TY - CONF A1 - Ramirez Caro, Alejandra A1 - Pauli, Jutta T1 - Study of the hydration of superplasticizer-cement pastes with optical spectroscopy N2 - Chemical admixtures like superplasticizers or stabilizing agents are of ever increasing importance for modern concrete technology. Although such admixtures have meanwhile become common practice in many applications of concrete technology, the understanding of these highly complex systems is still limited and the relevant parameters, which predominantly control the interaction between the superplasticizer and the cement components, have not been identified yet. Optical methods have been successfully used for the analysis and monitoring of the interactions between a broad variety of nanoscale and molecular systems like nanoparticles of various chemical composition and different types of organic ligands or biomolecules. This encouraged us to assess the potential of these methods, and particularly reflectance and fluorescence measurements, for the study of the interactions that occur at the interface between particle or hydrate surfaces and the fluid phase at a very early stage of concrete formation. Special emphasis is dedicated to search for and identify differences between commonly used superplasticizers. Here, we focus on hydration effects using commercial comb shape polycarboxylate ethers (PCEs) with different charge densities, which are known to allow a very low water/cement ratio (w/c of 0.20 or less) while maintaining good workability. Based upon changes of the intensity of the reflectance and fluorescence signal and spectral effects of a dye, acting as optical reporter, a model for the interactions of dye, PCE molecules and cement nanoparticles in the very first phase of cement hydration is derived T2 - Gesellschaft Deutscher Chemiker-Analytische Chemie-Anakon 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Cement hydration KW - Optical spectroscopy KW - Superplasticizers PY - 2017 AN - OPUS4-39882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Torge, Manfred T1 - Organic surface coatings on medieval stained glass and microbiological investigation N2 - Mediaeval stained glass has been treated with Polymethylmetacrylate coatings by Kwiatkowski in Poland during the 1950th. Such treated panels were found in the Johannis Church of Toruń (without protective glazing), in the Cathedral of Włocławek (behind a protective glazing), and on glass kept in exhibition cases in the museum of Toruń. Surface coatings have been detected and analyzed. There was no extensive contamination by fungi or bacteria if the glass was either coated or not. T2 - Glass Science in Art and Conservation 2017 CY - Lisbon, Portugal DA - 06.06.2017 KW - Microbiological investigation KW - Medieval stained glass KW - SEM analysis PY - 2017 AN - OPUS4-40573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Torge, Manfred T1 - SEM and Micro-XRF analysis to investigate stained glass windows N2 - Several restoration projects of stained-glass windows have been performed in Poland since 2010.Chemical analysis of glass samples was performed with SEM/EDX on a FEI ESEM-XL 30, (EDX-EDAX) and with Micro-XRF (M4 Tornado, Bruker).The chemical composition of medieval glass samples and of glass samples of the 19th Century have been determined. T2 - Technart2017 CY - Bilbao, Spain DA - 02.05.2017 KW - SEM KW - Micro-XRF KW - Glass composition PY - 2017 AN - OPUS4-40435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gluth, Gregor T1 - Additive manufacturing of geopolymers by selective laser curing N2 - Additive manufacturing (3D printing) of ceramics and other materials offers significant advantages compared to conventional production processes for several applications. While ceramics have been extensively investigated in this regard, additive manufacturing of geopolymers have received much less attention to date. In the present contribution we study a ‘standard’ metakaolin-based geopolymer, a fly ash-based geopolymer and a silica-based one-part geopolymer regarding their suitability for additive manufacturing via selective laser curing. Model geometries such as bars and cuboids could be produced by this route. After selective laser curing the specimens were additionally cured at 80 °C for 24 h. The specimens were studied by means of scanning electron microscopy (SEM) and powder X-ray diffraction (XRD). SEM showed that the precursors in all geopolymers had reacted partially and geopolymeric gel had formed. XRD confirmed these results and additionally revealed that the crystalline byproducts (zeolites) in the one-part geopolymer differed from the byproducts observed in conventionally produced samples. This indicates that also the geopolymerization reactions differ between the two synthesis routes. The mechanical strength after selective laser curing and 80 °C-curing appeared to be highest for the metakaolin-based geopolymer. However, SEM also showed that a significant volume of macropores remained in most regions of all specimens, while some regions in the metakaolin-based geopolymer appeared to be significantly denser. These preliminary results demonstrate that selective laser curing offers potential for the production of geopolymers, but more research has to be undertaken to optimize the process. T2 - 92. DKG Jahrestagung CY - Berlin, Germany DA - 19.03.2017 KW - Geopolymers KW - Inorganic polymers KW - Additive manufacturing KW - 3D printing KW - Selective laser curing PY - 2017 AN - OPUS4-39514 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stegemann, Robert T1 - Bewertung der magnetischen Mikrostruktur für die Schadensfrüherkennung N2 - Die Mikrostruktur ferromagnetischer Materialien hat einen maßgeblichen Einfluss auf deren magnetischen Eigenschaften. Gerade bei niedrigen Feldstärken zeigen sich Parameter wie Koerzitivität, Permeabilität und Verlustleistung hoch sensitiv. Wir zeigen am Beispiel des unlegierten Baustahls S235JR, dass die magnetische Mikrostruktur an der Probenoberfläche in hohem Maße mit inhomogenen Dehnungen übereinstimmt. Zur Detektion der Kleinststreufelder verwenden wir speziell designte GMR Sensorik, die Sensitivität (3mV/V/kA/m) mit hoher Ortsauflösung (180 µm) vereint. Infolgedessen können wir auf eine aktive magnetische Anregung verzichten. Wir nutzen allein die sich durch magneto-mechanische Prozesse ausbildende „spontane“ magnetische Mikrostruktur des Materials. Das hervorragende Signal-Rausch-Verhältnis unserer GMR-Sensorik für inhomogene Streufelder erlaubt, schon geringe und lokal abgegrenzte plastische Deformationen in Form und Position reproduzierbar zu visualisieren. Die zugehörigen Signale zeigen die typische Sequenz von erhöhten positiven und negativen Normalkomponenten wie sie bei einer Rissanzeige der aktiven Streuflussprüfung (MFL - Magnetic Flux Leakage) beobachtet wird. Magnetisch kann eine plastische Zone daher als Vorstufe eines Risses betrachtet werden, deren relative Permeabilität für den Riss als Grenzfall zu μr = 1 tendiert. T2 - DGZfP-Jahrestagung CY - Koblenz, Germany DA - 22.05.2017 KW - Baustahl KW - GMR-Sensorik KW - Heterogene plastische Deformation KW - Zugversuch PY - 2017 AN - OPUS4-40375 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiede, Tobias T1 - Residual stress analysis in selective laser melted parts of superalloy IN718 N2 - Additive Manufacturing (AM) by Selective Laser Melting (SLM) offers ample scope for producing geometrically complex parts in comparison to the traditional subtractive manufacturing strategies. Developing during the manufacturing process, residual stresses may limit the application of SLM parts by reducing the load bearing capacity as well as induce unwanted distortion depending on the boundary conditions specified in manufacturing. The present study aims to evaluate the bulk residual stresses in SLM parts by using neutron diffraction measurements performed at E3 line -BER II neutron reactor- of Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. Together with microstructure characterization and distortion measurements, it is possible to describe the stress state throughout the whole sample. The sample was measured in as-build condition (on a build plate) and after releasing from the build plate. The used material is the nickel based superalloy 718. This alloy is widely used in aerospace and chemical industries due to its superior corrosion and heat resistant properties. Obtained results indicated different residual stress states for each of the transversal, longitudinal and normal component. The normal and transversal component exhibits a rather compressive behavior while the longitudinal was tensile in the center part of the sample and became compressive towards the tip. As expected, the absolute values of all stress components decreased after releasing the sample from the building plate. A surface scan utilizing a coordinate-measuring machine (CMM) allowed us to present top surface distortion before and after releasing. The top surface showed a distortion around ±80µm after releasing. Microstructure evolution in the scanning-building cross-section is largely dominated by columnar grains. In addition, many small random orientated grains are prominent in the regions of a laser overlap during SLM. In summary, for the sample of superalloy 718 manufactured by SLM, a small distortion occurred when removing the sample from the build plate whereby the residual stress state decreases. Moreover, the observed columnar grains in the building direction could give a reason for the lowest stress values in that normal direction. However, the most important parameter controlling the residual stresses is the temperature gradient. Hence, future investigations are planned for a different scan strategy to distribute the laser impact in a more homogenous manner. T2 - 19th HERCULES Specialized Course CY - Grenoble, France DA - 15.05.2017 KW - Additive manufacturing KW - Selective laser melting KW - Residual stresses KW - Distortion KW - Microstructure PY - 2017 AN - OPUS4-40388 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stegemann, Robert T1 - Evaluation magneto-mechanischer Effekte in hochauflösenden Magnetfeldmessungen durch Neutronendiffraktion N2 - Die mechanische Spannung ist ein maßgeblicher Parameter ferromagnetischer Materialien. Wird ein solches Material unter die Curie Temperatur abgekühlt, zerfällt es spontan in nahezu selbstgesättigte magnetische Domänen. Diese Magnetisierung führt gleichzeitig zu einer Verformung der mit ihr gekoppelten Kristallgitter. Ein Effekt der auch reziprok gilt: wird die Gitterverformung durch eine Spannung behindert ändert sich zwangsweise der magnetische Zustand. Man kann annehmen, dass zwischen unterschiedlichen, für sich aber homogen verspannten Werkstoffbereichen, lokale magnetische Streufelder auftreten, weil magneto-mechanische Effekte eine Inkompatibilität der Domänenstruktur induzieren. Bekanntlich bilden sich Spannungsgradienten nach Schweißprozessen durch ungleichmäßigen Wärmeeintrag, thermischer Dehnung, und unterschiedlichen Abkühlraten aus. Unter dieser Prämisse untersuchen wir Wolfram-Inertgas geschweißte Blindnahtproben (250x100x4,8 mm^3) aus einem hypereutektoiden Baustahl. Der Spannungszustand der Proben wurde anhand von Neutronendiffraktometrie (ND) am Instrument E3 am Reaktor BERII (Helmholzzentrum Berlin, HZB) charakterisiert. ND ist ein Referenzverfahren für die quantitative Bestimmung von elastischen Dehnungen in kristallinen Materialien, deren Gitter selbst der Messmaßstab ist. Die Auswertung zeigt hohe Längsspannungen mit lokalen Maxima in Größenordnung von 600 MPa, die von umgebenen Druckspannungszonen kompensiert werden. Zur Detektion der magnetischen Kleinststreufelder verwenden wir speziell designte GMR-Sensorik (GMR - Giant Magneto Resistance), die aufgrund der geringen Größe ihrer aktiven Sensorelemente hohe Ortsauflösung mit Sensitivität vereint. Die Visualisierung der Messergebnisse lässt eine klare magnetische Mikrostruktur der Schweißnähte erkennen, in der die Streufelder lateral in Größenordnung des Erdmagnetfeldes variieren (~50 µT). Wir zeigen durch einen Vergleich beider Messverfahren, dass lokale magnetische Streufeldmaxima in hohem Maße mit den Spannungsgradienten übereinstimmen. T2 - DGZfP-Jahrestagung CY - Koblenz, Germany DA - 22.05.2017 KW - WIG-Blindschweißnaht KW - GMR-Sensorik KW - Neutronendiffraktion KW - Eigenspannungen PY - 2017 AN - OPUS4-40370 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiede, Tobias T1 - Influence of deposition hatch length on residual stress in selective laser melted Inconel 718 N2 - Additive Manufacturing (AM) by Selective Laser Melting (SLM) offers ample scope for producing geometrically complex parts in comparison to the traditional subtractive manufacturing strategies. Developing during the manufacturing process, residual stresses may limit the application of SLM parts by reducing the load bearing capacity as well as induce unwanted distortion depending on the boundary conditions specified in manufacturing. The present study aims to evaluate the bulk residual stresses in SLM parts by using neutron diffraction measurements performed at E3 line -BER II neutron reactor- of Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. Together with microstructure characterization and distortion measurements, it is possible to describe the stress state throughout the whole sample. The sample was measured in as-build condition (on a build plate) and after releasing from the build plate. The used material is the nickel based superalloy 718. This alloy is widely used in aerospace and chemical industries due to its superior corrosion and heat resistant properties. Obtained results indicated different residual stress states for each of the transversal, longitudinal and normal component. The normal and transversal component exhibits a rather compressive behavior while the longitudinal was tensile in the center part of the sample and became compressive towards the tip. As expected, the absolute values of all stress components decreased after releasing the sample from the building plate. A surface scan utilizing a coordinate-measuring machine (CMM) allowed us to present top surface distortion before and after releasing. The top surface showed a distortion around ±80µm after releasing. Microstructure evolution in the scanning-building cross-section is largely dominated by columnar grains. In addition, many small random orientated grains are prominent in the regions of a laser overlap during SLM. In summary, for the sample of superalloy 718 manufactured by SLM, a small distortion occurred when removing the sample from the build plate whereby the residual stress state decreases. Moreover, the observed columnar grains in the building direction could give a reason for the lowest stress values in that normal direction. However, the most important parameter controlling the residual stresses is the temperature gradient. Hence, future investigations are planned for a different scan strategy to distribute the laser impact in a more homogenous manner. T2 - HZB User Meeting 2017 CY - Berlin, Germany DA - 15.12.2017 KW - AM KW - SLM KW - IN 718 KW - Neutron diffraction KW - Residual stress KW - Hatch length KW - Microstructure PY - 2017 AN - OPUS4-43475 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Röhsler, Andreas T1 - The use of time-of-flight secondary ion mass spectrometry for the investigation of hydrogen-induced effects in austenitic steel AISI 304L N2 - In the course of 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 scientific community alike. The storage and transport of hydrogen, which is nowadays mainly realised by austenitic stainless steels, remains problematic. That is due to the degradation of mechanical properties and the possibility of phase transformation by hydrogen diffusion and accumulation. Development of materials and technologies requires a fundamental understanding of these degradation processes. Therefore, studying the behaviour 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 (ToF-SIMS) was conducted after electrochemical charging. To obtain furthermore information about the structural composition and cracking behaviour, electron-backscattered diffraction (EBSD) and scanning electron microscopy (SEM) were performed. Gathered data of chemical composition and topography was 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 behaviour, as well as solubility, allow nonetheless to draw conclusions from the experiments. T2 - SIMS21 CY - Krakau, Poland DA - 11.09.2017 KW - Austenitic stainless steel KW - ToF-SIMS KW - Hydrogen PY - 2017 AN - OPUS4-42315 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Butz, Adam T1 - Experimental and analytical investigation of notched components of a Nickel based superalloy under high temperature cyclic loading N2 - While the increase in use of renewable energy sources is a necessity in times of climate change the use of gas turbines as back-up requires them to be run in a much more flexible manner in order to compensate for side effects like sudden fluctuations of energy generation. The significant changes of stress and temperature levels in turbine blades due to start-up and shut down can cause crack initiation and growth in the blades‘ alloy. The aim of this research project is to identify a model for lifetime prediction for gas turbine components made of a Nickel base superalloy under high temperature with a Focus on stress concentration points such as cooling holes. T2 - HIDA-7 Conference on Life/Crack Assessment & Failures in Industrial Structures, UK CY - Portsmouth, UK DA - 15.05.2017 KW - LCF KW - Gas turbine KW - Service life model PY - 2017 AN - OPUS4-42274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saloga, Patrick E. J. T1 - Do non-thermal effects exist? - Microwave-assisted acceleration of silver nanoparticle synthesis and particle growth N2 - Ever since increasing a reaction’s yield while shortening the reaction time is the main objective in synthesis optimization. Microwave reactors meet these demands. In literature however their usage is under discussion due to claims of the existence of non-thermal effects resulting from the microwave radiation. Especially for nano-material syntheses it is of crucial importance to be aware of influences on the reaction pathway. Therefore, we compare ultra-small silver nanoparticles with mean radii of 3 nm, synthesized via conventional and microwave heating. We employed a versatile one-pot polyol synthesis of poly(acrylic acid) (PAA) stabilized silver nanoparticles, which display superior catalytic properties. No microwave specific effects in terms of particle size distribution characteristics, as derived by small-angle X-ray scattering (SAXS) and dynamic light scattering (DLS), are revealed. Due to the microwave reactor’s characteristics of a closed system, syntheses can be carried out at temperatures beyond the solvent’s boiling point. Particle formation was accelerated by a factor of 30 by increasing the reaction temperature from 200 °C to 250 °C. The particle growth process follows a cluster coalescence mechanism. A post-synthetic incubation step at 250 °C induces a further growth of the particles while the size distribution broadens. Thus, utilization of microwave reactors enables an enormous decrease of the reaction time as well as the opportunity of tuning the particles’ size. Possibly, decomposition of the stabilizing ligand at elevated temperatures results in reduced yields. A temperature of 250 °C and a corresponding reaction time of 30 s represent a compromise between short reaction times and high yields. T2 - 5th Nano Today Conference CY - Waikoloa Village, HI, USA DA - 06.12.2017 KW - Microwave synthesis KW - Small-angle scattering KW - Silver nanoparticles PY - 2017 AN - OPUS4-43497 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Theiler, Geraldine T1 - On the sliding behavior of PAEK composites in vacuum environment N2 - The tribological behavior of PAEK composites were investigated in air and vacuum environment. Results indicate that the tribological performance of these compounds depends on material compositions, fiber orientation as well as test conditions. In vacuum, very low friction and wear coefficient were obtained at low sliding speed while severe wear occurred at high speed. T2 - The 6th World Tribology Congress - WTC 2017 CY - Beijing, China DA - 17.09.2017 KW - PAEK KW - Sliding performances KW - Vacuum PY - 2017 AN - OPUS4-42447 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tschiche, Harald T1 - Determination of degradation products of thermoplastic polyurethane using fluorescent sensors in a model system N2 - Polyurethanes (PU) are formed by polyaddition reaction between diols and diisocyantes. They can be formed utilizing three building blocks, namely a polyol or long-chain diol, a chain extender or short-chain diol, and a diisocyanate. The derived multi-phase block copolymer has thermoplastic properties and is called thermoplastic PU (TPU). This modular approach allows for a variety of alternations yielding a broad range of structural properties and applications. TPUs are based on three main classes of polyols, i.e. polyethers, polyesters, and polycaprolactones. With these different polyols and the ability of changing the ratio of building blocks a variety of material properties can be obtained thus TPUs find numerous applications in e.g. lightweight construction1, insulation, flame retardants, lacquer and glue, as well as medicine. Linear, isocyanate terminated, polyurethane prepolymers prepared from non-equivalent amounts of diisocyanate such as methylene diphenyl diisocyanate (MDI) attached to a polyol are widely used as precursors of the correspondent polymers. Chain-extending reactions with low molecular weight compounds bearing different amounts of active hydrogens enable both linear and crosslinked polyurethane to be formed. Due to TPUs being used in a broad range of applications facing a variety of stress (e.g. mechanical, hydrolytic, thermal, radiative/UV, as well as its combinations) the complexity of possible degradation mechanism is high. A functional group derived from degradation of the bulk matrix can be detected utilizing a suited fluorogenic sensor molecule. There are several fluorogenic dyes known for the application as sensor for amine groups e.g. fluorescamine, pyrylium dyes, deriving a fluorescent signal upon reaction. T2 - ANAKON 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Bewitterung KW - Polyurethan KW - Functional group detection KW - Polyurethanes PY - 2017 AN - OPUS4-40262 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulla, Hannes T1 - In situ investigations of a mechanochemical cocrystal formation by X-ray diffraction for two different milling jar materials N2 - Mechanochemistry has become a valuable method for the synthesis of new materials, especially for pharmaceutical cocrystals. The Advantages of fast reactions in high purity and yield face a lack of understanding the underlying mechanism. Therefore, in situ setups to study mechanochemical reactions have been established. Herein, we present an in situ investigation of the mechanochemical cocrystal formation of pyrazinamide (PZA) with pimelic acid (PM) using synchrotron XRD. Two new polymorphs of PZA:PM (1:1) were synthesized by milling the starting materials in milling jars of different materials. While Form I is only obtained using a steel jar, Form II can be obtained purely in jars made of Perspex. In situ XRD experiments reveal a direct formation of Form II in Perspex and an intermediate formation of Form II in steel jars converting to Form I upon further grinding. Heating experiments and DFT calculations predict that Form II is the thermodynamically more stable polymorph. Therefore, the reaction progress in the steel jar contradicts Ostwald’s rules of stages as the more stable Form II converts into the metastable Form I. Hence, mechanochemistry offers the possibility to synthesize new materials that cannot be obtained using conventional methods. T2 - Adlershofer Forschungsforum 2017 CY - HU-Berlin, Erwin-Schrödinger Zentrum, Germany DA - 10.11.2017 KW - Cocrystal KW - Mechanochemistry KW - Polymorph KW - In situ KW - Milling PY - 2017 AN - OPUS4-42956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piedada, F. M. T1 - Polymorphism in Simvastatin: A Single Crystal X-ray Diffraction, Themodynamic, and MDSimulation Study N2 - Simvastatin is a prominent member of the statin family, a class of antilipidemic drugs widely used in the treatment of high plasma cholesterol levels, and thus in the prevention of atherosclerosis and cardiovascular diseases. Simvastatin is typically employed as a solid and it is well known that, in this case, the detection and characterization of polymorphism is of considerable importance. Polymorphs differ by their packing arrangements and also, occasionally, by the conformations of the molecules in the crystal lattice. These structural variations are normally reflected by differences in physical properties, such as solubility and dissolution rate in a given media, which may significantly affect the bioavailability of a drug. The lack of control of polymorphism can, therefore, play havoc with the safe use of a drug. T2 - COST Action CM1402 CY - Lincoln, United Kingdom DA - 26.06.2017 KW - Polymorphism KW - X-ry Diffraction PY - 2017 AN - OPUS4-41252 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nguyen, Thi Yen T1 - Guided crystallization: The influence of solvent and concentration N2 - Theoretical and experimental studies indicate that crystal nucleation can take more complex pathways than expected on the ground of the classical nucleation theory. A direct in situ observation of the different pathways of nucleation from solution is challenging since the paths can be influenced by heterogeneous nucleation sites, such as container walls. The custom-made acoustic levitator using in these experiments regulates the influence that solid surfaces, temperature, and humidity have on the crystallization process. The investigations of the crystallization process of paracetamol were performed with in situ analytical techniques and theoretical simulations to gain a comprehensive insight into processes, occurring intermediates, and required reaction conditions. The targeted choice of the solvent and the concentration enabled the guidance of the pathways, therefore, resulting in the isolation of one desired crystalline structure. T2 - Annual COST meeting CY - Lincoln, United Kingdom DA - 25.06.2017 KW - Crystallization KW - Polymorphism KW - Molecular dynamic simulation KW - Pair distribution function analysis KW - XRD PY - 2017 AN - OPUS4-41111 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Castro, R. A. E. T1 - New cocrystals of bexarotene with pyridinecarboxamide isomers sustained by the acid∙∙∙aromatic nitrogen supramolecular heterosynthon N2 - Pharmaceutical cocrystals are homogenous crystalline structures made up of two or more components in a definite stoichiometric ratio, where at least one of the components in the crystal lattice is an active pharmaceutical ingredient (API).1 Pharmaceutical cocrystals have opened the opportunity for engineering solid-state forms designed to have tailored properties to enhance drug product bioavailability and stability, as well a enhance processability of the solid material inputs in drug product manufacture. In this work the cocrystallization of bexarotene, an approved API by the U.S. Food and Drug Administration that belongs to Biopharmaceutics Classification System Class II (low solubility–high permeability), with pyridine carboxamide isomers (picolinamide, nicotinamide and isonicotinamide) was successfully undertaken. The synthesis was achieved by liquid assisted grinding (LAG) and the solids obtained were characterized by differential scanning calorimetry (DSC), infrared spectroscopy (FTIR-ATR), powder X-ray diffraction (XRPD), single crystal X-ray diffraction (SXD), and polarized light thermomicroscopy (PLTM). For bexarotene: picolinamide and bexarotene:isonicotinamide, 1:1 cocrystals were obtained directly from milling. SXD data of bexarotene:isonicotinamide cocrystal reveal acid∙∙∙aromatic nitrogen supramolecular heterosynthon and that the homosynthon amide∙∙∙amide in isonicotinamide is preserved. The bexarotene:nicotinamide mixtures prepared by ball milling give rise to simple binary solid–liquid phase diagram with an eutectic point, well described by the Schröder-van Laar equation. Melt crystallization of the 1:1 mixture gives rise to a cocrystal for which a complex phase behaviour is observed. T2 - 6th Meeting IAPC CY - Zagreb, Croatia DA - 04.09.2017 KW - Crystalline structure KW - Bexarotene KW - Powder X-ray diffraction KW - Single crystal X-ray diffraction KW - Infrared spectroscopy PY - 2017 AN - OPUS4-41063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nützmann, Kathrin T1 - Depth dependent phase identification of corrosion zones in ferritic alloys by micro-X-ray absorption near edge structure spectroscopy N2 - Ferritic steels with chromium contents up to 13 wt% are used as materials for power plant components as boiler materials (< 2 wt% Cr) and super heater tubes (> 9 wt% Cr). These materials are subject to aggressive corrosion caused by hot gases such as CO2, H2O, O2 and SO2. Especially SO2 causes fatal corrosion even as a minor component. To examine sulfurous corrosion mechanisms, experiments with pure SO2 were conducted. A proper analysis of the material changes requires phase identification and quantification with a high lateral resolution within the corrosion scale. T2 - ANAKON2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Corosion KW - Steel KW - XANES PY - 2017 AN - OPUS4-40415 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Breitfeld, Steffen T1 - High energy ball milling of a new representative of coordination polymers without organofluorine linkers N2 - Metal organic frameworks and coordination polymers play an important role in different fields of applications. Moreover, particularly fluorinated metal-organic frameworks (FMOFs) are in the focus of interest during the last years. In most cases, fluorine is implemented using perfluorinated organic linkers at the synthesis, usually performed by solvothermal synthesis. However, only few examples are known so far where fluorine is coordinated directly to the metal cation. Recently, we reported about mechanochemical syntheses and characterization of fluorine-containing coordination polymers of alkaline earth metals by milling M(OH) (M: Ca, Sr, Ba) with fluorinated benzene dicarboxylic acids 2 and we reported about mechanochemical syntheses of alkaline earth metal fluorides with ammonium fluoride. Now we are reporting about a combination of both synthesis routes. That is the first mechanochemical synthesis of coordination polymers where fluorine is coordinated directly to the metal cation. T2 - Konferenz CY - Berlin, Germany DA - 30.11.2017 KW - Metal organic frameworks KW - Coordination polymer KW - Mechanochemical syntheses KW - Direct fluorine-metal bond KW - Alkaline earth metal PY - 2017 AN - OPUS4-46898 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Li, Wei T1 - Crack propagation in filled and unfilled polymers: Separation of surface energy and irreversible deformation energy N2 - Fiber-reinforced-polymers (FRPs) are in current research focus in the lightweight construction industry, because of their extraordinary characteristics (stiffness and strength-to-density relation). The structure of polymer matrix and the interaction with reinforcement are crucial for optimization of the mechanical and thermal properties of FRPs. Due to the macromolecular chain structure, the mechanical properties of a polymer strongly vary with temperature: Below the glass transition, the chain segments of a polymer are “frozen”. Regarding fracture, the total changed energy during fracture if only dissipates for the generation of the new surfaces. However, in the region of the glass transition, the polymer chain segments start to get “unfrozen”, and the energy is not only required for generating new surfaces, but also for irreversibly deformation. This irreversible deformation is affected by the global temperature and the local temperature near the crack tip, which is affected by the local strain rate and crack propagation velocity. Hence, in this research project, the irreversible deformation of neat and reinforced polymers will be controlled by changing the global temperature as well as the local temperature. With using different fracture experiments, the amount of energy required for creating new surfaces and for the irreversible deformation will be separated. The fracture tests include the conventional tensile test, the macroscopic peel test and the single fiber peel – off test. T2 - PhD Day 2018 of BAM CY - Berlin, Germany DA - 31.05.2018 KW - Crack Propagation KW - Polymer PY - 2018 AN - OPUS4-48471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -