TY - CONF A1 - Holzweber, Markus A1 - Sobol, Oded A1 - Wirth, Thomas A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang T1 - Deuterium permeation and cracking in duplex steels as viewed by ToF-SIMS and HR-SEM with data fusion N2 - Better understanding of hydrogen assisted degradation and trapping mecha-nisms requires sufficient imaging techniques for respective hydrogen-microstructure interaction studies, in particular with multi-phase metallic micro-structures [1]. The present work is focusing on the elucidation of deuterium be-havior in two austenitic-ferritic duplex stainless steels (DSS) under the assumption that deuterium behaves in many ways similarly to hydrogen [2]. For case studies standard 2205 and lean 2101 DSSs were chosen due to the extensive use of these steels in industry [3]. The analyses were conducted by using a novel in-situ permeation and Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) imaging technique or by ex-situ ToF-SIMS imaging following electrochemical charging experiments. Another pioneering procedure was data fusion (including chemometry) of results of powerful laterally resolved chemical analysis and high resolution structural characterization techniques . Results for the ex-situ observations showed a different influence of deuterium loading on the two steel grades as well as different damage mechanisms in each phase. Formation of sub-surface blisters between the ferrite and austenite were obtained in both the standard and the lean DSS. In both steels, an increased deuterium concentration was observed around deformed regions such as cracks, confirming that they originate from the presence of deuterium [4]. The formation of parallel cracks was obtained only in the austenite within the standard duplex whereas in the lean duplex the highest intensity of deuterium was obtained in the austenite along the ferrite-austenite interphase. In comparison, application of the novel in-situ permeation technique enabled to register and record the deuterium permeation through the material and the respective saturation sequence of the two phases as well as the interfaces. Faster diffusion of the deuterium was observed in the ferrite and a direct proof for deuterium enrichment at the austenite-ferrite interface has been given [1]. The integration of the specified techniques gives a better insight into the processes leading to hydrogen induced failure. These two experimental techniques provide very valuable tools for elucidation of respective metallurgical failure mechanisms that can be used for the validation of respective numerical models for hydrogen assisted cracking (HAC). T2 - 19. Arbeitstagung Angewandte Oberflächenanalytik CY - Soest, Germany DA - 05.09.2016 KW - ToF-SIMS KW - Hydrogen assisted cracking KW - Data fusion KW - SEM PY - 2016 AN - OPUS4-37484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bäßler, Ralph T1 - Evaluation of metallic materials for geothermal applications N2 - Since geothermal wells are a feasible energy source to replace fossil fuel supply, many technologies have been developed to take advantage of geothermal energy. Nevertheless, service conditions in geothermal facilities are due to the chemical composition of hydrothermal fluids and temperatures, in many cases, extreme in terms of corrosion. Therefore, materials selection based on preliminary material qualification is essential to guarantee a secure and reliable operation of the facilities. The corrosion behavior of different high-alloyed metals including Duplex and austenitic stainless steels as well as a nickel alloy have been evaluated in artificial geothermal fluids simulating the conditions in some locations with geothermal potential in Germany as well as two sites in Indonesia. The suitability of carbon steel 25CrMo4, stainless steels X2CrNiMo17-12-2, X2CrNiMo-22-5, X2CrNiMoCuWN25-7-4 and super austenitic steel X1CrNiMoCu32-28-7 in these geothermal fluids obtained by electrochemical measurements and exposure tests is limited. The nickel alloy NiCr23Mo16Al shows an excellent corrosion resistance against pitting corrosion. Excluding its high cost, it is a very good alternative to be used in the construction of geothermal facilities having highly saline brines. Stainless and Duplex steels exhibit a limited corrosion resistance concerning pitting and crevice corrosion. Beside of the higher alloyed materials, also the lowalloyed steel 25CrMo4 could be employed as a constructional material for the geothermal power plant in stagnant highly acidic non Saline environments, as long as the wall thickness of the material vs. corrosion rate is taken into account. T2 - European Geothermal Congress CY - Strasbourg, France DA - 19.09.2016 KW - Localized corrosion KW - Stainless steel KW - Ni-based alloy KW - Geothermal energy PY - 2016 AN - OPUS4-37751 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hübert, Thomas A1 - Kemnitz, Erhard T1 - Wood protection with nanoparticles: MgF2 and CaF2 N2 - The potential of alkaline earth metal Fluoride nanoparticles was tested for protection of wood against fungi and termites. These nanoparticles are ideal for wood protection. T2 - School of Analytical Sciences Poster Session CY - Berlin, Germany DA - 06.12.2016 KW - Wood preservation KW - Fluorides KW - Nanoparticles PY - 2016 AN - OPUS4-39141 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Menzel, Friederike T1 - Semi-automated statistical quantification of initial colonization of bacteria on different materials under standardized conditions N2 - The formation of biofilms on different materials provokes high costs in industrial processes, as well as in medical applications. Therefore, the interest in development of new materials with improved surfaces to reduce bacterial colonization rises. In order to evaluate the quality and safety of these new materials, it is highly important to ensure world-wide comparable tests that are relying on statistical evidence. The only way to reach this statistical safety is through a high-throughput Screening under standardized test conditions. We developed a flow through system for cultivation of biofilm-forming bacteria under controlled conditions with a total capacity for testing up to 32 samples in parallel. Quantification of the surface colonization was done by staining the bacterial cells with a fluorescence marker, followed by epifluorescence microscopy. More than 100 images of each sample were automatically taken and the surface coverage was estimated with the free open source software gmic (http://gmic.eu), followed by a precise statistical evaluation. Overview images of all gathered pictures of the whole material coupon were generated to illuminate the colonization characteristics of the selected bacteria on certain materials. With this method, differences in bacterial colonization on different materials can be quantified in a statistically validated manner. The innovative and solid test procedure will support the design of improved materials for medical and industrial applications such as implants, ship hulls, pipelines, heat exchangers, aquaculture equipments, photovoltaic-panels and fundaments of wind power plants. T2 - Vereinigung für Allgemeine und Angewandte Mikrobiologie - Jahrestagung 2016 CY - Jena, Germany DA - 13.03.2016 KW - Biofilm cultivation KW - Image analysis KW - Microscopy PY - 2016 AN - OPUS4-37724 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Armatys, Kamila T1 - Corrosion and abrasion resistant protective coatings for biomass combustion N2 - One of the alternative renewable fuels is biomass but it is a difficult fuel because of its diversity and complexity. It can contain high percentages of K and Cl responsible for corrosion together with sand that have additionally an abrasive effect during combustion. Because of permanently extending the surface reaction due to abrasion the corrosion of the materials increases. In particular in power plants, the superheater tubes are exposed to a corrosive abrasive attack that is one of the main sources of concern. The development of new alloys for multilayer surface, which combines corrosive and abrasive resistance is therefore of high importance. Those new technical approaches must be at the same time cost-effective to be an alternative to conventional materials. The aim of the presented investigation methods is to test and develop suitable alloys for coatings for the super heater tubes of biomass power plants. First results of abrasion investigations show improved abrasion resistance compared to the multi-component reference material Alloy 625. T2 - Young Researchers Conference: Energy Efficiency & Biomass CY - Wels, Austria DA - 24.02.2016 KW - Coatings KW - Corrosion PY - 2016 AN - OPUS4-35713 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Peplinski, Burkhard T1 - Nanocrystalline and stacking-disordered beta-cristobalite AlPO4 stabilized at room temperature: synthesis and X-ray powder diffraction data N2 - X-ray powder diffraction (XRD) patterns of the high-temperature (HT) cristobalite form of SiO2 and its isoelectronic AlPO4 analogue are essentially influenced by the dynamic disorder of these crystal structures. The nature of this disorder and of the phase transition between the α- and β-form has been the subject of intensive research during the last four decades [1]. By 1989 it became possible to stabilize the HT-form of cristobalite SiO2 at room temperature in laboratory and engineering ceramic industries by applying solid solution forming techniques [2]. However, for the HT-form of cristobalite AlPO4 nothing similar has been known until 2014 when it was discovered that nanocrystalline and stacking-disordered β-cristobalite AlPO4 is the major component of the fly ash of a large incineration facility operated by the waste water treatment authorities of Frankfurt/M. [3]. Previous comprehensive investigations of this fly ash failed to interpret its complex XRD pattern – presumably mainly due to the lack of a matching experimental digital pattern in the Powder Diffraction Database. The present paper reports on a synthesis route that facilitates the crystallization of nanocrystalline and stacking-disordered β-cristobalite AlPO4 that is free of crystalline impurity phases and long-term stable at ambient. Its room temperature XRD pattern is presented with parameters traced back to certified reference materials. [1] Yuan F. and Huang L., Phys. Rev, B, 2012, 85, 134114. [2] Perrotta J.A., Grubbs D.K., Martin E.S., Dando N.R., McKinstry H.A. and Huang C.-Y., J. Am. Ceram. Soc., 1989, 72, 441. [3] Peplinski B., Adam C., Adamczyk B., Müller R., Michaelis M., Krahl Th. and Emmerling F., Powder Diffraction Journal, 2015, 30, 2, Supp. 1, S31. T2 - 15. European Powder Diffraction Conference (EPDIC15) CY - Bari, Italy DA - 12. June 2016 KW - Stabilization of HT-structures at room temperature KW - β-cristobalite structure type KW - Databases PY - 2016 AN - OPUS4-36727 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Electron irradiation of biomolecules under physiological conditions: Experimental realization and microdosimetric calculations N2 - In the last years, secondary low-energy electrons (LEE) emerged as important, if not predominant, reductive pathway in ionizing damage of biomolecules. These electrons are created in copious amount as result of inelastic scattering of high energy radiation at water. Until now, all experiments the quantification of the effects of LEEs on the biomolecular damage was either performed in vacuum with LEE sources or with DNA on surfaces in humid atmosphere. We present a new experimental setup to irradiate biomolecules with electrons under physiological conditions. In combination with monte carlo simulations this setup makes it possible to determine microdosimetric quantities for biomolecules in liquid environment under electron irradiation. This opens up new possibilities in radiation research to access the LEE damage under well defined physiological condition, for more complex systems, such as DNA-Protein complexes and even living cells. T2 - 14th International Congress of the International Radiation Protection Association CY - Cape Town, South Africa DA - 09.05.2016 KW - DNA KW - Dosimetry KW - Microdosimetry KW - Geant4 KW - Low energy electrons KW - Radicals KW - Radiation damage KW - Polymers PY - 2016 AN - OPUS4-36399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lauer, Franziska T1 - Multivariate statistics applied to MALDI-TOF MS data of pollen samples N2 - Current pollen screening information networks are based on time-consuming, microscopic determination of the genus-specific pollen morphology. Additionally, the given information relies on prediction of plant growth, wind direction and seasonal information. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) was introduced for rapid analysis of complex biological samples. MALDI-TOF provides the possibility to measure species-specific mass peak patterns of pollen and offers a powerful tool for investigation of taxonomic relations. Our objective is to develop a fast, reliable, routine method for detecting single pollen grains in pollen mixtures. The obtained spectra are analyzed by multivariate statistics. T2 - 49. Jahrestagung der Deutschen Gesellschaft für Massenspektrometrie CY - Hamburg DA - 28.02.2016 KW - Pollen KW - Datenanalyse KW - Hauptkomponentenanalyse PY - 2016 AN - OPUS4-35523 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bäßler, Ralph T1 - Korrosion von Rohrleitungswerkstoffen durch Kondensationseffekte infolge von SO2- und NO2-Begleitstoffen in CO2 N2 - Derzeit wird der Einsatz metallener Werkstoffe in CCU-/CCS-Anlagen hinsichtlich deren Korrosionsbeständigkeit und eine eventuell daraus resultierende Herausforderung diskutiert. Während des CO₂-Transportes vom Abscheide- zum Injektionsort kann es aufgrund der den CO₂-Strom begleitenden Beimengungen, wie Wasser, O₂, SOₓ , NOₓ , Temperaturschwankungen durchaus zu Kondensationseffekten und daraus resultierenden Schäden kommen. Es konnte gezeigt werden, dass die sich möglicherweise innerhalb einer CO₂-Rohrleitung bildenden Kondensate infolge von Begleitstoffen wie SO2 und NO2 eine viel korrosivere Wirkung auf Rohrleitungswerkstoffe entfalten, als in reinem CO₂. T2 - 48. Kraftwerkstechnisches Kolloquium CY - Dresden, Germany DA - 18.10.2016 KW - CO2-Korrosion KW - Edelstahl KW - Chromstahl KW - CCUS KW - Kondensation PY - 2016 AN - OPUS4-37753 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bäßler, Ralph T1 - Hochlegierte metallene Werkstoffe in Salzschmelzen N2 - In letzter Zeit kommen immer mehr alternative Energiequellen als Ersatz fossiler Brennstoffe zum Einsatz, so auch die Solarthermie. Jedoch sind die Betriebsbedingungen aufgrund der chemischen Zusammensetzung der Wärmeträgermedien und herrschenden Temperaturen extrem hinsichtlich Korrosion. Da die Kraftwerke bei maximaler Lebensdauer ökonomisch vertretbar sein müssen, ist eine Werkstoffauswahl basierend auf Voruntersuchungen notwendig, um einen sicheren und verlässlichen Betrieb dieser Anlagen zu gewährleisten. Die Werkstoffauswahl hängt von der Betriebstemperatur eines Kraftwerks bzw. der chemischen Zusammensetzung des Wärmeträgermediums ab. In hochkorrosiven Umgebungen werden aufgrund ihrer sehr guten Korrosionsbeständigkeit Nickelbasislegierungen nicht nur für stark korrosiv beanspruchte Bauteile als die Lösung angesehen. Jedoch kann es durchaus beständigkeitsbedingte Einschränkungen für den Einsatz geben, wofür die hier vorgestellten Ergebnisse dienen sollen. In diesem Beitrag wird die Beständigkeit ausgewählter hochlegierter Werkstoffe (inklusive einer neuentwickelten Legierung in einer Nitrat-Salzschmelze (60 % NaNO3/40 % KNO3) vorgestellt, die mittels elektrochemischer Messungen und Auslagerungsversuchen ermittelt wurde. T2 - 48. Kraftwerkstechnisches Kolloquium CY - Dresden, Germany DA - 18.10.2016 KW - Örtliche Korrosion KW - Nickelbasislegierungen KW - Solarenergie KW - Erneuerbare Energien KW - Elektrochemische Charakterisierung PY - 2016 AN - OPUS4-37754 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kömmling, Anja T1 - Discoloration effects of high-dose γ-irradiation and long-term thermal ageing of (U)HMW-PE N2 - Two polyethylene types with ultra high (UHMWPE) and high molecular weight (HMWPE), which are used as neutron radiation shielding materials in storage casks for radioactive waste, were subjected to gamma irradiation doses up to 600 kGy and subsequent thermal ageing at 125 °C for up to one year. One material was a medical grade UHMWPE and the other a HMWPE containing an antioxidant. Degradation effects in the materials were characterized using colorimetry, UV-Vis spectroscopy, MIR and FTIR measurements, DSC and, in the case of HMWPE, insoluble content determination. Both materials exhibited a yellowing upon irradiation. The discoloration of UHMWPE disappeared again after thermal ageing, which is why it was attributed to annealable color centers in the form of free radicals entrapped in the crystalline regions of the polymer that recombine during thermal ageing. Furthermore, oxidation species were observed with MIR and FTIR spectroscopy. For HMWPE, the yellowing occurred during both irradiation and thermal ageing and was correlated to antioxidant decomposition. Additionally, black spots were observed after thermal ageing of HMWPE that were attributed to reaction products of antioxidant derivatives and catalyst residues. While only little evidence of oxidation species was found in the light material parts, oxidation is expected to concentrate in the black spots as the catalyst residue promotes hydroperoxide decomposition and thus radical formation that initiate polymer oxidation T2 - Ionizing Radiation and Polymers Conference CY - Giens, France DA - 25.09.2016 KW - Polyethylene KW - Gamma-irradiation KW - Yellowing KW - Degradation PY - 2016 AN - OPUS4-38001 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hertwig, Andreas T1 - Measurement of Porous TiO2 Layers with spectroscopic ellipsometry – a multi-method study N2 - By means of an effective medium (EMA) based approach, it is possible to use spectroscopic ellipsometry to determine the mixing ratios between air and material in porous dielectrics and calculate a quantitative value of the porosity for these materials. As this method is model-based, it is very difficult to provide a quantitative measure for the accuracy of porosity values determined by this method. Valuable additional information can often be obtained by combining ellipsometry with other complementary methods. In the present study, the ellipsometry results were validated by Electron Probe Microanalysis (EPMA) with the option of layer analysis (by the socalled “STRATAGem” approach), gravimetry, and electron microscopy. We analysed porous TiO2 thin layers synthesised by means of a template synthesis approach (evaporation induced self assembly). Ellipsometry measurements on porous samples are difficult to analyse due to the complexity of the models necessary. Often it is difficult to decide if the measured data contains enough information to successfully determine the target quantities (mixing ratio, dielectric function of the matrix material). One method to decrease the complexity of the fit and therefore use the measurement data most efficiently is a multi-sample analysis. In the present case, multi-sample analysis was used for determining the porosity factors of the individual layers while using one common set of dielectric function values for the matrix in all cases. While the results of the fit analysis in this case can be used to show the feasibility and also the limitations of the multi-method approach, the porosity values themselves show a promising agreement between the independent methods. It can therefore be concluded that determining porosity values with ellipsometry is in accordance to other methods to the level of accuracy provided by the complementary methodologies. T2 - International conference on spectroscopic ellipsometry (ICSE-7) CY - Berlin, Germany DA - 06.06.2016 KW - Spectroscopic Ellipsometry KW - Electron Microscopy KW - Multi-method Metrology KW - Porous Materials KW - Thin Films KW - Titanium Dioxide PY - 2016 AN - OPUS4-37202 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rockenhäuser, Christian T1 - Microstructure evolution in aluminium alloy 2618 A during ageing and creep N2 - The Microstructure Evolution in Aluminium Alloy 2618 A during Ageing and Creep was presented and discussed. T2 - Microscopy & Microanalysis 2016 CY - Columbus, OH, USA DA - 24.07.2016 KW - Aluminium alloys KW - Coarsening KW - Transmission electron microscopy PY - 2016 AN - OPUS4-38268 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana T1 - The role of reinforcement orientation on the damage evolution of short fibre reinforced metal matrix composite under compression N2 - In the present study, internal damage to an AlSi12CuMgNi alloy reinforced with planar random Al2O3 short fibres was investigated after compression testing. Due to the alloy composition, this composite contains a second reinforcement phase in the form of eutectic Si, which builds interpenetrated networks in the volume and increases the creep resistance and load-bearing capacity of the material. Materials with their fibre plane parallel and transversal to the load direction were characterized in order to investigate the dependence of load partition and damage on fibre plane orientation. In-situ compression testing during neutron diffraction measurements showed that internal damage is strongly influenced by the load partition between matrix and reinforcement. Moreover, micro-computed tomography was performed in the same material after ex-situ compression for damage analysis. In the case of a fibre plane perpendicular to the applied load, breakage and interconnected cracks appeared in a significantly higher volume fraction than with a fibre plane parallel to load. T2 - RACIRI Summer School CY - Repino, Russia DA - 22.08.2016 KW - Metal matrix composite KW - Computed tomography KW - Neutron diffraction KW - Load transfer PY - 2016 AN - OPUS4-38107 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Optimization of Solid-State-Reactions of Calcium Cobaltite Ca3Co4O9 N2 - Calcium cobaltite is a promising p-type oxide thermoelectric material for high temperature applications due to its high figure of merit between 600 °C and 900 °C in air. The solid-state-reaction is well known for large scale powder synthesis of functional materials. As a high temperature process, the powder synthesis consumes a lot of energy. In different studies, different synthesis conditions were used for the preparation of calcium cobaltite powder. This study showed that a higher energy input (elevated temperatures, longer dwell times, or repeated calcinations) during powder synthesis does not increase but decrease the Seebeck coefficient and the electrical conductivity. The same correlation was determined for the densification. As a higher energy input leads to a larger grain size and therefore to a reduced sinter activity, it can be concluded that the thermoelectric properties are correlated with the sinter activity of the powder. These results can be used to minimize the energy demand for the powder synthesis of Ca₃Co₄ O₉. T2 - 14th European Conference on Thermoelectrics CY - Lisbon, Portugal DA - 20.09.2016 KW - Thermoelectrics KW - Solid-State-Reaction KW - Calcium cobaltite PY - 2016 AN - OPUS4-37543 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas T1 - Optimizing visibility of phase gratings for Talbot-Lau X-ray imaging N2 - We investigated the efficiency of phase gratings, i.e., the visibility upon variation of different parameters. Rotating around an axis parallel to the grid lines of the phase grating changes the grating’s shape and thereby the initial distribution of phase shifts. This yields high visibilities for shorter propagation distances than derived from box shapes. Tilting the grating in the scattering plane allows continuous tuning of the grating’s height that corresponds to an ideal phase shift for a particular photon energy. This opens the way for tuning the design energy suitable for the material under investigation. Our study included simulations for monochromatic sources with the sampling procedure for rectangular and triangular phase gratings. T2 - User-Meeting CY - Berlin, Germany DA - 8.12.2016 KW - Talbot-Lau interferomerty KW - Phase grating KW - Synchrotron radiation PY - 2016 AN - OPUS4-39096 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jürgens, Maria T1 - Ermüdungsverhalten, Lebensdauer und Schädigungsprozesse von P92 unter zyklischen Betriebsbedingungen N2 - Schnelle Lastwechsel mit hohen Temperaturgradienten führen zu thermischen und mechanischen Beanspruchungen v.a. in dickwandigen Bauteilen. Daraus ergibt sich ein komplexes Lastkollektiv, bei dem der Werkstoff sowohl durch Kriechermüdung als auch durch thermomechanische Ermüdung (TMF) geschädigt wird. Welche Auswirkungen hat eine gleichzeitige Änderung von Temperatur, mechanischer Beanspruchung und Arbeitsmedium auf die Schädigungsprozesse? T2 - KWT Dresden CY - Dresden, Germany DA - 18.10.2016 KW - LCF KW - P92 KW - TMF PY - 2016 AN - OPUS4-38587 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Chatzigiannakis, Emmanouil T1 - Influence of composition on the thermal ageing behaviour of EPDM N2 - Ethylene-propylenene-diene copolymer rubbers (EPDM) are used in a wide range of sealing applications e.g. in automotive industry or in containers for dangerous goods. Investigations with regard to the ageing behavior and lifetime prediction of commercial EPDM rubber seals consisting of 48 % polypropylene (PP) and 4.1 % of 5-ethylidene-2-norbornene (ENB) were conducted [1]. However, structural parameters (monomer ratio, diene type, curing agent etc.) and additives (filler, plasticizer etc.) are known to affect the ageing behavior of rubber compounds [2, 3]. The aim of the current study was to elucidate the influence of each component on the overall deterioration of material properties after thermal ageing. Therefore, different EPDM mixtures were prepared at BAM, the reference being an EPDM with 48 % PP and 4.1 % ENB reinforced with Sillitin. Five more formulations were prepared in order to assess the effect of (i) filler type (carbon black or sillitin), (ii) curing agent (sulfur or peroxide), (iii) plasticizer, (iv) ethylene-propylene ratio and (v) ENB content. Initially, the properties of the unaged materials were investigated by tensile testing, hardness and density measurements, TGA, DSC and DMA. Sulfur vulcanization resulted in higher elongation at break due to the flexibility of the sulfidic crosslinks. Carbon black resulted in better reinforcement compared to Sillitin. A higher ethylene and ENB content lead to higher hardness due to higher crystallinity and higher crosslink density, respectively. Thermal ageing for up to 30 days (with 10 days intervals) took place in circulating hot air ovens at 125 °C. Pronounced crosslinking was found to take place in all peroxide-cured materials, as the unreacted double bonds of the ENB units acted as starting points for oxidation and crosslinking. Increasing the ethylene content resulted in an increase in the ageing resistance of EPDM. This improvement was attributed to the higher crystallinity that inhibits oxygen diffusion and to the smaller number of chain scissions which occur in the PP units. Although significant loss of the plasticizer was observed, the remaining plasticizer adequately improved the tensile properties of the material. The filler type did not significantly affect the ageing behavior of EPDM. Finally, the lower thermal stability of the sulfidic crosslinks resulted in desulfurization and, thus, in an increase in the crosslinking density. To sum up, it has been shown that the monomer composition, curing agent and additives used in EPDM formulations greatly influence the properties and ageing resistance of these materials. T2 - 12. Kautschuk Herbst Kolloquium CY - Hanover, Germany DA - 22.11.2016 KW - Degradation KW - Elastomer KW - Compound PY - 2016 AN - OPUS4-38484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Greiser, Sebastian T1 - 29Si-27Al NMR to verify and distinguish Qn(mAl) sites in zeolites and geopolymers N2 - One-part-geopolymers, produced by addition of water to a mixture of solid silica and sodium alumi-nate, are a less exhaustively studied approach to form geopolymeric binders. Depending on the silica source, the reaction products show significant amounts of zeolite Na-A besides amorphous compounds. Previously, 29Si MAS NMR has been used to analyze the chemical structure of such one-part geopolymers, having crystalline structures and amorphous phases (Q2, Q3, Q4). In this work, pure zeolites and three different one-part-geopolymers cured for 1 day were investigated by 29Si-27Al TRAPDOR NMR. It was used to identify aluminum phases in overlapping silicon sites. Zeolites Na-X (Si/Al=1.4) and Na-Y (Si/Al=2.7) served as model systems to measure the TRAPDOR effect of the structural units Q4(mAl). Both materials show several Q4(mAl) signals, which are all separated by their chemical shifts. The more aluminum surrounds the silicon tetrahedron the higher are the normalized TRAPDOR difference signals (S0/∆S). The intensity ratios between Q4(mAl) to Q4({m-1}Al) of these signals is fixed but vary slightly between both zeolites. These results are transferred to the complex geopolymer structure. T2 - 57th Experimental nuclear magnetic resonance conference CY - Pittsburgh, PA, USA DA - 10.04.2016 KW - NMR KW - 29Si-27Al TRAPDOR MAS KW - Geopolymer KW - One-part formulation KW - Rice husk ash PY - 2016 AN - OPUS4-35864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thünemann, Andreas T1 - Characterization of silver nanoparticles in cell culture medium containing fetal bovine serum N2 - Nanoparticles are being increasingly used in consumer products worldwide, and their toxicological effects are currently being intensely debated. In vitro tests play a significant role in nanoparticle risk assessment, but reliable particle characterization in the cell culture medium with added fetal bovine serum (CCM) used in these tests is not available. As a step toward filling this gap, we report on silver ion release by silver nanoparticles, and changes in the particle radii and in their protein corona when incubated in CCM. Particles of a certified reference material (CRM), p1, and particles of a commercial silver nanoparticle material, p2, were investigated. The colloidal stability of p1 is provided by the surfactants polyethylene glycole-25 glyceryl trioleate and polyethylene glycole-20 sorbitan monolaurate, whereas p2 is stabilized by polyvinylpyrrolidone (PVP). Dialysis of p1 and p2 reveal that their silver ion release rates in CCM are much larger than in water. Particle characterization was performed with asymmetrical flow field-flow fractionation (FFF), small-angle X-ray scattering (SAXS), dynamic light scattering (DLS) and electron microscopy. p1 and p2 have similar hydrodynamic radii of 15 nm and 16 nm, respectively. The silver core radii are 9.2 and 10.2 nm. Gel electrophoresis and subsequent peptide identification reveal that albumin is the main corona component of p1 and p2 after incubation in CCM, which consists of Dulbeccos Modified Eagle Medium with 10% fetal bovine serum added. T2 - 6th International Colloids Conference CY - Berlin, Germany DA - 19.06.2016 KW - SAXS KW - Nanoparticle KW - Silver KW - Albumin PY - 2016 AN - OPUS4-36639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Hydrogen in Welded Microstructures of T24 Steel: Effect on Mechanical Properties and Corresponding Hydrogen Diffusion N2 - Low-alloyed CrMoV steels, such as T24, are widely used for welded components in fossil power stations due to their excellent creep-strength. Spectacular failure cases in the recent years exhibited severe cracking in T24 welds. The results showed that hydrogen-assisted cracking (HAC) occurring up to 200 degree Celsius cannot be excluded. Hence, a basic understanding is necessary on how hydrogen affects the material properties of welded microstructures. In this regard, each weld microstructure (HAZ and weld metal) has influence on the HAC susceptibility and respective hydrogen diffusion. Thus, the present contribution summarizes different results obtained from experiments with grades T24 (CrMoV alloy) and T22 (CrMo) and thermally simulated HAZ. Tensile tests were conducted with hydrogen charged specimens and compared to hydrogen-assisted stress corrosion cracking results obtained from slow strain rate tests (SSRT) up to 200 degree Celsius. Electrochemical permeation and degassing experiments were performed to identify a particular weld microstructure influence on hydrogen diffusion and trapping (especially in the HAZ). The results showed that T24 base material has improved resistance to hydrogen-assisted degradation/cracking. In contrast, the as-welded HAZ had remarkably increased susceptibility (tesnile tests at hydrogen concentration of 1 to 2 ppm). SSRT experiments confirmed this at elevated temperatures for both the T24 and the T22. Hence, the evaluation of a particular degradation of the mechanical properties should be performed independently for each weld microstructure. In addition, the HAZ showed decreased diffusion coefficients (at room temperature) of approximately one magnitude compared to the base materials. Trapped hydrogen was determined in the T24 at temperatures up to 120 degree Celsius compared to 75 degree Celsius in the T22. This has to be considered in case of changing operational temperatures, e.g. in the case of start-up and shutdown processes of boiler components. T2 - 10th Conference on Trends in Welding Research CY - Tokyo, Japan DA - 11.10.2016 KW - Degradation of Mechanical Properties KW - Hydrogen KW - Creep-resistant Steel KW - Weld Joint KW - Diffusion PY - 2016 AN - OPUS4-37827 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wurzler, Nina T1 - Investigation of the mechanisms of microbially induced corrosion on Fe/steel surfaces N2 - The role of metal reducing bacteria (MRB) in corrosion is being controversially discussed in the literature. They can utilize metals including iron, uranium and manganese as well as many organic compounds as electron acceptors. The reduction of Fe(III) compounds to soluble Fe(II) species leads to the destruction of passive films on steel, resulting in acceleration of general and local corrosion processes. Recent research shows that the secretion of electron shuttles like riboflavins also contribute to the extracellular electron transfer (EET). The aim of this project is to understand the chemical and electrochemical interaction mechanisms of MRB with steel surfaces by means of combined in situ techniques. An electrochemical XANES (x-ray absorption near edge spectroscopy) cell has been designed to study the changes of passive film chemistry in the presence of biomolecules and MRB. Electrochemical quartz crystal microbalance (eQCM) is used for studying the kinetics of bacterial cell attachment and diffusion of biomolecules in model biofilms. In situ investigations are complemented by ex situ spectroscopic and microscopic analysis to investigate the biofilm structure, composition and cell viability. Via the combination of electrochemical methods with spectroscopic techniques and QCM we are able to follow biological processes and resulting degradation of steel surfaces in a non-destructive manner. The selection of model systems and a defined biological medium allows the identification of the effects of individual surface and environmental parameters. The fundamental understanding of bacterial attachment mechanisms and initial steps of biofilm formation will contribute to the development of new antifouling strategies. T2 - Electrochemistry 2016 CY - Goslar, Germany DA - 26.09.2016 KW - MIC KW - Microbiologically influenced corrosion KW - XANES KW - Electrochemistry PY - 2016 AN - OPUS4-38199 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kathan, Michael T1 - Photocontrolling imine exchange kinetics to modulate inherent characteristics of self-healing polysiloxane networks N2 - Materials that respond to the environment by changing their properties are critical for developing autonomously adaptive systems. However, to reversibly influence a material's inherent characteristics, such as its ability to self-heal, from distance without continuously expending energy, remains a challenging task. Herein, we report on the modul at ion of imine exchange kinetics by light, manifested in a remote controllable dynamic covalent polymer network. Simple mixing of a commercially available amino-functionalized polysiloxane with small amounts of a photoswitchable diarylethene cross-linker, carrying two aldehyde groups, yields a rubbery material. Its viscoelastic and self-healing properties can be reversibly tuned with everyday light sources, such as sunlight. Our two-component system offers the unique advantage that self-healing takes place continuously without any additives at ambient conditions and is neither dependent on continuous illumination nor does it require recent damage. Overall, our approach allows for the local amplification of intrinsic material properties in a permanent yet reversible fashion. The availability of the inexpensive sta1ting materials on a multi-gram scale, the easy synthesis of the polymer network, and its convenient handling paired with high versatility make our Approach highly applicable to create custom-tailored adaptive materials. T2 - POLYDAYS 2016 CY - Potsdam, Germany DA - 28.09.2016 KW - Self-healing KW - Polymer PY - 2016 AN - OPUS4-37623 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Influence of Experimental Conditions and Calculation Method on Hydrogen Diffusion Coefficient Evaluation at Elevated Temperatures N2 - Hydrogen-assisted cracking (HAC) represents a significant failure risk for (high strength) creep resistant low-alloyed steel components in fossil-fired power plant applications at temperatures of up to and above 200 °C. This particularly applies to respective start-up and shut-down processes associated with alternating service-conditions in terms of load flexible power plants. For quantitative determination of localized crack critical hydrogen concentrations, the temperature dependent hydrogen diffusion coefficients have to be determined as exactly as possible. However, available literature provides a wide range of hydrogen diffusion coefficients for low alloyed steels with similar microstructures. Additionally, the available diffusion data seem not to be very reliable and their scatter increases with decreasing temperature. One reason is that the experimental boundary conditions can have a major impact on the determination of respective effective diffusion coefficients. Hence, the scope of this study is to evaluate the influence of the experimental boundary conditions on the derived diffusion coefficients. In addition, different methods for calculating diffusion coefficients are discussed. To elucidate such influences and to draw a line to practical application, the diffusion and trapping behavior in the creep resistant steel 7CrMoVTiB10 10 has been studied. For such purpose, hydrogen charged specimens were isothermally degassed at different temperatures using carrier gas hot extraction (CGHE). Based on experimental data, a numerical model has been developed by which the hydrogen transport behavior and the respective hydrogen distribution during CGHE can be assessed. It is demonstrated that the specimen heating rate has a large influence on the calculated diffusion coefficients under assumption of isothermal degassing which elsewhere has been underestimated in the assessment of diffusion data in creep-resistant steels. The numerical results suggest that calculation methods for diffusion coefficients are limited if compared to experimental results. It also turned out that the sample preparation time before CGHE can enormously influence determined diffusion coefficients. Consequently, non-homogeneous hydrogen concentration profiles have to be anticipated in the simulations to arrive at characteristic effusion curves consistent to respective CGHE experiments. In turn, validated diffusion coefficients are now available for the low-alloyed Cr-Mo-V steel, which can be helpful to calculate appropriate hydrogen removal heat treatment procedures. T2 - Project Meeting CAStLE CY - Colorado Springs, CO, USA DA - 07.09.2016 KW - Hydrogen KW - Diffusion Coefficient KW - Elevated Temperatures KW - Numerical Modeling KW - Carrier Gas Hot Extraction PY - 2016 AN - OPUS4-37408 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Influence of experimental conditions and calculation method on hydrogen diffusion coefficient evaluation at elevated temperatures N2 - Hydrogen-assisted cracking (HAC) represents a significant failure risk for (high strength) creep resistant low-alloyed steel components in fossil-fired power plant applications at temperatures of up to and above 200 °C. This particularly applies to respective start-up and shut-down processes associated with alternating service-conditions in terms of load flexible power plants. For quantitative determination of localized crack critical hydrogen concentrations, the temperature dependent hydrogen diffusion coefficients have to be determined as exactly as possible. However, available literature provides a wide range of hydrogen diffusion coefficients for low alloyed steels with similar microstructures. Additionally, the available diffusion data seem not to be very reliable and their scatter increases with decreasing temperature. One reason is that the experimental boundary conditions can have a major impact on the determination of respective effective diffusion coefficients. Hence, the scope of this study is to evaluate the influence of the experimental boundary conditions on the derived diffusion coefficients. In addition, different methods for calculating diffusion coefficients are discussed. To elucidate such influences and to draw a line to practical application, the diffusion and trapping behavior in the creep resistant steel 7CrMoVTiB10 10 has been studied. For such purpose, hydrogen charged specimens were isothermally degassed at different temperatures using carrier gas hot extraction (CGHE). Based on experimental data, a numerical model has been developed by which the hydrogen transport behavior and the respective hydrogen distribution during CGHE can be assessed. It is demonstrated that the specimen heating rate has a large influence on the calculated diffusion coefficients under assumption of isothermal degassing which elsewhere has been underestimated in the assessment of diffusion data in creep-resistant steels. The numerical results suggest that calculation methods for diffusion coefficients are limited if compared to experimental results. It also turned out that the sample preparation time before CGHE can enormously influence determined diffusion coefficients. Consequently, non-homogeneous hydrogen concentration profiles have to be anticipated in the simulations to arrive at characteristic effusion curves consistent to respective CGHE experiments. In turn, validated diffusion coefficients are now available for the low-alloyed Cr-Mo-V steel which might be helpful to calculate appropriate hydrogen removal heat treatment procedures, for instance. T2 - International Hydrogen Conference - Material Performance in Hydrogen Environments CY - Jackson Lake Lodge, Moran, Wyoming, USA DA - 11.09.2016 KW - Hydrogen diffusion KW - Elevated temperatures KW - Welding KW - Creep-resistant steel KW - Numerical modeling KW - Calculation PY - 2016 AN - OPUS4-37403 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fuhrmann, A. T1 - Conditional repair by locally switching the thermal healing ability of dynamic covalent polymers ON and OFF with light N2 - Healable materials are able to repair inflicted damages, herin often applied: dynamic covalent polymer networks. We have shown in this study that light of different colors shift the Diels-Alder and retro Diels-Alder crosslinking and decrosslinking equilibrium. This effect was utilized for self-healing of a polymer film. Small-angle X-ray scattering was used to quantifiy the polymeric mesh size on a nanoscale. T2 - Polydays 2016 CY - Potsdam, Germany DA - 28.09.2016 KW - Polymer KW - Small-angle X-ray scattering KW - SAXS KW - Self-healing PY - 2016 AN - OPUS4-37570 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Epping, Ruben T1 - Characterization of statistical EO-PO copolymers containing different end groups by UPLC/ESI-MS N2 - Commercial statistical ethylene oxide (EO) and propylene oxide (PO) copolymers of different monomer compositions and different average molar masses were studied by liquid chromatography under critical conditions (LCCC). Theoretical predictions of the existence of a critical adsorption point (CPA) for statistical copolymers with a given chemical and sequence distribution, could be studied and confirmed. An improved way to determine these critical conditions in a copolymer, alongside the inevitable chemical composition distribution (CCD), with the aid of mass spectrometric detection is described. Shift of the critical eluent composition with the monomer composition of the polymers could be observed. Due to the relatively low average molecular weight, broad molecular weight distribution (MWD) and the presumed existence of different end group functionalities as well as sequence distribution, gradient separation only by CCD was not possible. Therefore isocratic separations at the CPA of definite CCD’s were applied. Although the various present distributions partly superimposed the separation process the goal of separation by end group functionality could still be achieved on the basis of the additional dimension of ESI-MS. The existence of HO-H besides the desired AllylO-H end group functionalities could be confirmed and their amount could be estimated. T2 - International Symposium GPC/SEC and Related Techniques CY - Amsterdam, The Netherlands DA - 26.09.2016 KW - Polymers KW - UPLC KW - ESI-TOF-MS PY - 2016 AN - OPUS4-37632 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wurzler, Nina T1 - Chemical interaction mechanisms of metal reducing bacteria on steel surfaces N2 - Metal reducing bacteria (MRB) are able to utilize various materials such as iron, uranium and manganese as well as many organic compounds as electron acceptors. This process leads to the conversion of Fe(III) containing passive film species to soluble Fe(II) oxides and hydroxides. The reduction process triggers the acceleration of general and local corrosion processes. Electron transfer mechanisms are not yet fully understood. In literature it has been controversially discussed to which extend secreted electron shuttles contribute to the extracellular electron transfer (EET). To understand the chemical and electrochemical interaction mechanisms of MRB with steel surfaces this project combines a variety of in-situ techniques. The changes in oxide chemistry on Fe/steel surfaces in the presence of biomolecules and MRB are under investigation using a newly designed electrochemical cell for in situ XANES (x-ray absorption near edge structure) spectroscopy. Electrochemical quartz crystal microbalance (eQCM) studies support the spectroscopic investigations to gain information about the kinetics of attachment processes and changes in biofilm viscosity. The biofilm structure and composition as well as cell viability are investigated by complementary ex situ spectroscopic and microscopic analysis. Combining spectroscopic techniques and eQCM data with electrochemical measurements, biological processes and the resulting degradation of steel surfaces can be observed in a non-destructive manner. Selecting model systems and a defined biological medium allows the determination of individual effects of diverse surface and environmental parameters. The fundamental understanding of bacterial attachment mechanisms and initial steps of biofilm formation will contribute to the development of new antifouling strategies. T2 - 12th International Conference on Biology and Synchrotron Radiation CY - San Francisco, CA, USA DA - 21.08.2016 KW - Microbially influenced corrosion (MIC) KW - Metal reducing bacteria KW - XANES KW - Electrochemistry PY - 2016 AN - OPUS4-37238 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Akhmetova, Irina T1 - In situ investigation of mechanochemical syntheses of metal phosphonates N2 - We report on the in situ investigation of mechanochemical syntheses of metal phosphonates. The metal phosphonates are formed in milling reactions starting from a metal acetate and a phosphonic acid. The conversions are observed by synchrotron PXRD and Raman spectroscopy to shed light on the reaction mechanisms including possible intermediates. T2 - 8th HZB User Meeting CY - Berlin, Germany DA - 07.12.2016 KW - Mechanochemistry KW - In situ KW - Metal phosphonates KW - XRD KW - Raman spectroscopy PY - 2016 AN - OPUS4-38780 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fischer, Franziska T1 - In situ investigation of the mechanochemical formation of cocrystals unsing combined PXRD and Raman spectroscopy N2 - We present an in situ investigation of the mechanochemical formation of cocrystals using synchrotron XRD and Raman spectroscopy. This combination allows to study milling processes on the level of the molecular and crystalline structure thus obtaining reliable data for mechanistic studies. Thereby, mechanochemical syntheses can be optimized to isolate new crystal structures. T2 - Joint BER II and BESSY II User Meeting 2016 CY - Berlin, Germany DA - 07.12.2016 KW - Intermediate KW - Mechanochemistry KW - Cocrystal KW - In situ KW - Milling PY - 2016 AN - OPUS4-38722 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fischer, Franziska T1 - Survival of the fittest - Competetive cocrystal reactions in the ball mill N2 - Mechanochemistry is increasingly used for synthesizing various materials including cocrystals and metal organic compounds. Although this synthesis approach offers a fast and pure synthesis in high yields there is a lack in understanding the mechanisms of milling reactions. The driving forces triggering the formation of cocrystals under milling conditions were investigated using a set of multi-component competitive milling reactions. In these reactions, different active pharmaceutical ingredients were ground together with a further compound acting as coformer. The study was based on new cocrystals including the coformer anthranilic acid. The results of the competitive milling reactions indicate that the formation of cocrystals driven by intermolecular recognition are influenced and inhibited by kinetic aspects including the formation of intermediates and the stability of the reactants. T2 - Berliner Chemie Symposium CY - Berlin, Germany DA - 12.04.2016 KW - milling KW - cocrystal KW - mechanochemistry PY - 2016 AN - OPUS4-35862 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nguyen, Thi Yen T1 - Direct evidence of polyamorphism in paracetamol N2 - While polymorphism is a common phenomenon in the crystallization processes of organic compounds, polyamorphism has gained importance only recently. Using sophisticated sample environments and applying in situ scattering methods and vibrational spectroscopy, the complete crystallization process of organic compounds from solution can be traced and characterized. Diffuse scattering from amorphous intermediates can be investigated by analyzing the atomic pair Distribution function (PDF) to gain further insights into molecular pre-orientation. The crystallization behavior of Paracetamol was studied exemplarily under defined, surface-free conditions. Based on the choice of the solvent, the formation of different polymorphs is promoted. The thermodynamically stable form I and the metastable orthorhombic form II could be isolated in pure form directly from solution. For both polymorphs, the crystallization from solution proceeds via a distinct amorphous precursor phase. PDF analyses of these different amorphous states indicate a specific pre-orientation of the analyte molecules introduced by the solvent. The resulting crystalline polymorph is already imprinted in these proto-crystalline precursors. Direct experimental evidence for the polyamorphism of paracetamol is provided. T2 - Annual CM1402 crystallize COST meeting CY - Coimbra, Portugal DA - 06.04.2016 KW - Paracetamol KW - Crystallization KW - In situ analysis KW - Active pharmaceutical ingredient (API) PY - 2016 AN - OPUS4-35873 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kabelitz, Anke T1 - Time-resolved studies on the formation of maghemite nanoparticles combining fast-XANES and SAXS N2 - Iron oxide nanoparticles find application in different areas like sensing, magnetic storage media, and biomedicine, due to their magnetic properties and environment-friendliness. In the present contribution, we report on the in situ investigation of an iron oxide nanoparticle synthesis by coupled X-ray absorption near-edge structure (XANES) and small-angle X-ray scattering (SAXS). The combination provides simultaneously information about the size of particles (SAXS) and on the oxidation state and the local structure of the iron atoms (XANES). The co-precipitation synthesis was exemplary studied, using a stabilization agent to decelerate the fast precipitation of the iron oxides. This allows to detect intermediates in situ. The measurements were performed using a custom-made acoustic levitator as sample holder. From the data, a mechanism was derived indicating different phases of particle Formation and oxidation state changes. T2 - The European Materials Research Society-Spring Meeting 2016 CY - Lille, France DA - 01.05.2016 KW - Iron oxide nanoparticles KW - SAXS KW - XANES KW - Time-resolved PY - 2016 AN - OPUS4-36351 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulla, Hannes T1 - In situ investigation of mechanochemical reactions with PXRD and Raman spectroscopy - cocrystals of pyrazinamide with dicarboxylic acids N2 - - Cocrystal formation of pyrazinamide with dicarboxylic acids proceeds either directly or via a crystalline intermediate. - Two new crystal structures were discovered by in situ investigations. T2 - ICS 2016 CY - Granada, Spain DA - 30.05.2016 KW - In situ KW - Mechanochemie KW - XRD KW - Cocrystal PY - 2016 AN - OPUS4-36620 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fischer, Franziska T1 - Polymorphism of mechanochemically synthesized Cocrystals: an in situ study N2 - In situ investigations using PXRD coupled with Raman spectroscopy permit the evaluation of the formation pathways of milling reactions. The liquid-assisted grinding cocrystallisation of theophylline with benzamide leading to polymorphic compounds was investigated. The dipole moment of the solvent used in the synthesis determines the structure of the polymorphic product. A detailed investigation allows determining the kinetically and thermodynamically favored product. In situ observations of the formation pathway during the grinding process of both polymorphs show that the thermodynamically favored cocrystal is formed in a two-step mechanism with the kinetic cocrystal as intermediate. The evaluation of the mechanochemical formation pathways reveals the importance of in situ investigations for an in depth understanding of mechanochemical synthesis mechanisms. Our study demonstrates that the choice of the solvent in the LAG synthesis is decisive for the controlled formation of a desired polymorphic final product. T2 - CGOM/ BACG 47th Annual British Association of Crystal Growth Conference CY - Leeds, UK DA - 28.06.2016 KW - Cocrystal KW - Mechanochemistry KW - Milling PY - 2016 AN - OPUS4-36764 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gollwitzer, Christian T1 - Synchrotron based absorption edge tomography for §D characterization of the microstructure of MG-Y-Zn alloys N2 - Absorption edge tomography is a method which exploits the sudden change of the attenuation coefficient, when the photon energy crosses the absorption edge of an element. The beamline BAMline at BESSY II, which is operated by the Federal Institute for Materials Research and Testing, can provide a monochromatized beam in a photon energy range from 5 keV up to 80 keV with a bandwidth of 2%. Together with the microtomography setup, this enables differential tomography sensitive to any element with N >= 24 (Cr) by using an appropriate K- or L-edge in this range. Here, absorption edge tomography at the Yttrium edge is employed to perform a non-destructive 3D characterization of the microstructure of a high strength Mg-Y-Zn alloy. The long period stacking ordered (LPSO) phase which forms fibres in this material was extracted based on the Yttrium content and the fibre length distribution was analysed. T2 - Ninth Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 13.12.2017 KW - Synchrotron KW - Computed Tomography KW - Absorption edge KW - BAMline PY - 2017 AN - OPUS4-43854 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Moldenhauer, Laura T1 - Experimental modeling approach for determining the moisture damping exponent of a bluetooth low energy signal in moist building material N2 - We investigated, the damped Received Signal Strength Indicator (RSSI) of a Bluetooth Low Energy (BLE) signal, transmitted from the BLE-module embedded in building materials with changing moisture content, Fig. 1. The BLE-module communicates with a mobile Smart Device as tablet via 2.45 GHz-ISM-frequency band where water dipoles start to oscillate, Fig. 2. The damping model demonstrates this damping effect on RSSI by the abstraction of the reality observed in a real system. Through the reproduction of the active relationships, the system behavior is decomposed in such a way that a separate consideration of the required system parameters is possible. T2 - 34th DANUBIA ADRIA SYMPOSIUM on Advances in Experimental Mechanics (DAS 2017) CY - Trieste, Italy DA - 18.09.2017 KW - Structural health monitoring KW - Long-term monitoring KW - Bluetooth Low Energy KW - BLE KW - Moisture KW - Network Communication KW - Experimental study KW - Modellierung PY - 2017 AN - OPUS4-42966 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koclega, D. T1 - High temperature corrosion resistance of Inconel 686 coatings in aggresive environments N2 - The work presents the microstructure, chemical composition and mechanical properties of Inconel 686 coatings after high - temperature corrosion in environment of aggressive gases. To produce the Ni - base weld overlays the QS Nd:YAG laser beam was used. The substrates were 13Mo4-5 boilers plate steel. Ni - base alloys characterize the excellent high temperature corrosion resistance, good strength and good ability to work in aggressive environments. Applied overlays had a proper combination of the metal substrate in particular small amount of Fe. This could be achieved by the reduction of the melting of the substrate and its dissolution into the overlays. The microstructure, chemical composition of the obtained overlays were investigated by means of a light microscope, a scanning electron microscope (SEM) equipped with the EDS detector. The overlays had cellular-dendritic structure. The variations of the chemical composition (especially Mo, Ni and W ) in the interdendritic and dendritic regions were observed. The interdendritic regions were enriched during solidifications in Mo and W and had lower content of Ni. T2 - EUROCORR 2017 CY - Prague, Czech Republic DA - 03.09.2017 KW - Inconel 686 KW - Corrosion resistance KW - Laser cladding PY - 2017 AN - OPUS4-44197 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koclega, D. T1 - The microstructure of weld overlay Ni - base alloy deposited on carbon steel by laser QS-Nd:YAG N2 - Ni- base alloys are used as a one of the most important coating material and can be applied in a different environments and elements of devices having various applications. To protect the surface of the material from aggressive gases at high temperature, there are use different kinds of the Ni- base alloys. One of such alloy is Ni-Cr-Mo-W called commercial Inconel 686. This alloy based on NiCr22Mo9Nb (Inconel 625), in which content of molybdenum increased and niobium was replaced with the addition of tungsten, in order to counteract the strong segregation in the microstructure, which results in homogeneity of the chemical composition of the structure. Inconel 686 is also characterized by greater resistance to high temperature corrosion and heat resistance than Inconel 625. The Inconel 686 alloy was deposited on 13CrMo4-5 steel by laser QS - Nd:YAG. In the poster the microstructure (SEM) and chemical composition (EDS) of obtained weld overlays were investigated. T2 - EUROMAT 2017 CY - Thessaloniki, Greece DA - 17.09.2017 KW - Nickel based alloy KW - Laser cludding KW - High temperature corrosion resistance PY - 2017 AN - OPUS4-44195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reinsch, Stefan A1 - Patzig, C. T1 - Surface-initiated microstructure formation in glass ceramics N2 - Up to now, the mechanisms of surface nucleation and surface-induced texture formation are far from being understood. Corresponding phenomena are discussed hypothetically or even controversial, and related studies are restricted to very few glasses. As a main drawback, the vast majority of previous work on oriented growth of surface crystals do not consider the possible effects of glass surface treatments (like polishing defects, adhered particles and cracks, …) or ambient annealing conditions (vacuum or atmospheric pressure) which both can influence crystal nucleation and growth. Moreover, very few observations of crystal orientation related to surface crystallization were focused on separately growing crystals. In conclusion, up to now, no systematic studies on initially oriented crystal growth or nucleation from defined active nucleation sites have been pursued. Therefore, the main objective of the proposed project is to gain a basic understanding of the mechanisms of surface-induced microstructure formation in glass ceramics. We shall answer the question whether preferred orientation of surface crystals is the result of oriented nucleation or caused by other orientation selection mechanisms acting during early crystal growth. In both cases, crystal orientation may be caused by the orientation of the glass surface itself or the anisotropy and orientation of active surface nucleation defects. New techniques of experimental characterization of surface-crystallized glasses shall be applied to find answers to the questions posed above. Based on a controlled preparation and annealing of the glass sample surfaces, that includes the defined creation of active nucleation defects, and followed by the microstructural characterization especially during the very early growth stages of separated surface crystals, the orientation relations between defect and initiated surface crystal will be analyzed. In order to gain new insights, a couple of entirely new microstructure diagnostics techniques, including chemically contrasted XRM, laser-based sample preparation for XRM, and 3D electron backscatter diffraction shall be developed or applied. This way, using X-ray microscopy as a pivotal technique for the non-destructive 3D characterization of relatively large samples at superior spatial resolution (but also complemented by other microstructure diagnostics techniques, e.g. TEM elemental mappings at cross-sectioned samples) unprecedented insights into the microstructure evolution upon surface crystallization of model glasses will be gained. T2 - DFG Begutachtungskolloquium (PAK 949/1 und PAK 950/1) CY - Bonn, Germany DA - 07.03.2017 KW - Oberflächenkeimbildung KW - Glaskeramik KW - Orientierung PY - 2017 AN - OPUS4-44221 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koclęga, Damian T1 - Optimization of laser treatment parameters of Inconel 686 overlay weld on carbon steel 13Mo4-5 N2 - The work presents the effects of the change of the laser cladding parameters on microstructure, chemical composition and mechanical properties of Inconel 686 overlays (coatings). To obtain the best quality of these coatings the various parameters of laser cladding such as the power density of the laser beam, the laser beam velocity and overlapping ratio of the weld tracks were applied. The substrates were boilers plate made of the 13Mo4-5 steel. Ni - base alloys characterize by the excellent high-temperature corrosion resistance, good strength and good ability to work in aggressive environments. Applied overlays had a proper combination of the metal substrate in particular small amount of Fe. This could be achieved by the reduction of the substrate melting and its dissolution into the overlays. The microstructure, chemical composition of the obtained overlays were investigated by means of a light microscope, a scanning electron microscope (SEM) equipped with the EDS detector. The overlays had cellular-dendritic structure. The variations of the chemical composition (especially Mo, Ni and W ) in the interdendritic and dendritic regions were observed. The interdendritic regions were enriched during solidifications in Mo and W and had lower content of Ni. T2 - METAL 2017 CY - Brno, Czech Republic DA - 24.05.2017 KW - Laser cladding KW - Overlay KW - Chemical composition KW - Inconel 686 PY - 2017 AN - OPUS4-44464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Raedel, Martina T1 - Research and reconstruction of historic gold mosaics N2 - A research project of reconstructing historical gold mosaics deals with reconstructing weatherproof gold and silver mosaics according to historical models. The gold mosaics examinded originate mainly from germany from 1880 to 1920 and are composed of three parts. They consist of a matching support glass, the gold or silver layer and a cover glass. By examining the morphology and layer thicknesses with the ESEM, and using chemical analysis with the EDX, the relationship of glass composition and damage patterns was established. The glass analysis provided quantitative composition data and made it possible to determine its chemical stability. It supplied the basis for calculating glass characteristics and was referred to when casting suitable historical mosaic glass. The analysis of the qualitative composition of the gold and silver layers also served as a model for reconstruction. After testing selected reconstructed gold mosaics in the climate chamber, the ESEM was used for capturing leaching and other process data and the glass composition was optimized accordingly. Over 100 predominantly historical gold mosaics were analyzed and the results entered into a database which can now be consulted for comparative investigations to determine both origin and date. T2 - What comes to mind when you hear mosaics, conserving mosaics from ancient to modern CY - Barcelona, Spain DA - 15.10.2017 KW - Gold mosaics KW - Leaching process KW - Composition KW - Database PY - 2017 AN - OPUS4-43216 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hiller, Th. A1 - Costabel, S. A1 - Müller-Petke, M. A1 - Kruschwitz, Sabine T1 - Evaluation of different laboratory NMR devices in a tripartite round robin test N2 - Nuclear magnetic resonance (NMR) is a well established laboratory / borehole method to characterize the storage and transport properties of rocks due to its direct sensitivity to the corresponding pore fluid saturation (water or oil) and pore sizes. For petrophysical applications there are several different NMR laboratory devices commercially available varying over a wide range of e.g. magnetic field strength / frequency (2 MHz to 30 MHz), applicable measurement protocols (T1, T2, T1-T2, T2-D, etc.) and sample sizes (2.5 cm to 10 cm in diameter). In this work we present NMR measurements, layed out in a round robin like manner, on a set of 20 sandstone samples. We use three different NMR devices containing two standard setups with homogenous magnetic fields (LIAG and RWTH) and one single-sided setup with gradient field (BGR) to measure T1 and T2 relaxation data. In our evaluation we especially focus on the comparison of the individually inverted relaxation time distributions to quantify the differences arising from different laboratory setups. Diverging results can be deduced on the one hand to the inherit differences between homogeneous and gradient fields but on the other hand also due to quality differences between the two homogeneous setups. Additionally, we also examine the influence of the individually chosen inversion parameters (signal processing, distribution sampling points, error weighting, regularization, etc.) to establish a general standardized best practice recommendation for future petrophysical NMR laboratory measurements. T2 - 77. Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Potsdam, Germany DA - 27.03.2017 KW - Nuclear Magnetic Resonance KW - Sandstone PY - 2017 AN - OPUS4-43244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lüth, Peter T1 - CEQAT-DGHS Ringversuchsprogramm für die Chemikaliensicherheit – Methodenvalidierung N2 - Bei der Bewertung der Verlässlichkeit der im Labor gewonnenen Prüfergebnisse spielen Ringversuche eine entscheidende Rolle. Die Bundesanstalt für Materialforschung und –prüfung (BAM) unterstützt deshalb den weiteren Ausbau des Ringversuchsprogramms des im Jahr 2007 gegründeten Kompetenzzentrums zur Qualitätssicherung für Prüfungen von Gefahrgütern und Gefahrstoffen auf physikalische Gefahren (Centre for quality assurance for testing of dangerous goods and hazardous substances, CEQAT-DGHS). Bei allen bisher untersuchten Prüfmethoden besteht ein Verbesserungsbedarf. Die RV müssen daher zunächst auf die Methodenentwicklung, -verbesserung und -validierung und auf die Bestimmung der Messunsicherheit der jeweiligen Prüfmethode abzielen und nicht auf Leistungstests. T2 - 13. Fachtagung Anlagen-, Arbeits- und Umweltsicherheit CY - Köthen, Germany DA - 16.11.2017 KW - Gefahrgut KW - Gefahrstoff KW - Ringversuch KW - Prüfmethode KW - Validierung KW - Qualitätssicherung PY - 2017 AN - OPUS4-43301 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kirner, Sabrina V. T1 - Laser-induced periodic surface structures on steel for tribological applications N2 - Laser-induced periodic surface structures (LIPSS) can be generated by irradiation of almost any material with linearly polarized laser beams, particularly when using ultrashort laser pulses. Within this work, different types of steel were irradiated at optimized conditions for the processing of large surface areas. For these nanostructured surfaces, the coefficient of friction (COF) using different lubricants was determined and the corresponding wear tracks were characterized by scanning electron microscopy (SEM). Our experiments provide a qualification of the tribologicalperformance of the fs-LIPSS on different steel surfaces, which are relevant for technical applications. T2 - International Conference on Laser Ablation (COLA) CY - Marseille, France DA - 3.09.2017 KW - Femtosecond laser ablation KW - Laser-induced periodic surface structures (LIPSS) KW - Tribology KW - Friction and wear KW - Steel PY - 2017 AN - OPUS4-42358 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kirner, Sabrina V. T1 - LiNaBioFluid Laser-induced nanostructures as biomimetic model of fluid transport in the integument of animals N2 - Laser-induced Nanostructures as Biomimetic Model of Fluid Transport in the Integument of Animals”, aims on laser-fabrication of biomimetic surfaces with unique wetting properties, which are inspired by the hierarchical micro- and/or nano- structures of animal body surfaces. LiNaBioFluid is a Research and Innovation Action funded by the European Commissions’ Horizon 2020 - FET Open Programme, which supports early-stage research on any idea for a new technology (Grant Agreement no: 665337). It brings together 7 partners from 4 different countries and is strongly interdisciplinary combining renowned experts from the fields of zoology, physics, mechatronics, life sciences, materials sciences, laser-matter interaction, production technology, tribology, and biomimetics. www.laserbiofluid.eu/ T2 - Science Sets Sail CY - Baltic Sea DA - 2.08.2017 KW - Laser-induced periodic surface structures (LIPSS) KW - EU H2020 project KW - Biomimetics KW - Wetting KW - Tribology KW - Friction and wear KW - Laser ablation PY - 2017 AN - OPUS4-42359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schulte, Petra T1 - Kritische Bewertung der Prüfergebnisse in chemikalienrechtlichen Verfahren: Wie agiert die Behörde? Welche Folgen haben die Ergebnisse für die Rechtsetzung? N2 - Mit nicht-konformen oder schlecht dokumentierten Prüfergebnissen können weder Behörden noch Unternehmen etwas anfangen. Belastbare und eindeutige Informationen aus den Registrierungsdossiers sind entscheidend, damit industrielle und gewerbliche Verwender der Stoffe das Gefahrenpotenzial einschätzen und ggf. Maßnahmen zum Schutz von Menschen und Umwelt treffen können. Darüber hinaus benötigen die Behörden verlässliche Daten aus den Registrierungen, um ihrer Verantwortung bei der Identifizierung regulierungsbedürftiger Stoffe nachkommen zu können. T2 - 13. Fachtagung "Anlagen-, Arbeits- und Umweltsicherheit" CY - Köthen, Germany DA - 16.11.2017 KW - Prüfmethoden KW - Einstufung KW - REACH KW - CLP KW - Registrierungsdossiers KW - SIEF KW - Qulitätssicherung KW - IUCLID KW - ECHA KW - OECD PY - 2017 AN - OPUS4-43081 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griepentrog, Michael T1 - Size effects in electrodeposited Ni-coatings N2 - Polycrystalline Ni materials with grain sizes less than 100 nm (nano crystalline NC) and with grain sizes in the micrometer range (micro crystalline MC) in form of thin films have become important in many technologies due to their improved physical, chemical and mechanical properties. Usual the mechanical properties of such coatings are described by a Hardness value and a Young´s modulus measured by Instrumented Indentation Testing (IIT).The behavior of such coatings during indentation test is influenced by different size effects having their representative length scale – grain size, coating thickness, length that characterizes the depth dependence of the hardness (Indentation Size Effect ISE). To estimate realistic values for the intrinsic coating Hardness and Young´s modulus all size effects have to be considered. For this work thin nano crystalline Ni – coatings (average grain size 30 nm) with thickness from 1 μm to 5 μm were electrodeposited on brass substrates. Indentation tests in the continuous stiffness measurement (CSM) mode were provided on as prepared Ni – coatings using a G200 Nanoindentation system (Fa. Keysight). For estimation of the intrinsic hardness of the coatings from composite hardness values calculated from the measured force –displacement curve using the Oliver & Pharr method, the model described by Z.S. Ma [1] was used. It was found that the experimental data can be well described by the model. The fitted values for the intrinsic hardness and the fitting parameters will be given. The different values of intrinsic hardness and of length characterizing depth dependence of the hardness for different coating thickness are discussed as results of changes in the coating structure because of changes in deposition parameters. [1] Z.S. Ma, Y.C. Zhou, S.G. Long, C. Lu: On the intrinsic hardness of a metallic film/substrate system: Indentation size and substrate effects. International Journal of Plasticity 34 (2012) 1-11. This work is supported by European Metrology Program for Innovation and Research (EMPIR) (JRP 14IND03 Strength – ABLE) T2 - Conference: Nanomechanical Testing in Materials Research and Development CY - Dubrovnik, Croatia DA - 01.10.2017 KW - Size effect KW - Substrate effect KW - Electrodeposited Ni - coatings KW - Instrumented indentation testing PY - 2017 AN - OPUS4-42664 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hilgenberg, Kai T1 - Localized laser dispersing of titanium-di-boride with pulsed fiber laser N2 - In this paper, titanium-di-boride is dispersed on a cold-working tool steel by use of a pulsed fiber laser with high beam quality to produce separated and elevated surface features. The potential to adjust the geometry as well as the mechanical properties of the produced structures in dependence on the process parameters (pulse power, pulse duration) is described by means of metallographic and topographical investigations. It can be ascertained that very hard (hardness > 1000 HV1) surface features of different shape (spots and short lines) can be produced. They are characterized by a fine-grained microstructure resulting from a rapid solidification and finely dispersed TiB2 particles. Finally, the paper proposes different applications for this structuring technique. T2 - ICALEO 2017 - International congress on applications of lasers & electro-optics CY - Atlanta, GA, USA DA - 22.10.2017 KW - Laser dispersing KW - Titanium-di-boride KW - Surface structuring KW - Laser implantation PY - 2017 AN - OPUS4-42867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Myrach, Philipp A1 - Ziegler, Mathias T1 - Online Laser-thermografische Rissprüfung an Stahl bei hohen Temperaturen N2 - Die Detektion bzw. Charakterisierung von Oberflächenrissen in Stahl ist eine herausfordernde Aufgabe für die zerstörungsfreie Prüfung. Dies gilt insbesondere, wenn eine solche Prüfung bereits während der Produktion selbst erfolgen soll. Die hier vorgefundenen Randbedingungen, wie z.B. die hohen Probentemperaturen (>700°C) oder Vorschubgeschwindigkeiten von bis zu 0,9 m/min, machen die Anwendung etablierter und vor allem berührender ZfP-Methoden praktisch meist unmöglich. Laser-thermografische Verfahren können hier eine Alternative bieten, da sie berührungslos und schnell arbeiten. Wir stellen die Ergebnisse einer Weiterentwicklung der Laser-thermografischen Prüfung vor, bei der die Anwendbarkeit bzw. die Übertragbarkeit der Methode auf die Bedingungen der Stahlproduktion untersucht wurde. Neben der Simulation der Produktionsbedingungen im Labor und der experimentellen Untersuchung der entscheidenden Einflussgrößen, wurden umfangreiche FEM-Simulationen durchgeführt. Mit Hilfe dieser theoretischen und experimentellen Ergebnisse wurde das Verfahren auch hinsichtlich der Analyse-Algorithmen weiterentwickelt, um eine zuverlässige und schnelle In-Line Prüfung während des Produktionsprozesses zu ermöglichen. Um zudem die Fähigkeiten der Thermografiekamera für schnelle online-Messungen und ihre Integrierbarkeit in verschiedene Anwendungssysteme zu verbessern, wurde die für die Verarbeitung der Detektordaten erforderliche Non-Uniformity Correction der Pixeldaten auf schneller Spezialhardware innerhalb der Kamera implementiert. T2 - Thermografie-Kolloquium 2017 CY - Berlin, Germany DA - 28.09.2017 KW - Rissprüfung KW - Laserthermografie KW - Thermografie KW - Risse PY - 2017 AN - OPUS4-42922 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosemann, Paul T1 - Wärmebehandlung und Korrosionsbeständigkeit druckaufgestickter nichtrostender Stähle N2 - Gefüge und Eigenschaften nichtrostender Stählen werden maßgeblich von ihrer chemischen Zusammensetzung und der Wärmebehandlung bestimmt. Eine spezielle Werkstoffgruppe der austenitischen nichtrostenden Stähle enthält ca. 19 Gew.-% Mangan und 0,8 Gew.-% Stickstoff, um das austenitische Gefüge ohne das Legieren mit Nickel sicherzustellen. Die herausragenden mechanischen Eigenschaften dieser Werkstoffe (Rm von 900 2.000 MPa, A5 > 50 %, Av > 350 J) werden nach der Wärmebehandlung (Lösungsglühen und Abschrecken) durch gezielte Kaltverfestigung eingestellt. Das Lösungsglühen beseitigt vorhandene Kaltverfestigung und unerwünschte Ausscheidungsphasen (Cr2N, M23C6 und Sigma-Phase) und bewirkt die homogene Verteilung der Legierungselemente (insbesondere Stickstoff) im Austenit. Dies ist zur Erzielung der Korrosionsbeständigkeit von entscheidender Bedeutung. Im Poster werden systematische Untersuchungen zur Korrosionsbeständigkeit dieser vielversprechenden Werkstoffklasse vorgestellt und die Interaktion zwischen Legierungszusammensetzung, Wärmebehandlung, Gefüge und Korrosionsbeständigkeit dargestellt. Insbesondere der Einfluss von Warmauslagerungsversuchen nach dem Abschrecken wird dabei charakterisiert. Die vom Gefüge bedingten Veränderungen der Korrosionsbeständigkeit werden durch verschiedene Methoden (EPR, KorroPad, Lochkorrosionspotentiale) ermittelt und interpretiert. T2 - Werkstoffwoche 2017 CY - Dresden, Germany DA - 27.09.2017 KW - Wärmebehandlung KW - Korrosion KW - Nichtrostender Stahl KW - EPR KW - KorroPad KW - Sensibilisierung KW - Stickstoff KW - ThermoCalc PY - 2017 AN - OPUS4-42831 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dieck, S. A1 - Ecke, M. A1 - Harnisch, K. A1 - Rosemann, Paul A1 - Halle, T. T1 - Gefüge- und Phasenanalyse biokompatibler Co-Cr-Mo-Legierung N2 - Co-Cr-Mo-Werkstoffe sind im Bereich der Biomaterialien weit verbreitet und werden für Endoprothesen eingesetzt. Deren Lebensdauer ist jedoch durch tribologische und korrosive Dauerbelastung begrenzt. Um die Anzahl operativer Eingriffe am Patienten zu minimieren, ist es notwendig den Werkstoff hinsichtlich Verschleißbeständigkeit und Korrosionsbeständigkeit zu optimieren. Hierfür ist ein umfassendes Verständnis der legierungsabhängigen Phasenbildung und –entwicklung während Herstellung und Wärmebehandlung notwendig. An einer speziellen Co-Cr-Mo Legierung werden verschiedene Untersuchungen zur Gefügecharakterisierung durchgeführt. Dabei werden die auftretenden Phasen thermodynamisch berechnet, mittels XRD nachgewiesen, die Phasenmorphologie durch EBSD analysiert, die Elementverteilung durch EDX-Analyse ermittelt und die Ergebnisse durch Farbätzen verifiziert. Das Ziel der Untersuchungen ist es, Optimierungspotentiale bei Herstellung und Wärmebehandlung zu identifizieren. T2 - Werkstoffwoche 2017 CY - Dresden, Germany DA - 27.09.2017 DA - 29.09.2017 KW - CoCrMo KW - Gefüge KW - ThermoCalc KW - EBSD KW - Farbätzen PY - 2017 AN - OPUS4-42832 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, C. T1 - Wärmebehandlung und Korrosionsbeständigkeit druckaufgestickter nichtrostender Stähle N2 - Gefüge und Eigenschaften nichtrostender Stählen werden maßgeblich von ihrer chemischen Zusammensetzung und der Wärmebehandlung bestimmt. Eine spezielle Werkstoffgruppe der austenitischen nichtrostenden Stähle enthält ca. 19 Gew.-% Mangan und 0,8 Gew.-% Stickstoff, um das austenitische Gefüge ohne das Legieren mit Nickel sicherzustellen. Die herausragenden mechanischen Eigenschaften dieser Werkstoffe (Rm von 900 2.000 MPa, A5 > 50 %, Av > 350 J) werden nach der Wärmebehandlung (Lösungsglühen und Abschrecken) durch gezielte Kaltverfestigung eingestellt. Das Lösungsglühen beseitigt vorhandene Kaltverfestigung und unerwünschte Ausscheidungsphasen (Cr2N, M23C6 und Sigma-Phase) und bewirkt die homogene Verteilung der Legierungselemente (insbesondere Stickstoff) im Austenit. Dies ist zur Erzielung der Korrosionsbeständigkeit von entscheidender Bedeutung. Im Poster werden systematische Untersuchungen zur Korrosionsbeständigkeit dieser vielversprechenden Werkstoffklasse vorgestellt und die Interaktion zwischen Legierungszusammensetzung, Wärmebehandlung, Gefüge und Korrosionsbeständigkeit dargestellt. Die vom Gefüge bedingten Veränderungen der Korrosionsbeständigkeit werden durch verschiedene Methoden ermittelt und interpretiert. T2 - GfKORR-Jahrestagung 2017 CY - Frankfurt a. M., Germany DA - 07.11.2017 KW - Wärmebehandlung KW - Korrosion KW - Nichtrostender Stahl KW - EPR KW - KorroPad KW - Sensibilisierung KW - Stickstoff KW - ThermoCalc PY - 2017 AN - OPUS4-42833 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kauss, N. A1 - Rosemann, Paul T1 - Sensibilisierungsverhalten vom nichtrostenden Lean-Duplexstahl 1.4062 N2 - Der nichtrostende Lean-Duplexstahl 1.4062 (X2CrNiN22-2) verbindet die hohe Festigkeit des Ferrits mit der Duktilität und Zähigkeit des Austenits in einem zweiphasigen Gefüge mit sehr hoher Korrosionsbeständigkeit. Die höchste Korrosionsbeständigkeit wird erreicht, wenn das ferritisch-austenitische Gefüge frei von weiteren Sekundärphasen ist. Dies wird durch ein gezieltes Lösungsglühen bei 1050 °C mit anschließender Abschreckung in Wasser erreicht. Durch thermische Beeinflussung (z.B. beim Schweißen) können Sekundärphasen ausgeschieden und die Korrosionsbeständigkeit des Werkstoffs gesenkt werden. Dies wurde durch eine isotherme Warmauslagerung bei 500 °C bis 900 °C für 0,1 h bis zu 72 h simuliert. Die Veränderung der Korrosionsbeständigkeit wurde mit dem DL-EPR-Verfahren und durch die angepasste KorroPad-Prüfung ermittelt. Die ermittelten Anfälligkeitsbereiche wurden miteinander Verglichen und in zwei Sensibilisierungsschaubildern zusammengefasst. T2 - GfKORR-Jahrestagung CY - Frankfurt a. M., Germany DA - 07.11.2017 KW - Duplexstahl KW - Nichtrostender Stahl KW - Wärmebehandlung KW - Korrosion KW - EPR KW - KorroPad KW - Sensibilisierung PY - 2017 AN - OPUS4-42834 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulla, Hannes T1 - In situ PXRD monitoring of a mechanochemical cocrystal formation in milling jars of different material N2 - We present an in situ PXRD investigation of the mechanochemical cocrystal formation of pyrazinamide with pimelic acid in two milling jar materials. In the steel jar a polymorph transformation presenting an exception of Ostwald’s rule of stages is observed. T2 - BESSY User Meeting 2017 CY - Bessy II (HZB), Berlin, Germany DA - 14.12.2017 KW - In situ KW - XRD KW - Polymorph KW - Cocrystal KW - Milling PY - 2017 AN - OPUS4-43502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kormunda, M. T1 - Study of magnetron sputtering deposited ultrathin FeSnOx films for Surface Plasmon Resonance sensors towards gas sensing applications N2 - In this study, series of coatings with the goal of sensitising gold SPR sensors towards CO, NH4, etc. were prepared. To better understand the mechanism behind the sensitizing effect and to enable the targeted production of optimized layers, the wide range of coatings was studied by multiple methods from spectroscopic ellipsometry for their dielectric function, by XPS for chemical composition and SEM, TEM to determine their microscopic structure. The coatings were deposited at inert Ar gas and reactive Ar/O2 gas mixture by RF magnetron sputtering or DC pulsed magnetron sputtering with settable RF bias on the substrates. The plasma processes were monitors by mass spectrometry. The metal oxide coatings in SPR sensors have to be prepared reproducible with thickness about 5 nm therefore lower deposition rate conditions were advantages. T2 - THE 14th INTERNATIONAL SYMPOSIUM ON SPUTTERING & PLASMA PROCESSES,ISSP 2017 CY - Kanazawa, Japan DA - 05.07.2017 KW - Surface Plasmon Resonance KW - Magnetron sputtering KW - FeSnOx PY - 2017 AN - OPUS4-43536 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In situ investigations of mechanochemical reactions - new insights in formation pathways N2 - Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals. The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms. We recently introduced a setup enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. In situ Raman spectroscopy coupled with thermography revealed a low temperature increase during milling reactions due to the mechanical impact and clear temperature increases because of the reaction heat. Based on the data, temperature rises as postulated in the magma plasma and hot spot theory can be excluded for soft matter milling syntheses. Our results indicate that in situ investigation of milling reactions offer a new approach to tune and optimize mechanochemically synthesized compounds. T2 - Wissenschaftsforum Chemie CY - Berlin, Germany DA - 10.09.17 KW - Mechanochemistry KW - In situ PY - 2017 AN - OPUS4-43563 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kelly, U. A1 - Richter, S. A1 - Schladitz, K. A1 - Scheuerlein, C. T1 - Nb3Sn wire shape and cross sectional area inhomogeneity in Rutherford cables N2 - During Rutherford cable production the wires are plastically deformed and their initially round shape is distorted. Using X-ray absorption tomography we have determined the 3D shape of an unreacted Nb3Sn 11 T dipole Rutherford cable, and of a reacted and impregnated Nb3Sn cable double stack. State-of-theart image processing was applied to correct for tomographic artefacts caused by the large cable aspect ratio, for the segmentation of the individual wires and subelement bundles inside the wires, and for the calculation of the wire cross sectional area and shape variations. The 11 T dipole cable cross section oscillates by 2% with a frequency of 1.24 mm (1/80 of the transposition pitch length of the 40 wire cable). A comparatively stronger cross sectional area variation is observed in the individual wires at the thin edge of the keystoned cable where the wire aspect ratio is largest. T2 - 13th European Conference on Applied Superconductivity, EUCAS 2017 CY - Geneva, Switzerland DA - 17.09.2017 KW - X-ray computer tomography KW - Image processing KW - Superconducting KW - CERN KW - µCT PY - 2017 AN - OPUS4-43493 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falk, Florian A1 - Menneken, Martina T1 - Early oxidation and sulfidation of high temprature alloys: An EDXRD in-situ study N2 - P92 is one of the important steels for super heater tubes used in combustion plants. However, in fossil fuel fired environments the formation of oxides and sulfides are challenging the material. To understand early corrosion mechanisms, which are important for process prediction, high temperature in-situ ageing experiments of Fe-Cr-Mn alloys in SO2 and SO2+H2O atmosphere were performed, applying energy dispersive X-ray diffraction (EDXRD) analysis. T2 - Bessy usermeeting CY - Berlin, Germany DA - 05.12.2017 KW - Corrosion KW - In-situ KW - EDXRD PY - 2017 AN - OPUS4-45368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wollschläger, N. A1 - Nützmann, Kathrin T1 - What happens during S-corrosion in Fe13Cr in the early stage? N2 - Ferritic alloys containing Cr form Cr5S6 precipitates along grain boundaries in hot SO2 environment. Grain boundary precipitates may influence the steel’s mechanical behavior. Cr5S6 precipitates were reconstructed three-dimensionally using FIB tomography analysis to determine the volume, number, and penetration depth. The volume growth of Cr5S6 precipitates increased only for the initial aging time of 3 h but became constant after 6 h. The number of precipitates increased linearly. T2 - Meeting on Focused Ion Beams in Berlin - FIBiB2017 CY - Berlin, HZB Wannsee Campus, Germany DA - 06.11.2017 KW - Grain boundary corrosion KW - 3D tomography KW - Sulfidation PY - 2017 AN - OPUS4-45061 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane T1 - Real time observation of crystallization and growth of corrosion products by energy dispersive X-ray diffraction N2 - Ferritic-martensitic high temperature alloys are widely used as boiler tube and heat exchanger materials in combustion based power plants. All technologies have in common that the applied materials are exposed to different temperatures, process pressures and reactive atmospheres which lead to a change of the material properties and a further degradation of the material. To date corrosion analytics mainly proceeds via the use of various microscopic techniques and the analysis of the corrosion products after the reaction is completed. Comprehensive efforts have been made to study high temperature corrosion by the use of environmental SEM’s or in-situ TEM technologies. The here presented work will show a different approach to study high temperature gas corrosion in a multiple gas atmosphere by energy dispersive X-ray diffraction (EDXRD). For this technique high energetic white X-ray radiation (10-100 keV) was used as radiation source instead of conventional monochromatic radiation. It enables us to study crystallization procedures on short and medium time scales (1 min < t < 24 h) and the collection of Bragg-Signals of the phases of interest as a function of process time. Their occurrence can directly be correlated with thermodynamic and kinetic parameters. A special designed corrosion reactor was used to combine high temperature gas corrosion experiments with the collection of diffraction patter. The crystallization and reaction paths for oxide and sulfide formation was followed in-situ on Fe-Cr and Fe-Cr-Mn model alloys in a hot SO2 containing (T=650 °C) atmosphere. T2 - Gordon Research Conference on High Temperature Corrosion and Protection of Materials CY - New London, NH, USA DA - 09.07.2017 KW - Corrosion KW - In situ diffraction KW - Crystallization PY - 2017 AN - OPUS4-44717 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Barnefske, Lena T1 - Self-healing silicone rubber for F-POF partial discharge sensors in HV cable accessories N2 - To avoid a catastrophic failure of insulation in high-voltage (HV) applications, a monitoring of partial discharges (PD) is necessary. Fluorescently labelled polymer optical fibres (F-POF) offer an electrically passive method for PD detection in HV facilities. F-POF could be embedded into HV cable insulation material, which are usually made of silicone rubber. Due to the difficult accessibility of HV cable accessories, a self-healing silicone rubber, based on incorporated capsules, with prolonged service life after PD detection represents an attractive material design for HV electrical insulation. T2 - 26th International Conference on Plastic Optical Fibres CY - Aveiro, Portugal DA - 13.09.2017 KW - Fluorescent polymer optical fibres KW - Partial discharge detection KW - High voltage cable accessories KW - Self-healing KW - Silicone rubber PY - 2017 AN - OPUS4-42511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stajanca, Pavol T1 - Post-fabrication cladding doping of commercial PMMA polymer optical fiber N2 - Possibility of post-fabrication doping of commercial PMMA fibers using well-known solution doping technique is presented. The cladding of 1 mm PMMA fiber is doped with Rhodamine B with the help of methanol-mediated diffusion of the dye molecules into the fiber material. Doping of the fiber core was not possible even at extended doping times. The proposed method represents rather simple and cheap way for preparing custom cladding-doped POFs with high flexibility of dopant choice and fiber length. Produced cladding-doped fibers have potential for various sensing or lighting applications. T2 - 26th International Conference on Plastic Optical Fibres (POF 2017) CY - Aveiro, Portugal DA - 13.09.2017 KW - Polymer optical fibers KW - Fluorescent dyes KW - Solution doping KW - Polymethyl methacrylate PY - 2017 AN - OPUS4-42321 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosemann, Paul T1 - Einfluss der Schweißnaht-Nachbehandlung auf die Korrosionsbeständigkeit von nichtrostenden Duplexstählen N2 - Der Duplexstahl 1.4062 (X2CrNiN22-2) hat sich im Bauwesen als Werkstoffalternative zu den nichtrostenden Austeniten etabliert. Die Korrosionsbeständigkeit von Schweißverbindungen wird, neben dem Grundwerkstoff, dem Schweißzusatzwerkstoff und dem Schweißverfahren, auch sehr stark von der Oberflächennachbehandlung der Schweißnaht beeinflusst. Je nach zukünftigem Anwendungsbereich und geforderter Optik sowie Korrosionsbeständigkeit wird der Schweißnahtbereich anschließend geschliffen, gebeizt, elektropoliert, oder gestrahlt, um die beim Schweißen entstehenden Zunderschicht zu entfernen. Gestrahlte Oberfläche sind in der industriellen Praxis häufig anzutreffen, da sie deutlich einfacher und kostengünstiger herzustellen sind als gebeizte oder elektropolierte Oberflächen. Die Auswahl des Strahlmittels bestimmt auch die Prozesskosten, wobei das Strahlen mit Korund effektiver als das Strahlen mit Glasperlen ist. In den letzten Jahren wurden bei nichtrostenden Stählen korrosionsanfällige Oberflächen beobachtet, wenn diese mit Korund geschliffen wurden. Daher wird nun auch beim Strahlen kritisch hinterfragt, ob das Strahlmittel die Korrosionsbeständigkeit verändert. Diese Fragestellung wird beantwortet indem geschliffene, gebeizte, mit Korund gestrahlte und mit Glasperlen gestrahlte Schweißverbindungen vergleichend untersucht werden. Die Ergebnisse der REM-Untersuchungen von den Strahlmitteln und den gestrahlten Oberflächen werden dazu mit den Ergebnissen verschiedener Korrosionsuntersuchungen (KorroPad-Indikatortest, Potentialmessungen und Bestimmung der kritischen Lochkorrosionspotentiale) korreliert und vorgestellt. T2 - Werkstoffwoche 2017 CY - Dresden, Germany DA - 27.09.2017 KW - Duplexstahl KW - Korrosion KW - Nichtrostender Stahl KW - Oberflächenbearbeitung KW - Schweißen KW - Strahlen PY - 2017 AN - OPUS4-42830 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Babutzka, Martin T1 - Einfluss von Korundschleifprozessen auf die Korrosionsbeständigkeit nichtrostender Stähle N2 - Das Poster stellt aktuelle Eregbnisse des AiF-Vorhabens 18823 N/1 zum Einfluss von Schleifprozessen auf die Korrosionsbeständigkeit nichtrostender Stähle vor. T2 - Jahrestagung 2017 der GfKORR CY - Frankfurt a. M., Germany DA - 07.11.2017 KW - Korrosion KW - Corrosion KW - Korundschleifen KW - Corundum grinding KW - Nichtrostende Stähle KW - Stainless Steels PY - 2017 AN - OPUS4-42773 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Höhne, Patrick T1 - Utilization of an ultra sound atomizer for spray granulation of oxide ceramic fine powder N2 - Spray drying based granulation processes aim for flowable granules neither containing voids nor hard shells thus leading to a homogenous microstructure in the green and sinter bodies without strength reducing large pores. The increase of the specific surface area due to the utilization of finer powders as raw materials makes the production of granules of demanded quality more sophisticated. Innovations regarding additives as well as process engineering are therefore required. While conventional spray granulation processes of ceramic materials are based on rotational, one stream or two stream nozzles for nebulization, the investigations in the ZIM project concentrate on the applicability of an ultra sound atomizer unit. A spray dryer comprised of the aforementioned ultra sound atomization unit implemented in a commercial spray dryer (Niro, Denmark) was used as test system. Potential advantages of the ultra sound nebulization are investigated for model systems of alumina, zirconia and a ZTA composite while focusing on solids content, yield, pressability and granule properties (size, size distribution, flowability, shape and microstructure) as well as the final sinter body properties (density, microstructure and flexural strength). First ultra sound spray drying experiments yielded granules with excellent processability. Spray drying of identical slurries, as before tested and optimized for a two stream nozzle atomization process, resulted in a more suitable size distribution for dry pressing (less particles below 20 µm) and a higher yield. Furthermore, sinter bodies produced of ultra sound granules seem to have less large pores and a more homogenous microstructure T2 - 92. Jahrestagung der deutschen keramischen Gesellschaft CY - Berlin, Germany DA - 20.03.2017 KW - Ceramics KW - Spray drying KW - Ultra sound KW - Atomization KW - Microstructure PY - 2017 AN - OPUS4-39588 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sentker, Kathirn A1 - Yildirim, Arda T1 - Fabrication of organic nanowires by melt infiltration of a discotic liquid crystal: A combined X-ray diffraction and optical birefringence study N2 - Optical polarimetry and angle dependent X-ray scattering in employed to study the structure of a discotic liquid crystal confined into nanochannels. The pore size dependence of the obtauned data are discussed in detail. T2 - DPG Spring Meeting 2017 CY - Dresden, Germany DA - 20.03.2017 KW - Discotic Liquid Crystals KW - Nanoconfinement PY - 2017 AN - OPUS4-39591 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Yildirim, Arda T1 - Structure, Dynamics and Phase Behavior of a Discotic Liquid Crystal Confined in Nanoporous Anodic Aluminum Oxide Membranes N2 - The interest in porous anodic aluminum oxide (AAO) has been rapidly growing due to its numerous applications in separation, catalysis, energy generation and storage, electronics, and sensors. From the scientific point of view, AAO is a topical interest in soft matter fields. Spatial confinement of soft matter in nanoporous media influences its structure, thermodynamics, and mobility. Embedding polymers and liquid crystals into nanopores of AAO results in a 2D nanoconfinement of these materials. This confinement affects their properties, compared to the bulk, such as phase transition temperatures and enthalpies, molecular mobility, and architecture of the crystallization. On the other hand, discotic liquid crystals (DLCs) are a promising class of soft matter for electronic applications. This is due to their ability to organize and stack themselves into columns in a hexagonal columnar mesophase, a mesophase in between the plastic crystalline and isotropic phase, driven by the overlap of the π orbitals of their aromatic core. This leads to a high charge-carrier mobility along the column axis. Further, these columns could then be considered as “molecular nanowires”. In this study, 2,3,6,7,10,11 hexakis[hexyloxy] triphenylene (HAT6), a triphenylene based DLC, was confined into nanoporous AAO membranes. The structure, dynamics and the phase behavior of the confined HAT6 were investigated by broadband dielectric spectroscopy (BDS) and differential scanning calorimetry (DSC). HAT6 was embedded into nanoporous AAO membranes by melt infiltration in the isotropic phase under argon atmosphere. The membranes have parallel aligned cylindrical nanopores, with pore diameter of 10, 20, 25, 40, 80, 120 and 180 nm. The filling degree for each sample was checked by thermogravimetric analysis (TGA) in order to ensure complete filling. Bulk HAT6 forms a hexagonal columnar phase; in between the isotropic phase above 371 K and the plastic crystalline phase below 340 K. Unlike the bulk, the confined HAT6 split the plastic crystalline-to-hexagonal columnar phase transition in two, which might be interpret as two different phase structures; close to the wall and at the pore center. Moreover, the isotropic-to-columnar transition of the confined HAT6 shifted, with decreasing pore diameter, to lower temperatures. Furthermore, pore surfaces of a series of membranes were chemically modified, resulting in a more hydrophobic pore surface than the unmodified ones. HAT6 was embedded into the modified membranes by the same aforementioned preparation. The influence of the changed host-guest-interaction, on the structure, dynamics, and the phase behavior of HAT6 confined in the modified membranes, was also investigated by BDS and DSC. T2 - 9th International Conference on Porous Media & Annual Meeting CY - Rotterdam, The Netherlands DA - 08.05.2017 KW - Nanoporous media KW - Anodic Aluminum Oxide KW - Discotic Liquid Crystal PY - 2017 AN - OPUS4-40089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schadow, Florian T1 - Sende-Empfangs-Prüfköpfe auf Ferroelektret-Basis für Luftultraschall-Anwendungen N2 - Leichtbaustrukturen aus Verbundwerkstoffen stellen einen immer größeren Anteil im Flugzeug- und Automobilbau dar. Hiermit steigt die Nachfrage nach zuverlässigen, zerstörungsfreien Prüfmethoden, welche an solche Strukturen angepasst sind. Besonders Luftultraschall (LUS) eignet sich für diese Aufgabe, da hier kein Koppelmedium benötigt wird. Derzeit wird für diese Methode jedoch oft ein beidseitiger Bauteilzugang für eine Prüfung in Durchschallung vorausgesetzt. Handelsübliche Prüfköpfe für Luftultraschallanwendungen nutzen zudem meist Anpassschichten um den Impedanzunterschied zwischen Schwinger und Luft zu reduzieren. Sowohl Signal-Rausch-Abstand als auch die Bandbreite der resultieren-den Prüfköpfe ist für viele Anwendungen jedoch nicht ausreichend. Durch den Einsatz von Ferroelektreten wie zellulärem Polypropylen (zPP) kann hingegen vollständig auf Anpassschichten verzichtet werden. Hierbei handelt es sich um polarisierte, zelluläre Polymerschichten mit sehr geringer Dichte, Steifigkeit und Schallgeschwindigkeit. In diesem Beitrag stellen wir drei verschiedene Sende-Empfangs-Prüfköpfe vor, welche auf zellulärem Polypropylen basieren. Anhand von Schallfeld, Signal-Rausch-Abstand und Sendepegel werden diese Prüfköpfe charakterisiert. Die Ergebnisse werden mit den Ergebnissen von Referenzprüfköpfen ohne Sende-Empfangs-Charakteristik verglichen. Bei den Referenzprüfköpfen werden sowohl handelsübliche LUS-Prüfköpfe, sowie bisher entwickelte Prüfköpfe aus zellulärem Polypropylen berücksichtigt. T2 - DGZFP Jahrestagung 2017 CY - Koblenz, Germany DA - 22.05.2017 KW - Sende-Empfangs Prüfkopf KW - Ferroelektret KW - Zelluläres Polypropylen KW - Charakterisierung KW - Luftultraschall PY - 2017 AN - OPUS4-40430 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Otremba, Frank T1 - Testing of pressurized vessels N2 - The results are based on data1. Figure 3 displays temperatures of the tank wall and of the gas phase over testing time. It can be seen that a complete coating strongly delayed the heating of tank wall and gas phase, whereas the partly coated tanks only had a minor influence on temperature development. There was no significant difference between a half coated and a thirdly coated tank measurable. Figure 4 shows the internal pressure of tanks over testing time. Only the fully coated tank enabled a low pressure over 90 min testing time. Hence, a complete coating is necessary to guarantee the fire safety of hazmat tanks and a partly coating is not sufficient. T2 - Annual Conference on Engineering and Information Technology CY - Nagoya - Japan DA - 29.03.2017 KW - Fire KW - Testing KW - Vessels KW - Dangerous goods PY - 2017 AN - OPUS4-39843 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schlichting, S. A1 - Hönig, Gerald T1 - Tuning of the quantum-confined Stark effect in wurtzite [0001] nanostructures by the internal-field-guarded-active-region design N2 - In this work we eliminate the QCSE without having any special requirements on the growth procedure or the material. Hönig et al. developed the Internal-Field-Guarded-Active-Region Design (IFGARD), which we experimentally investigate in this work based on GaN/AlN nanodiscs (NDs). T2 - Compound Semiconductor Week 2017 CY - Berlin, Germany DA - 14.05.2017 KW - Halbleiterphysik KW - Nanophysik KW - Optoelektronik KW - Piezopolarisation KW - Spontane Polarisation PY - 2017 AN - OPUS4-40174 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schulz, Bärbel T1 - High-temperature stability of ceramic springs N2 - Metallic springs undergo oxidation and creep at elevated temperatures and their use is limited to temperature of about 650°C. Therefore, there is a need for stable materials which can easily withstand temperatures up to 1000°C for long periods in different atmospheres. Ceramic materials have been drawing attention due to their excellent properties. This work aimed at investigating the high-temperature stability of zirconia and alumina ceramic springs at elevated temperatures under different atmospheres (air, N2 and H2) in order to determine the limitation of use of these ceramic springs. T2 - DKG 2017 CY - Berlin, Germany DA - 20.03.2017 KW - Ceramic spring KW - High-temperature stability KW - Harsh environments KW - Spring constant PY - 2017 AN - OPUS4-40289 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Czarnecki, Sebastian T1 - Synthesis of hybrid inorganic/organic homopolymers via ATRP and RAFT: A practical comparison N2 - The synthesis of hybrid inorganic/organic copolymers, using reversible deactivation radical polymerization (RDRP) techniques, has been an intensively studied research topic over recent years. A plethora of hybrid inorganic/organic copolymers were synthesized, including hybrid inorganic/organic block copolymers as well as random copolymers,[1–4] that showed great potential in fabricating hybrid (nano)materials with tailored properties [5]. Two widely employed RDRP techniques to prepare such hybrid inorganic/organic copolymers are atom transfer radical polymerization (ATRP) [1,2] and reversible addition-fragmentation chain transfer (RAFT) polymerization [3,4]. In order, to afford hybrid inorganic/organic copolymers with narrow dispersity, high conversions and precise structures, it is required to choose proper reaction conditions. Due to the importance of both ATRP and RAFT in the preparation of such hybrid polymers, we aim to compare both RDRP techniques by preparing 2-acetoxyethyl methacrylate (AcEMA) and 3-(triethoxysilyl)propyl methacrylate (TESPMA) based homopolymers. For this purpose, AcEMA and TESPMA were polymerized in 1,4-dioxane at 60 °C mediated by CuBr/N,N,N',N'-pentamethyldiethylenetriamine (PMDETA) and 2-(2-carboxylethylsulfanylthiocarbonyl-sufanyl) propionic acid (TTC) as well as cumyl dithiobenzoate (CDB) to evaluate the suitability and reliability of ATRP and RAFT to prepare such hybrid (co)polymers. T2 - Berlin Chemie Symposium 2017 CY - TU Berlin, Berlin, Germany DA - 06.04.2017 KW - Hybrid inorganic/organic copolymers KW - ATRP KW - RAFT PY - 2017 UR - https://bcs.jcf-berlin.de/BCS2017/BoA2017.pdf AN - OPUS4-40280 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel T1 - Hochauflösende Reinheitsgradbestimmung – Fertigung von Referenzfehlern N2 - Regelwerke zur zerstörungsfreien Bestimmung des Reinheitsgrades wie das SEP 1927 und die ASTM E588 erreichen ihre Vergleichbarkeit unter Anwendung von - vergleichsweise einfachen - Referenzfehlern. Hinsichtlich Realisierbarkeit wird somit der Kompromiss zwischen Herstellung des Referenzfehlers und der erreichbaren Nachweisgrenze gefunden. Zur Weiterentwicklung über die Grenzen der SEP1927 hinaus, wurde der Versuch unternommen Fehler kleiner 500 μm herzustellen - welche aufgrund der geringen geometrischen Ausdehnung fertigungsbedingt schwierig zu realisieren sind. Bei den vergleichenden Untersuchungen kristallisierten sich zwei Fertigungsverfahren, Funkenerosion (EDM: electrical discharge maching) und die Fertigung der Bohrungen unter Verwendung eines Hochleistungslasers, als vielversprechend heraus. Zunächst wurden die Fehler mit beiden Verfahren in unterschiedlichen Größen (100, 250 und 100 μm) und Tiefen (1, 1,5 und 2 mm) unter Anwendung von computertomographischen Verfahren der Röntgenprüfung, die Geometrie der eingebrachten Fehlstellen und anschließend durch hochauflösende Tauchtechnikmessungen das Reflektionsverhalten charakterisiert. T2 - DGZfP Jahrestagung CY - Koblenz, Germany DA - 22.05.2017 KW - Materialcharakterisierung KW - Reinheitsgradbestimmung KW - Ultraschalltauchtechnik PY - 2017 AN - OPUS4-40353 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Woydt, Mathias T1 - Potentials of niobium carbide (NbC) as cutting tools and for wear protection N2 - Niobium is today largely available. NbC grades displayed lower dry sliding friction over WC grades. The softer Ni- and NiMo-bondes NbC1.0-grades have a higher abrasive wear resistance (ASTM G65), even with lower toughnesses, as the tougher WC-Co grades. T2 - 19. Plansee Seminar CY - Reutte, Austria DA - 29.05.2017 KW - Niobium carbide (NbC) KW - Cutting tools KW - Hardness PY - 2017 AN - OPUS4-40512 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wäsche, Rolf T1 - Colloidal processing of metal bonded niobium carbide (NbC-Ni) N2 - The manufacturing of NbC with Ni binder with addition of titanium carbide by using a colloidal process for blending the different powders without a milling step were investigated. The the sintering process and formation of the resulting microstructures, the phase relations and the hardness of the produced cermet materials are characterized. T2 - 19. Plansee Seminar CY - Reutte, Austria DA - 29.05.2017 KW - Niobium carbide (NbC) KW - Cermets KW - Hardness PY - 2017 AN - OPUS4-40513 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kabelitz, Anke T1 - A02: Time-resolved WAXS studies on the crystallization of Al13 keggin clusters N2 - Polynuclear aluminium species (Al13 keggin cluster) find application in different areas like water purification, contaminant transport, and as pilling clays with high specific surface areas, due to their strong binding ability to aggregates and high positive charge. In the present contribution, we report on the in situ investigation of the Al13 sulfate synthesis by synchrotron wide-angle X-ray scattering (WAXS). Al13 cluster were crystallized by precipitating hydrolyzed aluminum solutions by the addition of sodium sulfate. The measurements were performed using a custom-made acoustic levitator as sample holder. The study provides information about the intermediates during the crystallization process. From the data, a mechanism was derived indicating the influence of the crystallization process. T2 - International Symposium of the CRC 1109 CY - Berlin, Germany DA - 19.02.2017 KW - WAXS KW - In situ KW - Crystallization PY - 2017 AN - OPUS4-39367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosignuolo, F. T1 - A comparison between empirical models and FDS simulation to predict the ceiling gas temperature distribution in a tunnel fire N2 - A comparison between the results obtained from a Computational Fluid Dynamic (CFD) simulation and from the application of an empirical formula for determining the temperature distribution inside a tunnel in case of fire is presented. The temperature is measured and calculated at different distances from the location of the fire and at different time intervals. The fire considered varies with time following a time-heat release rate curve which has a parabolic growing phase, a constant period and a linear decay. The comparison reveals differences in the results. The temperatures calculated with the empirical formula resulted higher than the temperatures obtained by means of the CFD simulation. A list of possible reasons for this limited correspondence is also presented and commented. A proposal for further studies to better define the limitations of both the procedures and to define the influence of each parameter involved is finally presented. T2 - World Tunnel Congress 2017 – Surface challenges – Underground solutions CY - Bergen, Norway DA - 09.06.2017 KW - CFD KW - Fire KW - Tunnel KW - Design Fire PY - 2017 AN - OPUS4-40655 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Uhlmann, E. T1 - Cutting tools made from niobium carbide N2 - The Federal Institute for Materials Research and Testing (BAM) and the Institute for Machine Tools and Factory Management (IWF) of the Technical University Berlin analyzed the suitability of various NbC types in comparison to tungsten carbide (WC) for use as a tool in cutting processes. The focus was placed on the optimization of the functional profile of NbC-based cutting materials with reproducible industrial production. T2 - 19. Plansee Seminar CY - Reutte, Austria DA - 29.05.2017 KW - Niobium carbide (NbC) KW - Tungsten carbide (WC) KW - Cutting material PY - 2017 AN - OPUS4-40515 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisermann, René T1 - Reducing sensitivity fading in C-OTDR by use of enhanced scattering fiber segments N2 - We have shown that for C-ODTR based DAS two UV-inscribed scattering segments within an optical fiber have a significant influence on the local sensitivity Fading characteristics. This method was experimental proven to be suitable for distributed dynamic strain measurement in a thermally unstable environment. Signal-to-noise ratio analyses for detecting a signal peak within the time-dependent spectra were performed. Results show an increase in SNR and additionally that the occurrence of total loss of sensitivity (SNR <1) could be decreased by a factor of six when compared to an untreated standard fiber. T2 - 25th International Conference on Optical Fiber Sensors CY - Jeju-City, Jeju, Republic of Korea DA - 24.04.2017 KW - Coherent Rayleigh OTDR KW - Distributed acoustic sensing KW - Distributed vibration sensing KW - Fiber sensors KW - Quasi-distributed sensing KW - Rayleigh scattering PY - 2017 AN - OPUS4-40643 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Huang, S. G. T1 - Effect of carbon content on the microstructure and mechanical properties of NbC-Ni based cermets N2 - The aim of this work was to correlate the carbon content in NbC-Ni starting powders with the resulting microstructure, hardness and fracture toughness of Ni-bonded NbC cermets. T2 - 19. Plansee Seminar CY - Reutte, Austria DA - 29.05.2017 KW - Cermet KW - Liquid phase sintering KW - Microstructure KW - Hardness KW - Carbon PY - 2017 AN - OPUS4-40647 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Genga, R. M. T1 - Microstructure and wear behavior of improved NbC cermets for (BS-1452) grey cast iron machining N2 - Tungsten carbide (WC) and cobalt (Co) based cermets are the most successful commercial cermets beacuse of the good combination of physical, mechanical and behavioral properties. Niobium carbide (NbC) has good mechanical and physical properties, such as high hardness, very high melting point and low density. SPS refined the NbC grains and increased the hardness, while substitution of Co with Ni improved the fracture toughness. T2 - 19. Plansee Seminar CY - Reutte, Austria DA - 29.05.2017 KW - Cermets KW - Grey cast iron machining KW - Tungsten carbide (WC) KW - Niobium carbide (NbC) KW - Wear PY - 2017 AN - OPUS4-40603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - Material properties and their impact on laserinduced plasmas for concrete analysis N2 - For concrete production aggregates, cement and water are mixed together and after 28 days of hydration a porous and multiphase material is formed. To consider the heterogeneity of concrete a 2D scanning system is used. The coarse aggregates (limit > 2 X d ) can be excluded. laser spot The remaining content is a mixture of flour grains and cement particles (micro heterogeneity). Harmful species like chlorides may penetrate together with water through the capillary pore space. A quantification of Cl regarding to the cement content only (European standard EN 206) is necessary for the damage assessment. A LIBS system operating with a NdCr:YAG laser (pulse energy of 3 mJ, a wavelength of 1064 nm, a pulse width of 1.5 ns, a repetition rate of 100 Hz) and two Czerny-Turner spectrometer (UV and NIR range) have been used. T2 - EMSLIBS Konferenz 2017 CY - Pisa, Italy DA - 12.06.2017 KW - Concrete KW - LIBS KW - Micro-heterogeneity PY - 2017 AN - OPUS4-40938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Martin T1 - Development of a material model for the crush of spruce wood N2 - Typical transport packages used in Germany are equipped with wooden impact limiting devices. In this paper we give an overview of the latest status regarding the development of a finite element material model for the crush of spruce wood. Although the crush of wood – mainly in longitudinal direction – is a phenomenon governed by macroscopic fracture and failure of wood fibres we smear fracture and failure mechanisms over the continuous voume. In first step we altered an existing LS-DYNA material model for foams, which considers an ellipse shaped yield surface written in terms of the first two stress invariants. The evolution of the yield surface in the existing model depends on the volumetric strain only. For the use with spruce wood, we modified the existing material model to consider the deviatoric strain for the evolution of the yield surface as well. This is in accordance with the results of crush tests with spruce wood specimens, where the crushing deformation was rather deviatoric for uniaxial stress states and rather volumetric for multiaxial stress states We rate the basic idea of this approach to be reasonable, though other problems exist regarding the shape of the yield surface and the assumption of isotropic material properties. Therefore we developed a new transversal isotropic material model with two main directions, which considers different yield curves according to the multiaxiality of the stress state via a multi-surface yield criterion and a non-associated flow rule. The results show the ability to reproduce the basic strength characteristics of spruce wood. Nevertheless, problems with regularization etc. show that additional investigations are necessary. T2 - ASME PVP 2017 CY - Waikaloa, HY, USA DA - 16.07.2017 KW - Crush KW - Wood KW - Spruce KW - FEM PY - 2017 AN - OPUS4-41617 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Babutzka, Martin A1 - Reinemann, Steffi T1 - Influence of corundum grinding processes on the corrosion behaviour of austenitic stainless steels N2 - The scientific poster shows by means of corrosion testing in combination with surface analytical methods to which degree corundum grinding influences the corrosion behaviour of stainless steel surfaces. The austenitic stainless steel AISI 304 from a consistent heat was used for all investigations to guarantee the same chemical composition and thus no additional influences caused by the material itself. A wide range of different grinding parameters such as pressure, cooling medium and grain size of the abrasive was varied. Thus, comparison of the corrosion behaviour of different surface states and the evaluation of an optimum grinding process using corundum abrasives were possible. The results will contribute to present discussions and give novel impulses for companies in the metalworking industry. T2 - Eurocorr 2017 CY - Prague, Czech Republic DA - 03.09.2017 KW - Korrosion KW - Corrosion KW - Korundschleifen KW - Corundum grinding KW - Nichtrostende Stähle KW - Stainless steels PY - 2017 AN - OPUS4-41896 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sahre, Mario T1 - Electroplated magnetostrictive actuator layer enabling the external diagnosis of strain sensors N2 - Embedded fibre-opticaloptical strain sensors are suitable for structural health monitoring. In order to validate long-term performance (e.g.sensors integrated in airplane wings or wind power turbine blades) an external diagnostics is required. A strain-detecting region of the optical fibre, the fibre Bragg grating (FBG, is encased by a magnetostrictive layer system serving as actuator. For the validation of the correct sensor function, an external magnetic field introduces mechanical strain resulting in a defined shift of the Bragg wavelength. The layer system is realized by acombined PVD /ECD process optimized regarding magnetostrictive and mechanical properties. The long -term stability of layer adhesion and actuator function has been verified. T2 - 12. Thementage Grenz- und Oberflächentechnik (ThGOT) und das 5. Kolloquium Dünne Schichten in der Optik CY - Zeulenroda, Germany DA - 14.03.2017 KW - Magnetostrictive actuator layer KW - PVD /ECD process KW - Magnetostrictive layer KW - Strain sensors PY - 2017 AN - OPUS4-41800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lange, Thorid T1 - Mehr-Proben-Kleb-Vorrichtung (MPKV) zur Validierung der Klebfestigkeit N2 - Mit der Verfügbarkeit der Mehr-Proben-Prüfung von bis zu 8 Klebverbunden mittels CAT-Technologie (CAT: centrifugal adhesion testing) wurde im Forschungsvorhaben OKTETT ein durchgehendes Mehr-Proben-Konzept zur Validierung der Klebfestigkeit angewendet. Dazu gehört ein universeller Probenteller (Abb.1) zur Mehr-Proben-Handhabung bei Vorbehandlung, Lagerung, Transport und Klebung. Für das Mehr-Proben-Kleben wurde die MSB-Technologie (MSB: multiple sample bonding) unter Verwendung einer instrumentierten hydraulischen Mehr-Proben-Kleb-vorrichtung entwickelt. Damit kann der Klebandruck für bis zu 8 Prüfkörper über einen Drucksensor definiert eingestellt und die gesamte Vorrichtung beim Kleben Temperaturen von bis zu 180°C ausgesetzt werden. T2 - 12. Thementage Grenz- und Oberflächentechnik (ThGOT) und das 5. Kolloquium Dünne Schichten in der Optik CY - Zeulenroda, Gemany DA - 14.03.2017 KW - Zentrifugentechnologie KW - Mehr-Proben-Kleben (MSB) KW - Mehr-Proben-Prüfen (CAT) KW - Haftfestigkeit KW - Verbundfestigkeit PY - 2017 AN - OPUS4-41291 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sentker, K. A1 - Yildirim, Arda T1 - Characterization of the thermotropic phase behavior and microscopic structure of a confined discotic liquid crystal N2 - Discotic liquid crystals (DLC) filled into cylindrical nanopores exhibit a liquid crystalline phase with their molecules arranged in hexagonal columns. The columns orient perpendicular (radially) or parallel (axially) with respect to the pore axis depending on surface anchoring conditions and pore size. Axially oriented columns enable the fabrication of organic nanowires utilizing the high conductivity in the stacking direction due to overlapping π-electrons. This leads to interesting applications in e.g. organic semiconductorbased devices. The molecular ordering of the liquid crystalline columns can be probed by temperature dependent optical retardation measurements supplemented by X-ray diffraction sensitive to the translational order. We investigated the DLC 2, 3, 6, 7, 10, 11 - hexakis [hexyloxy] triphenylene (HAT6) embedded in nanoporous alumina and silica membranes as function of the pore diameter (12 nm - 180 nm). Due to their hydrophilic nature porous membranes enforce face-on anchoring leading to a radial orientation. To obtain edge-on anchoring conditions, and thus favoring axial orientation, the silica membrane surface is chemically modified. The optical retardation measurements show that the columns orient radially in these membranes independent of the anchoring conditions. Interestingly, a quantized phase transition of each molecular layer is found indicated by a distinct increase of the optical orientation. Additionally, an axial orientation of HAT6 filled into alumina membranes with a pore diameter of 25 nm is achieved. A Landau-de Gennes ansatz semi-quantitatively describes the phase transition behavior observed. X-ray diffraction experiments performed at the 3rd generation synchrotron radiation source PETRA III at DESY giving detailed information about the translational order support these findings. Summarizing, this study shows the existence of a phase transition in the molecular range as well as the suitability of the membrane with 25 nm pores as a template for preparing organic nanowires. T2 - Liquids 2017 – 10th Liquid Matter Conference CY - Ljubljana, Slovenia DA - 17.07.2017 KW - Discotic Liquid Crystals PY - 2017 AN - OPUS4-41180 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertin, Annabelle T1 - Upper critical solution temperature (UCST)- type thermoresponsive polymers from acrylamide-based monomers N2 - UCST-type thermoresponsive polymers that phase separate from solution upon cooling present a tremendous potential not only in aqueous media where they can be used in drug delivery, diagnostic and microfluidic applications, but also in water/alcohol mixtures, where they can be used for instance in sensing systems for alcohol-soluble drugs. However, only a few thermoresponsive polymers have been reported that present an UCST in a relevant temperature range and “green” solvents such as water or ethanol. In this context, acrylamide-based monomers can be very useful building blocks for designing novel UCST-type polymers because of their hydrophilic nature (with the right side chain) and propensity to form hydrogen bonds. We want to present our latest results on the copolymer poly(acrylamide-co-acrylonitrile) (P(AAm-co-AN)) that present a UCST in water as well as on two homopolymers based on an acrylamide derivative of 2,6-diaminopyridine, namely poly(N-(6-aminopyridin-2-yl)acrylamide) (PNAPAAm) and poly(N-(6-acetamidopyridin-2-yl)acrylamide) (PNAcAPAAm) that show UCST-type thermoresponsiveness in water/alcohol mixtures. Our focus for P(AAm-co-AN)) is its aggregation behaviour above and below its phase transition temperature as the size of thermoresponsive polymeric systems is of prime importance for biomedical applications (as size dependent processes take place in the body) and is linked to the optical properties of a material that matter in materials science. In the case of PNAPAAm and PNAcAPAAm, we focused on the co-solvency/co-non solvency effect on the phase transition temperature in water/alcohol mixture. Indeed, polymers with UCST behavior below 60°C in water/alcohol mixtures are extremely promising for the preparation of “smart” materials for sensing. T2 - 31st Conference of the European Colloid and Interface Society (ECIS 2017) CY - Madrid, Spain DA - 03.09.2017 KW - Thermoresponsive polymers KW - UCST polymers KW - Acrylamide based polymers PY - 2017 AN - OPUS4-41902 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Erdmann, Maren T1 - Effect of surface degradation on high-density polyethylene for initial attachment of bacillus and pseudomonas N2 - High-density polyethylene (PE-HD) is a widely applied plastic for fuel storage tank applications. But such tanks, filled with diesel or biodiesel, provide excellent environmental conditions for growth of a broad spectrum of fungi and various bacteria1. This can result in fuel contamination, engine plugging or possible (bio-) degradation2. Our research focusses on the initial attachment phase of Bacillus sp. and Pseudomonas aeruginosa isolated from a „dieselpest“2 on two distinctly PE-HD materials, typical for fuel storage tank applications, pre-damaged thermally and by UV-irradiation. T2 - PDDG CY - Taormina, Sicily, Italy DA - 04.09.2017 KW - PE-HD KW - UV-irradiation KW - Initial attachment KW - Bacteria PY - 2017 AN - OPUS4-41908 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Erdmann, Maren T1 - Long-term storage of high-density polyethylene in biodiesel and diesel fuels N2 - Sustainable energy and clean engine fuels receive more and more attention. Petrodiesel could be substituted by biofuels such as biodiesel produced from renewable resources. Biodiesel is derived by transesterification of oils with alcohols for example vegetable oils, animal fats or food waste. Its chemical composition of unsaturated fatty methyl acids causes biodiesels susceptibility to oxidation. Especially, the polymer-biodiesel performance under long-term conditions has been considered only in few researches. Our study addresses a long-term storage scenario of a polymeric fuel tank containing biodiesel or diesel. T2 - PDDG CY - Taormina, Sicily, Italy DA - 04.09.2017 KW - PE-HD KW - Degradation KW - Biodiesel KW - Diesel PY - 2017 AN - OPUS4-41909 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schreier, Andy T1 - Analytical model for mode-based insertion loss in ball-lensed coupling of graded-index silica and polymer fibres N2 - Analytical model for ball-lensed couplers to calculate the insertion loss for each optical mode. The basis for the calculation are commercial perfluorinated polymer optical (PFGI-POFs) and silica based fibres (SOFs). The modal power distribution for given misalignments are presented as well as the reflection-based losses at all optical interfaces. Additionally, the ball-lensed interconnection between PFGI-POF and SOF was theoretically demonstrated. T2 - POF 2017: 26th International Conference on Plastic Optical Fibres CY - Aveiro, Portugal DA - 13.09.2017 KW - Polymer optical fibre KW - Optical connector PY - 2017 AN - OPUS4-41974 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fontana, P. T1 - Healthier life with eco-innovative components for housing constructions N2 - The project has developed a variety of new multifunctional and flexible building components for a healthier indoor environment. [H] house solutions are durable, energy efficient, safe and affordable. They are suitable for use in new buildings and for renovation. [H] house solutions cover aspects of long service life, reduced maintenance and long-term improvement of energy efficiency. T2 - H-House Abschluss-Kolloquium, Dauerausstellung am Demonstrator-Gebäude CY - Warsaw, Poland DA - 23.08.2017 KW - Building materials KW - Beton KW - UHPC PY - 2017 AN - OPUS4-43003 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waurischk, Tina T1 - New device for inert crack growth measurements in ultra-strong glasses N2 - The practical strength of glasses under ambient conditions is substantially lower compared to its intrinsic strength because of sub-critical crack growth (SCCG) from microscopic flaws. While SCCG is related to the humidity of the ambient atmosphere, leading to stress corrosion phenomena, the detailed kinetics are still not fully understood. To get better insight to the contribution of water on the crack-tip, highly water bearing glasses will be investigated by a new device for inert SCCG-measurements using double cantilever beam (DCB) geometry specimens. This device was designed to investigate the stress intensity factor in modus I and crack velocity in vacuum, but different atmospheres can also be introduced. For validation of the new device, first experiments were performed on microscope slides as well as on a soda-lime silicate and a borosilicate crown glass. The results achieved will be presented in comparison to the published results of Wiederhorn. T2 - 91. Glastechnische Tagung CY - Weimar, Germany DA - 29.05.2017 KW - Double cantilever beam KW - DCB KW - Crack intensity factor KW - Crack growth velocity KW - Glass PY - 2017 AN - OPUS4-40680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Welter, T. T1 - Glass structures with low helium and hydrogen permeability N2 - An efficient energy provision using fuel cells is linked to effecitve hydrogen storage capabilities. Because of its low intrinsic hydrogen permeability, glass has a huge potential in modern concepts of hydrogen storage. Previous studies on oxidic glasses showed an empirical connection between glass composition and gas permeation, which was mainly derived from the behavior of silica glass. In this study we focus on the relationship between topologic (free volume; network polymerization) and thermodynamic (configurational entropy) parameters. The comparison of three glasses within the meta (earth-) alkaline alumino silicate system to silica glass shows that an increase of the atomic packing factor (APF) does not necessarily decrease the permeability. Furthermore, the results suggest a connection between ΔCp at Tg and hydrogen permeability of the glass. All experiments were performed assuming that chemical hydrogen solubiltity in glass is negligible at temperatures well below the glass transition temperature. T2 - 91. Glastechnische Tagung CY - Weimar, Germany DA - 29.05.2017 KW - Hydrogen permeability KW - Glass composition KW - Atomic packing factor KW - Configurational entropy KW - Diffusion coefficient PY - 2017 AN - OPUS4-40488 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Marzok, Ulrich T1 - 3D High-temperature laser profilometry during sintering N2 - Most crucial for components of complex shape or heterogeneous micro structure, precise control of sintering has decisive influence on dimensional accuracy, mechanical integrity and reliability of sintered components. In these cases, only in situ 3D high-temperature shape screening during shrinkage would allow revealing temporary sinter warpage and hereby caused potential defects. Against this background, nokra Optische Prüftechnik und Automation GmbH, HTM Reetz GmbH and BAM developed a testing device for in situ 3D shape screening for ceramic and glass-ceramic tapes up to 1000°C by means of high-temperature laser profilometry. The local repeatability of the sample-sensor distance (sample height profile) is 10 µm at 1000°C. Current work is focused on dropping these restrictions in sample shape and temperature. In a second testing device, currently being in development, samples up to 5 cm x 5 cm x 5 cm can be measured at temperatures up to 1500°C.The presentation illustrates the current state of this work and possible applications of the method. T2 - 92. DKG Jahrestagung CY - Berlin, Germany DA - 19. 03. 2017 KW - Laser profilometry KW - 3D High-temperatue shape screening KW - Sintering PY - 2017 AN - OPUS4-40449 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Marzok, Ulrich T1 - Measurement of H2 permeability of glasses with VHE powder method N2 - The development of glassy hydrogen barriers requires the determination of low H2 permeabilities. Previous studies and numerical simulations have shown that the VHE powder method (vacuum hot extraction with mass spectrometric gas detection) is suitable for this purpose. The measured isothermal gas emission is fitted to a classical diffusion model for spherical particles from which the diffusion coefficient of the glass is calculated. The H2 permeability is determined by means of the solubility determined from the same measurement data. This presentation is referring to the optimization of the method regarding sample preparation and measurement data evaluation using suitable experimentally determined particle size distributions is reported. For quartz glass, it is shown that the accuracy of classical measuring methods is achieved with the VHE powder method. Furthermore, other examples of substantially gas-tighter glasses are given. T2 - 91. Glastechnische Tagung CY - Weimar, Germany DA - 29.05.2017 KW - Hydrogen permeation KW - Glass KW - Vacuum hot extraction KW - Powder method KW - Diffusion coefficient PY - 2017 AN - OPUS4-40441 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waurischk, Tina T1 - New device for inert sub-critical crack growth: measurements in crystallized glasses N2 - Compared to its intrinsic strength, the practical strength of glasses is substantially lowered by microscopic flaws. Their sub critical growth from the surface is strongly affected by ambient humidity. A new device was designed to enable the observation of sub critical crack growth (SCCG) in vacuum and controlled atmosphere. It allows measurements in transparent and semi-transparent materials in double cantilever beam (DCB) geometry. The aim of the present work is to study the effect of crystals on crack growth. T2 - 12th International Symposium on Crystallization in Glasses and Liquids CY - Segovia, Spain DA - 10.09.2017 KW - Double cantilever beam KW - DCB KW - Crack intensity factor KW - Crack growth velocity KW - Glass KW - Glass ceramic PY - 2017 AN - OPUS4-41995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Thoralf A1 - Rosemann, Paul T1 - Influence of the post-weld surface treatment on the corrosion resistance of duplex stainless steel 1.4062 N2 - The duplex stainless steel 1.4062 (X2CrNiN22-2) is used as alternative material to austenitic stainless steels in the construction industry. The corrosion resistance of welded seams is influenced by the base material, the weld filler material, the welding process and also by the final surface treatment. The scale layer next to the weld seam can be removed by grinding, pickling, electro-polishing or blasting depending on the requested corrosion resistance. Blasted surfaces are often used in the industrial practice due to the faster and cheaper manufacturing process compared to pickled or electro-polished surfaces. Furthermore blasting with corundum-grain is more effective than blasting with glass-beads which also lower the process costs. In recent years, stainless steel surfaces showed an unusually high susceptibility to pitting corrosion after grinding with corundum. For this reason, it is now also questioned critically whether the corrosion resistance is influenced by the applied blasting agent. This question was specifically investigated by comparing grinded, pickled, corundum-grain- and glass-bead-blasted welding seams. Results of the SEM analyses of the blasting agents and the blasted surfaces will be presented and correlated with the results of different corrosion tests (KorroPad-testing and pitting potentials). T2 - Eurocorr 2017 CY - Prague, Czech Republic DA - 03.09.2017 KW - Duplexstahl KW - Korrosion KW - Nichtrostender Stahl KW - Oberflächenbearbeitung KW - Schweißen KW - Strahlen PY - 2017 AN - OPUS4-41915 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotaka, M. T1 - Unique growth behavior of ferroelastic beta’-Gd2(MoO4)3 crystals in glasses N2 - An understanding on crystallization behavior and kinetics in glasses is one of the important topics in the glass science and technology. Tsukada et al.1) found an extremely unique and curious phenomenon in the crystallization of multiferroic (ferroelectric and ferroelastic properties) ’-Gd2(MoO4)3 crystals in Gd2O3-MoO3-B2O3 glasses. That is, crystals formed in the crystallization break into small pieces with a triangle prism or pyramidal shape having a length of 50-150 um spontaneously during the crystallization in the inside of an electric furnace, not during the cooling in air after the crystallization. They proposed to call this phenomenon “self-powdering phenomenon”. To the best of our knowledge, such a self-powdering phenomenon has not been observed in the crystallization of any other glasses. To investigate this phenomenon is very important for the glass science and for the preparation of bulk crystallized glasses with ferroelastic crystals. In this work, the preparation of crystallized glasses keeping the original shape is challenged, and the mechanism of self-powdering phenomenon is proposed. Glasses with the compositions of 21Gd2O3-63MoO3-(16-x)B2O3-xTeO2 (mol%) (x=0, 2, 4, 8) such as 21Gd2O3-63MoO3-16B2O3 (GM16B) and 21Gd2O3-63MoO3-8B2O3-8TeO2 (GM8T8B) were prepared using a conventional melt quenching technique. The quenched glasses were heat-treated at some temperatures, and the crystalline phase present in the crystallized samples was identified by X-ray diffraction (XRD) analyses, and the morphology and birefringence of crystals formed were observed using a polarized optical microscope (POM). The densities of GM16B and GM8T8B glasses are 4.76 g/cm3 and 4.91 g/cam3, respectively, and these values are higher than the density of ’-Gd2(MoO4)3 crystal, 4.555 g/cm3. These differences in the density might induce the large stresses in the inside of crystals during the crystal growth. The crystallized glasses of GM16B with ’-Gd2(MoO4)3 crystals do not keep the original glass shape, showing self-powdering phenomenon (breaking into small pieces). However, the crystallized glasses of GM8T8B keep the original glass shape without indicating any self-powdering. It is proposed that the stress at the interface between the glassy phase and ’-Gd2(MoO4)3 crystalline phase might be reduced in GM8T8B glasses containing TeO2 with weak Te-O bonds. T2 - Crystallization 2017 CY - Segovia, Spain DA - 10.09.2017 KW - Glass KW - Crystallization KW - Self-powdering PY - 2017 AN - OPUS4-44403 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -