TY - CONF A1 - Beck, Uwe A1 - Griepentrog, Michael A1 - Hertwig, Andreas A1 - Hielscher-Hofinger, Stefan A1 - Lange, Thorid A1 - Weise, Matthias T1 - Uncertainty budgets in surface technology: stepheigt, layerthickness, indentation hardness, adehesive strength N2 - The object (sample) and the measurement/testing procedure may always have unknown degrees of freedom, i.e. instead of 𝐯 ≄ n – 1 in many cases 𝐯 ≫ n - 1 may apply, in particular in the micro- and nano-world! T2 - 10. VDI-Fachtagung, Messunsicherheit und PrĂŒfprozesse CY - Erfurt, Germany DA - 10.11.2021 KW - Methodology in metrology KW - Methodology in testing KW - Spectroscopic Ellipsometry KW - Instrumented Indentation Testing (IIT) KW - Centrifugal Adhesion Testing (CAT) PY - 2021 AN - OPUS4-53986 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sachse, RenĂ© A1 - Moor, MaĂ«lle A1 - Kraehnert, Ralph A1 - Hodoroaba, Vasile-Dan A1 - Hertwig, Andreas T1 - Ellipsometry-based approach for the characterization of mesoporous thin films for H2 technologies N2 - Porous thin layer materials are gaining importance in different fields of technology and pose a challenge to the accurate determination of materials properties important for their function. In this work, we demonstrate a hybrid measurement technique using ellipsometry together with other independent methods for validation. Ellipsometry provides information about the porosity of different mesoporous films (PtRuNP/OMC = 45%; IrOx = 46%) as well as about the pore size (pore radius of ca. 5 nm for PtRuNP/OMC). In addition, the electronic structure of a material, such as intraband transitions of a mesoporous IrOx film, can be identified, which can be used to better understand the mechanisms of chemical processes. In addition, we show that ellipsometry can be used as a scalable imaging and visualization method for quality assurance in production. These require accurate and traceable measurements, with reference materials playing an important role that include porosity and other related properties. We show that our novel analytical methods are useful for improving analytical work in this entire field. KW - Porous materials KW - Electrolysis KW - Spectroscopic ellipsometry KW - Hybrid metrology measurement KW - Electron microscopy PY - 2021 DO - https://doi.org/10.1002/adem.202101320 SP - 1 EP - 17 PB - Wiley-VCH AN - OPUS4-53960 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Frisch, M. A1 - Raza, M. H. A1 - Ye, M.-Y. A1 - Sachse, RenĂ© A1 - Paul, B. A1 - Gunder, R. A1 - Pinna, N. A1 - Kraehnert, R. T1 - ALD-coated mesoporous iridium-titanium mixed oxides: Maximizing iridium utilization for an outstanding OER performance N2 - With the increasing production of renewable energy and concomitant depletion of fossil resources, the demand for efficient water splitting electrocatalysts continues to grow. Iridium (Ir) and iridium oxides (IrOₓ) are currently the most promising candidates for an efficient oxygen evolution reaction (OER) in acidic medium, which remains the bottleneck in water electrolysis. Yet, the extremely high costs for Ir hamper a widespread production of hydrogen (H₂) on an industrial scale. Herein, the authors report a concept for the synthesis of electrode coatings with template-controlled mesoporosity surface-modified with highly active Ir species. The improved utilization of noble metal species relies on the synthesis of soft-templated metal oxide supports and a subsequent shape-conformal deposition of Ir species via atomic layer deposition (ALD) at two different reaction temperatures. The study reveals that a minimum Ir content in the mesoporous titania-based support is mandatory to provide a sufficient electrical bulk conductivity. After ALD, a significantly enhanced OER activity results in dependency of the ALD cycle number and temperature. The most active developed electrocatalyst film achieves an outstanding mass-specific activity of 2622 mA mg(Ir)⁻Âč at 1.60 V(RHE) in a rotating-disc electrode (RDE) setup at 25 °C using 0.5 m H₂SO₄ as a supporting electrolyte. KW - Acidic oxygen evolution reaction KW - Atomic layer deposition KW - Electrocatalysis KW - Iridium oxide KW - Soft-templated mesoporous films PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542651 DO - https://doi.org/10.1002/admi.202102035 SN - 2196-7350 SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54265 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Griepentrog, Michael A1 - Hertwig, Andreas A1 - Hielscher-Hofinger, S. A1 - Lange, Thorid A1 - Weise, Matthias T1 - Uncertainty budgets in surface techno-logy: step height, layer thickness, indentation hardness, adehesive strength N2 - The object (sample) and the measurement/testing procedure may always have unknown degrees of freedom, i.e. instead of 𝐯 ≄ n – 1 in many cases 𝐯 ≫ n - 1 may apply, in particular in the micro- and nano-world! T2 - 10. VDI-Fachtagung, Messunsicherheit und PrĂŒfprozesse CY - Erfurt, Germany DA - 10.11.2021 KW - Methodology in metrology KW - Methodology in testing KW - Spectroscopic Ellipsometry KW - Instrumented Indentation (IIT) KW - Centrifugal Adhesion Testing (CAT) PY - 2021 AN - OPUS4-53739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ermilova, Elena A1 - Hertwig, Andreas A1 - Beck, Uwe A1 - Schneider, S. A1 - Peters, S. T1 - Development of a standard series for ellipsometry N2 - Ellipsometry is a powerful tool, which allows the investigation of material properties over a broad spectral range. Over the course of several years, the ellipsometry lab at BAM has become an accredited testing lab according to ISO/IEC 17025 laying bare the need of better methods for accuracy and traceability. Despite its wide range of application in both research and development as well as industry, there have been no generally accepted standards dealing with model validation and measurement uncertainties. Based on the first German standard DIN 50989 – 1: 2018 Ellipsometry - Part 1: Principles (currently international standard ISO 23131: 2021) and under consideration of GUM [1] a series of standards for ellipsometry was developed. The entire 6-part series covers several model-based application cases. This standards series avoids having narrow and material specific application cases but instead classifies applications of ellipsometry according to the sample complexity. The concept of ellipsometric transfer quantities (Κ and Δ or alternatively the elements of transfer matrices) is implemented in the series. For each application case a model-based validation strategy was developed. Thus, the standards are applicable to all materials, instruments and measuring principles. The uniform structure concept of the series facilitates its practical applicability for users. The standards include the model-based GUM-compliant determination/estimation of the measurement uncertainties. In addition, the appendices of the documents contain numerous measurement and simulation examples as well as recommendations for measuring practice. In this contribution we present the application cases and basic structure of the standards developed in collaboration with Accurion GmbH and SENTECH Instruments GmbH in the project SNELLIUS. T2 - 11th Workshop Ellipsometry (WSE 11) CY - Steyr, Austria DA - 06.09.2021 KW - Standardization of ellipsometry KW - DIN 50989 Parts 1 – 6 KW - ISO 23131: 2021 KW - Validation concepts of ellipsometric measurements KW - Uncertainty budgets KW - GUM-compliance PY - 2021 AN - OPUS4-53250 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Beck, Uwe A1 - Ermilova, Elena A1 - Schneider, S. A1 - Peters, S. T1 - Gemeinsamer Abschlussbericht WIPANO-Vorhaben „Standardisierung und Normung der Ellipsometrie als universeller Spektroskopie“ N2 - Im Vorhaben SNELLIUS wurden in enger Zusammenarbeit der BAM mit den Firmen Accurion und SENTECH Instruments aufbauend auf der Norm DIN 50989-1 „Ellipsometrie - Teil 1: Grundlagen; Ellipsometry – Part 1: Principles“ insgesamt fĂŒnf NormenentwĂŒrfe erarbeitet, die fĂŒnf Modell-basierten AnwendungsfĂ€llen der Ellipsometrie entsprechen. Unter BerĂŒcksichtigung des neuartigen Modell-basierten Normungskonzepts wurde in den NormenentwĂŒrfen erstmals eine GUM- und DIN EN ISO/IEC 17025:2018 konforme Bestimmung bzw. AbschĂ€tzung der Messunsicherheit umgesetzt. Dies erforderte neben der textlichen Erstellung auch umfangreiche experimentelle Arbeiten bei den Firmen, Vergleichsversuche und komplementĂ€re Modell- und Datenevaluierungen, da sowohl die verwendete ellipsometrische Hardware (unterschiedliche ellipsometrische Funktionsprinzipien) als auch die ellipsometrische Software (Modell-Randbedingungen, Fitalgorithmus) firmenspezifisch zum Teil sehr unterschiedlich sind. Hierbei mussten in einem Konsensprozess Lösungen gefunden werden, die die beiden deutschen Ellipsometer-Anbieter Accurion (Imaging-Ellipsometrie) und SENTECH Instruments (Mapping Ellipsometrie) gleichermaßen akzeptieren konnten und die zudem einen Transfer auf die Internationale Ebene (ISO Norm) ermöglichen, also vom Grundsatz her auch auf weitere Ellipsometerhersteller wie (J. A. Woollam Co., USA; SEMILAB, Ungarn; HORIBA, Japan) mit wieder anderen ellipsometrischen Funktionsprinzipien, Hard- und Softwarelösungen anwendbar sind. Die weitgehende UnabhĂ€ngigkeit von ellipsometrischen Funktionsprinzipien, Hard- und Softwarelösungen wurde dadurch erreicht, dass normativ festgelegt wurde, dass die ellipsometrischen GrĂ¶ĂŸen PSI und DELTA im Sinne von DIN ENISO/IEC 17025 als Rohdaten fungieren. KW - Ellipsometrie-Norm KW - Messunsicherheit ellipsometrischer Messungen KW - Validierungskonzepte ellipsometrischer Messungen KW - DIN 50989, Teile 1 bis 6 KW - DIN EN ISO/IEC 17025:2018 und GUM KompatibilitĂ€t PY - 2021 SP - 1 EP - 16 AN - OPUS4-52857 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Baier, Jennifa A1 - Fischer, Daniel A1 - Griepentrog, Michael A1 - Hertwig, Andreas A1 - Hielscher-Hofinger, Stefan A1 - Sahre, Mario A1 - Stockmann, Jörg Manfred A1 - Weise, Matthias T1 - Mapping und Imaging modifizierter OberflĂ€chen: Generische KenngrĂ¶ĂŸen, Fehlstellen, Reinigungszustand und Haftfestigkeit N2 - Der Vortrag widmet sich dem Mapping und Imaging modifizierter OberflĂ€chen: Generische KenngrĂ¶ĂŸen, Fehlstellen, Reinigungszustand und Haftfestigkeit. Es werden Untersuchungsmethoden zu ihrer PrĂŒfung dargestellt. T2 - 37. ak-adp 2021, Jena CY - Online meeting DA - 16.06.2021 KW - QualitĂ€tssicherung KW - Mapping modifizierter OberflĂ€chen KW - Generische KenngrĂ¶ĂŸen KW - Haftfestigkeit KW - Klebfestigkeit PY - 2021 AN - OPUS4-52870 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Baier, Jennifa A1 - Fischer, Daniel A1 - Griepentrog, Michael A1 - Hertwig, Andreas A1 - Hielscher-Hofinger, Stefan A1 - Stockmann, Jörg Manfred A1 - Weise, Matthias T1 - Mapping und Imaging modifizierter OberflĂ€chen: Generische KenngrĂ¶ĂŸen, Fehlstellen, Reinigungszustand und Haftfestigkeit N2 - Der Vortrag widmet sich dem Mapping und Imaging modifizierter OberflĂ€chen: generische KenngrĂ¶ĂŸen, Fehlstellen, Reinigungszustand und Haftfestigkeit. Es werden Untersuchungsmethoden zu ihrer PrĂŒfung dargestellt. T2 - 37. ak-adp 2021 CY - Jena, Germany DA - 16.06.2021 KW - QualitĂ€tssicherung KW - Mapping modifizierter OberflĂ€chen KW - Imaging modifizierter OberflĂ€chen KW - Generische KenngrĂ¶ĂŸen KW - Haftfestigkeit KW - Klebfestigkeit PY - 2021 SP - 1 EP - 10 AN - OPUS4-52893 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Duwe, M. A1 - Florian, C. A1 - Fischer, Daniel A1 - Freiberg, K. A1 - Sahre, Mario A1 - Schneider, S. A1 - Hertwig, Andreas A1 - KrĂŒger, Jörg A1 - Rettenmayr, M. A1 - Beck, Uwe A1 - Undisz, A. A1 - Bonse, Jörn T1 - Thickness Profiling of the Superficial Amorphization and Re-Crystallization of Silicon Induced by Femtosecond Laser Pulses N2 - Crystalline Silicon undergoes a complex phase-change dynamic of melting, amorphization, ablation and re-crystallization upon irradiation with high intensity ultra-short laser pulses [1]. The final state of such a modified surface spot depends on many factors, most notably the local fluence and the surface’s crystal orientation. In this study, we induced superficial structure and phase changes in Silicon <111> and <100> wafers using single femtosecond laser pulses (790 nm, 30 fs) for a range of different peak fluences. The resulting surface modifications were studied in great detail using a number of different techniques, including spectroscopic imaging ellipsometry (SIE), atomic force microscopy, high-resolution transmission electron microscopy (HRTEM), and energy dispersive X-ray spectroscopy within scanning transmission electron microscopy (STEM-EDX). Playing a pivotal role in this work, SIE provided non-destructive measurements for the calculation of the radial amorphous layer-thickness profiles of the irradiated spots using a two-layer thin-film model (Silicon dioxide and amorphous Silicon on a crystalline Silicon substrate). The measurements further allowed for the analysis of the oxide-layer modifications induced by the laser treatment. The results of the SIE-calculations were cross-checked by an in-depth material lamella via HRTEM and STEM-EDX. T2 - 11th Workshop Ellipsometry (WSE 11) CY - Steyr, Austria DA - 06.09.2021 KW - Femtosecond Laser KW - Spectroscopic imaging ellipsometry KW - Amorphization KW - Ablation KW - Re-crystallization PY - 2021 AN - OPUS4-53363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirabella, Francesca A1 - Mezera, Marek A1 - Wasmuth, Karsten A1 - Hertwig, Andreas A1 - Richter, Anja A1 - Schwibbert, Karin A1 - KrĂŒger, Jörg A1 - Bonse, Jörn A1 - Hodoroaba, Vasile-Dan T1 - ToF-SIMS as a new tool for nano-scale investigation of ps-laser-generated surface structures on titanium substrates N2 - In recent years, the fabrication of laser-generated surface structures on metals such as titanium surfaces have gained remarkable interests, being technologically relevant for applications in optics, medicine, fluid transport, tribology, and wetting of surfaces. The morphology of these structures, and so their chemistry, is influenced by the different laser processing parameters such as the laser fluence, wavelength, pulse repetition rate, laser light polarization type and direction, angle of incidence, and the effective number of laser pulses per beam spot area. However, the characterization of the different surface structures can be difficult because of constraints regarding the analytical information from both depth and the topographic artifacts which may limit the lateral and depth resolution of elemental distributions as well as their proper quantification. A promising technique to investigate these structures even at the nano-scale is Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS), a very surface sensitive technique that at the same time allows to perform depth-profiling, imaging and 3D-reconstruction of selected ion-sputter fragment distributions on the surface. In this study we combine chemical analyses such as Energy Dispersive X-ray spectroscopy (EDX) and high-resolution scanning electron microscopy (SEM) analyses with ToF-SIMS to fully characterize the evolution of various types of laser-generated micro- and nanostructures formed on Ti and Ti alloys at different laser fluence levels, effective number of pulses and at different pulse repetition rates (1 – 400 kHz), following irradiation by near-infrared ultrashort laser pulses (925 fs, 1030 nm) in air environment or under argon gas flow. We show how this combined surface analytical approach allows to evaluate alteration in the surface chemistry of the laser-generated surface structures depending on the laser processing parameters and the ambient environment. T2 - European Materials Research Society (EMRS) Fall Meeting 2021 CY - Online meeting DA - 20.09.2021 KW - ToF SIMS KW - Nano characterization PY - 2021 AN - OPUS4-53366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -