TY - CONF A1 - Kromm, Arne A1 - Cabeza, Sandra A1 - Mishurova, Tatiana A1 - Thiede, Tobias A1 - Nadammal, Naresh A1 - Bruno, Giovanni T1 - Residual stress formation in selective laser melted parts of alloy 718 N2 - Additive Manufacturing (AM) through the Selective Laser Melting (SLM) route offers ample scope for producing geometrically complex parts compared to the conventional subtractive manufacturing strategies. Nevertheless, the residual stresses which develop during the fabrication can limit application of the SLM components by reducing the load bearing capacity and by inducing unwanted distortion, depending on the boundary conditions specified during manufacturing. The present study aims at characterizing the residual stress states in the SLM parts using different diffraction methods. The material used is the nickel based superalloy Inconel 718. Microstructure as well as the surface and bulk residual stresses were characterized. For the residual stress analysis, X-ray, synchrotron and neutron diffraction methods were used. The measurements were performed at BAM, at the EDDI beamline of -BESSY II synchrotron- and the E3 line -BER II neutron reactor- of the Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. The results reveal significant differences in the residual stress states for the different characterization techniques employed, which indicates a dependence of the residual state on the penetration depth in the sample. For the surface residual stresses, longitudinal and transverse stress components from both X-ray and synchrotron agree well and the obtained values were around the yield strength of the material. Furthermore, synchrotron mapping disclosed gradients along the width and length of the sample for the longitudinal and transverse stress components. On the other hand, lower residual stresses were found in the bulk of the material measured using neutron diffraction. The longitudinal component was tensile and decreased towards the boundary of the sample. In contrast, the normal component was nearly constant and compressive in nature. The transversal component was almost negligible. The results indicate that a stress re-distribution takes place during the deposition of the consecutive layers. Further investigations are planned to study the phenomenon in detail. T2 - Forschungsseminar OvGU Magdeburg CY - Magdeburg, Germany DA - 15.11.2018 KW - Additive Manufacturing KW - Selective Laser Melting KW - Residual Stresses PY - 2018 AN - OPUS4-46876 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenberg, Rainer A1 - Charmi, Amir T1 - Virtual-lab-based determination of a macroscopic yield function for additively manufactured parts N2 - This work presents a method for the yield function determination of additively manufactured parts of S316L steel. A crystal plasticity model is calibrated with test results and used afterwards to perform so-called virtual experiments, that account for the specific process-related microstructure including crystallographic and morphological textures. These simulations are undertaken on a representative volume element (RVE), that is generated from EBSD/CT-Scans on in-house additively manufactured specimen, considering grain structure and crystal orientations. The results of the virtual experiments are used to determine an anisotropic Barlat yield function, that can be used in a macroscopical continuum-sense afterwards. This scale-bridging approach enables the calculation of large-scale parts, that would be numerically too expensive to be simulated by a crystal plasticity model. T2 - 3. Tagung des DVM-Arbeitskreises Additiv gefertigte Bauteile und Strukturen CY - Berlin, Germany DA - 07.11.2018 KW - Virtual experiments KW - Additive manufacturing KW - Anisotropy KW - Crystal plasticity KW - Scale-bridging PY - 2018 AN - OPUS4-46895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trappe, Volker A1 - Nielow, D. A1 - Hickmann, Stefan A1 - Kupsch, Andreas A1 - Gaal, Mate A1 - Redmer, Bernhard A1 - Krankenhagen, Rainer T1 - Sandwich-Schalenstrukturen in situ charakterisiert mit Thermographie und Felddehnungsmessungen N2 - An der BAM wurde ein Schalenprüfstand entwickelt, mit dem typische Sandwichschalenstrukturen unter simulierter Betriebsbeanspruchung belastet werden können. Im mechanischen Ermüdungsversuch wurden in situ die Entstehung von Schäden in Schalenprüfkörpern mit Test-Imperfektionen mittels der passiven Thermographie und Felddehnungsmessungen verfolgt. Damit konnten der Zeitpunkt, der Schadensursprung und der Schadensfortschritt zerstörungsfrei bestimmt werden. Zudem wurden vergleichend Schalenprüfkörper mit Luftultraschall und der Röntgen-Laminographie untersucht. Im Rahmen eines BMWi-Forschungsvorhabens wurden die Schädigungsmechanismen evaluiert und Empfehlungen für die Praxis der Fertigung von Rotorblättern abgeleitet. In diesem Beitrag wird sich auf die Darstellung der ZfP-Verfahren und der ZfP-Ergebnisse konzentriert. T2 - DGZfP-Jahrestagung 2018 CY - Leipzig, Germany DA - 07.05.2018 KW - Windkraft KW - Rotorblatt KW - Schalenprüfstand KW - Thermographie KW - Laminographie KW - Luftultraschall PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-469395 VL - 166 SP - 1 EP - 11 AN - OPUS4-46939 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Prasetiadi, A. E. A1 - Jost, M. A1 - Schulz, Baerbel A1 - Quibeldey, M. A1 - Rabe, Torsten A1 - Follmann, R. A1 - Jakoby, R. T1 - Liquid-crystal-based amplitude tuner and tunable SIW filter fabricated in LTCC technology N2 - Tunable microwave devices will play an important role in future wireless systems, in which high-frequency bands, e.g. millimeter waves, will become promising, due to its huge spectrum availability. At such frequency bands, liquid crystals (LCs) exhibit low microwave loss, which is excellent compared with the other tuning elements. In this paper, LC-based microwave components are fabricated by using low temperature co-fired ceramic technology, allowing the integration of the LC into microwave structures. The first component, the Amplitude tuner, controls the signal’s amplitude by using the interference concept, which exhibits a tunable attenuation range from 11 dB to 30 dB at 30 GHz. The second component is a 3-pole tunable bandpass filter, which is realized by using a substrate integrated waveguide topology, enabling a device with comparatively high-quality factors (Q-factors). The measurement results show Q-factors in the range of 68 to 100 for a frequency tuning of 29.4–30.1 GHz, i.e. a tuning range of 700 MHz, accompanied by an insertion loss 2 dB to 4 dB. KW - Passive components and circuits KW - Filters KW - Microwave technology PY - 2018 DO - https://doi.org/10.1017/S1759078718000600 SN - 1759-0787 VL - 10 IS - 5-6 SP - 674 EP - 681 PB - Cambridge University Press AN - OPUS4-46985 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lüchtenborg, Jörg A1 - Mühler, T. A1 - Zocca, Andrea A1 - Günster, Jens T1 - Additive Manufacturing of Dense Ceramics with Laser Induced Slip Casting (LIS) N2 - Most additive manufacturing processes which produce dense ceramics are nowadays limited in size because of inevitable post-processing steps like for example binder removal in stereolithography. The additive manufacturing of voluminous ceramic parts is realized by powder bed based processes which, however, generate parts with residual porosity. Via infiltration these parts can be processed to dense parts like for example SiC but this is not possible for all ceramics like for example Si3N4. There is a lack of methods for the additive manufacturing of dense voluminous parts for most ceramics. We have developed a new additive manufacturing technology, the Laser Induced Slip casting (LIS), based on the layerwise deposition of slurries and their local drying by laser radiation. Laser Induced Slip casting generates ceramic green bodies which can be sintered to dense ceramic components like traditional formed ceramic powder compacts. We will introduce the LIS technology, green bodies and sintered parts will be shown and their microstructure and mechanical properties will be discussed. T2 - CIMTEC 2018 14th Ceramics Congress CY - Perugia, Italy DA - 04.06.2018 KW - Additive Manufacturing PY - 2018 AN - OPUS4-45781 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lüchtenborg, Jörg A1 - Mühler, T. A1 - Zocca, Andrea A1 - Günster, Jens T1 - Additive manufacturing of dense ceramics with laser induced slip casting (LIS) N2 - Most additive manufacturing processes which produce dense ceramics are nowadays limited in size because of inevitable post-processing steps like for example binder removal in stereolithography. The additive manufacturing of voluminous ceramic parts is realized by powder bed based processes which, however, generate parts with residual porosity. Via infiltration these parts can be processed to dense parts like for example SiC but this is not possible for all ceramics like for example Si3N4. There is a lack of methods for the additive manufacturing of dense voluminous parts for most ceramics. We have developed a new additive manufacturing technology, the Laser Induced Slip casting (LIS), based on the layerwise deposition of slurries and their local drying by laser radiation. Laser Induced Slip casting generates ceramic green bodies which can be sintered to dense ceramic components like traditional formed ceramic powder compacts. We will introduce the LIS technology, green bodies and sintered parts will be shown and their microstructure and mechanical properties will be discussed. T2 - yCAM (Young Ceramists Additive Manufacturing Forum) CY - Padua, Italy DA - 03.05.2018 KW - Additive manufacturing PY - 2018 AN - OPUS4-45782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rockenhäuser, Christian A1 - Skrotzki, Birgit T1 - The long-term ageing process of alloy 2618A N2 - The long-term ageing process of alloy 2618A was introduced and discussed The dark-field transmission electronmicroscopical resilts werde shown and evaluated regarding the precipitate radii. The influence of the precipitate radii regarding ageing was used for a preliminary ageing assessment. T2 - 19th International Microscopy Congress (IMC19) CY - Sydney, Australia DA - 09.09.2018 KW - Alloy 2618A KW - Degradation KW - Coarsening KW - S-phase KW - Dark-field transmission electron microscopy (DFTEM) PY - 2018 AN - OPUS4-46120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rockenhäuser, Christian A1 - Skrotzki, Birgit T1 - The long-term ageing process of alloy 2618A N2 - The long-term ageing process of alloy 2618A was introduced and discussed The dark-field transmission electronmicroscopical resilts werde shown and evaluated regarding the precipitate radii. The influence of the precipitate radii regarding ageing was used for a preliminary ageing assessment. T2 - 19th International Microscopy Congress (IMC19) CY - Sydney, Australia DA - 09.09.2018 KW - Alloy 2618A KW - Degradation KW - Coarsening KW - S-phase KW - Dark-field transmission electron microscopy (DFTEM) PY - 2018 AN - OPUS4-46123 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabe, Torsten A1 - Schulz, Bärbel A1 - Hollesch, Martin A1 - Börner, Andreas T1 - Keramikfedern – Herstellung, Eigenschaften und Applikation N2 - Entwickelt wurde eine mehrstufige Fertigungstechnologie (Schruppen, Schlichten, Trennschnitt) zur Herstellung keramischer Federn aus gesinterten Hohlzylindern. Durch Optimierung von Maschinenparametern, Schleifscheiben sowie Werkstück- und Werkzeugaufnahmen ist es gelungen, Federn aus Hochleistungskeramik (Aluminiumoxid und Zirkonoxid) mit hoher Kanten- und Oberflächenqualität reproduzierbar herzustellen. Eine hohe Variabilität bezüglich Außen- und Innendurchmesser, Steigung, Windungsquerschnitt und Abstand zwischen den Windungen ermöglicht es, die Federkonstante über drei Größenordnungen zu variieren. Untersucht wurden Federstabilität und Spannungs-Dehnungs-Verhalten unter konstanter und zyklischer Druckbelastung sowie die thermomechanische Stabilität der Keramikfedern. Aluminiumoxid-Federn können bis etwa 800°C, Zirkonoxid-Federn bis etwa 600°C ohne bleibende geometrische Verformung eingesetzt werden. Unter konstanter Spannung zeigen Federn aus Y-stabilisiertem TZP (Zirkonoxid)-Werkstoffen, von anderen Keramikwerkstoffen abweichend, bei Raumtemperatur eine zeitabhängige, elastische, Verformung (Superelastizität), die nach Entlastung über einen Zeitraum von mehreren Stunden reversibel verläuft. Als Ursache wird eine spannungsinduzierte reversible Phasenumwandlung zwischen austenitischer (tetragonales ZrO2) und martensitischer (monoklines ZrO2) Phase postuliert. Diskutiert wird das Anwendungspotenzial der entwickelten Federn für kapazitive keramische Federsensoren für Gravimeter und Wägetechnik. T2 - AK-Sitzung "Keramikbearbeitung" des Fraunhofer IPK CY - Berlin, Germany DA - 27.09.2018 KW - Keramikfeder KW - Spannungs-Dehnungs-Verhalten KW - Zyklische Belastung KW - Thermomechanische Eigenschaften KW - Fertigungstechnologie PY - 2018 AN - OPUS4-46231 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Müller, Alexander T1 - Schädigungscharakterisierung an Faser-Kunststoff-Verbunden im Schwingversuch mittels Röntgenrefraktionstopographie unter Berücksichtigung der Matrixeigenschaften N2 - In der vorliegenden Arbeit wurden verschiedene Epoxidharzsysteme charakterisiert. Zwei Systeme mit großen bruchmechanischen Unterschieden wurden zur Fertigung äquivalenter GFK- und CFK-Laminate mit Faserausrichtungen in 0/90° und ±45° ausgewählt. In quasi-statischen Zugversuchen und Einstufenschwingversuchen mit einem Beanspruchungsverhältnis von R= 0,1 wurden diese Laminate hinsichtlich ihres Schädigungsbeginns und ihrer Schädigungsentwicklung untersucht. Die Detektion der Schädigungen sowie die Dokumentation der Schädigungsentwicklung wurde anhand der Lichtabsorptionsanalyse an GFK-Laminaten und anhand der Röntgenrefraktionsanalyse an CFK-Laminaten umgesetzt. Auf diese Weise konnten Einflüsse der bruchmechanischen Eigenschaften der Matrix auf die Schädigungsentwicklung im Verbund aufgezeigt werden. Zudem wurden für die untersuchten Laminate die Schädigungsgrenzen bei schwingender Beanspruchung ermittelt. Anhand durchgeführter Schwingversuche an CFK-Laminaten im Very High Cycle Fatigue-(VHCF)-Lastwechselbereich bis 108 konnten Rückschlüsse vom Schädigungsverhalten im High Cycle Fatigue-(HCF)-Lastwechselbereich bis 106 auf die Dauerfestigkeit im VHCF-Bereich gezogen werden und damit VHCF-Dauerfestigkeitsgrenzen bestimmt werden. Mit dem Ziel die Ermüdung der Laminate auf die Beanspruchung der Matrix zurückzuführen, wurden die Erweiterte Inverse Laminattheorie, mikromechanikbasierte Mischungsregeln sowie eine Vergleichsspannungshypothese auf die untersuchten Laminate angewendet. Die Schädigungsgrenzen konnten damit in Form der Matrixbeanspruchung wiedergegeben werden. Die Abbildung der Ermüdung verschiedener Laminate anhand einer matrixspezifischen normierten Masterschädigungslinie ist für die behandelten CFK- und GFK-Laminate gelungen. T3 - BAM Dissertationsreihe - 162 KW - CFK KW - GFK KW - Ermüdung KW - Epoxidharz KW - Masterschädigungslinie KW - Röntgenrefraktion KW - ZfP PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-467833 SN - 1613-4249 VL - 162 SP - 1 EP - 204 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-46783 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thiede, Tobias A1 - Cabeza, S. A1 - Mishurova, Tatiana A1 - Nadammal, N. A1 - Kromm, Arne A1 - Bode, Johannes A1 - Haberland, C. A1 - Bruno, Giovanni T1 - Residual stress in selective laser melted Inconel 718: Influence of the removal from base plate and deposition hatch length N2 - The residual stress distribution in IN718 elongated prisms produced by Selective Laser Melting was studied by means of neutron (bulk) and laboratory X-ray (surface) diffraction. Two deposition hatch lengths were considered. A horizontal plane near the top surface (perpendicular to the building direction) and a vertical plane near the lateral surface (parallel to the building direction) were investigated. Samples both in as-built (AB) condition and removed (RE) from the base plate were characterized. While surface stress fields seem constant for AB condition, X-ray diffraction shows stress gradients along the hatch direction in the RE condition. The stress profiles correlate with the distortion maps obtained by tactile probe measurements. Neutron diffraction shows bulk stress gradients for all principal components along the main sample directions. We correlate the observed stress patterns with the hatch length, i.e. with its effect on temperature gradients and heat flow. The bulk stress gradients partially disappear after removal from the baseplate. KW - Residual stress KW - Additive manufacturing KW - Neutron diffraction KW - Selective laser melting KW - Laboratory X-ray diffraction KW - Coordinate measurement machine KW - IN718 PY - 2018 DO - https://doi.org/10.1520/MPC20170119 SN - 2379-1365 VL - 7 IS - 4 SP - 717 EP - 735 PB - ASTM International CY - USA, West Conshohocken AN - OPUS4-46673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waurischk, Tina A1 - Balzer, R. A1 - Kiefer, P. A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Behrens, H. A1 - Deubener, J. T1 - The influence of volatile constituents on mechanical properties of glasses N2 - Im Rahmen des Young Researcher Day des SPP1594 wurden die bisherigen Inhalte der Projekte zusammengefasst und vorgetragen. T2 - Annual Meeting and Young Researcher Day CY - Jena, Germany DA - 11.09.2018 KW - Glass KW - Crack growth KW - Vickers KW - DCB KW - Water speciation PY - 2018 AN - OPUS4-46728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Nofz, Marianne T1 - High temperature coatings (Book review) N2 - All in all, practicing professionals as well as researchers can read this book with pleasure and great benefit. It presents a comprehensive collection of data and practical examples manifested in about 100 graphs, 80 schemes of processes and devices, a manifold of images showing the microstructure of alloys or details of components and several phase diagrams. Tables containing data on commercially available coatings, alloys, compositions of corrosive salts, function of constituents of coatings add further important pieces of information. Thus, this book is a valuable source of information for anyone engaged in work with or research on high temperature coatings. KW - Coating KW - High temperature PY - 2018 DO - https://doi.org/10.1002/maco.201870104 SN - 0947-5117 VL - 69 IS - 10 SP - 1490 EP - 1490 PB - Wiley‐VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-46749 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tielemann, Christopher A1 - Kirzdörfer, Adrian A1 - Reinsch, Stefan A1 - Müller, Ralf T1 - First hints on reorientation of surface crystals N2 - Up to now, the mechanisms of surface nucleation and surface-induced texture formation are far from being understood. Very few observations of crystal orientation were focused on separately growing surface crystals. In conclusion, no systematic studies on initially oriented crystal growth or nucleation from defined active surface nucleation sites exists. Therefore, the main objective of this just is to advance the basic understanding of the mechanisms of surface-induced microstructure formation in glass ceramics. As a first attempt, we focus on reorientation of separately growing surface crystals during their early growth. T2 - 92nd Annual Meeting of the German Society of Glass Technology in Conjunction with the Annual Meetings of the Czech Glass Society & the Slovak Glass Society CY - Bayreuth, Germany DA - 28. Mai 2018 KW - Glass KW - Crystallization KW - BCS PY - 2018 AN - OPUS4-47536 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hlavacek, Petr A1 - Mühler, T. A1 - Lüchtenborg, Jörg A1 - Sturm, Patrick A1 - Gluth, Gregor A1 - Kühne, Hans-Carsten A1 - Günster, Jens T1 - Additive manufacturing of geopolymers by local laser curing N2 - For the additive manufacturing of large components typically powder-based methods are used. A powder is deposited layer by layer by means of a recoater, then, the component structure is printed into each individual layer. We introduce here the new method of local laser drying, which is a suspension-based method specially developed for the manufacturing of large voluminous ceramic parts. The structure information is directly written into the freshly deposited layer of suspension by laser drying. Initially, the technology was developed for ceramic suspensions, however, first experiments with geopolymers reveal a high potential for this class of materials. Metakaolin, fly ash and lithium aluminate-based one-part geopolymers were used in first experiments. The local annealing of the geopolymer slurry results in a drying and crosslinking reaction and, thus, in a local consolidation of the material. First parts made are introduced and their properties are discussed. T2 - CIMTEC 2018 CY - Perugia, Italy DA - 04.06.2018 KW - Additive manufacturing KW - Laser curing KW - Geopolymers PY - 2018 AN - OPUS4-47447 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Knauer, S A1 - Kratzig, Andreas A1 - Bettge, Dirk A1 - Kranzmann, Axel T1 - Droplet corrosion of CO2 transport pipeline steels N2 - This work examined the droplet corrosion of CO2 pipeline steels caused by impurities in CO2 supercritical/dense phase at 278 K, simulating the underground transport condition. The wetting properties of carbon steels (X52 and X70) as well as martensitic steel UNS S41500, and superaustenite UNS N08031 were studied by contact angle measurement, revealing reactive wetting behavior of carbon steels. Exposure tests with CO2 saturated water droplet on steel surface showed that the impurities (220 ppmv SO2 and 6700 ppmv O2) diffused into the droplet and then reacted with metal coupons in supercritical/dense phase condition, forming the corrosion product instantly during pumping process. Due to the active wetting behavior, the carbon steels suffered from heavily attack, while negligible corrosion product was observed in cases of martensitic steel UNS S41500 and superaustenite UNS 08031 coupons. Condensation experiments that were carried out on fresh polished coupons in CO2 with 1200 ppmv H2O showed that the formation and aggregation of droplet is dependent on the presence of impurities. Without SO2 and O2, the same concentration of H2O did not cause observable corrosion process after a week of exposure. With 220 ppmv SO2 and 6700 ppmv O2 even low water concentration (5-30 ppmv) still resulted in heterogeneous nucleation and subsequent growth of droplets, leading to corrosive process on carbon steel surface albeit to a lesser extent. T2 - CORROSION 2018 CY - Phoenix, AZ, USA DA - 15.04.2018 KW - CCUS KW - Supercritical/dense phase CO2 KW - Carbon steels KW - Martensitic steel KW - Superaustenite steel KW - Droplet corrosion PY - 2018 SP - Paper 10845, 1 EP - 11 PB - NACE International Publications Division CY - Houston, Texas, USA AN - OPUS4-44798 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo T1 - Effect of a circular notch on [001] tensile creep behavior of the Ni-base superalloy single crystal LEK 94 at 1020 °C N2 - Ni-base superalloy single crystals have been used in turbine blades for hot sections of gas turbines for over four decades. In order to increase the efficiency of the turbines, a continuous increase in the inlet temperature of combustion gases into the turbine has driven the design of turbine blades to complicated shapes and the presence of a complex pattern of cooling channels. These three-dimensional shapes, together with the inhomogeneous distribution of stresses along the blade, induce an also complicated triaxial stress state, which does not compare to uniaxial tests that are performed to characterize high temperature properties such as creep. A round notch on a test piece represents a simple configuration that generates a quasi-isostatic stress state across the notch. In the present contribution, the effect of a sharp round notch on the microstructural micromechanisms within the notched region cylindrical bars, loaded along [001] at 1020 °C and 160 MPa net stress, is studied. To this end, a series of interrupted creep tests is conducted on plain and notched bars and the microstructure is compared. Results are discussed in terms of degree microstructural coarsening, and dislocation activity. The effect of notch generation via grinding is also discussed in these terms. The presence of carbides evolving in from residual carbon is also shown and discussed. .Funding by the German Research Association (DFG) [grant number AG 191/1] is acknowledge T2 - DGM-Arbeitskreis mechanisches Werkstoffverhalten bei hoher Temperatur CY - Hochschule Augsburg, Germany DA - 20.09.2018 KW - Superalloy single crystals KW - Microstructure KW - Electron microscopy KW - Creep KW - Multiaxial stress state PY - 2018 AN - OPUS4-46050 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane A1 - Nützmann, Kathrin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Menneken, Martina A1 - Falk, Florian T1 - High temperature oxidation/sulfidation meets X-ray absorption near edge structure spectroscopy (XANES) N2 - Ferritic-martensitic alloys with 12-16 % Cr in weight are subject to devices for various energy systems, such as coal power plants and waste incineration plants. These materials are exposed to a highly corrosive environment which lead to a degradation of the material. Especially the simultaneous oxidation and sulfidation is thereby of special interest. Proper spatially resolved measurements that determine not only chemical compositions but phases are rare. However, precise phase identification and quantification of corrosion products within the multi-phase corrosion scales is a key aspect to understand diffusion paths of metal ions and gas ions/molecules. This study investigated Fe-Cr model alloys with Cr contents from 0 to 13 % in weight in 0.5 % SO2 and 99.5 % Ar atmosphere to aim in a fundamental and systematic analysis. Samples were aged at 650 °C for time scales from 12 h to 250 h. The results presented here correspond to depth dependent phase identification of oxide and sulphide phases in the corrosion scales by using X-ray absorption near edge spectroscopy (XANES). Per sample a series of ca. 20 spots (1-5 µm spot size) from scale-gas to scale-metal interface were measured. XANES spectroscopy was performed at the Fe-K edge (7.11 keV) on polished cross sections. The collected spectra were fitted to a combination of reference materials to quantify the present phases at different positions within the scale.The phase distribution differs with Cr content and the Cr diffusion through pure Fe-oxide and mixed Fe-Cr-oxide phases is discussed. T2 - EFC Workshop "High Temperature Corrosion" CY - Frankfurt am Main, Germany DA - 26.09.2018 KW - High temperature corrosion KW - XANES PY - 2018 AN - OPUS4-47277 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Röhsler, Andreas A1 - Sobol, Oded A1 - Nolze, Gert A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang T1 - Analysis of deuterium in austenitic stainless steel AISI 304L by Time-of-Flight Secondary Ion Mass Spectrometry N2 - Due to their excellent combination of ductility, strength and corrosive resistance, austenitic stainless steels (ASS) are widely used in many industrial applications. Thus, these steel grades can be found as structural components in the (petro-)chemical industry, in offshore applications and more recent for storage and transport of hydrogen fuel. Steels employed for these applications are exposed to aggressive environments and hydrogen containing media. The ingress and accumulation of hydrogen into the microstructure is commonly observed during service leading to a phenomenon called “hydrogen embrittlement”. A loss in ductility and strength, the formation of cracks and phase transformations are typical features of this hydrogen-induced degradation of mechanical properties. Although, great efforts are made to understanding hydrogen embrittlement, there is an ongoing debate of the underlying mechanisms. This knowledge is crucial for the safe use and durability of components on the one side and the development of new materials on the other. Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was proven to be a powerful tool for depicting the distribution of the hydrogen isotope deuterium in the microstructure of austenitic and duplex steels. The combination with imaging techniques such as electron backscatter diffraction (EBSD) and scanning electron microscopy (SEM), delivering structural and morphological information, creates a comprehensive picture of the hydrogen/deuterium-induced effects in the materials. All the gathered data is treated with principal component analysis (PCA) and data fusion to enhance the depth of information. The mobility of hydrogen and deuterium in a steel microstructure is affected by external mechanical stress. To investigate the behaviour of deuterium in a strained microstructure, a new in situ experimental approach was developed. This gives the possibility of analysing samples in the SIMS instrument simultaneously to four-point-bending-tests. Specimens made from ASS AISI 304L were electrochemically charged with deuterium instead of hydrogen. This necessity stems from the difficulty to separate between artificially charged hydrogen and hydrogen existing in the pristine material or adsorbed from the rest gas in the analysis chamber. Nonetheless, similar diffusion, permeation and solubility data allow to draw qualitative conclusions from the experiments, which are relevant for the application addressed. T2 - SIMS Europe 2018 CY - Münster, Germany DA - 16.09.2018 KW - Hydrogen KW - Deuterium KW - Austenitic stainless steel KW - SIMS PY - 2018 AN - OPUS4-46029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nützmann, Kathrin A1 - Menneken, Martina A1 - Agudo Jácome, Leonardo A1 - Stephan-Scherb, Christiane T1 - Orientation dependent corrosion N2 - Ferritic-martensitic Fe-Cr alloys are widely utilised as materials for high temperature applications such as super heater tubes in coal, biomass or co-fired power plants. Various corrosive gases are produced in combustion processes, but especially SO2 is known to cause catastrophic application failure. In order to understand the effect of orientation and grain size of the alloy on the initial corrosion processes we analysed metal coupons of Fe-Cr- alloys (2-13 wt. % Cr) by electron backscattered diffraction (EBSD) before and after exposure to SO2 containing atmospheres in 650°C for short time spans (2 min – 12 h). An infra red heated furnace with integrated water-cooling was used for the ageing procedures to conduct short time experiments and to keep the reaction products in a ‘frozen’ state. EBSD characterization of oxides formed on the surface of the alloys showed a topotactic relationship between grain orientation of the alloys and the oxides. With increasing scale thickness this relation diminishes possibly due to lattice strain. There appears to be no correlation between oxide growth and absolute, initial orientation, grain size, or the quality of polishing. An initially topotactic relationship between scale and steel had been already described for the formation of magnetite in hot steam environments, indicating that the initial corrosion mechanisms are mainly depending on the presence of Oxygen, and not changed by the presence of Sulphur. However, Sulphur is incorporated into the oxide scale in the low Cr alloy, and mainly observable in the inner corrosion zone for the higher alloyed material. Furthermore, oxides formed directly on grain boundaries in higher Cr alloyed materials are enriched in Cr compared to oxides on grain faces. T2 - EFC Workshop Dechema CY - Frankfurt am Main, Germany DA - 26.09.2018 KW - Crystal Orientation KW - High Temperature Corrosion PY - 2018 AN - OPUS4-47279 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sommer, Konstantin A1 - Kranzmann, Axel A1 - Reimers, W. T1 - Microstructure characterization of additive produced parts N2 - Due to the advantages of additive manufacturing (AM), it has been increasingly integrated into many industrial sectors. The application of AM materials for safety-critical parts requires the detailed knowledge about their microstructure stability under thermo-mechanical or mechanical load and knowledge on ageing process mechanisms. Ageing processes are characterized by change of the material microstructure that is to be initially investigated. This work deals with the Investigation of 316L stainless steel manufactured by selective laser melting (SLM). Describing Parameters must be defined and applied on the microstructure of these materials in their initial state and after loads were applied. The findings of this work form the basis for the investigation of AM material ageing. T2 - FEMS Junior EUROMAT 2018 CY - Budapest, Hungary DA - 08.07.2018 KW - Additive manufacturing KW - Selective laser melting KW - 316L KW - Material characterization KW - Microstructure PY - 2018 AN - OPUS4-47176 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Knauer, S. A1 - Kratzig, Andreas A1 - Bettge, Dirk A1 - Kranzmann, Axel T1 - Droplet corrosion of CO2 transport pipeline steels N2 - In this work, the focus was set on the corrosion process of condensate as drops on the surface of carbon steels (X52, X70), martensitic steel UNS S41500, and superaustenite UNS 08031 in CO2 atmosphere with impurities at 278 K (to simulate the transportation condition in a buried pipeline). Exposure tests were performed at both normal pressure and high pressure where CO2 is supercritical or in dense phase. The drop, 1 ‑ 10 µL in volume, was prepared by dropping CO2 saturated ultra-pure water onto the surface of steel coupons in a one-liter-autoclave. The CO2 gas stream, simulating the oxyfuel flue gas with varying concentration of impurities (SO2 and O2), was then pumped into the autoclave to observe the condensation and corrosion impacts of impurities. Comparable exposure tests were carried out with the same gas mixture and the same volume of water as vapor to observe the drop formation and the corrosion process that follows. The wettability and stability of drops on the surface of steel coupons in CO2 supercritical/dense phase environment was evaluated additionally by contact angle measurement. T2 - NACE 2018 CY - Phoenix, Arizona, USA DA - 15.04.2018 KW - Droplet corrosion KW - CCUS KW - Supercritical/dense phase CO2 KW - Carbon steels KW - Martensitic steel KW - Superaustenite steel PY - 2018 AN - OPUS4-44767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Olbricht, Jürgen A1 - Jürgens, Maria A1 - Mosquera Feijoo, Maria A1 - Agudo Jácome, Leonardo A1 - Roohbakhshan, Farshad A1 - Saliwan Neumann, Romeo A1 - Nolze, Gert A1 - Fedelich, Bernard A1 - Kranzmann, Axel A1 - Skrotzki, Birgit T1 - Performance of 9-12%Cr steels under cyclic loading and cyclic oxidation conditions N2 - 9-12% Cr ferritic-martensitic stainless steels are widely used as high temperature construction materials in power plants due to their excellent creep and oxidation resistance. The growing share of renewable energy sources in power generation forces many of these plants into more flexible operation with frequent load shifts or shutdowns. These cyclic operation profiles constitute a major lifetime issue. The present contribution reports on current findings obtained in a multidisciplinary project which combines cyclic mechanical and cyclic oxidation testing with detailed microstructural analyses. Mechanical analyses are carried out on P92 and P91 steel grades to give an overview of softening phenomena and lifetimes obtained in isothermal cyclic loading (low cycle fatigue, LCF), non-isothermal cyclic loading (thermo-mechanical fatigue, TMF), and service-like combinations of creep and fatigue periods (creep-fatigue interaction). Oxidation testing focuses on the grades P92 and VM12 with the intention of clarifying the impact of frequent passes through intermediate temperature levels on the kinetics of steam-side oxidation and the characteristics of the evolving oxide scales. An attempt is made to evaluate their composition, strength, integrity and adhesion after up to 250 temperature cycles. Flat coupons as well as curved tube sections are tested to assess the mutual influence of geometry on oxide scale integrity. Complementary microstructural investigations by scanning and transmission electron microscopy plus EBSD are used for phase identification and substrate/oxide interface characterisation. The evolutions of grain size and dislocation density under different test conditions are quantified. T2 - International Conference on Power Plant Operation & Flexibility CY - London, UK DA - 04.07.2018 KW - Ferritic-martensitic steels KW - Low cycle fatigue KW - Thermo-mechanical fatigue KW - Cyclic oxidation PY - 2018 AN - OPUS4-47115 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Olbricht, Jürgen A1 - Jürgens, Maria A1 - Agudo Jácome, Leonardo A1 - Nolze, Gert A1 - Roohbakhshan, Farshad A1 - Fedelich, Bernard A1 - Skrotzki, Birgit T1 - Cyclic loading and creep-fatigue performance of P92 N2 - 9-12% Cr ferritic-martensitic stainless steels are widely used as high temperature construction materials in power plants due to their excellent creep and oxidation resistance. The growing share of renewable energy sources in power generation forces many of these plants into more flexible operation with frequent load shifts or shutdowns. These cyclic operation profiles constitute a major lifetime issue. The present contribution reports on current findings obtained in a multidisciplinary project which combines cyclic mechanical and cyclic oxidation testing of different 9-12% Cr grades with detailed microstructural analyses. Mechanical analyses are carried out on P92 and P91 steel grades to give an overview of softening phenomena and lifetimes obtained in isothermal cyclic loading (low cycle fatigue, LCF), non-isothermal cyclic loading (thermo-mechanical fatigue, TMF), and service-like combinations of creep and fatigue periods. Complementary microstructural investigations by scanning and transmission electron microscopy plus EBSD are used for phase identification, substrate/oxide interface characterization and quantification of the microstructure evolution under cyclic conditions. T2 - 44th MPA-Seminar CY - Leinfelden/Stuttgart, Germany DA - 17.10.2018 KW - Ferritic-martensitic steels KW - Fatigue KW - Creep-fatigue PY - 2018 AN - OPUS4-47116 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klinger, Christian A1 - Bettge, Dirk A1 - Ell, Matthias T1 - Failure analysis on medical implants N2 - The application of implants e.g. for osteosynthesis or substitution of worn out joints is common practice since decades. Successes in surgery and orthopedics are highly dependent on the use of artificial parts for implanting into the human body. Over the years the number of surgical procedures and the number of different implants were growing rapidly. Implants, however, are exposed to complex mechanical, corrosive and tribological loads along with restriction in geometric dimension. While being essentially successful, the sheer number of cases leads to a rising number of implant failures. Such failures are painful for the affected patients and are very costly. The failure cases presented in this paper occurred from 1981 to 2016. The predominant failure mechanism of all kinds of implants is fatigue fracture. Fatigue cracks are initiated due to a whole bunch of reasons: Material defects and fabrication defects are rare events. The main factors are cyclic overload due to improper fitting with delayed bone healing, corrosion and unauthorized modification of the implant during surgery T2 - Int. Conf. on Engineering Failure Analysis 2018 CY - Budapest, Hungary DA - 08.07.2018 KW - Implant failures KW - Complex loading KW - Fatigue fracture PY - 2018 AN - OPUS4-50198 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nadammal, Naresh A1 - Kromm, Arne A1 - Saliwan Neumann, Romeo A1 - Farahbod, Lena A1 - Haberland, Christoph A1 - Portella, Pedro Dolabella T1 - Influence of support configurations on the characteristics of selective laser-melted Inconel 718 N2 - Samples fabricated using two different support configurations by following identical scan strategies during selective laser melting of superalloy Inconel 718 were characterized in this study. Characterization methods included optical microscopy, electron back-scattered diffraction and x-ray diffraction residual stress measurement. For the scan strategy considered, microstructure and residual stress development in the samples were influenced by the support structures. However, crystallographic texture intensity and the texture components formed within the core part of the samples were almost independent of the support. The formation of finer grains closer to the support as well as within the columnar grain boundaries resulted in randomization and texture intensity reduction by nearly half for the sample built on a lattice support. Heat transfer rates dictated by the support configurations in addition to the scan strategy influenced the microstructure and residual stress development in selective laser-melted Inconel 718 samples. KW - Additive manufacturing KW - Selective laser melting KW - Support configurations KW - Microstructure and texture KW - Residual stress PY - 2018 DO - https://doi.org/10.1007/s11837-017-2703-1 SN - 1047-4838 SN - 1543-1851 VL - 70 IS - 3 SP - 343 EP - 348 PB - Springer CY - USA AN - OPUS4-44175 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Butz, Adam A1 - Fedelich, Bernard A1 - Rehmer, Birgit A1 - Skrotzki, Birgit T1 - Crack identification by data fusion in fatigued flat specimens with through-holes - A feasibility study N2 - A numerical pre-study has shown that cracks in a flat sample featuring a drilled hole can be classified into one of three crack shape classes based on the combined evaluation of various types of test data. T2 - Fatigue 2018 CY - Poitiers, France DA - 27.05.2018 KW - LCF KW - Crack KW - Data Fusion PY - 2018 AN - OPUS4-45936 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Uckert, Danilo A1 - Kühn, Hans-Joachim A1 - Matzak, Kathrin A1 - Rehmer, Birgit A1 - Skrotzki, Birgit T1 - Ermüdungsverhalten des warmfesten austenitischen Gusseisens EN-GJSA-XNiSiCr35-5-2 bei hoher Temperatur N2 - Die warmfeste austenitische Gusseisenlegierung EN-GJSA-XNiSiCr35-5-2 (häufig auch als Ni-Resist D-5S bezeichnet) wurde hinsichtlich ihres mechanischen Verhaltens bei hoher Temperatur charakterisiert. Dazu wurden (isotherme) niederzyklische (LCF-) und (nicht-isotherme) thermomechanische Ermüdungsversuche (TMF) zwischen Raumtemperatur und 900 °C durchgeführt. Diese Ergebnisse dienten (zusammen mit weiteren Versuchsdaten) der Kalibrierung werkstoffmechanischer Modelle. Bei den höchsten Prüftemperaturen wurde Schädigung in Form von Kriechen beobachtet und metallographisch dokumentiert. T2 - Langzeitverhalten warmfester Stähle und Hochtemperaturwerkstoffe CY - Dusseldorf, Germany DA - 30.11.2018 KW - Kriechen KW - LCF KW - Lebensdauer KW - Ni-Resist KW - Schädigung KW - TMF PY - 2018 SN - 978-3-00-061694-5 SP - 29 EP - 38 CY - Düsseldorf AN - OPUS4-46919 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Butz, Adam A1 - Fedelich, Bernard A1 - Rehmer, Birgit A1 - Skrotzki, Birgit A1 - Schmitz, Sebastian ED - Moninger, G. T1 - Risserkennung an Bohrlochproben: Numerische Voruntersuchung für eine neuartige Methode zur Rissformerkennung T1 - Crack Detection on Borehole Specimens: Numerical pre-examination for a novel crack shape detection method N2 - Es konnte anhand einer numerischen Voruntersuchung gezeigt werden, dass anhand der kombinierten Auswertung der im Versuch verwendeten Sensorik eine Einteilung der unter Ermüdung in Bohrlochproben auftretenden Rissformen in verschiedene Hauptkategorien (Eckriss, Oberflächenriss, Durchgangsriss) möglich ist. N2 - When fatigued specimens with a hole are to be investigated regarding crack growth, it may be the case that the shape of the crack can’t be identified with sufficient certainty. If marking the fracture surface e.g. using beach marks is not possible, a method is required that nevertheless allows for the determination of the crack shape in order to calculate the corresponding fracture mechanics parameters. This paper describes a numerical pre-study for a method that allows for the classification of cracks in a sample featuring a drill hole into one of three crack shape classes based on the combined evaluation of various types of test data. T2 - Tagung Werkstoffprüfung 2018 CY - Bad Neuenahr, Germany DA - 06.12.2018 KW - Crack KW - LCF KW - Data Fusion KW - Risse KW - Rissform KW - Datenfusion PY - 2018 VL - 2018 SP - 249 EP - 254 AN - OPUS4-46976 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bettge, Dirk A1 - Portella, Pedro Dolabella T1 - Fraktographische online-Datenbank: Beispiele Kunststoffe N2 - Im Rahmen der DGM/DVM AG Fraktographie wird an der BAM eine fraktographische online-Datenbank aufgebaut. Während von metallischen Werkstoffen viele Beispiele vorliegen, die auch gut verstanden sind, sind die Brüche von Kunststoffen bislang weniger prominent vertreten. Eine teils ungeklärte Frage ist, in welcher Form sich an Kunststoffen klassische Schwingbrüche nachweisen lassen, wie sie von metallischen Werkstoffen bekannt sind. Der Vortrag zeigt einige Beispiele im Detail und stellt diese zur Diskussion. T2 - VDI Expertenkreis Kunststoffe CY - Wuppertal, Germany DA - 08.11.2018 KW - Schwingbrüche KW - Kunststoffe KW - Fraktographie PY - 2018 AN - OPUS4-47388 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bettge, Dirk A1 - Portella, Pedro Dolabella A1 - Buggisch, Enrico A1 - Schneider, Hannes T1 - Fraktographische online-Datenbank: Erste Ergebnisse aus Schwingversuchen an Sinterstählen N2 - Im Rahmen der Erstellung einer fraktographischen online-Datenbank an der BAM wurden systematisch Schwingversuche an einem Sinterstahl vorgenommen, dessen Sinterdichte variiert wurde. Die erzeugten Bruchflächen wurden analysiert, mit der Literatur verglichen und Datensätze in die Datenbank eingefügt. T2 - VDI Expertenkreis Sinterstähle CY - Berlin, Germany DA - 12.04.2018 KW - Fraktographie PY - 2018 AN - OPUS4-47389 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Skrotzki, Birgit A1 - Häusler, I. A1 - Schwarze, C. A1 - Umer Bilal, M. A1 - Hetaba, W. A1 - Darvishi Kamachali, Reza T1 - Age hardening of a high purity Al‐4Cu‐1Li‐0.25Mn alloy: Microstructural investigation and phase‐field simulation N2 - Research results considering the "Age Hardening of a High Purity Al‐4Cu‐1Li‐0.25Mn Alloy: Microstructural Investigation and Phase‐Field Simulation" were presented. T2 - ICAA16 CY - Montreal, Canada DA - 17.06.2018 KW - Age hardening KW - Aluminium KW - Phase-field simulation KW - Precipitates KW - Transmission electron microscopy PY - 2018 AN - OPUS4-45286 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Darvishi Kamachali, Reza A1 - Rockenhäuser, Christian A1 - Saxena, A. A1 - Skrotzki, Birgit A1 - Umer Bilal, M. A1 - Ramirez, Daniela Valencia A1 - Schwarze, C. A1 - Häusler, I. T1 - Chemo-mechanical Coupling Effect During Precipitation in AlLi and AlLiCu systems N2 - The chemo-mechanical coupling effect during precipitation in AlLi and AlLiCu systems is presented and effects of chemo-mechanical coupling on materials with different microstructures is discussed. The results of the simulations are then compared to electron-microscopical investigations. T2 - Plenary meeting DFG Priority program 1713 ("Chemomechanics") CY - Bochum, Germany DA - 17.12.2018 KW - Al-Li alloys KW - Phase field simulation KW - Precipitation KW - Inverse ostwald ripening KW - Transmission electron microscopy PY - 2018 AN - OPUS4-46961 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rockenhäuser, Christian A1 - Häusler, Ines A1 - Darvishi Kamachali, Reza A1 - Heidl, Daniel A1 - Skrotzki, Birgit T1 - Influence of heat treatment and creep loading on an Al-Cu-Li alloy N2 - The influence of heat treatment and creep loading on the microstructure of an Al-Cu-Li alloy was investigated. Especially the formation of different precipitates (T1 and Theta') were characterized and the microstructural changes under different ageing conditions (with and without external strain) were investigated to determine the effect od stress on the ageing process. T2 - 19th International Microscopy Congress (IMC19) CY - Sydney, Australia DA - 09.09.2018 KW - Aluminium KW - Degradation KW - Coarsening KW - Dark-field transmission electron microscopy PY - 2018 AN - OPUS4-46129 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rockenhäuser, Christian A1 - Häusler, Ines A1 - Darvishi Kamachali, Reza A1 - Heidl, Daniel A1 - Skrotzki, Birgit T1 - Influence of heat treatment and creep loading on an Al-Cu-Li alloy N2 - The influence of heat treatment and creep loading on the microstructure of an Al-Cu-Li alloy was investigated. Especially the formation of different precipitates (T1 and Theta') were characterized and the microstructural changes under different ageing conditions (with and without external strain) were investigated to determine the effect od stress on the ageing process. T2 - 19th International Microscopy Congress (IMC19) CY - Sydney, Australia DA - 09.09.2018 KW - Aluminium KW - Degradation KW - Coarsening KW - Dark-field transmission electron microscopy PY - 2018 AN - OPUS4-46131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kindrachuk, Vitaliy A1 - Titscher, Thomas A1 - Unger, Jörg F. T1 - A Fourier transformation-based method for gradient-enhanced modeling of fatigue N2 - A key limitation of the most constitutive models that reproduce a Degradation of quasi-brittle materials is that they generally do not address issues related to fatigue. One reason is the huge computational costs to resolve each load cycle on the structural level. The goal of this paper is the development of a temporal Integration scheme, which significantly increases the computational efficiency of the finite element method in comparison to conventional temporal integrations. The essential constituent of the fatigue model is an implicit gradient-enhanced formulation of the damage rate. The evolution of the field variables is computed as amultiscale Fourier series in time.On a microchronological scale attributed to single cycles, the initial boundary value problem is approximated by linear BVPs with respect to the Fourier coefficients. Using the adaptive cycle jump concept, the obtained damage rates are transferred to a coarsermacrochronological scale associated with the duration of material deterioration. The performance of the developedmethod is hence improved due to an efficient numerical treatment of the microchronological problem in combination with the cycle jump technique on the macrochronological scale. Validation examples demonstrate the convergence of the obtained solutions to the reference simulations while significantly reducing the computational costs. KW - Accelerated temporal integration KW - Fourier series KW - Gradient-enhanced fatigue model PY - 2018 DO - https://doi.org/10.1002/nme.5740 SN - 1097-0207 SN - 0029-5981 VL - 114 IS - 2 SP - 196 EP - 214 PB - Wiley AN - OPUS4-44008 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Jörg F. A1 - Kindrachuk, Vitaliy A1 - Titscher, Thomas T1 - Concrete under cyclic loading a continuum damage model and a temporal multiscale approach N2 - The durability of concrete structures and its performance over the lifetime is strongly influenced by many interacting phenomena such as e.g. mechanical degradation due to fatigue loading, loss of prestress, degradation due to chemical reactions or creep and shrinkage. Failure due to cyclic loading is generally not instantaneous, but characterized by a steady damage accumulation. Many constitutive models for concrete are currently available, which are applicable for specific loading regimes, different time scales and different resolution scales. A key limitation is that the models often do not address issues related to fatigue on a structural level. Very few models can be found in the literature that reproduce deterioration of concrete under repeated loading-unloading cycles. The objective of this paper is the presentation of numerical methods for the simulation of concrete under fatigue loading using a temporal multiscale method. First, a continuum damage model for concrete is developed with a focus on fatigue under compressive stresses. This includes the possibility to model stress redistributions and capture size effects. In contrast to cycle based approaches, where damage is accumulated based on the number of full stress cycles, a strain based approach is developed that can capture cyclic degradation under variable loading cycles including different amplitudes and loading frequencies. Second, a multiscale approach in time is presented to enable structural computations of fatigue failure with a reduced computational effort. The damage rate within the short time scale corresponding to a single cycle is computed based on a Fourier based approach. This evolution equation is then solved on the long time scale using different time integration schemes. T2 - 6th European Conference on Computational Mechanics (ECCM 6) CY - Glasgow, UK DA - 11.06.2018 KW - Cycle jump KW - Fatigue damage KW - Concrete PY - 2018 AN - OPUS4-45696 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kindrachuk, Vitaliy A1 - Titscher, Thomas A1 - Hirthammer, Volker A1 - Unger, Jörg F. ED - Meschke, G. ED - Pichler, B. ED - Rots, J.G. T1 - A continuum damage model for the simulation of concrete under cyclic loading N2 - Lifetime aspects including fatigue failure of concrete structures were traditionally only of minor importance. Because of the growing interest in maxing out the capacities of concrete, its fatigue failure under compression has become an issue. A variety of interacting phenomena such as e.g. loss of prestress, degradation due to chemical reactions or creep and shrinkage influence the fatigue resistance. Failure due to cyclic loads is generally not instantaneous, but characterized by a steady damage accumulation. Therefore, a reliable numerical model to predict the performance of concrete over its lifetime is required, which accurately captures order effects and full three-dimensional stress states. Many constitutive models for concrete are currently available, which are applicable for specific loading regimes, different time scales and different resolution scales. However, a key limitation of those models is that they generally do not address issues related to fatigue on a structural level. Very few models can be found in the literature that reproduce deterioration of concrete under repeated loading-unloading cycles. This is due to the computational effort necessary to explicitly resolve every cycle which exceeds the currently available computational resources. The limitation can only be overcome by the application of multiscale methods in time. The objective of the paper is the development of numerical methods for the simulation of concrete under fatigue loading using temporal multiscale methods. First, a continuum damage model for concrete is developed with a focus on fatigue under compressive stresses [1]. This includes the possibility to model stress redistributions and capture size effects. In contrast to cycle based approaches, where damage is accumulated based on the number of full stress cycles, a strain based approach is developed that can capture cyclic degradation under variable loading cycles including different amplitudes and loading frequencies. The model is designed to represent failure under static loading as a particular case of fatigue failure after a single loading cycle. As a consequence, most of the material parameters can be deduced from static tests. Only a limit set of additional constitutive parameters is required to accurately describe the evolution under fatigue loading. Another advantage of the proposed model is the possibility to directly incorporate other multi-physics effects such as creep and shrinkage or thermal loading on the constitutive level. Second, a multiscale approach in time is presented to enable structural computations of fatigue failure with a reduced computational effort. The damage rate within the short time scale corresponding to a single cycle is computed based on a Fourier based approach [2]. This evolution equation is then solved on the long time scale using different implicit and explicit time integration schemes. Their performance and some limitations for specific loading regimes is discussed. Finally, the developed methods will be validated and compared to experimental data. [1] Vitaliy Kindrachuk, Marc Thiele, Jörg F. Unger. Constitutive modeling of creep-fatigue interaction for normal strength concrete under compression, International Journal of Fatigue, 78:81-94, 2015 [2] Vitaliy Kindrachuk, Jörg F. Unger. A Fourier transformation-based temporal integration scheme for viscoplastic solids subjected to fatigue deterioration, International Journal of Fatigue, 100:215-228, 2017 T2 - Conference on Computational Modelling of concrete and concrete structures (EURO_C 2018') CY - Bad Hofgastein, Austria DA - 26.02.2018 KW - Fatigue KW - Concrete KW - Damage PY - 2018 SN - 978-1-138-74117-1 DO - https://doi.org/10.1201/9781315182964-19 SP - 155 EP - 164 PB - CRC Press, Taylor & Francis Group CY - Boca Raton, Lodon, New York, Leiden AN - OPUS4-47999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kindrachuk, Vitaliy A1 - Unger, Jörg F. T1 - A novel computational method for efficient evaluation of structural fatigue N2 - The methods of computational damage mechanics are well-established for the description of degradation of materials under monotone loading. An extension to structural damage induced by cyclic loading is however significantly limited. This is due to enormous computational costs required to resolve each load cycle by conventional temporal incremental integration schemes while a typical fatigue loading history comprises between thousands and millions of cycles. Despite the permanent increase of computational resources and algorithmic performance, a successful approach is rather based on the development of novel multiscale in time integration schemes. A Fourier transformation-based temporal integration (FTTI) is represented, which takes advantage of temporal scale separation incorporated into the cycle jump method. The response fields are approximated by a Fourier series whose coefficients undergo the evolution on a long-time scale. This is correlated with the evolution of the history variables, including damage, by means of the adaptive cycle jump method of various orders. The necessary extrapolation rates are obtained from the underlying solution of a short-time scale problem, which results from the oscillatory boundary condition and fulfills the global equilibrium of the Fourier coefficients. In this way, a remarkable speedup is achieved because the number of cycles to be fully integrated dramatically decreases. The key idea behind the FTTI method is that the global in space equilibrium problem is linear since it is decoupled from the evolution equations. The latter are solved in the quadrature points under response fields prescribed throughout the whole load cycle. Consequently, integration of a single load cycle is much more efficient than the conventional single scale integration where the global equilibrium iteration and the local iteration of the evolution equations are coupled. This results in an additional speedup of the FTTI method. The performance of the FTTI technique is demonstrated for two different constitutive behaviors: a viscoplastic model with a damage variable governed by the local equivalent viscoplastic strain; a quasi-brittle response where the damage variable is driven by a non-local equivalent strain. The latter is implicitly introduced as proposed by Peerlings. Both, the explicit and implicit extrapolation schemes are validated. The FTTI solutions agree very well with the reference cycle-by -cycle solutions, while significantly reducing the computational costs. The adaptive determination of the jump length can properly recognize the particular responses throughout the fatigue loading history (stationary fatigue, acceleration of fatigue damage when approaching failure) as well as stress redistribution phenomena. T2 - International Fatigue International Fatigue International Fatigue International Fatigue International Fatigue International Fatigue Congress Congress Congress 2018 CY - Poitiers, France DA - 27.05.2018 KW - Fatigue KW - Accelerated integration scheme PY - 2018 AN - OPUS4-46975 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Jörg F. A1 - Kindrachuk, Vitaliy A1 - Titscher, Thomas A1 - Hirthammer, Volker T1 - A continuum damage model for the simulation of concrete under cyclic loading N2 - Lifetime aspects including fatigue failure of concrete structures were traditionally only of minor importance. Because of the growing interest in maxing out the capacities of concrete, its fatigue failure under compression has become an issue. A variety of interacting phenomena such as e.g. loss of prestress, degradation due to chemical reactions or creep and shrinkage influence the fatigue resistance. Failure due to cyclic loads is generally not instantaneous, but characterized by a steady damage accumulation. Therefore, a reliable numerical model to predict the performance of concrete over its lifetime is required, which accurately captures order effects and full three-dimensional stress states. Many constitutive models for concrete are currently available, which are applicable for specific loading regimes, different time scales and different resolution scales. However, a key limitation of those models is that they generally do not address issues related to fatigue on a structural level. Very few models can be found in the literature that reproduce deterioration of concrete under repeated loading-unloading cycles. This is due to the computational effort necessary to explicitly resolve every cycle which exceeds the currently available computational resources. The limitation can only be overcome by the application of multiscale methods in time. The objective of the paper is the development of numerical methods for the simulation of concrete under fatigue loading using temporal multiscale methods. First, a continuum damage model for concrete is developed with a focus on fatigue under compressive stresses. This includes the possibility to model stress redistributions and capture size effects. In contrast to cycle based approaches, where damage is accumulated based on the number of full stress cycles, a strain based approach is developed that can capture cyclic degradation under variable loading cycles including different amplitudes and loading frequencies. The model is designed to represent failure under static loading as a particular case of fatigue failure after a single loading cycle. As a consequence, most of the material parameters can be deduced from static tests. Only a limit set of additional constitutive parameters is required to accurately describe the evolution under fatigue loading. Another advantage of the proposed model is the possibility to directly incorporate other multi-physics effects such as creep and shrinkage or thermal loading on the constitutive level. Second, a multiscale approach in time is presented to enable structural computations of fatigue failure with a reduced computational effort. The damage rate within the short time scale corresponding to a single cycle is computed based on a Fourier based approach. This evolution equation is then solved on the long time scale using different implicit and explicit time integration schemes. Their performance and some limitations for specific loading regimes is discussed. Finally, the developed methods will be validated and compared to experimental data. T2 - Conference on Computational Modelling of concrete and concrete structures (EURO_C 2018') CY - Bad Hofgastein, Austria DA - 26.02.2018 KW - Fatigue KW - Concrete KW - Damage PY - 2018 AN - OPUS4-48001 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kindrachuk, Vitaliy ED - Titscher, Thomas ED - Hirthammer, Volker ED - Unger, Jörg F. T1 - A continuum damage model for the simulation of concrete under cyclic loading N2 - A continuum damage model for concrete is developed with a focus on fatigue under compressive stresses. This includes the possibility to model stress redistributions and capture size effects. In contrast to cycle based approaches, where damage is accumulated based on the number of full stress cycles, a strain based approach is developed that can capture cyclic degradation under variable loading cycles including different amplitudes and loading frequencies. The model is designed to represent failure under static loading as a particular case of fatigue failure after a single loading cycle. As a consequence, most of the material parameters can be deduced from statictests. Only a limit set of additional constitutive parameters is required to accurately describe the evolution under fatigue loading. Another advantage of the proposed model is the possibility to directly incorporate other multi-physics effects such as creep and shrinkage or thermal loading on the constitutive level. A multiscale approach in time is presented to enable structural computations of fatigue failure with a reduced computational effort. The damage rate within the short time scale corresponding to a single cycle is computed based on a Fourier based approach. This evolution equation is then solved on the long time scale using different implicit and explicit time integration schemes. Their performance and some limitations for specific loading regimes is discussed. T2 - Euro-C, March 1st 2018 CY - Bad Hofgastein, Austria DA - 26.02.2018 KW - Continnum damage model KW - Simulation of concrete KW - Under cyclic loading PY - 2018 UR - https://euro-c.tuwien.ac.at/home/ SN - 978-1-315-18296-4 SN - 978-1-138-74117-1 VL - 2018 SP - 155 EP - 164 PB - CRC Press, Taylor & Francis Group CY - Leiden, The Netherland AN - OPUS4-48400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kindrachuk, Vitaliy A1 - Titscher, Thomas A1 - Hirthammer, Volker A1 - Unger, Jörg F. T1 - A continuum damage model for the simulation of concrete under cyclic loading N2 - A continuum damage model for concrete is developed with a focus on fatigue under compressive stresses. This includes the possibility to model stress redistributions and capture size effects. In contrast to cycle based approaches, where damage is accumulated based on the number of full stress cycles, a strain based approach is developed that can capture cyclic degradation under variable loading cycles including different amplitudes and loading frequencies. The model is designed to represent failure under static loading as a particular case of fatigue failure after a single loading cycle. As a consequence, most of the material parameters can be deduced from statictests. Only a limit set of additional constitutive parameters is required to accurately describe the evolution under fatigue loading. Another advantage of the proposed model is the possibility to directly incorporate other multi-physics effects such as creep and shrinkage or thermal loading on the constitutive level. A multiscale approach in time is presented to enable structural computations of fatigue failure with a reduced computational effort. The damage rate within the short time scale corresponding to a single cycle is computed based on a Fourier based approach. This evolution equation is then solved on the long time scale using different implicit and explicit time integration schemes. Their performance and some limitations for specific loading regimes is discussed. T2 - Computational Modelling of concrete and concrete Structures Euro-C, March 1st 2018 CY - Bad Hofgastein, Austria DA - 26.02.2018 KW - Continnum damage model KW - Simulation of concrete KW - Under cyclic loading PY - 2018 UR - https://euro-c.tuwien.ac.at/home/ AN - OPUS4-48399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Skrotzki, Birgit A1 - Uckert, Danilo A1 - Kühn, Hans-Joachim A1 - Matzak, Kathrin A1 - Rehmer, Birgit T1 - Ermüdungsverhalten des warmfesten austenitischen Gusseisens EN-GJSA-XNiSiCr35-5-2 bei hoher Temperatur N2 - Die warmfeste austenitische Gusseisenlegierung EN-GJSA-XNiSiCr35-5-2 (häufig auch als Ni-Resist D-5S bezeichnet) wurde hinsichtlich ihres mechanischen Verhal-tens bei hoher Temperatur charakterisiert. Dazu wurden (isotherme) niederzyklische (LCF-) und (nicht-isotherme) thermomechanische Ermüdungsversuche (TMF) zwischen Raumtemperatur und 900 °C durchgeführt. Diese Ergebnisse dienten (zu-sammen mit weiteren Versuchsdaten) der Kalibrierung werkstoffmechanischer Modelle. Bei den höchsten Prüftemperaturen wurde Schädigung in Form von Kriechen beobachtet und metallographisch dokumentiert. T2 - 41. Vortragsveranstaltung Langzeitverhalten warmfester Stähle und Hochtemperaturwerkstoffe CY - Dusseldorf, Germany DA - 30.11.2018 KW - Ni-Resist KW - LCF KW - TMF KW - Kriechen KW - Lebensdauer KW - Schädigung PY - 2018 AN - OPUS4-46851 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Butz, Adam A1 - Fedelich, Bernard A1 - Rehmer, Birgit A1 - Schmitz, Sebastian T1 - Risserkennung an Bohrlochproben N2 - Es wird eine neu entwickelte Methode zur Thermographiebasierten Rissmessung vorgestellt. Darüber hinaus wird eine numerische Vorarbeit präsentiert, die zeigt, dass anhand der gemeisamen Auswertung der Versuchsdaten aus unterschiedlicher Sensorik die Möglichkeit besteht, die unter Ermüdungsbelastung in Bohrlochproben auftretenden Risse in Geometriekategorien zu unterteilen. T2 - Tagung Werkstoffprüfung 2018 CY - Bad Neuenahr, Germany DA - 06.12.2018 KW - LCF KW - Crack KW - Data Fusion KW - Thermographie PY - 2018 AN - OPUS4-46977 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kromm, Arne A1 - Cabeza, S. A1 - Mishurova, Tatiana A1 - Thiede, Tobias A1 - Nadammal, Naresh A1 - Bruno, Giovanni A1 - Portella, Pedro Dolabella T1 - Residual stress Formation in selective laser melted parts of Alloy 718 N2 - Additive Manufacturing (AM) through the Selective Laser Melting (SLM) route offers ample scope for producing geometrically complex parts compared to the conventional subtractive manufacturing strategies. Nevertheless, the residual stresses which develop during the fabrication can limit application of the SLM components by reducing the load bearing capacity and by inducing unwanted distortion, depending on the boundary conditions specified during manufacturing. The present study aims at characterizing the residual stress states in the SLM parts using different diffraction methods. The material used is the nickel based superalloy Inconel 718. Microstructure as well as the surface and bulk residual stresses were characterized. For the residual stress analysis, X-ray, synchrotron and neutron diffraction methods were used. The measurements were performed at BAM, at the EDDI beamline of -BESSY II synchrotronand the E3 line -BER II neutron reactor- of the Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. The results reveal significant differences in the residual stress states for the different characterization techniques employed, which indicates the dependence of the residual state on the penetration depth in the sample. For the surface residual stresses, longitudinal and transverse stress components from X-ray and synchrotron agree well and the obtained values were around the yield strength of the material. Furthermore, synchrotron mapping disclosed gradients along the width and length of the sample for the longitudinal and transverse stress components. On the other hand, lower residual stresses were found in the bulk of the material measured using neutron diffraction. The longitudinal component was tensile and decreased towards the boundary of the sample. In contrast, the normal component was nearly constant and compressive in nature. The transversal component was almost negligible. The results indicate that a stress re-distribution takes place during the deposition of the consecutive layers. Further investigations are planned to study the phenomenon in detail. T2 - European Conference on Residual Stresses - ECRS10 CY - Leuven, Belgium DA - 11.09.2018 KW - Additive Manufacturing KW - Selective Laser Melting KW - Residual Stresses PY - 2018 AN - OPUS4-45979 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Häusler, Ines A1 - Darvishi Kamachali, Reza A1 - Hetaba, W. A1 - Skrotzki, Birgit T1 - Thickening of T-1 Precipitates during Aging of a High Purity Al–4Cu–1Li–0.25Mn Alloy N2 - The age hardening response of a high-purity Al–4Cu–1Li–0.25Mn alloy (wt. %) during isothermal aging without and with an applied external load was investigated. Plate shaped nanometer size T1 (Al2CuLi) and θ′ (Al2Cu) hardening phases were formed. The precipitates were analyzed with respect to the development of their structure, size, number density, volume fraction and associated transformation strains by conducting transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) studies in combination with geometrical Phase analysis (GPA). Special attention was paid to the thickening of T1 phase. Two elementary types of single-layer T1 precipitate, one with a Li-rich (Type 1) and another with an Al-rich (Defect Type 1) central layer, were identified. The results show that the Defect Type 1 structure can act as a precursor for the Type 1 structure. The thickening of T1 precipitates occurs by alternative stacking of These two elementary structures. The thickening mechanism was analyzed based on the magnitude of strain associated with the precipitation transformation normal to its habit plane. Long-term aging and aging under load resulted in thicker and structurally defected T1 precipitates. Several types of defected precipitates were characterized and discussed. For θ′ precipitates, a ledge mechanism of thickening was observed. Compared to the normal aging, an external load applied to the peak aged state leads to small variations in the average sizes and volume fractions of the precipitates. KW - Al-Cu-Li-alloy KW - Precipitation KW - T1 precipitate KW - Microstructure evolution KW - Thickening KW - Creep KW - Volume fraction KW - Number density KW - Strain difference PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471207 DO - https://doi.org/10.3390/ma12010030 SN - 1996-1944 VL - 12 IS - 1 SP - 30, 1 EP - 23 PB - MDPI AN - OPUS4-47120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Donėlienė, J. A1 - Rudzikas, M. A1 - Rades, Steffi A1 - Dörfel, Ilona A1 - Peplinski, Burkhard A1 - Sahre, Mario A1 - Pellegrino, F. A1 - Maurino, V. A1 - Ulbikas, J. A1 - Galdikas, A. A1 - Hodoroaba, Vasile-Dan T1 - Morphology and structure of TixOy nanoparticles generated by femtosecond laser ablation in water N2 - In this work femto-second pulsed laser ablation in liquid (PLAL) procedure for the generation of titanium oxide nanoparticles (NP) is reported with the purpose of understanding morphology and structure of the newly generated NPs. Ablation duration was varied for optimization of NP generation processes between 10 and 90 min. Surface morphology of NPs as well as their size and shape (distribution) were analysed by various complementary electron microscopy techniques, i.e. SEM, TSEM and TEM. The crystalline structure of titanium oxide particles was investigated byXRD(two instruments operated in different geometries) and HR-TEM. Concentration of generated titanium oxide NPs in liquid was analysed by ICP-MS. A mix of crystalline (mainly anatase), partly crystalline and amorphous spherical titanium oxide NPs can be reported having a mean size between 10 and 20 nm, which is rather independent of the laser ablation (LA) duration. A second component consisting of irregularly shaped, but crystalline titanium oxide nanostructures is co-generated in the LA water, with more pronounced occurrence at longer LA times. The provenance of this component is assigned to those spherical particles generated in suspension and passing through the converging laser beam, being hence subject to secondary irradiation effects, e. g. fragmentation. KW - Titanium oxide KW - Nanoparticles KW - Laser ablation in liquid KW - Particle morphology KW - Nanoparticle structure PY - 2018 DO - https://doi.org/10.1088/2053-1591/aaba56 SN - 2053-1591 VL - 5 IS - 4 SP - 045015-1 EP - 045015-12 PB - IOP Publishing CY - London, UK AN - OPUS4-44678 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. A1 - Petrushin, N. A1 - Gerstein, G. A1 - Maier, J. A1 - Nolze, Gert T1 - Investigation of the gamma'-strengthened quaternary co-based alloys Co-Al-W-Ta N2 - The alloying system Co-Al-W-Ta is comprehensively investigated in the vicinity of the compositional point Co-9Al-10W-2Ta, at. pct. These investigations provided a large amount of quantitative information, which can be used for alloy development, namely, the compositional dependences of the The alloying system Co-Al-W-Ta is comprehensively investigated in the vicinity of the compositional point Co-9Al-10W-2Ta, at. pct. These investigations provided a large amount of quantitative information, which can be used for alloy development, namely, the compositional dependences of the γ‘-solvus, solidus, and liquidus temperatures; fraction of the extrinsic phases after casting; the compositional dependence of the γ/γ‘-lattice misfit; the element partitioning between γ- and γ‘-phases; and the two Phase compositional area γ/γ‘ in the Co-rich part of the Co-Al-W-Ta phase diagram at 900°C. It is shown that additions of Ta elevate the γ‘-solvus temperature and increase the γ/γ‘-lattice misfit, but adding more than about 3 at. pct Ta results in a large amount of undissolvable extrinsic phases. Additionally, two Co-Al-W-Ta alloys with lower content of W were developed and solidified as [001] single crystals for mechanical testing in a temperature range between 20 and 1200°C. These tests included measurement of the Young modulus, tensile tests with constant strain rate, and stress rupture tests. It was found that at temperatures up to about 750°C the ultimate tensile strength of Co-Al-Ta-W alloys can be at the same level or even higher than of Ni-based superalloys. KW - Cobald based alloy KW - Microstructur KW - Segregation PY - 2018 DO - https://doi.org/10.1007/s11661-018-4756-3 SN - 1543-1940 SN - 1073-5623 VL - 49A IS - 9 SP - 4042 EP - 4057 PB - Springer Sciences & Business Media CY - New York, NY AN - OPUS4-45395 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eh Hovsepian, P. A1 - Ehiasarian, A. P. A1 - Purandare, Y. P. A1 - Mayr, P. A1 - Abstoss, K. G. A1 - Mosquera Feijoo, Maria A1 - Schulz, Wencke A1 - Kranzmann, Axel A1 - Lasanta, M. I. A1 - Trujillo, J. P. T1 - Novel HIPIMS deposited nanostructured CrN/NbN coatings for environmental protection of steam turbine components N2 - To increase efficiency, modern steam plants are pushing their operational regime from super-critical (600 °C/300 bar) to ultra-super-critical (740/760 °C/350 bar) stretching existing turbine materials to their limits. The focus is on new generation functional materials and technologies which complement the inherent properties of existing materials. Current work proposes a novel High Power Impulse Magnetron Sputtering (HIPIMS) Deposition technology, for the first time, for deposition of a ceramic based CrN/NbN coating with a nanoscale multilayer structure (bi-layer thickness Δ = 1.9 nm) with superior adhesion (LC2 = 80 N) to protect low Chromium P92 steel widely used in steam power plants. Thermodynamic calculations predict the equilibrium phases and aggressive gaseous compounds generated by the interaction of steam with the coating. CrN/NbN coated P92 steel samples oxidised at 600 °C in a high pressure (50 bar) 100% steam atmosphere for up to 1000 h reveal the coating's superior oxidation resistance and protective mechanisms, especially against the detrimental effect of Hydrogen. High temperature (650 °C) Tensile Strength, Low Cycle Fatigue and Creep tests confirm that, unlike other state-of-the-art PVD technologies, HIPIMS is not detrimental to the mechanical properties of the substrate material. Water droplet erosion tests confirm no measurable weight loss after 2.4 X 10⁶ impacts. KW - Hipims KW - CrN/NbN KW - Nanoscale multilayers KW - Steam oxidation resistance KW - Water droplet erosion resistance PY - 2018 DO - https://doi.org/10.1016/j.jallcom.2018.02.312 SN - 0925-8388 SN - 1873-4669 VL - 746 SP - 583 EP - 593 PB - Elsevier AN - OPUS4-44800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nützmann, Kathrin A1 - Kranzmann, Axel A1 - Stephan-Scherb, Christiane T1 - The influence of chromium on early high temperature corrosion of ferritic alloys under SO₂ atmosphere N2 - Comprehensive insights into the early stages of corrosion mechanisms provide fundamental knowledge to further understand and model long time material behaviour. The present work studies the early stages of combined oxidation and sulphidation of ferritic model alloys for time scales up to 250 h at 650 °C to observe the influence of chromium during the corrosion under SO2. Model alloys were used to focus on the reaction of the intended elements: Fe, Cr, S, and O. Pure iron simultaneously forms magnetite and iron sulphide in an early stage of corrosion, covered by a pure oxide layer after 100 h. Iron with 13 wt% Cr shows hematite and mixed Fe-Cr-oxides first, before sulphides nucleate in the inner corrosion zone. With increasing ageing time a magnetite layer is observed below the hematite layer. Quantitative phase fractions of all corrosion products observed were determined from cross section images. Characterization of the Fe13Cr corrosion scale by FIB revealed a highly porous structure in the inner corrosion zone where Cr-rich (Fe, Cr)-sulphides are present, and caused the scale to spall easily. KW - Early stages KW - Sulphidation KW - High temperature corrosion PY - 2018 DO - https://doi.org/10.1080/09603409.2018.1446705 SN - 0960-3409 VL - 36 IS - 6 SP - 558 EP - 568 PB - Taylor & Francis AN - OPUS4-44707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dmitriev, A. I. A1 - Nikonov, A. Y. A1 - Österle, Werner T1 - Molecular dynamics modeling of the sliding performance of an amorphous silica nano-layer - The impact of chosen interatomic potentials N2 - The sliding behavior of an amorphous silica sample between two rigid surfaces is in the focus of the present paper. Molecular Dynamics using a classical Tersoff’s potential and a recently developed ReaxFF potential was applied for simulating sliding within a thin film corresponding to a tribofilm formed from silica nanoparticles. The simulations were performed at different temperatures corresponding to moderate and severe tribological stressing conditions. Simulations with both potentials revealed the need of considering different temperatures in order to obtain a sound interpretation of experimental findings. The results show the striking differences between the two potentials not only in terms of magnitude of the resistance stress (about one order of magnitude) but also in terms of friction mechanisms. The expected smooth sliding regime under high temperature conditions was predicted by both simulations, although with Tersoff’s potential smooth sliding was obtained only at the highest temperature. On the other hand, at room temperature Tersoff-style calculations demonstrate stick-slip behavior, which corresponds qualitatively with our experimental findings. Nevertheless, comparison with a macroscopic coefficient of friction is not possible because simulated resistance stresses do not depend on the applied normal pressure. KW - Molecular dynamics KW - Thin tribofilm KW - Resistance stress KW - Sliding simulation KW - Amorphous silica PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-449366 DO - https://doi.org/10.3390/lubricants6020043 SN - 2075-4442 VL - 6 IS - 2 SP - 43, 1 EP - 11 PB - MDPI CY - Basel AN - OPUS4-44936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nofz, Marianne A1 - Dörfel, Ilona A1 - Sojref, Regine A1 - Wollschläger, Nicole A1 - Mosquera Feijoo, Maria A1 - Schulz, Wencke A1 - Kranzmann, Axel T1 - Thin Sol-Gel Alumina Coating as Protection of a 9% Cr Steel Against Flue Gas Corrosion at 650 °C N2 - Samples of sol-gel alumina coated and uncoated P92 steel were exposed to flue gas at 650 °C for 300 h. As result of this treatment a 50 µm thick bi-layered oxide scale had formed on the surface of the uncoated sample. Below the scale a 40 µm thick inner oxidation zone was detected. In contrast, the porous, micron thick alumina coating enabled the formation of a chromium oxide scale with a thickness of some nanometers at the interface between steel substrate and coating. In this case high temperature corrosion of the steel was prevented so far. KW - Steel KW - Oxide coatings KW - High-temperature corrosion KW - TEM KW - SEM PY - 2018 DO - https://doi.org/10.1007/s11085-017-9799-0 SN - 0030-770X SN - 1573-4889 VL - 89 IS - 3-4 SP - 453 EP - 470 PB - Springer AN - OPUS4-44472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böllinghaus, Thomas A1 - Lüders, V. A1 - Nolze, Gert T1 - Microstructural insights into natural silver wires N2 - Due to the increasing global demand for pure silver, native wire silver aggregates in very high purities are gaining more industrial attention. Up to the present, no substantial metallurgical Investigation of natural wire silver exists in the accessible literature. To convey urgently needed cross-disciplinary fundamental knowledge for geoscientists and metallurgical engineers, twenty natural wire silver specimens from eight different ore deposits have been investigated in detail for the first time by EBSD (Electron Back Scattering Diffraction), supported by light microscopy and micro-probe analyses. The improved understanding of the natural silver wire microstructure provides additional Information regarding the growth of natural silver aggregates in comparison to undesired artificial growth on electronic devices. Clear evidence is provided that natural silver curls and hairs exhibit a polycrystalline face-centered cubic microstructure associated with significant twinning. Although the investigated natural wire silver samples have relatively high purity (Ag > 99.7 wt.-%), they contain a variety of trace elements such as, S, Cu, Mn, Ni, Zn, Co and Bi, As and Sb. Additionally, Vickers micro-hardness measurements are provided for the first time which revealed that natural silver wires and curls are softer than it might be expected from conversion of the general Mohs hardness of 2.7. KW - Natural silver wires PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-451655 UR - http://www.nature.com/articles/s41598-018-27159-w DO - https://doi.org/10.1038/s41598-018-27159-w SN - 2045-2322 VL - 8 IS - 1 SP - Article 9053, 1 EP - 9 PB - nature publishing group CY - London, United Kingdom AN - OPUS4-45165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. A1 - Chyrkin, A. A1 - Nolze, Gert A1 - Midtlyng, Jan A1 - Mayer, H. M. A1 - Petrushin, N. A1 - Reimers, W. T1 - Interdiffusion in the Face-Centered Cubic Phase of the Co-Al-W-Ta System Between 1090 and 1240 °C N2 - Interdiffusion of Al, W, Ta and Co in a Co-base alloy at temperatures between 1090 and 1240 °C has been investigated. The interdiffusion coefficients were found to be close to those reported for these elements in Ni-base alloys. Combining the diffusion simulation software DICTRA with the Ni-base diffusion databases TCNi5 and MobNi3, the interdiffusion profiles of Co, Al W, and Ta were modeled for Co9Al8W2Ta/Co diffusion couples annealed at different temperatures and for different times. The results show that interdiffusion in the Co-Al-W-Ta alloys can be modeled reasonably well using the available commercial databases for thermodynamics and kinetics of Ni-base systems. KW - Alloys KW - Interdiffusion KW - Modeling PY - 2018 DO - https://doi.org/10.1007/s11669-018-0620-9 VL - 39 IS - 2 SP - 176 EP - 185 PB - Springer AN - OPUS4-44463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wollschläger, Nicole A1 - Nofz, Marianne A1 - Dörfel, Ilona A1 - Schulz, Wencke A1 - Sojref, Regine A1 - Kranzmann, Axel T1 - Exposition of sol-gel alumina-coated P92 steel to flue gas: Time-resolved microstructure evolution, defect tolerance, and repairing of the coating N2 - Technically relevant P92 steel (9% Cr) was coated with a micron-thick porous alumina layer prepared by sol-gel technique and treated with flue gas (60 CO2-30 H2O-2 O2-1 SO2-7 N2 (mole fraction in %)) at 650 ° to mimic an oxyfuelcombustion process. Local defects in the coating were marked using focused ion beam (FIB) technique and were inspected after exposition to hot flue gas atmosphere at 300, 800, and 1300 h, respectively. Local defects like agglomerated alumina sol particles tend to spall off from the coating uncovering the underlying dense chromia scale. Re-coating was found to restore the protection ability from oxidation when repeatedly treated with hot flue gas. Cracks and voids did not promote the local oxidation due to the formation of crystalline Mn/S/O species within and on top of the coating. The protective character of the steel-coating system is a result of (i) the fast formation of a dense chromia scale at the surface of sol-gel alumina-coated P92 steel bars in combination with (ii) the porous alumina coating acting as diffusion barrier, but also as diffusion partner in addition with (iii) fast Mn outward diffusion capturing the S species from flue gas. KW - Alumina coatings KW - Oxyfuel KW - Steel P92 KW - High temperature corrosion PY - 2018 DO - https://doi.org/10.1002/maco.201709712 SN - 1521-4176 SN - 0947-5117 SN - 0043-2822 VL - 69 IS - 4 SP - 492 EP - 502 PB - Wiley-VCH Verlag GmbH&Co. KGaA CY - Weinheim AN - OPUS4-45300 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nützmann, Kathrin A1 - Wollschläger, Nicole A1 - Rockenhäuser, Christian A1 - Kranzmann, Axel A1 - Stephan-Scherb, Christiane T1 - Identification and 3D reconstruction of Cr5S6 precipitates along grain boundaries in Fe13Cr N2 - Metal sulfide grain boundary precipitates of a ferrous model alloy with 13 wt.% chromium formed at 650°C under a gas atmosphere containing 0.5% SO2 and 99.5% Ar were investigated after ageing for 3 h, 6 h, and 12 h. The precipitates formed along grain boundaries were identified as Cr5S6 using energy-dispersive x-ray spectroscopy in transmission electron microscopy and electron backscatter diffraction analysis. Serial focused ion beam slicing was conducted followed by three-dimensional reconstruction to determine the number, size, and penetration depth of the precipitates evolved at the different time steps. There was a linear increase in the number of precipitates with time, while their average size increased only for the initial aging time but became constant after 6 h. Based on these results, a model for grain boundary sulfidation of ferritic alloys is discussed. KW - Internal Sulfidation KW - Grain Boundary Corrosion KW - FIB Tomography PY - 2018 DO - https://doi.org/10.1007/s11837-018-2940-y SN - 1047-4838 SN - 1543-1851 VL - 70 IS - 8 SP - 1478 EP - 1483 PB - Springer Science + Business Media CY - New York, NY AN - OPUS4-45090 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Kratzig, Andreas A1 - Bettge, Dirk A1 - Kranzmann, Axel A1 - Knauer, S. T1 - Droplet corrosion of CO2 transport pipeline steels N2 - In this work, the focus was set on the corrosion process of condensate as drops on the surface of carbon steels (X52, X70), martensitic steel UNS S41500, and superaustenite UNS N08031 in CO2 atmosphere with impurities at 278 K (to simulate the transportation condition in a buried pipeline). Exposure tests were performed at both normal pressure and high pressure where CO2 is supercritical or in dense phase. The drop, 1 ‑ 10 μL in volume, was prepared by dropping CO2 saturated ultra-pure water onto the surface of steel coupons in a one-liter-autoclave. The CO2 gas stream, simulating the oxyfuel flue gas with varying concentration of impurities (SO2 and O2 ), was then pumped into the autoclave to observe the condensation and corrosion impacts of impurities. Comparable exposure tests were carried out with the same gas mixture and the same volume of water as vapor to observe the drop formation and the corrosion process that follows. The wettability and stability of drops on the surface of steel coupons in CO2 supercritical/dense phase environment was evaluated additionally by contact angle measurement. T2 - NACE International Annual Corrosion Conference CY - Phoenix, AZ, USA DA - 15.04.2018 KW - Geothermal KW - Coating KW - SiO2 KW - Polyaniline KW - Corrosion PY - 2018 SP - 10845, 1 EP - 11 PB - Omnipress CY - Houston AN - OPUS4-44917 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pfennig, A. A1 - Wolf, M. A1 - Kranzmann, Axel T1 - In-situ testing of corrosion and corrosion fatigue behavior of stainless steels in geothermal environment N2 - In CCS environment (carbon capture and storage) pipes are loaded statically and/or cyclically and at the same time exposed constantly to the highly corrosive hot thermal water. Experimental procedures such as ambient pressure immersions tests, in-situ corrosion fatigue experiments using a flexibly designed corrosion chamber at ambient pressure and a specially designed corrosion chamber at high pressure. Experimental set-ups for push/pull and rotation bending load are introduced. The corrosion behavior and lifetime reduction of high alloyed steels (X46Cr13, 1.4043), (X5CrNiCuNb16-4, 1.4542) and (X2CrNiMoN22-5-3, 1.4462) is demonstrated (T=60 °C, geothermal brine: Stuttgart Aquifer flow rate: 9 l/h, CO2 ). T2 - 10th International Conference on Chemical, Biological and Environmental Engineering ICBEE 2018 CY - Berlin, Germany DA - 27.09.2018 KW - Adiabatic calorimeter KW - Thermal energy storage KW - Phase change material KW - Salt eutectics PY - 2018 DO - https://doi.org/10.7763/IPCBEE.2018.V103.5 VL - 103 SP - 13 EP - 20 AN - OPUS4-50364 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pfennig, A. A1 - Simkin, Roman A1 - Kranzmann, Axel T1 - Construction of an adiabatic calorimeter for investigation of high tempertarue salt - based phase change material N2 - The commercial usage of latent thermal energy storages primarily depends on the development of a suitable phase change material (PCM). For industrial high temperature applications above 400 °C multicomponent chloride eutectics are promising and therefore discussed seriously. The profound thermodynamic investigation of such eutectics requires a much greater amount of specimen material than conventional calorimeter can handle. Therefore, a special adiabatic calorimeter was developed and designed. With a specimen mass of > 100 g the typical thermodynamic measurements with a commercial calorimeter can be extended by cycle stability measurements, which are often decisive for practical application of PCM. Furthermore, by implementing corrosion specimens inside the calorimeter high temperature corrosion experiments according to ISO 21608 can be performed inside the calorimeter. Adiabatic measuring conditions can be provided by using two separate heating systems. Therefore, the outer “protective system” follows the temperature curve of the inner “measuring system” minimizing the temperature difference between the heating systems and simultaneously preventing heat losses from the measuring systems. T2 - 10th International Conference on Chemical, Biological and Environmental Engineering ICBEE 2018 CY - Berlin, Germany DA - 27.09.2018 KW - Adiabatic calorimeter KW - Thermal energy storage KW - Phase change material KW - Salt eutectics PY - 2018 DO - https://doi.org/10.7763/IPCBEE.2018.V103.6 VL - 103 SP - 21 EP - 28 AN - OPUS4-50363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koclega, Damian A1 - Radziszewska, A. A1 - Kranzmann, Axel A1 - Marynowski, P. A1 - Wozny, K. T1 - Morphology and chemical composition of inconel 686 after high-temperature corrosion N2 - The work presents the microstructure, chemical composition and mechanical properties of Inconel 686 coatings after high - temperature corrosion in environment of aggressive gases and ashes. To produce the Ni - based coatings the QS Nd:YAG laser cladding process was carried out. As the substrate used 13CrMo4-5 boilers plate steel. Ni - base alloys characterize the excellent high-temperature corrosion resistance, good strength and ability to work in aggressive environments. Formed clad were characterized by high quality of metallurgical bonding with the substrate material and sufficiently low amount of the iron close to the clad layer surface. After corrosion experiment the oxide scale on the substrate and clad created. The scale on 13CrMo4-5 steel had 70 μm thickness while the scale of the clad had less than 10 μm. The microstructure, chemical composition of the obtained clad and scales were investigated by scanning electron microscope (SEM) and electron probe microanalyzer (EPMA) equipped with the EDS detectors. T2 - 27th International conference on metallurgy and materials CY - Brno, Czech Republic DA - 23.05.2018 KW - laser cladding KW - Inconel 686 KW - High - temperature corrosion KW - Aggressive environment KW - Oxide scale PY - 2018 SP - 1010 EP - 1016 AN - OPUS4-49660 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Peetz, Christoph A1 - Buggisch, Enrico A1 - Bettge, Dirk A1 - Kranzmann, Axel T1 - Electrochemical study on wellbore constellations for CO2 injection N2 - Carbon Capture and Storage (CCS) is identified as an excellent technology to reach the target of CO2 reduction. However, the safety issue and cost effectiveness hinder the future of CCS. For the reliability and safety issues of injection wells the corrosion resistance of the materials used needs to be determined. In this study, representative low cost materials including carbon steel 1.8977 and low alloyed steel 1.7225 were embedded in cement to mimic the realistic casing-cement interface. Electrochemical studies were carried out using these metal-cement specimens in comparison with those made of metal only in CO2 saturated synthetic aquifer fluid, at 333 K, to reveal the effect of cement on the steel performance. The results showed the protective effect of cement on the performance of pipeline metals during polarisation process. However, the corrosion current density was high in all cases, with and without cement, indicating that the corrosion resistance of these materials is low. This conclusion was supported by the surface analysis of the polarized specimens, which revealed both homogenous and pitting corrosions. T2 - EUROCORR 2018 CY - Krakow, Poland DA - 09.09.2018 KW - CCUS KW - Supercritical/dense phase CO2 KW - Carbon steels KW - Martensitic steel KW - Superaustenite steel KW - Injection KW - Impurities PY - 2018 SP - 1 EP - 4 PB - EFC CY - Krakau, Poland AN - OPUS4-46291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pfennig, Anja A1 - Kranzmann, Axel T1 - Impact of saline aquifer water on surface and shallow pit corrosion of martensitic stainless steels during exposure to CO2 environment (CCS) N2 - Pipe steels suitable for carbon capture and storage technology (CCS) require resistance against the corrosive environment of a potential CCS-site, e.g. heat, pressure, salinity of the aquifer, CO2-partial pressure. Samples of different mild and high alloyed stainless injection-pipe steels partially heat treated: 42CrMo4, X20Cr13, X46Cr13, X35CrMo4 as well as X5CrNiCuNb16-4 were kept at T=60 °C and ambient pressure as well as p=100 bar for 700 h - 8000 h in a CO2-saturated synthetic aquifer environment similar to possible geological on-shore CCS-sites in the northern German Basin. Main corrosion products are FeCO3 and FeOOH. Corrosion rates obtained at 100 bar are generally much lower than those measured at ambient pressure. Highest surface corrosion rates are 0.8 mm/year for 42CrMo4 and lowest 0.01 mm/year for X5CrNiCuNb16-4 in the vapour phase at ambient pressure. At 100 bar the highest corrosion rates are 0.01 mm/year for 42CrMo4, X20Cr13 (liquid phase), X46Cr13 and less than 0.01 mm/year for X35CrMo4 and X5CrNiCuNb16-4 after 8000 h of exposure with no regard to atmosphere. Martensitic microstructure offers good corrosion resistance. T2 - 8th International Conference on Future Environment and Energy (ICFEE 2018) CY - Phuket, Thailand DA - 10.01.2018 KW - CCS KW - CO2 corrosion KW - Pipeline PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-465896 DO - https://doi.org/10.1088/1755-1315/150/1/012012 VL - 150 SP - 81 EP - 90 PB - IOP Publ. AN - OPUS4-46589 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Olbricht, Jürgen A1 - Agudo Jácome, Leonardo A1 - Jürgens, Maria A1 - Roohbakhshan, Farshad A1 - Fedelich, Bernard A1 - Skrotzki, Birgit T1 - Cyclic loading performance and related microstructure evolution of ferritic-martensitic 9-12% Cr steels N2 - The current competitive situation on electricity markets forces power plants into cyclic operation regimes with frequent load shifts and starts/shutdowns. In the present work, the cyclic mechanical behavior of ferritic-martensitic 9-12 % Cr steels under isothermal and thermomechanical loading was investigated for the example of grade P92 material. A continuous softening was observed under all loading conditions. The introduction of hold periods to the applied cycles reduced material lifetime, with most prominent effects at technologically relevant small strain levels. The microstructural characterization reveals a coarsening of the original “martensitic” lath-type microstructure to a structure with polygonal subgrains and reduced dislocation density. The microstructural data forms the input for a physically-based modelling approach. T2 - 44th MPA-Seminar CY - Leinfelden/Stuttgart, Germany DA - 17.10.2018 KW - Ferritic-martensitic steels KW - Cyclic loading KW - Microstructure evolution PY - 2018 SP - 259 EP - 265 AN - OPUS4-47118 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koclega, Damian A1 - Radziszewska, A. A1 - Kranzmann, Axel T1 - The influence of the aggressive environments on the Inconel 686 coating in high-temperature corrosion experiments N2 - This work presents the microstructure and chemical composition of oxide scales created on Ni – base coating after corrosion experiments in aggressive gases and ashes. The Inconel 686 coating applied on the low carbon steel 13CrMo4-5 was performed by a CO2 laser cladding process. The experiments were carried out in oxidizing gas atmospheres containing O2, COx, SOx. The second Variation of corrosion experiments were performed in a reducing atmosphere with ashes containing elements such as: Na, Cl, Ca, Si, C, Fe, Al etc. After 240 h and 1.000 h corrosion experiments the oxide scales on the substrate and overlay were created in both cases. The sulfur compounds were found on the top of the coating surface (EPMA) and also higher contents of silica compounds were revealed on specimens covered by ashes during the experiments. The microstructure and chemical composition of the clad and scales were investigated by means of a light microscope and an electron microscope (SEM)equipped with an EDS detector. T2 - 50. Kraftwerkstechnisches Kolloquium CY - Dresden, Germany DA - 23.10.2018 KW - Nickel based coatings KW - Inconel 686 KW - High temperature corrosion PY - 2018 SP - 599 AN - OPUS4-46590 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koclega, Damian A1 - Petrzak, P. A1 - Kowalski, K. A1 - Rozmus-Gornikowska, M. A1 - Debowska, A. A1 - Jedrusik, M. T1 - Annealing effect on microstructure and chemical composition of Inconel 625 alloy N2 - Our research focused on Inconel 625 weld overlays on 16Mo3 steel boiler pipes. The Investigation focused on the characterization of changes in the microstructure and chemical composition after annealing. The annealing was performed for ten hours at temperatures from 600 to 1000°C. Changes in the microstructure were observed with a scanning and transmission electron microscope (SEM and TEM). The investigation was supplemented by hardness measurements. KW - Inconel 625 KW - Microsegregation KW - Annealing PY - 2018 DO - https://doi.org/10.7494/mafe.2018.44.2.73 SN - 1230-2325 SN - 0860-6307 SN - 2300-8377 VL - 44 IS - 2 SP - 73 EP - 80 PB - AGH University of Science and Technology Press CY - Cracow AN - OPUS4-49659 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stegemann, Robert A1 - Cabeza, Sandra A1 - Pelkner, Matthias A1 - Lyamkin, Viktor A1 - Pittner, Andreas A1 - Werner, Daniel A1 - Wimpory, R. A1 - Boin, M. A1 - Kreutzbruck, Marc A1 - Bruno, Giovanni T1 - Influence of the microstructure on magnetic stray fields of low-carbon steel welds N2 - This study examines the relationship between the magnetic mesostructure with the microstructure of low carbon steel tungsten inert gas welds. Optical microscopy revealed variation in the microstructure of the parent material, in the heat affected and fusion zones, correlating with distinctive changes in the local magnetic stray fields measured with high spatial resolution giant magneto resistance sensors. In the vicinity of the heat affected zone high residual stresses were found using neutron diffraction. Notably, the gradients of von Mises stress and triaxial magnetic stray field modulus follow the same tendency transverse to the weld. In contrast, micro-X-ray fluorescence characterization indicated that local changes in element composition had no independent effect on magnetic stray fields. KW - TIG-welding KW - GMR sensors KW - Magnetic stray field KW - Neutron diffraction KW - Residual stress KW - Microstructure KW - Low carbon steel PY - 2018 DO - https://doi.org/10.1007/s10921-018-0522-0 SN - 0195-9298 SN - 1573-4862 VL - 37 IS - 3 SP - 66,1 EP - 18 PB - Springer US CY - New York AN - OPUS4-45855 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eggeler, G. A1 - Wieczorek, N. A1 - Fox, F. A1 - Berglund, S. A1 - Bürger, D. A1 - Dlouhý, A. A1 - Wollgramm, P. A1 - Neuking, K. A1 - Schreuer, J. A1 - Agudo Jácome, Leonardo A1 - Gao, S. A1 - Hartmaier, A. A1 - Laplanche, G. T1 - On shear testing of single crystal Ni-base superalloys N2 - Shear testing can contribute to a better understanding of the plastic deformation of Ni-base superalloy single crystals. In the present study, shear testing is discussed with special emphasis placed on its strengths and weaknesses. Key mechanical and microstructural results which were obtained for the high-temperature (T ≈ 1000 °C) and low-stress (τ ≈ 200 MPa) creep regime are briefly reviewed. New 3D stereo STEM images of dislocation substructures which form during shear creep deformation in this regime are presented. It is then shown which new aspects need to be considered when performing double shear creep testing at lower temperatures (T < 800 °C) and higher stresses (τ > 600 MPa). In this creep regime, the macroscopic crystallographic [11−2](111) shear system deforms significantly faster than the [01−1](111) system. This represents direct mechanical evidence for a new planar fault nucleation scenario, which was recently suggested (Wu et al. in Acta Mater 144:642–655, 2018). The double shear creep specimen geometry inspired a micro-mechanical in-situ shear test specimen. Moreover, the in-situ SEM shear specimen can be FIB micro-machined from prior dendritic and interdendritic regions. Dendritic regions, which have a lower γ′ volume fraction, show a lower critical resolved shear stress. T2 - EuroSuperalloys 2018 CY - Oxford, UK DA - 09.09.2018 KW - Superalloy single crystals KW - Shear testing KW - Creep mechanisms KW - In-situ SEM micro shear deformation KW - Transmission electron microscopy PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-456591 DO - https://doi.org/10.1007/s11661-018-4726-9 SN - 1073-5623 SN - 1543-1940 VL - 49A IS - 9 SP - 3951 EP - 3962 PB - Springer US CY - New York AN - OPUS4-45659 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winkelmann, A. A1 - Nolze, Gert A1 - Cios, G. A1 - Tokarski, T. T1 - Mapping of local lattice parameter ratios by projective Kikuchi pattern matching N2 - We describe a lattice-based crystallographic approximation for the analysis of distorted crystal structures via Electron Backscatter Diffraction (EBSD) in the scanning electron microscope. EBSD patterns are closely linked to local lattice parameter ratios via Kikuchi bands that indicate geometrical lattice plane projections. Based on the transformation properties of points and lines in the real projective plane, we can obtain continuous estimations of the local lattice distortion based on projectively transformed Kikuchi diffraction simulations for a reference structure. By quantitative image matching to a projective transformation model of the lattice distortion in the full solid angle of possible scattering directions, we enforce a crystallographically consistent approximation in the fitting procedure of distorted simulations to the experimentally observed diffraction patterns. As an application example, we map the locally varying tetragonality in martensite grains of steel. KW - EBSD KW - Scanning electron microscopy KW - Orientation refinement PY - 2018 DO - https://doi.org/10.1103/PhysRevMaterials.2.123803 SN - 2475-9953 VL - 2 IS - 12 SP - 123803, 1 EP - 15 PB - American Physical Society CY - College Park, MD AN - OPUS4-47296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, Anja A1 - Kranzmann, Axel T1 - Local Corrosion of Martensitic Stainless Steels during Exposure to Saline Aquifer Water and CO2 Environment N2 - Carbon Capture and Storage (CCS) is well acknowledged to mitigate climate change. Therefore, pipe Steels suitable for CCS technology require resistance against the corrosive environment of a potential CCS-site, e.g. heat, pressure, salinity of the aquifer, CO2-partial pressure. Samples of different mild and high alloyed stainless injection-pipe Steels partially heat treated: 42CrMo4, X20Cr13, X46Cr13, X35CrMo4 as well as X5CrNiCuNb16-4 were kept at T=60 °C and ambient pressure as well as p=100 bar for 700 h - 8000 h in a CO2-saturated synthetic aquifer environment similar to possible geological on-shore CCS-sites in the northern German Basin. Main corrosion products analysed on pits are FeCO3 and FeOOH. The carbon content does not show significant influence on the pitting behaviour. Generally, higher chromium Content results in better corrosion resistance. Although X35CrMo17-1 and X5CrNiCuNb16-4 show low surface corrosion rates, their resistance against local corrosion in CCS environment is not significantly better compared to the much less costly Steels X20Cr13 and X46Cr13. KW - Corrosion KW - CCS KW - Carbon storage KW - Aquifer KW - Heat treatment PY - 2018 DO - https://doi.org/10.18178/ijcea.2018.9.1.694 SN - 2010-0221 VL - 9 SP - 26 EP - 31 PB - International Association of Computer Science and Information Technology Press CY - Singapore AN - OPUS4-46627 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mujica Roncery, L. A1 - Agudo Jácome, Leonardo A1 - Aghajani, A. A1 - Theisen, W. A1 - Weber, S. T1 - Subsurface characterization of high-strength high-interstitial austenitic steels after impact wear N2 - The microstructure of the subsurface after impact wear of three high-strength high interstitial austenitic steels has been analysed using transmission electron microscopy (TEM) in alloys with C and N as interstitial elements. In all cases, a nanocrystalline region followed by a transition zone and a cold-worked area are present. Additionally, microhardness and nano-scratching tests were conducted to study the wear-related properties of the impact subsurface and the base material. The results of the microstructural analysis reveal that the following mechanisms are involved during impact wear: abrasion (ploughing), microcrack formation associated with contact fatigue, entrapment and adhesion of SiO2 particles. The analysis of the wear-related properties indicates that the subsurface acts as a self-protective layer that prevents the deterioration of the substrate. KW - Impact wear KW - TEM KW - Nano-scratch test KW - High interstitial austenitic steel PY - 2018 DO - https://doi.org/10.1016/j.wear.2018.02.016 SN - 0043-1648 VL - 402-403 SP - 137 EP - 147 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-44290 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stephan-Scherb, Christiane A1 - Nützmann, Kathrin A1 - Kranzmann, Axel A1 - Klaus, M. A1 - Genzel, C. T1 - Real time observation of high temperature oxidation and sulfidation of Fe-Cr model alloys N2 - Insights into early damage mechanisms during high-temperature gas corrosion provide important aspects for the prediction of the long-term stability of hightemperature materials exposed to a hot and corrosive environment. The current work presents a real time study concerning the combined oxidation and sulfidation of ferritic model alloys in a hot SO2 containing atmosphere using energy dispersive X-ray diffraction. The applied high temperature reactor allows the transmittance of high energetic X-rays in order to collect X-ray diffraction pattern of the sample surface in situ during the reaction with the reactive environment. The results revealed that the first phases crystallizing on iron with 2 wt% chromium and with 9 wt% chromium are oxides. The aging experiments at T = 650° C with 0.5% SO2 and 99.5% Ar were followed in situ and caused an external mixed oxide-sulfide layer on top of iron with 2 wt% chromium. On the higher alloyed material the external scale consists of iron oxides and the inner scale of mixed (Fe,Cr)-oxides and chromium-sulfides. The oxide content continuously increases parallel to an increase of the sulfide amount. Thus, the initially formed (Fe,Cr)-oxides do not have a protective character and support the transport of sulfur through the growing oxide scale. KW - High temperature corrosion KW - In situ diffraction KW - Sulfidation PY - 2018 DO - https://doi.org/10.1002/maco.201709892 SN - 0947-5117 VL - 69 IS - 6 SP - 678 EP - 689 PB - Wiley VCH Verlag AN - OPUS4-44776 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Agudo Jácome, Leonardo A1 - Pöthkow, K. A1 - Paetsch, O. A1 - Hege, H.-C. T1 - Three-dimensional reconstruction and quantification of dislocation substructures from transmission electron microscopy stereo pairs N2 - A great amount of material properties is strongly influenced by dislocations, the carriers of plastic deformation. It is therefore paramount to have appropriate tools to quantify dislocation substructures with regard to their features, e.g., dislocation density, Burgers vectors or line direction. While the transmission electron microscope (TEM) has been the most widely-used equipment implemented to investigate dislocations, it usually is limited to the two-dimensional (2D) observation of three-dimensional (3D) structures. We reconstruct, visualize and quantify 3D dislocation substructure models from only two TEM images (stereo pairs) and assess the results. The reconstruction is based on the manual interactive tracing of filiform objects on both images of the stereo pair. The reconstruction and quantification method are demonstrated on dark field (DF) scanning (S)TEM micrographs of dislocation substructures imaged under diffraction contrast conditions. For this purpose, thick regions (> 300 nm) of TEM foils are analyzed, which are extracted from a Ni-base superalloy single crystal after high temperature creep deformation. It is shown how the method allows 3D quantification from stereo pairs in a wide range of tilt conditions, achieving line length and orientation uncertainties of 3% and 7°, respectively. Parameters that affect the quality of such reconstructions are discussed. KW - Dislocation KW - Diffraction contrast KW - Scanning transmission electron microscopy (STEM) KW - Stereoscopy KW - Visualization PY - 2018 DO - https://doi.org/10.1016/j.ultramic.2018.08.015 SN - 0304-3991 VL - 195 SP - 157 EP - 170 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-46355 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Jürgens, Maria A1 - Olbricht, Jürgen A1 - Winkelmann, Aimo T1 - Improving the precision of orientation measurements from technical materials via EBSD pattern matching N2 - We use pattern matching of experimental and dynamically simulated backscattered Kikuchi diffraction (BKD) patterns to increase the orientation precision of electron backscatter diffraction (EBSD) measurements. In order to quantify the improvement in orientation precision, we analyze the experimental distribution of the kernel average misorientation (KAM) angles. We find that for the same raw data, i.e. the same EBSD data acquisition time budget, the pattern matching approach improves the KAM resolution by an order of magnitude compared to orientation data delivered from the conventional Hough-transform based data analysis. This quantitative improvement enables us to interpret small orientation changes in plastically deformed materials which are hidden in noisy orientation data delivered from the reference EBSD system. As an application example, we analyze a ferritic-martensitic steel (P92) sample before and after low-cycle fatigue (LCF) loading (±0.3% strain) at 620 °C. Whereas the low precision of the EBSD orientation data from the manufacturer software does not allow a reliable discrimination of the gradually changing microstructure, we find very clear systematic differences of the local microstructure after the pattern matching orientation refinement of the initial, raw pattern data. For the investigated P92 sample, the KAM-angle histograms are well described by two log-normal distributions indicating the already tempered and the remaining and mostly untempered martensite. KW - Misorientation KW - Thermo-mechanical loading KW - Martensite KW - Log-normal distribution KW - Bimodal distribution PY - 2018 DO - https://doi.org/10.1016/j.actamat.2018.08.028 VL - 159 SP - 408 EP - 415 PB - Elsevier Ltd. AN - OPUS4-46454 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Han, M. A1 - Chen, C. A1 - Zhao, G. A1 - Li, L. A1 - Yo, B. A1 - Huang, X. A1 - Zhu, Y. T1 - Blind lattice-parameter determination of cubic and tetragonal phases with high accuracy using a single EBSD pattern N2 - The Bravais lattices and their lattice parameters are blindly determined using electron backscatter diffraction (EBSD) patterns of materials with cubic or tetragonal crystal structures. Since the geometric relationships in a single EBSD pattern are overdetermined, the relative errors of determining the lattice parameters as well as the axial ratios are confined to about 0.7 ± 0.4% and 0.07 ± 0.03%, respectively, for ideal simulated EBSD patterns. The accuracy of the crystal orientation determination reaches about 0.06 ± 0.03°. With careful manual band detection, the accuracy of determining lattice parameters from experimental patterns can be as good as from simulated patterns, although the results from simulated patterns are often better than expermental patterns, which are lower quality and contain uncertain systematic errors. The reasonably high accuracy is obtained primarily because the detection of the diffracting-plane traces and zone axes is relatively accurate. The results here demonstrate that the developed procedure based on the EBSD technique presents a reliable tool for crystallographic characterization of the Bravais lattices of unknown phases. KW - EBSD KW - Bravais lattice KW - Lattice parameters KW - Kikuchi pattern PY - 2018 DO - https://doi.org/10.1107/S2053273318010963 SN - 2053-2733 VL - 74 IS - 6 SP - 630 EP - 639 PB - International Union of Crystallography AN - OPUS4-46455 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Donėlienė, J. A1 - Rudzikas, M. A1 - Rades, Steffi A1 - Dörfel, Ilona A1 - Peplinski, Burkhard A1 - Sahre, Mario A1 - Pellegrino, F. A1 - Maurino, V. A1 - Ulbikas, J. A1 - Galdikas, A. A1 - Hodoroaba, Vasile-Dan T1 - Electron Microscopy and X-Ray Diffraction Analysis of Titanium Oxide Nanoparticles Synthesized by Pulsed Laser Ablation in Liquid N2 - A femto-second pulsed laser ablation in liquid (PLAL) procedure for the generation of titanium oxide nanoparticles (NP) is reported with the purpose of understanding morphology and structure of the newly generated NPs. Ablation duration was varied for optimization of NP generation processes between 10 and 90 min. Surface morphology of NPs as well as their size and shape (distribution) were analysed by various complementary electron microscopy techniques, i.e. SEM, TSEM and TEM. The crystalline structure of titanium oxide particles was investigated by XRD(two instruments operated in different geometries) and HR-TEM. Concentration of generated titanium oxide NPs in liquid was analysed by ICP-MS. A mix of crystalline (mainly anatase), partly crystalline and amorphous spherical titanium oxide NPs can be reported having a mean size between 10 and 20 nm, which is rather independent of the laser ablation (LA) duration. A second component consisting of irregularly shaped, but crystalline titanium oxide nanostructures is co-generated in the LA water, with more pronounced occurrence at longer LA times. The provenance of this component is assigned to those spherical particles generated in suspension and passing through the converging laser beam, being hence subject to secondary irradiation effects, e. g. fragmentation. KW - Laser ablation in liquid KW - Nanoparticles KW - Titanium oxide KW - Particle morphology PY - 2018 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/electron-microscopy-and-xray-diffraction-analysis-of-titanium-oxide-nanoparticles-synthesized-by-pulsed-laser-ablation-in-liquid/AE368446FAC70E08C514F9AEABFD131B DO - https://doi.org/10.1017/S1431927618009030 VL - 24 IS - S1 (August) SP - 1710 EP - 1711 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-45949 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reith, F. A1 - Rea, M.A.D. A1 - Sawley, P. A1 - Zammit, C.M. A1 - Nolze, Gert A1 - Reith, T. A1 - Rantanen, K. A1 - Bissett, A. T1 - Biogeochemical cycling of gold: Transforming gold particles from arctic Finland N2 - (Bio)geochemical cycling of gold (Au) has been demonstrated in present-day (semi)-arid, (sub)-tropical and temperate environment. Hereby biofilms on Au-bearing mineral- and Au-particle surfaces drive Au dispersion and reconcentration, thereby (trans)forming the particles. However, it is unknown if biogeochemical cycling of Au occurs in polar environments, where air temperatures can reach −40 °C and soils remain frozen for much of the year. Therefore, placer Au-particles, soils and waters were collected at two placer mining districts in arctic Finland, i.e., the Ivalojoki and Lemmenjoki goldfields. Sites were chosen based on contrasting settings ((glacio)-fluvial vs. glacial-till deposits) and depths (surface to 5m below current surface). Gold particles were studied using a combination of tagged 16S rRNA gene next generation sequencing and electron microscopic/microanalytical techniques. Across all sites a range of Au-particle morphologies were observed, including morphotypes indicative of Au dissolution and aggregation. Elevated Au concentrations indicative of Au mobility were detected in placer particle bearing soils at both districts. Typically Au-particles were coated by polymorphic biofilm layers composed of living and dead cells embedded in extracellular polymeric substances. Intermixed were biominerals, clays and iron-sulfides/oxides and abundant secondary Au morphotypes, i.e., nano-particles, microcrystals, sheet-like Au, branched Au networks and overgrowths and secondary rims. Biofilms communities were composed of Acidobacteria (18.3%), Bacteroidetes (15.1%) and Proteobacteria (47.1%), with β-Proteobacteria (19.5%) being the most abundant proteobacterial group. Functionally, biofilms were composed of taxa contributing to biofilm establishment, exopolymer production and nutrient cycling, abundant taxa capable of Au mobilization, detoxification and biomineralization, among them Cupriavidus metallidurans, Acinetobacter spp. and Pseudomonas spp., were detected. In conclusion, these results demonstrate that placer Au-particle transformation and Au dispersion occur in cold, arctic environments. This corroborates the existence of biogeochemical Au cycling in present-day cold environments. KW - Gold KW - Bacteria KW - Biogeochemistry KW - Mobility KW - Finland KW - Cupriavidus metallidurans KW - NGS PY - 2018 DO - https://doi.org/10.1016/j.chemgeo.2018.03.021 SN - 0009-2541 VL - 483 SP - 511 EP - 529 PB - Elsevier AN - OPUS4-44805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, A. A1 - Kranzmann, Axel T1 - Degradation of AISI 630 exposed to CO2-saturated saline aquifer at ambient pressure and 100 bar N2 - In general high alloyed steels are suitable as pipe steels for carbon capture and storage technology (CCS), because they provide sufficient resistance against the corrosive environment of CO2-saturated saline aquifer which serves as potential CCS-site in Germany. High alloyed martensitic steel AISI 630 has been proven to be sufficient resistant in corrosive environments, e.g. regarding heat, pressure, salinity of the aquifer, CO2-partial pressure), but reveals a distinct corrosion pattern in CCS environment. Therefore coupons of AISI 630 heat treated using usual protocols were kept at T=60 °C and ambient pressure as well as p=100 bar up to 8000 h in an a) water saturated supercritical CO2 and b) CO2-saturated synthetic aquifer environment similar to on-shore CCS-sites in the Northern German Basin. AISI 630 precipitates a discontinuous ellipsoidal corrosion layer after being exposed for more than 4000 hours. Best corrosion resistance in the CO2-saturated synthetic aquifer environment phase is achieved via normalizing prior to exposure. In water saturated supercritical CO2 tempering at medium temperatures after hardening gives lowest corrosion rates. Corrosion fatigue via push-pull tests with a series of 30 specimens was evaluated at stress amplitudes between 150 MPa and 500 MPa (sinusoidal dynamic test loads, R=-1; resonant frequency ~ 30 Hz). The endurance limit of AISI 630 is reduced by more than 50% when exposed to CCS environment (maximum number of cycles (10 x 106) at a stress amplitude of 150 MPa). KW - Corrosion Fatigue KW - High Cycle Fatigue KW - Steel KW - Ccs KW - Co2-Storage PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503783 DO - https://doi.org/10.22587/jasr.2018.14.6.3 SN - 1819-544X SN - 1816-157X SP - 11 EP - 17 PB - INSInet Publications CY - Faisalabad AN - OPUS4-50378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Knauer, S A1 - Jaeger, P A1 - Kratzig, Andreas A1 - Bettge, Dirk A1 - Kranzmann, Axel T1 - Droplet corrosion of CO2 transport pipeline steels in simulated oxyfuel flue gas N2 - The research focus of this study was set on the corrosion process of condensate as droplets on the surface of carbon steels (X52, X70) martensitic steel UNS S41500, and super austenite UNS N08031 in CO2 atmosphere with impurities at 278 K (to simulate the offshore transportation condition in a buried pipeline). The possibility of dew/droplet formation on the steel surface and wetting behavior of corresponding materials were evaluated by contact angle measurement in dense CO2 at 278 K. To observe the effect of impurities (SO2 and O2) on droplet corrosion process, exposure tests were carried out in the mixed atmosphere with a drop, 1 ‑ 10 µL in volume, of CO2 saturated ultra-pure water on steel surface. Comparable exposure tests were carried out with the same gas mixture and the same volume of water, as vapor, to observe the droplet formation and the corrosion process that follows. Effects of surface roughness on the droplet formation and its corrosion process were further studied and showed no significant role upon long time exposure. The results from droplet experiments were compared to those from the bulk electrolyte for the further recommendation on the quality control of gas stream along with the use of carbon steels as transport pipelines in CCS - Carbon Capture and Storage system. KW - CCUS, supercritical/dense phase CO2, carbon steels, martensitic steel, superaustenite steel, droplet corrosion PY - 2018 UR - http://corrosionjournal.com/doi/abs/10.5006/2927 DO - https://doi.org/10.5006/2927 SN - 0010-9312 SN - 1938-159X VL - 74 IS - 12 SP - 1406 EP - 1420 PB - NACE International CY - Houston, Texas, USA AN - OPUS4-46903 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hinrichs, R. A1 - Zen Vasconcellos, M.A. A1 - Österle, Werner A1 - Prietzel, C. T1 - Amorphization of graphite flakes in gray cast iron under tribological load N2 - A gray cast iron disc, which had been submitted to a heavy duty automotive brake test, was examined with energy filtered transmission electron microscopy. A graphite flake in a convenient angular position showed the shear interaction of graphite layers with the iron matrix in nano-scale resolution. Atomic layers of graphite were wedged into the ferritic bulk, allowing the entrance of oxygen and the subsequent formation of magnetite. The exfoliated few-layer graphene batches deformed heavily when forced into the matrix. When Raman spectra from the disc surface, which show distinctive carbonaceous bands, were compared with Raman spectra from graphite subjected to deformation in a shaker mill with different milling times, it could be seen that the shear stress on the brake surface was much more effective to induce disorder than the milling, where compressive and impact forces had been additionally exerted on the sample. During shear load the high anisotropy of elastic modulus in the graphite crystalline structure and the low adhesion between graphite basal planes allowed the exfoliation of wrinkled few-layer grapheme batches, causing the formation of more defect related Raman bands than the mechanical stress during high-energy milling. KW - Graphite KW - Shear load KW - Amorphization KW - EFTEM KW - Raman spectroscopy PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-469227 DO - https://doi.org/10.1590/1980-5373-MR-2017-1000 SN - 1516-1439 SN - 1980-5373 VL - 21 IS - 4 SP - e20171000, 1 EP - 6 PB - Universidade Federal de São Carlos CY - São Carlos AN - OPUS4-46922 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koclęga, Damian A1 - Radziszewska, A. A1 - Kranzmann, Axel A1 - Dymek, S. T1 - Microstructure characterization of the Inconel 686 clad layer after high-temperature corrosion tests in aggressive gases and ashes N2 - The Ni-Cr-Mo-W alloy is characterized by the excellent high-temperature corrosion resistance, good strength and ability to work in aggressive environments. To protect the surface of the substrate 13CrMo4-5 steel against aggressive environments the Inconel 686 as clad layer was used. The corrosion process was performed in oxidizing mixture of gases like O2, COx, SOx. The second part of corrosion Experiment concerned the corrosion test of the coating in reducing atmosphere of the specified gases with ashes, which contained e.g. Na, Cl, Ca, Si, C, Fe, Al. T2 - Junior EUROMAT 2018 CY - Budapest, Hungary DA - 08.07.2018 KW - Laser Cladding KW - Inconel 686 KW - High temperature corrosion KW - Aggressive environement KW - Material oxidation PY - 2018 AN - OPUS4-45627 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koclega, Damian A1 - Radziszewska, Agnieszka A1 - Kranzmann, Axel A1 - Dymek, Stanislaw T1 - The microstructure characterization of the oxide scale created on Inconel 686 clad N2 - The Ni-Cr-Mo-W alloy is characterized by the excellent high-temperature corrosion resistance, good strength and ability to work in aggressive environments. To protect the surface of the substrate 13CrMo4-5 steel against aggressive environments the Inconel 686 as clad layer was used. The corrosion process was performed in oxidizing mixture of gases like O2, COx, SOx. The second part of corrosion Experiment concerned the corrosion test of the coating in reducing atmosphere of the specified gases with ashes, which contained e.g. Na, Cl, Ca, Si, C, Fe, Al. T2 - EUROCORR 2018 CY - Crocow, Poland DA - 09.09.2018 KW - Laser cladding KW - Inconel 686 coating KW - High-temperature corrosion KW - Aggressive gases PY - 2018 AN - OPUS4-47393 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Donėlienė1, J. A1 - Rudzikas, M. A1 - Rades, Steffi A1 - Dörfel, Ilona A1 - Peplinski, Burkhard A1 - Sahre, Mario A1 - Pellegrino, F. A1 - Maurino, V. A1 - Ulbikas, J. A1 - Galdikas, A. T1 - Electron Microscopy and X-Ray Diffraction Analysis of Titanium Oxide Nanoparticles Synthesized by Pulsed Laser Ablation in Liquid N2 - A femto-second pulsed laser ablation in liquid (PLAL) procedure for the generation of titanium oxide nanoparticles (NP) is reported with the purpose of understanding morphology and structure of the newly generated NPs. Ablation duration was varied for optimization of NP generation processes between 10 and 90 min. Surface morphology of NPs as well as their size and shape (distribution) were analysed by various complementary electron microscopy techniques, i.e. SEM, TSEM and TEM. The crystalline structure of titanium oxide particles was investigated by XRD and HR-TEM. Concentration of generated titanium oxide NPs in liquid was analysed by ICP-MS. A mix of crystalline (mainly anatase), partly crystalline and amorphous spherical titanium oxide NPs can be reported having a mean size between 10 and 20 nm, which is rather independent of the laser ablation (LA) duration. A second component consisting of irregularly shaped, but crystalline titanium oxide nanostructures is co-generated in the LA water, with more pronounced occurrence at longer LA times. The provenance of this component is assigned to those spherical particles generated in suspension and passing through the converging laser beam, being hence subject to secondary irradiation effects, e. g. fragmentation. T2 - Microscopy & Microanalysis 2018 CY - Baltimore, MD, USA DA - 05.08.2018 KW - Nanoparticles KW - Titanium oxide KW - Laser ablation in liquid KW - Electron microscopy KW - XRD PY - 2018 AN - OPUS4-46502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo A1 - Pöthkow, K. A1 - Paetsch, O. A1 - Hege, H.-C. T1 - 3D reconstruction and quantification of dislocation substructures from TEM stereo pairs N2 - Dislocations are the carriers of plastic deformation. As such, their characterization offers important information on the properties they affect. In this contribution, a new tool is presented, which is incorporated in Amira ZIB Edition and allows for three-dimensional (3D) imaging and quantification of dislocations substructures from thick regions an electron-transparent specimen. In the tool, the dislocation segments are traced on diffraction contrast images that are obtained in the transmission electron microscope (TEM). The uncertainties related to the experimental setup and to the proposed method are discussed on the base of a tilt series. T2 - AVIZO / AMIRA User Meeting CY - Berlin, Germany DA - 14.11.2018 KW - Dislocation KW - Diffraction contrast KW - Scanning transmission electron microscopy (STEM) PY - 2018 AN - OPUS4-47394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zerbst, Uwe A1 - Klinger, Christian A1 - Bettge, Dirk T1 - Defects as a root cause for fatigue failure of metallic components N2 - The Topic of the presentationis a discussion on defects which can cause failure in cyclically loaded metallic components. Although also touching Features such as material defects such as pores or micro-shrinkages, etc. and geometric defects such as surface roughness and secondary notches (which are not considered in the design process) which origin in manufacturing, and others the presentation concentrates on non-metallic inclusions. It is prefaced by an introduction to the life cycle of a fatigue crack from initiation up to fracture. Special emphasis is put on the fact that only cracks which are not arrested during one of their distinct Propagation stages can grow to a critical size. T2 - VIII. International Conference on Engineering Failure Analysis CY - Budapest, Ungarn DA - 08.06.2018 KW - Metallic components KW - Material defects KW - Micro-shrinkages PY - 2018 AN - OPUS4-46875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bettge, Dirk A1 - Kratzig, Andreas A1 - Peetz, Christoph A1 - Kranzmann, Axel T1 - Interaction of Oxidizing and Reductive Impurities in CO2 Streams with Transport Pipeline Steel N2 - A main goal of CLUSTER CCS project at BAM was to study the corrosion behaviour of pipeline steel with dense phase carbon dioxide containing impurities. Depending on the kind of impurities specific corrosion mechanisms and corrosion rates were determined. T2 - CO2 and H2 Technologies for the Energy Transition CY - BAM, Berlin, Germany DA - 28.11.2018 KW - Carbon capture KW - Carbon dioxide KW - Corrosion KW - CCS PY - 2018 AN - OPUS4-47016 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa A1 - Knauer, S A1 - Bäßler, Ralph A1 - Peetz, Christoph A1 - Kratzig, Andreas A1 - Bettge, Dirk A1 - Kranzmann, Axel A1 - Jaeger, P A1 - Schulz, S T1 - Impact of acid condensation on wetting and corrosion behavior of CO2 transport-pipeline steel N2 - Es ist allgemein akzeptiert, das Korrosion in CO2-Transport-Pipelines vernach¬lässigbar ist, solange der Wassergehalt des CO2-Stroms deutlich unter der maximal löslichen Menge liegt. Bisher gibt es keinen allgemeinen Konsens darüber, welcher maximale Wassergehalt in zu transportierendem CO2 zugelassen werden sollte. Bei einem Druck von 100 bar und im Temperaturbereich von 277 K bis 298 K beträgt die Löslichkeit von Wasser in CO2 ca. 1.900 bis 3.200 ppmv, aber die Korrosionsrate von Stählen steigt schon ab einem Wassergehalt von 500 ppmv deutlich an. Bei Anwesenheit von Begleitstoffen wie SO2, NO2 und O2, können sich HNO3, H2SO3 und H2SO4 bilden. Menge und Zusammensetzung von kondensierter Säure sind von der Gaszusammensetzung abhängig, und der Korrosionsmechanismus und die Korrosionsform sind vom Kondensationsverhalten abhängig. T2 - CLUSTER Symposium: CO2 and H2 Technologies for the Energy Transition CY - BAM, Berlin, Germany DA - 28.11.2018 KW - CCUS KW - Supercritical/dense phase CO2 KW - Carbon steels KW - Martensitic steel KW - Superaustenite steel KW - Droplet corrosion PY - 2018 AN - OPUS4-46907 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Peetz, Christoph A1 - Buggisch, Enrico A1 - Bettge, Dirk A1 - Kranzmann, Axel T1 - Electrochemical study on wellbore constellations for CO2 injection N2 - Carbon Capture and Storage (CCS) is identified as an excellent technology to reach the target of CO2 reduction. However, the safety issue and cost effectiveness hinder the future of CCS. For the reliability and safety issues of injection wells the corrosion resistance of the materials used needs to be determined. In this study, representative low cost materials including carbon steel 1.8977 and low alloyed steel 1.7225 were embedded in cement to mimic the realistic casing-cement interface. Electrochemical studies were carried out using these metal-cement specimens in comparison with those made of metal only in CO2 saturated synthetic aquifer fluid, at 333 K, to reveal the effect of cement on the steel performance. The results showed the protective effect of cement on the performance of pipeline metals during polarisation process. However, the corrosion current density was high in all cases, with and without cement, indicating that the corrosion resistance of these materials is low. This conclusion was supported by the surface analysis of the polarized specimens, which revealed both homogenous and pitting corrosions. Furthermore, to reveal the possible protective performance of FeCO3, the pipeline steels were pre-carbonated and then tested in the same condition as freshly polished specimens. T2 - EUROCORR 2018 CY - Krakow, Poland DA - 09.09.2018 KW - CCUS KW - Supercritical/dense phase CO2 KW - Carbon steels KW - Martensitic steel KW - Superaustenite steel KW - Injection KW - Impurities PY - 2018 AN - OPUS4-46279 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded A1 - Röhsler, Andreas A1 - Nolze, Gert A1 - Unger, Wolfgang A1 - Böllinghaus, Thomas T1 - Sputtering derived artefacts in austenitic steel during Time-of-Flight Secondary Ion Mass Spectrometry analyses N2 - Among the very few techniques to localize hydrogen (H) at the microscale in steels, Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was proven to be a reliable tool. The necessity to detect hydrogen stems from its deleterious effects in metals, that are often used as structural components and to obtain better understanding of the underlying metallurgical mechanisms of hydrogen embrittlement (HE) which are still unclear. Austenitic stainless steels are nowadays commonly used in a wide variety of application, from hydrogen transport and storage facilities to petrochemical and offshore applications where they are exposed to aggressive environments and therefore prone to HE. One of the greater risks in the austenitic class is the embrittlement of the material due to the instability of the γ austenite and its transformation into a brittle α martensitic phase. This transformation takes place due to the local stresses that are induced by the uptake of hydrogen during service. Nonetheless, it was shown that this transformation can occur as an artefact during SIMS analysis itself where Cs-sputtering is necessary not only to remove surface contaminations but mainly to enhance H/D secondary ion yield. In the following contribution we show the influence of different sputtering conditions on AISI 304L austenitic stainless steel in order to distinguish the artefact from the hydrogen induced transformation. The material was charged electrochemically in a deuterium based electrolyte. Deuterium (D) must be in these experiments as a replacement for hydrogen which cannot be used because adsorbed hydrogen superimposes hydrogen originating from charging the sample in the SIMS images. ToF-SIMS analyses were conducted by ToF SIMS IV (IONTOF GmbH, Münster, Germany). The experiments were carried out on deuterium charged and non-charged samples. The structural characterization was carried out by SEM and EBSD examinations before and after charging, both with a Leo Gemeni 1530VP field-emission scanning electron microscope and a Zeiss Supra 40 instrument (Carl Zeiss Microscopy GmbH, Oberkochen, Germany). The results showed that the use of 1keV Cs+ beam induces stacking faults while higher sputter beam energies results in γ→α transformation. T2 - SIMS Europe 2018 CY - Münster, Germany DA - 16.09.2018 KW - Austenitic steel KW - Hydrogen KW - ToF-SIMS KW - Artefact PY - 2018 AN - OPUS4-46701 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kratzig, Andreas A1 - Bettge, Dirk A1 - Peetz, Andreas A1 - Kranzmann, Axel T1 - Interaction of Reactive Components in CO2 Streams with Transport Pipeline Steel X70 N2 - In context of CLUSTER project, impacts of impurities (SO2, NO2, O2, CO, H2S, H2, N2, Ar and H2O) in CO2 streams captured from different sources in a regional cluster on transport, injection and storage were investigated. Corrosion studies of oxidizing, reductive or mixed atmospheres towards transport pipeline steel X70 were carried out applying high pressure (10 MPa) at low temperatures (278 K or 313 K). T2 - GHGT-14 Conference CY - Melbourne, Australia DA - 22.10.2018 KW - Carbon capture KW - CCS KW - Carbon dioxide KW - Corrosion PY - 2018 AN - OPUS4-47017 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falk, Florian A1 - Menneken, Martina A1 - Stephan-Scherb, Christiane T1 - Early oxidation and sulfidation of high temperature model alloys: An EDXRD in situ study N2 - The fundamental impact of sulfur and water on corrosion rates and potential failure of the exposed material is well known. However, the access to the related corrosion mechanism causing material degradation is often a problem to solve. This study investigates the effect of SO2 and water vapor in the initial stages of corrosion of an Fe9Cr0.5Mn model alloy at 650 °C in situ. The analysis was carried out under laboratory conditions using energy-dispersive X-ray diffraction (EDXRD). T2 - Dechema EFC Workshop CY - Frankfurt am Main, Germany DA - 26.09.2018 KW - Sulfidation KW - Model alloy KW - Oxidation PY - 2018 AN - OPUS4-46134 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Menneken, Martina A1 - Falk, Florian A1 - Stephan-Scherb, Christiane T1 - Early stages of corrosion in hot, aggressive environments N2 - We investigated the effect of water vapor in the initial stages of SO2 corrosion of an Fe-9Cr-0.5Mn model alloy at 650 °C. Two separate experiments were run, one with 99.5%-Ar + 0.5%-SO2 and one with 69.5%-Ar + 0.5%-SO2 with 30%-H2O atmosphere. During the experiment the scale growth was observed in-situ, using energy dispersive X-ray diffraction (EDXRD). Our results confirm an increased speed of oxygen transport into the material, with the addition of water, while the transport of sulfur appears to be less affected. T2 - Sektionstreffen der DMG Sektionen "Angewandte Mineralogie in Umwelt & Technik" und "Chemie, Physik und Kristallographie der Minerale" CY - Bad Windsheim, Germany DA - 28.02.2018 KW - Corrosion KW - In-situ KW - EDXRD PY - 2018 AN - OPUS4-45369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Kratzig, Andreas A1 - Bettge, Dirk A1 - Kranzmann, Axel A1 - Knauer, S. T1 - Droplet corrosion of CO2 transport pipeline steels N2 - In this work, the focus was set on the corrosion process of condensate as drops on the surface of carbon steels (X52, X70), martensitic steel UNS S41500, and superaustenite UNS 08031 in CO2 atmosphere with impurities at 278 K (to simulate the transportation condition in a buried pipeline). Exposure tests were performed at both normal pressure and high pressure where CO2 is supercritical or in dense phase. The drop, 1 ‑ 10 µL in volume, was prepared by dropping CO2 saturated ultra-pure water onto the surface of steel coupons in a one-liter-autoclave. The CO2 gas stream, simulating the oxyfuel flue gas with varying concentration of impurities (SO2 and O2), was then pumped into the autoclave to observe the condensation and corrosion impacts of impurities. Comparable exposure tests were carried out with the same gas mixture and the same volume of water as vapor to observe the drop formation and the corrosion process that follows. The wettability and stability of drops on the surface of steel coupons in CO2 supercritical/dense phase environment was evaluated additionally by contact angle measurement. T2 - NACE International Annual Corrosion Conference CY - Phoenix, AZ, USA DA - 15.04.2018 KW - CCUS KW - Supercritical/dense phase CO 2 KW - Carbon steels KW - Martensitic steel KW - Superaustenite steel KW - Droplet corrosion PY - 2018 AN - OPUS4-44922 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Röhsler, Andreas A1 - Sobol, Oded A1 - Nolze, Gert A1 - Unger, Wolfgang A1 - Böllinghaus, Thomas T1 - In-situ observation of the hydrogen behaviour in austenitic stainless steel by time-of-flight secondary ion mass spectrometry during mechanical loading N2 - The reduction of harmful emissions to the environment is one of the most urgent challenges of our time. To achieve this goal, it is inevitable to shift from using fossil fuels to renewable energy sources. Within this transition, hydrogen can play a key role serving as fuel in transportation and as means for energy storage. The storage and transport of hydrogen using austenitic stainless steels as the infrastructure, as well as the use of these grades in hydrogen containing aggressive environments, remains problematic. The degradation of the mechanical properties and the possibility of phase transformation by ingress and accumulation of hydrogen are the main drawbacks. Advanced studies of the behaviour of hydrogen in austenite is necessary to fully understand the occurring damage processes. This knowledge is crucial for the safe use of components in industry and transportation facilities of hydrogen. A powerful tool for depicting the distribution of hydrogen in steels, with high accuracy and resolution, is time-of-flight secondary ion mass spectrometry (ToF-SIMS). We here present a comprehensive research on the hydrogen degradation processes in AISI 304L based on electrochemical charging and subsequent ToF-SIMS experiments. To obtain furthermore information about the structural composition and cracking behaviour, electron-backscattered diffraction (EBSD) and scanning electron microscopy (SEM) were performed afterwards. All the gathered data was treated employing data fusion, thus creating a thorough portrait of hydrogen diffusion and its damaging effects in AISI 304L. Specimens were charged with deuterium instead of hydrogen. This necessity stems from the difficulty to separate between artificially charged hydrogen and traces existing in the material or adsorbed from the rest gas in the analysis chamber. Similar diffusion and permeation behaviour, as well as solubility, allow nonetheless to draw onclusions from the experiments. T2 - International Conference on Metals and Hydrogen; Steely Hydrogen 2018 CY - Ghent, Belgium DA - 29.05.2018 KW - Hydrogen KW - Deuterium KW - ToF-SIMS KW - AISI 304L PY - 2018 AN - OPUS4-45079 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Röhsler, Andreas A1 - Sobol, Oded A1 - Nolze, Gert A1 - Unger, Wolfgang A1 - Böllinghaus, Thomas T1 - Use of time-of-flight secondary ion mass spectrometry for the investigation of hydrogen-induced effects in austenitic steel AISI 304L N2 - During the energy transformation from fossil fuels to renewable energy sources, the use of hydrogen as fuel and energy storage can play a key role. This presents new challenges to industry and the scientific community alike. The storage and transport of hydrogen, which is nowadays mainly realized by austenitic stainless steels, remains problematic, which is due to the degradation of mechanical properties and the possibility of phase transformation by hydrogen diffusion and accumulation. The development of materials and technologies requires a fundamental understanding of these degradation processes. Therefore, studying the behavior of hydrogen in austenitic steel contributes to an understanding of the damage processes, which is crucial for both life assessment and safe use of components in industry and transportation. As one of the few tools that is capable of depicting the distribution of hydrogen in steels, time-of-flight secondary ion mass spectrometry was conducted after electrochemical charging. To obtain further information about the structural composition and cracking behavior, electron-backscattered diffraction and scanning electron microscopy were performed. Gathered data of chemical composition and topography were treated employing data fusion, thus creating a comprehensive portrait of hydrogen-induced effects in the austenite grade AISI 304L. Specimens were electrochemically charged with deuterium instead of hydrogen. This arises from the difficulties to distinguish between artificially charged hydrogen and traces existing in the material or the rest gas in the analysis chamber. Similar diffusion and permeation behavior, as well as solubility, allow nonetheless to draw conclusions from the experiments. T2 - 21st International Conference on Secondary Ion Mass Spectrometry CY - Kraków, Poland DA - 10.09.2017 KW - AISI 304L KW - Hydrogen KW - ToF-SIMS KW - Austenitic stainless steel PY - 2018 DO - https://doi.org/10.1116/1.5013931 SN - 1071-1023 VL - 36 IS - 3 SP - Article 03F103, 1 EP - 6 PB - American Vacuum Society (AVS) AN - OPUS4-44840 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Goedecke, Caroline A1 - Altmann, Korinna A1 - Bannick, C. G. A1 - Kober, E. A1 - Ricking, M. A1 - Schmitt, T. A1 - Braun, Ulrike T1 - Detection of polymers in treated waste water using TED-GC-MS N2 - The presence of large quantities of plastic waste and its fragmentation in various environmental compartments are an important subject of current research. In the environment, (photo ) oxidation processes and mechanical abrasion lead to the formation of microplastics. However, until now, there are no established quality assurance concepts for the analysis of microplastic (<5 mm) in environmental compartments, including sampling, processing and analysis. The aim of the present work is the development of suitable examination methods and protocols (sampling, sample preparation and detection) to qualify and quantify microplastic in urbane water management systems. At first a fractional filtration system for sampling and the analytical tool, the so-called TED-GC-MS (thermal desorption gas chromatography mass spectrometry) were developed. The TED-GC-MS method is a two-step analytical procedure which consists of a thermal extraction where the sample is annealed and characteristic decomposition products of the polymers are collected on a solid phase. Afterwards these products are analysed using GC-MS. The developed fractional filtration for sampling and the TED-GC-MS for detection were used for quantitative analysis to screen the waste water influent and effluent of a Berlin waste water treatment plant for the most relevant polymers, polyethylene (PE), polypropylene (PP), polystyrene (PS), polyethylene terephthalate (PET) and polyamide (PA). The results of the study revealed that the polymeres PE, PS and PP were detected in the effluent, and PE and PS were find in the raw waste water of the sewage treatment plant in Ruhleben, Berlin. Differences in polymer types and amounts were detected at different sampling dates and within different sieve fractions. Much higher amounts of polymers were observed in the raw waste water. The peak areas of the decomposition products, used for quantification of the polymers, were adjusted using so-called response factors since the TED-GC-MS method is more sensitive for PP and PS than for PE. It has been shown that PE is the most dominant polymer in the samples. Comparing the masses of polymers in the effluent and in the raw sewage, a removal of 99 % of the polymers in the water treatment plant can be assumed. These results are consistent with the literature where removal rates between 98-99 % were described. T2 - SETAC Europe CY - Rom, Italy DA - 13.05.2018 KW - Microplastics KW - Thermogravimetry KW - Waste water KW - Chromatography PY - 2018 AN - OPUS4-44968 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna A1 - Goedecke, Caroline A1 - Bannick, C.G. A1 - Ricking, M. A1 - Kober, E. A1 - Schmitt, T. A1 - Braun, Ulrike T1 - Detektion von Polymeren im Abwasser eines Klärwerks mittels TED-GC_MS N2 - In den Umweltmedien Wasser, Boden und Luft wird Mikroplastik (MP) gefunden. Mögliche Eintragspfade, besonders Einträge über den Klarlauf kommunaler Klärwerke, sind unklar. Dazu wurde das Klärwerk Ruhleben in Berlin an jeweils vier Tagen im Sommer- und Winterbetrieb beprobt. Es wurde jeweils 1 m3 Klarlauf fraktioniert filtriert (500, 100 und 50 µm Siebe). Weiterhin wurde Rohabwasser exemplarisch untersucht. Als Analyse-methoden wurden die TED-GC-MS und die FTIR Mikroskopie verwendet. Bei der TED-GC-MS wird die Probe zunächst thermisch extrahiert, bevor die charakteristischen Zersetzungsgase mittels einer GC-Säule getrennt und im MS detektiert werden [1,2]. Es ist hier erstmals gelungen, nicht nur das MP zu identi-fizieren, sondern auch eine Massenbilanz zu erstellen und so eine quantitative Auswertung vorzunehmen. Es wurde PE, PS ganzjährig und PP im Sommer gefunden. Das Klärwerk Ruhleben hat einen Rückhalt an MP von 99%. T2 - Wasser 2018 CY - Papenburg, Germany DA - 07.05.2018 KW - Mikroplastik KW - Abwasser KW - TED-GC-MS KW - Bilanzierung PY - 2018 AN - OPUS4-44889 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mair, Georg A1 - Becker, B. A1 - Gesell, Stephan A1 - Wang, Bin T1 - Monte-Carlo-analysis of minimum load cycle requirements for composite cylinders for hydrogen N2 - Hydrogen is an attractive energy carrier that requires high effort for safe storage. For ensuring safety, storage cylinders must undergo a challenging approval process. Relevant standards and regulations for composite cylinders used for the transport of hydrogen and for its onboard storage are currently based on deterministic (e.g. ISO 11119-3) or to some respect semi-probabilistic criteria (UN GTR No. 13; with respect to burst strength). This paper provides a systematic analysis of the load cycle properties resulting from these regulations and standards. Their characteristics are compared with the probabilistic approach of the Federal Institute for Materials Research and Testing BAM. The most important aspect of comparing different concepts is the rate for accepting designs with potentially unsafe or critical safety properties. This acceptance rate is analysed by operating Monte-Carlo simulations over the available range of production properties. T2 - ICHS 2017 CY - Hamburg, Germany DA - 11.09.2017 KW - Safety assessment KW - Failure rate KW - Ageing KW - Degradation KW - End of life KW - Production scatter PY - 2018 DO - https://doi.org/10.1016/j.ijhydene.2018.09.185 SN - 0360-3199 VL - 44 IS - 17 SP - 8833 EP - 8841 PB - Elsevier Ltd AN - OPUS4-46341 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wander, Lukas A1 - Braun, Ulrike A1 - Becker, Roland A1 - Maiwald, Michael A1 - Paul, Andrea T1 - Mikroplastikanalyse: Nahinfrarotspektroskopie und chemometrische Auswertung N2 - Für die Erfassung der Verbreitung von Mikroplastik (MP) in der Umwelt ist die zeit- und kostenaufwendige Analysestrategie und der damit verbundene geringe Probendurchsatz eine limitierende Größe. Eine große Zahl verschiedener Studien dokumentriet das Auftreten von MP über den gesamten Globus. Meist sind die Studien aufgrund des großen analytischen Aufwands auf exemplarische, stichpunktartige Untersuchungen kleiner Umweltaliquoten und zahlenmäßig kleiner Probenumfänge begrenzt. Um die Verbreitung, die Eintragspfade und den Verbleib von MP in der Umwelt besser zu verstehen und effektive Vermeidungsstrategien abzuleiten, ist es jedoch notwendig, analytisch mehr Proben erfassen zu können. Bildgebende mikro-spektroskopische Methoden wie das Raman- und FTIR-Imaging ermöglichen eine zeitaufwendige, umfassende Charakterisierung kleiner Umweltaliquoten. Neben der Partikelanzahl sind zusätzlich Informationen zu Partikelgröße, Größenverteilung und Oberflächenmorphologie zugänglich. Chemische und thermische Extraktionsverfahren sind bereits deutlich schneller und können diese Informationen durch eine Massenbilanz vervollständigen. Die analysierbare Probenmenge ist jedoch auf Milligramm Mengen beschränkt. Wir schlagen daher vor, die Analyse von Proben auf MP durch ein vorangestelltes Screening mit der Nahinfrarot-Spektroskopie (NIRS) zur komplementieren. In diesem wird bereits eine erste Einschätzung über die Präsenz von MP in einer Probe gefällt und dadurch die wertvolle Messzeit anderer Methoden effizienter genutzt. NIR zur Analyse von Polymeren wird seit langem eingesetzt, jedoch bisher lediglich im Rahmen einer Studie zur Mikroplastikuntersuchung mittels Hyperspektraler Bildgebung beschrieben. Der NIR Spektralbereich findet sich zwischen dem sichtbaren Licht und dem mittleren Infrarot (MIR). MIR Spektren sind durch klar definierte Banden charakterisiert, welche mehrheitlich von den Grundschwingungen der Moleküle stammen. Die höheren Energien im nahen Infrarot regen hingegen Kombinations- und Oberschwingungen der Streck und Biegeschwingungen an. Die resultierenden Absorptionsbanden sind oft breit und relativ unspezifisch. Erst mit Hilfe einer computergestützten Datenauswertung lassen sich aus diesen Spektren nützliche Informationen gewinnen. Dies erklärt die steigende Popularität der NIR-Spektroskopie in der jüngeren Vergangenheit mit einem Schwerpunkt als prozessanalytische Methode. NIR Spektrometer für das industrielle Prozessmonitoring zeichnen sich durch eine kompakte und robuste Konstruktionsweise aus. Die verfügbaren faseroptischen Reflexionssonden eignen sich gut um pulverförmige Proben zu untersuchen. Der räumlich erfassbare Messbereich kann durch die Sondengeometrie variiert werden. Sind die untersuchten Partikel im Verhältnis zur abgetasteten Fläche klein, wird als spektrale Information die Summe der Absorption aller Partikel im Sichtfeld erfasst. Die Methode ist deshalb nicht für Detailuntersuchungen von MP geeignet, erlaubt es jedoch innerhalb weniger Minuten eine Einschätzung über das Vorkommen von Mikroplastik in einer Probe zu treffen. Exemplarisch wurden für diese Untersuchungen vier der am weitesten verbreiteten Kunststoffe Polyethylen (PE), Polyethylenterephthalat (PET), Polypropylen (PP) und Polystyrol (PS) gewählt. Aus den additivfreien Polymeren wurden nach einer Kryo-vermahlung und anschließender Siebung (< 125 µm) Modellproben generiert. Die Polymere wurden dafür zu einem Massenanteil von 1 % mit einem Standardboden (LUFA2.3, gesiebt < 125 µm) vermischt. Die Gesamtmenge von 1 g je Probe wurde in Aluminiumbehältern präpariert und 8 Messungen an unterschiedlichen, zufällig gewählten Positionen vorgenommen. Die erhaltenen Spektren wurden zur Kalibrierung chemometrischer Modelle genutzt. In einem hierarchischen Ansatz wurde anhand der NIR-Spektren eine Klassifizierung vorgenommen: 1. Bestimmung ob eine Probe MP enthält (Ja/Nein). 2. Identifikation der Polymere in der Probe. Eine aussagekräftige Klassifizierung beruht auf einer Vorbehandlung der Spektren. Hierdurch werden die Unterschiede zwischen den einzelnen Polymerbanden hervorgehoben. Die Eignung der so erstellten Modelle wurde anhand eines Referenzmaterials und am Beispiel von Realproben erfolgreich getestet. Dabei zeigte sich, dass nicht nur in den erstellten Polymer-Bodenmischungen, sondern auch in den Rückständen von fermentiertem Bioabfall und in Filterrückständen einer Waschmaschine, MP richtig erkannt wurde. Weiterhin zeigten Tests mit Mikroplastik-freien Bodenproben unterschiedlicher Herkunft, dass keine falsch-positive Resultate erzeugt wurden. Alle vier untersuchten Polymere, d.h. PE, PET, PS und PP mit einem Massenanteil von 1 % in einer Bodenmatrix werden auch bei einer gemischten Polymerzusammensetzung mit der NIR-Spektroskopie erkannt. Der kombinierte Einsatz von NIRS und Chemometrie ermöglicht die Entscheidung über ein potenzielles Vorkommen sowie die Zuordnung des Materials der enthaltenen Polymerpartikel für eine Massefraktion ≥ 1 % in einer (trockenen) Probenmenge von 1 g innerhalb von 10–15 min. Der zeitaufwendige Schritt der Methode liegt hier in der Erstellung geeigneter chemometrischer Modelle sowie deren Validierung. Wesentliche Voraussetzung ist dabei, dass bei der Kalibrierung die Varianz der zu erwartenden Partikel und der Matrix realistisch abgebildet wird. T2 - GDCh Jahrestagung der Wasserchemischen Gesellschaft CY - Papenburg, Ems, Germany DA - 07.05.2018 KW - Mikroplastik KW - Nahinfrarotspektroskopie KW - Chemometrie KW - Boden PY - 2018 AN - OPUS4-44887 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Andrea A1 - Wander, Lukas A1 - Becker, Roland A1 - Goedecke, Caroline A1 - Braun, Ulrike T1 - High-throughput NIR spectroscopic (NIRS) detection of microplastics in soil N2 - The increasing pollution of terrestrial and aquatic ecosystems with plastic debris leads to the accumulation of microscopic plastic particles of still unknown amount. To monitor the degree of contamination analytical methods are urgently needed, which help to quantify microplastics (MP). Currently, time-costly purified materials enriched on filters are investigated both by micro-infrared spectroscopy and/or micro-Raman. Although yielding precise results, these techniques are time consuming, and are restricted to the analysis of a small part of the sample in the order of few micrograms. To overcome these problems, here we tested a macroscopic dimensioned NIR process-spectroscopic method in combination with chemometrics. For calibration, artificial MP/soil mixtures containing defined ratios of polyethylene, polyethylene terephthalate, polypropylene, and polystyrene with diameters < 125 µm were prepared and measured by a process FT-NIR spectrometer equipped with a fiber optic reflection probe. The resulting spectra were processed by chemometric models including support vector machine regression (SVR), and partial least squares discriminant analysis (PLS-DA). Validation of models by MP mixtures, MP-free soils and real-world samples, e.g. and fermenter residue, suggest a reliable detection and a possible classification of MP at levels above 0.5 to 1.0 mass% depending on the polymer. The benefit of the combined NIRS chemometric approach lies in the rapid assessment whether soil contains MP, without any chemical pre-treatment. The method can be used with larger sample volumes and even allows for an online prediction and thus meets the demand of a high-throughput method. KW - Microplastics KW - Soil KW - Chemometrics KW - PLS-DA KW - Support vector machines KW - Near Infrared Spectroscopy PY - 2018 DO - https://doi.org/10.1007/s11356-018-2180-2 SN - 1614-7499 SN - 0944-1344 VL - 26 IS - 8 SP - 7364 EP - 7374 PB - Springer AN - OPUS4-45405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Usmani, Shirin A1 - Stephan, Ina A1 - Huebert, Thomas A1 - Kemnitz, E. T1 - Nano metal fluorides for wood protection against fungi N2 - Wood treated with nano metal fluorides is found to resist fungal decay. Sol−gel synthesis was used to synthesize MgF2 and CaF2 nanoparticles. Electron microscopy images confirmed the localization of MgF2 and CaF2 nanoparticles in wood. Efficacy of nano metal fluoride-treated wood was tested against brown-rot fungi Coniophora puteana and Rhodonia placenta. Untreated wood specimens had higher mass losses (∼30%) compared to treated specimens, which had average mass loss of 2% against C. puteana and 14% against R. placenta, respectively. Nano metal fluorides provide a viable alternative to current wood preservatives. KW - Brown-rot fungi KW - Coniophora puteana KW - Fluoride nanoparticles KW - Fluorolytic sol−gel KW - Rhodonia placenta KW - SEM wood characterization KW - Wood protection PY - 2018 DO - https://doi.org/10.1021/acsanm.8b00144 SN - 2574-0970 VL - 2018 SP - 1 EP - 6 PB - American Chemical Society (ACS) CY - Washington DC, US AN - OPUS4-44730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -