiley CY - Chichester AN - OPUS4-27139 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abou-Ras, D. A1 - Caballero, R. A1 - Fischer, C.-H. A1 - Kaufmann, C.A. A1 - Lauermann, I. A1 - Mainz, R. A1 - Mönig, H. A1 - Schöpke, A. A1 - Stephan, C. A1 - Streeck, C. A1 - Schorr, S. A1 - Eicke, A. A1 - Döbeli, M. A1 - Gade, B. A1 - Hinrichs, J. A1 - Nunney, T. A1 - Dijkstra, H. A1 - Hoffmann, V. A1 - Klemm, D. A1 - Efimova, V. A1 - Bergmaier, A. A1 - Dollinger, G. A1 - Wirth, Thomas A1 - Unger, Wolfgang A1 - Rockett, A.A. A1 - Perez-Rodriguez, A. A1 - Alvarez-Garcia, J. A1 - Izquierdo-Roca, V. A1 - Schmid, T. A1 - Choi, P.-P. A1 - Müller, M. A1 - Bertram, F. A1 - Christen, J. A1 - Khatri, H. A1 - Collins, R.W. A1 - Marsillac, S. A1 - Kötschau, I. T1 - Comprehensive comparison of various techniques for the analysis of elemental distributions in thin films JF - Microscopy and Microanalysis N2 - The present work shows results on elemental distribution analyses in Cu(In,Ga)Se2 thin films for solar cells performed by use of wavelength-dispersive and energy-dispersive X-ray spectrometry (EDX) in a scanning electron microscope, EDX in a transmission electron microscope, X-ray photoelectron, angle-dependent soft X-ray emission, secondary ion-mass (SIMS), time-of-flight SIMS, sputtered neutral mass, glow-discharge optical emission and glow-discharge mass, Auger electron, and Rutherford backscattering spectrometry, by use of scanning Auger electron microscopy, Raman depth profiling, and Raman mapping, as well as by use of elastic recoil detection analysis, grazing-incidence X-ray and electron backscatter diffraction, and grazing-incidence X-ray fluorescence analysis. The Cu(In,Ga)Se2 thin films used for the present comparison were produced during the same identical deposition run and exhibit thicknesses of about 2 µm. The analysis techniques were compared with respect to their spatial and depth resolutions, measuring speeds, availabilities, and detection limits. KW - Elemental distributions KW - Comparison KW - Depth profiling KW - Chemical mapping KW - Thin films KW - Solar cells KW - Chalcopyrite-type KW - Cu(In,Ga)Se2 PY - 2011 DO - https://doi.org/10.1017/S1431927611000523 SN - 1431-9276 SN - 1435-8115 VL - 17 IS - 5 SP - 728 EP - 751 PB - Cambridge University Press CY - New York, NY AN - OPUS4-24506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Silbernagl, Dorothee A1 - Cappella, Brunero T1 - Mechanical properties of thin polymer films on stiff substrates JF - Scanning N2 - Force–displacement curves have been acquired with a commercial atomic force microscope on thin films of poly(n-butyl methacrylate) on glass substrates in order to examine the so-called 'mechanical double layer' topic, i.e. the influence of the substrate on the mechanical properties of the film in dependence of the film thickness. The hyperbolic fit, a novel semi-empirical equation introduced in previous articles, has been further corroborated. The interpretation of this equation has been deepened, yielding a quantitative and demonstrative characterization of the mechanical properties of double layers. Provided that the Young's moduli of bulk polymer and substrate are measured from the deformation curves, this mathematical model permits to fit the deformation–force curves on the double layers and to determine the thickness of the polymer films in wide range (0–200 nm). KW - Atomic force microscopy KW - Indentation KW - Rheology KW - Polymers KW - Thin films PY - 2010 DO - https://doi.org/10.1002/sca.20196 SN - 0161-0457 SN - 1932-8745 VL - 32 IS - 5 SP - 282 EP - 293 PB - Wiley CY - Hoboken, NJ AN - OPUS4-22681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rybachuk, Maksym A1 - Hertwig, Andreas A1 - Weise, Matthias A1 - Sahre, Mario A1 - Männ, Marion A1 - Beck, Uwe A1 - Bell, J. M. T1 - Near infrared optical materials from polymeric amorphous carbon synthesized by collisional plasma process JF - Applied physics letters N2 - The synthesis of polymerlike amorphous carbon (a-C:H) thin-films by microwave excited collisional hydrocarbon plasma process is reported. Stable and highly aromatic a-C:H were obtained containing significant inclusions of poly(p-phenylene vinylene) (PPV). PPV confers universal optoelectronic properties to the synthesized material. That is a-C:H with tailor-made refractive index are capable of becoming absorption-free in visible (red)-near infrared wavelength range. Production of large aromatic hydrocarbon including phenyl clusters and/or particles is attributed to enhanced coagulation of elemental plasma species under collisional plasma conditions. Detailed structural and morphological changes that occur in a-C:H during the plasma synthesis are also described. KW - Kohlenstoffschichten KW - Plasmachemie KW - PA-CVD KW - Amorphous state KW - Carbon KW - Coagulation KW - Hydrogen KW - Optical materials KW - Plasma collision processes KW - Plasma deposition KW - Refractive index KW - Thin films PY - 2010 DO - https://doi.org/10.1063/1.3431292 SN - 0003-6951 SN - 1077-3118 VL - 96 IS - 21 SP - 211909-1 - 211909-3 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-21365 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Labahn, Diana A1 - Mix, Renate A1 - Schönhals, Andreas T1 - Dielectric relaxation of ultrathin films of supported polysulfone JF - Physical review E N2 - The dynamic glass transition (α relaxation, structural relaxation) of ultrathin polysulfone films prepared between aluminum electrodes is investigated by dielectric relaxation spectroscopy. As a main result, it is found that the glass transition temperature Tg does not depend on the thickness of the polymeric layer down to a thickness of 10 nm. For thicknesses lower than 10 nm, an increase of Tg is observed. A more detailed analysis of the temperature dependence of the relaxation rates reveals that the Vogel temperature increases and the fragility decreases systematically with decreasing film thickness d. Further, the dielectric strength Δε decreases with decreasing d. This is discussed by the formation of a surface layer of adsorbed polysulfone segments having a reduced molecular mobility with regard to the time scale characteristic of the glassy dynamics of bulk polysulfone. Plotted versus inverse film thickness Δε decreases linearly with 1/d and becomes zero for an extrapolated length scale of 10 nm. From that it is concluded that the thickness of the adsorbed boundary layer is about 5 nm. Contact-angle measurements were carried out to confirm the strong interaction between aluminum and polysulfone. It is also shown that preparation details like annealing conditions strongly influence the glass transition of supported ultrathin films. KW - Adsorbed layers KW - Aluminium KW - Annealing KW - Contact angle KW - Dielectric relaxation KW - Electrodes KW - Glass transition KW - Polymer films KW - Thin films PY - 2009 DO - https://doi.org/10.1103/PhysRevE.79.011801 SN - 1539-3755 SN - 1063-651X VL - 79 IS - 1 SP - 011801-1 - 011801-9 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-19050 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Swaraj, Sufal A1 - Oran, Umut A1 - Lippitz, Andreas A1 - Schulze, Rolf-Dieter A1 - Friedrich, Jörg Florian A1 - Unger, Wolfgang T1 - Surface Analysis of Plasma-Deposited Polymer Films, 4 - In situ Characterization of Plasma-Deposited Ethylene Films by XPS and NEXAFS JF - Plasma processes and polymers N2 - XPS and NEXAFS spectroscopy were used for the chemical characterization of pulsed plasma-deposited ethylene films before and after exposure to ambient air. The influence of external plasma parameters on the spectroscopic results was investigated. Information on the chemical character of the plasma-polymerized films, such as the regularity of the primary structure, the amount of long-living radicals, and branching or cross-linking or both was derived from this data. Irregularity and radical concentration for post-plasma reactions of the plasma-deposited films increased with the duty cycle or power. A decreased level of monomer fragmentation and, consequently, an increase in regularity is partially concluded from the experimental data when the monomer pressure is increased. The concentration of surface radicals available for post-plasma reactions also increased with monomer pressure. The correlation found between the degree of the post-plasma oxygen incorporation and the variation of the various external parameters agreed with earlier ToF-SSIMS findings. KW - ESCA/XPS KW - NEXAFS KW - Plasma polymerization KW - Polyethylene (PE) KW - Thin films PY - 2005 DO - https://doi.org/10.1002/ppap.200400070 SN - 1612-8850 SN - 1612-8869 VL - 2 IS - 4 SP - 310 EP - 318 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-11940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hübert, Thomas A1 - Shimamura, Aki A1 - Klyszcz, Andreas T1 - Electrical Properties of Carbon Black and Ruthenium Dioxide Embedded Silica Films JF - Journal of sol gel science and technology N2 - The electrical properties of sol–gel-derived films can be tailored by embedding conductive particles of ruthenium dioxide or carbon black in an insulating amorphous SiO2 silica matrix. The preparation process included an acid hydrolysis of tetraethoxysilane and methyltrimethoxysilane. Then alcohol solutions of ruthenium chloride or carbon black were added. Films of filler concentration up to 60 vol.% were prepared by dip coating and then dried and heat-treated at various temperatures up to 600_°C. The D.C. resistance of the films can be varied within the range of 109 to 10–2 OHgr sdot cm. A non-linear dependence on filler composition in the films was observed for both systems, which is explained by a modified percolation theory. A percolation threshold of 5.5 vol.% for SiO2-RuO2 or 50 vol.% for SiO2-C films, whereby the resistance drastically decreases, was determined. Moreover the temperature dependency of resistance and the current-voltage characteristics of the films can also be explained by this geometric model. KW - Sol-gel KW - Thin films KW - Carbon black KW - Ruthenium dioxide KW - Percolation phenomena PY - 2004 DO - https://doi.org/10.1007/s10971-004-5777-5 SN - 0928-0707 SN - 1573-4846 VL - 32 SP - 131 EP - 135 PB - Kluwer Academic Publ. CY - Dordrecht AN - OPUS4-6909 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -