TY - CONF A1 - Müller, Ralf A1 - Behrens, H. A1 - Deubener, J. T1 - Impact of structure and relaxation on fatigue and micromechanical properties of oxide glasses: the role of volatiles and bonding state N2 - As subcritical crack growth (SCCG) can reduce tensile strength of glasses by many orders of magnitude, the potential for improvement of fatigue behaviour is most intriguing in developing ultra-strong glasses. An essential bottleneck is the basic understanding of the numerous interplaying pressure-, temperature- and water-affected relaxation phenomena at the crack tip and related toughening strategies. Therefore, the present project aims to advance the basic understanding of structural relaxation effects and local properties caused by increased water concentration and tensile stresses at the crack tip as they are a key for structural toughening designs to develop SCCG-free glasses and glass surfaces. Our first studies give clear evidence that glass structure and dynamics is strongly modified upon hydration of glasses. These changes are highly related to the nature of network formers but are affected as well by the counter ions (network modifier). Results of the 1st project part suggest that structural relaxation below glass transition temperature, i.e. overlapping of short-range (beta) and long-range (alpha) interactions can contribute to SCCG in water-free environments and that structurally dissolved water in the glasses can have decisive impact on this effect. In the 2nd project stage specific glasses compositions will be investigated to gain an improved understanding on the relation of sub-Tg relaxation and inert SCCG as well as to shed light to the related effects of dissolved water and its speciation. These glasses cover a broader range of different glass topologies and binding partners, whereby the coupling of alpha and beta relaxations is varied systematically by alkali-, alkaline earth ions and water species concentrations. Preparation of hydrous glasses (up to 8 wt% water) will be performed by high pressure syntheses. Structure will be resolved by NMR, Raman and IR spectroscopy while structural relaxation is accessed in the temperature and frequency domain using dynamic mechanical spectroscopy and ultrasonic damping. We will focus on measurements of inert SCCG (region III) conducting experiments in vacuum and dry gas atmospheres using indentation techniques and stressing of glass specimens in DCB geometry. Experimental data on SCCG will be provided to SPP groups, which deals with fatigue in metallic glasses and vice versa we will test theoretical predictions of ab-initio simulations of partner within SPP 1594 in order to quantify the effect of water on the crack tip. In summa topological factors controlling the subcritical crack growth with respect to water will be identified from which structural toughening designs for highly fatigue resistant-glasses can be derived. N2 - Subkritisches Risswachstum (SCCG) kann die Zugfestigkeit von Glas um viele Größenordnungen erniedrigen. Deshalb birgt die Verbesserung des Ermüdungsverhaltens ein hohes Potential für das topologische Design hochfester Gläser. Ein diesbezüglicher Engpass ist das Verständnis der zahlreichen interagierenden druck-, temperatur- und wasserbeeinflussten Relaxationsphänomene an der Rissspitze und hieraus abgeleitete Verstärkungsstrategien. Ziel des Projekts ist es daher, das grundlegende Verständnis der Effekte, die infolge erhöhter Wasserkonzentrationen und Zugspannungen an der Rissspitze entstehen, zu vertiefen, da sie als ein Schlüssel für künftige strukturelle Designprinzipien zur Entwicklung schadenstoleranter Gläser und Glasoberflächen gelten. Unsere ersten Studien zeigen, dass die Struktur und Dynamik von Gläsern nach einer Hydration stark verändert sind. Diese Modifikationen sind mit der Art der Netzwerkbildner stark verknüpft, aber auch von ihren Gegenionen (Netzwerkwandler) abhängig. Die Ergebnisse des ersten Projektabschnitts legen nahe, dass strukturelle Relaxation unterhalb der Glasübergangstemperatur, d. h. ein Überlappen von kurz-reichweitigen (beta) und lang-reichweitigen (alpha) Wechselwirkungen, zum subkritisches Risswachstum in wasserfreien Umgebungen beitragen kann und, dass strukturell gelöstes Wasser in Gläsern sich entscheidend auf diese Effekt auswirken kann. Im zweiten Projektabschnitt werden daher spezielle Glaszusammensetzungen untersucht, die zu einem besseren Verständnis der Verbindung zwischen sub-Tg Relaxation und SCCG führen aber auch den Einfluss von gelöstem Wasser und dessen Speziation näher beleuchten. Diese Gläser weisen eine großen Breite an verschiedenen Topologien und Bindungspartnern auf, wobei die Kopplung von alpha und beta Relaxation durch Veränderungen in den Gehalten von Alkali-, Erdalkalionen und der Wasserspezies systematisch variiert wird. Die Präparation hydratisierter Gläser (bis zu 8 Ma.%) erfolgt mittels Hochdrucksynthesen. Die Glasstruktur wird durch NMR, Raman und IR Spektroskopie aufgeklärt während die Strukturrelaxation anhand dynamische mechanische Spektroskopie und Ultraschalldämpfung im Temperatur- und Frequenzraum erfasst wird. Im Fokus werden Messungen des inerten subkritischen Risswachstums (Region III) stehen, die Indenter-Experimente im Vakuum und trockenen Gasatmosphären sowie Verspannen von Glasproben in DCB Geometrie beinhalten. Experimentelle SCCG Daten werden Gruppen im Schwerpunktprogramm zur Verfügung stellen, die sich mit Ermüdung in metallischen Gläsern beschäftigen und im Gegenzug werden wir theoretische Vorhersagen aus ab initio Simulationen der Partner im SPP 1594 testen, um den Einfluss von Wasser auf die mechanischen Eigenschaften an der Rissspitze und deren Einfluss auf SCCG zu quantifizieren. In summa werden topologische Faktoren bezüglich Wasser, die SCCG kontrollieren, identifiziert, um daraus Designprinzipien für hoch ermüdungsresistente Gläser abzuleiten. T2 - Kolloquium des DFG-PP 1594 CY - Jena, Germany DA - 17.9.2015 KW - Glass KW - Fatigue PY - 2015 AN - OPUS4-38334 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Selleng, Christian T1 - Effect of 90°C thermal treatment on Ultra-High Performance Concrete N2 - Ultra High Performance Concrete (UHPC) is characterized by high strength and high durability. This is achieved by an optimized grain size distribution, especially within fine grains, and addition of superplasticizer, which allow the reduction of the water/cement ratio in the cement paste and thereby the increase of the density of UHPC. Thermal treatment, i.e. curing at elevated temperature and pressure, contributes to a further increase of compressive strength. The aim of the presented study was to analyze the effect of thermal treatment at 90 ◦C and atmospheric pressure on UHPC samples. Varying factors were the age of the samples when heat treatment started (initial storage time), the duration of heat treatment and the type of heat treatment. It was applied in three ways: 1. treated without any protection, 2. sealed in plastic foil and 3. treated in hot water. Afterwards the samples were analyzed with respect to their mechanical properties and their phase composition. Furthermore, the weight (water absorption) of the samples was observed over 28 days and was correlated with the strength test results. The development of strength depends on the combination of initial storage time and the duration of heat treatment and is also influenced by the type of thermal treatment. The highest compressive strengths have been observed by implementing the hot water treatment. Thereby the weight of the samples increase due to additional absorbed water. This enables an increased hydration of cement clinker inducing a higher strength. T2 - GeoBerlin 2015: Dynamic Earth - from Alfred Wegener to today and beyond CY - Berlin, FU Berlin DA - 04.10.2015 PY - 2015 AN - OPUS4-34504 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blaeß, Carsten T1 - Sintering and crystallization of new bioactive glasses N2 - Bioglass® 45S5 is mainly used clinically as powders, granules or pastes instead of sintered compacts. This is due to the inherent problem of crystallization during the sintering, which results in poor mechanical properties and reduced bioactivity. Recently, new bioactive glasses with improved crystallization stability have been developed as promising candidates for manufacturing of sintered powder compacts for bone regeneration, which combine improved sintering behavior with bioactivity. Compared with the well-known Bioglass® 45S5 (SiO2-P2O5-CaO-Na2O) the calcium/alkali oxide ratio was increased, sodium oxide was partially replaced by potassium oxide and up to 3 mol% calcium fluoride were added, in order to stabilize the glass against crystallization. The aim of this study was to investigate the sintering and crystallization behavior of these new bioactive glasses. Sintering and crystallization were characterized by heating microscopy, XRD, FTIR, SEM, and DTA. The results show that a sintered density of 88-99 % is achieved in contrast to only 57-67% for Bioglass® 45S5. In addition, FTIR and XRD analyses show that Bioglass® 45S5 crystallized during sintering while for the new glasses no crystalline phases are detected. The thermal properties of all glasses were studied by DTA measurements, and the influence of grain size was characterized. These studies showed that full densification can be attained for particle size < 32 µm, whereas coarser particles progressively increase residual porosity. Observed foaming phenomena, are strongly retarded by crystallization of beta-HAp. T2 - ICG 2016 CY - Shanghai, China DA - 07.04.2016 KW - Bioactive KW - Glass KW - Crystallization KW - Sintering PY - 2015 AN - OPUS4-38304 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blaeß, Carsten T1 - New bioactive glasses with improved sintering behavior N2 - Nowadays, the use of bioactive glasses is established for bone regeneration; however glasses are used mostly as powders, granules or in a paste. Sintered scaffolds are not used clinically, because of the in inherent problem of crystallization during the sintering process, resulting in poor mechanical properties and reduced bioactivity. The aim of this study was therefore to design new bioactive glasses, which combine improved processing and sintering with bioactivity. Compared with the well-known Bioglass® 45S5 (SiO2-P2O5-CaO-Na2O) the calcium/alkalioxide ratio was increased, sodiumoxide was partially replaced by potassiumoxide and up to 8 mol% calciumflorid were added, in order to stabilize the glass against crystallization. The sintering behavior of the new glasses was characterized by heating microscopy and compared to Bioglass® 45S5. The results showed that the new glasses achieved a sintered density of 88-99 % in contrast to only 57-67% for Bioglass® 45S5. In addition FTIR and XRD analyses showed that Bioglass® 45S5 crystallized during sintering while for the new glasses no crystalline phases were detected. The thermal properties of all glasses were studied by DTA and DSC measures, and the influence of grain size and heating rate were characterized. These studies showed a shift of start and end temperature of sintering process as well as the final density. The structure of sintered specimens during and after sintering was examined using light and electron microscopy (REM). T2 - Crystallization 2015 CY - Nagaoka, Japan DA - 11.10.2015 KW - Bioactive KW - Glass KW - Crystallization KW - Sintering PY - 2015 AN - OPUS4-38308 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo T1 - Nano-sized precipitates in an Fe-13Cr alloy formed under oxidizing water vapor atmosphere N2 - Oxidation of a Fe-13Cr alloy under water vapor at 600 °C produced a zone of nano-sized precipitation underneath the outside scale formed by iron oxides and Fe‒Cr spinel. The majority of the spinel layer shows a mixed orientation relationship to the ferritic matrix {100}α || {100}sp & <011>α || <001>sp. However, also the discovered precipitated particles are characterized by the same crystallographic orientation relationship to the respective ferritic parent grain. The habit of the precipitates is best described by a lath morphology with their main axis parallel to <100> of ferrite. Energy dispersive X-ray spectroscopy (EDX) and electron backscatter diffraction (EBSD) in an scanning electron microscope (SEM) have been applied to characterize the oxide layer in the micrometer scale. The clearly smaller precipitates were subsequently investigated by transmission electron microscopy (TEM). Specimens have been prepared by focused ion-beam (FIB) milling at an area previously characterized by EBSD. They cover the ferritic base material, but mainly the precipitation zone and the Fe‒Cr spinel layer. Energy filtered selected area diffraction (SAD) in the conventional (C)TEM and high-angle annular darkfield (HAADF) imaging in the scanning (S)TEM mode were employed in the characterization of the specimens. T2 - International Conference on Solid-Solid Phase Transformations in Inorganic Materials (PTM) 2015 CY - Whistler, British Columbia, Canada DA - 28.06.2015 KW - Precipitation KW - Oxidation KW - Microscopy KW - Topotactic transformation KW - Spinel PY - 2015 AN - OPUS4-42169 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rübner, Katrin T1 - Studies on the Pore Structure of Lightweight Recycling Granules N2 - Lightweight granules are mineral, spherical and porous particles with bulk density less than 2000 kg m . New types of lightweight granules are made from masonry -3 rubble as an alternative to the commonly used expanded clay and shale. They are produced in a multistage manufacturing process by thermal or hydrothermal treatment. Studies of the microstructure of the new lightweight granules are very important to optimise the engineering properties with regard to different applications from lightweight concrete to planting substrates and wastewater treatment. Here, the results of porosity and pore structure measurements are presented. Characteristic samples with different bulk densities of both thermally and hydrothermally hardened granules have been analysed by means of various methods. T2 - 27. Deutsche Zeolith-Tagung CY - Oldenburg, Germany DA - 25.02.2015 PY - 2015 AN - OPUS4-32835 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Laquai, René A1 - Schaupp, Thomas A1 - Müller, Bernd R. A1 - Griesche, Axel A1 - Bruno, Giovanni A1 - Kannengießer, Thomas T1 - 3D imaging of hydrogen assisted cracking using analyser-based imaging N2 - To better understand the mechanism of hydrogen assisted cracking (HAC), it is important to investigate the 3D structure of the cracks non-destructively. Since, cracks introduced by HAC are usually very small, conventional x-ray imaging methods often lack the required spatial resolution. However, the detection of those cracks can be enhanced by taking advantage of refraction at interfaces within the sample. To image this refractive deflection we employ analyser based imaging (ABI). In this work we aim at proving the enhanced crack detection of ABI by investigating an alluminum alloy weld. T2 - BESSY User Meeting 2015 CY - Berlin, Germany DA - 09.12.2015 KW - X-ray refraction KW - Synchrotron KW - Analyser-based imaging KW - Hydrogen assisted cracking KW - Welding PY - 2015 AN - OPUS4-38278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shashev, Yuri T1 - Optimizing the performance of phase gratings for better visibility in Talbot- Lau interferometry 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. T2 - PhD Day 2015 CY - Berlin, Germany DA - 14.7.2015 KW - Talbot-Lau interferometry PY - 2015 AN - OPUS4-38325 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stroh, Julia T1 - High resolution in situ monitoring of the initial cement hydration influenced by organic admixtures N2 - Numerous admixtures are used in the building practice to customize the properties of the cement paste during application. The influences of admixtures on the course of cement hydration and formation of hydrate phases have to be considered. Polycarboxylate ether (PCE) based polymeric superplasticizers (SPs) are known to retard the setting of the cement paste. The extent of the retardation differs depending on the molecular structure of the SP. Additionally, the presence of a stabilizing agent (SA) in the cement paste has a retarding side effect on the setting. The initial cement hydration processes and the detailed mechanisms of the retardation influenced by PCEs, as well as their interactions with particular SAs, are insufficiently understood. Up to now, only the results of phenomenological studies were taken into account to describe this retardation process. A detailed structure analysis monitoring the change of the phase composition during the hydration was never applied. Both SP and SA affect the adsorption of the sulphate ions on the clinker particles, causing changes in the formation of ettringite during the initial hydration, and are therefore a crucial part of the setting process itself. Here, the initial hydration of cement influenced by the interaction of SP and SA was monitored in situ by synchrotron X-ray diffraction. The high time resolution of the measurements allowed a continuous detection of the hydrates formed. The hydration was followed from the starting point of water addition and for couple of hours afterwards. The hydration of the levitated cement pellets containing starch as SA was initialized by adding aqueous solutions of different commercial SPs. Changes in the ettringite formation were detected in comparison to the reference hydration of pure cement. T2 - Early Age Concrete: From the Research Lab to the Construction Site CY - Tomsk, Russia DA - 02.06.2015 KW - Portland cement KW - Initial hydration KW - Superplasticizer KW - Stabilizer KW - Synchrotron XRD PY - 2015 AN - OPUS4-35470 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oesch, Tyler T1 - In-situ CT investigation of pull-out failure for reinforcing bars embedded in conventional and high-performance concretes N2 - The use of high-performance concretes holds great promise for many structural applications. This paper investigates the performance of these materials when used in combination with traditional reinforcing bars. An improved understanding of failure during reinforcing bar pull-out from high-performance concretes is needed in order to better predict the embedment length required to develop full reinforcing bar pull-out strength and the required thickness of reinforcing bar cover for adequate corrosion protection. The cracking structures surrounding the reinforcing bars were analyzed using x-ray computed tomography (CT) in order to determine the stress states causing failure. This was accomplished by conducting in-situ reinforcing bar pull-out experiments during CT scanning. A conventional concrete, a high-strength concrete, and a high-strength fiber reinforced concrete were all tested during the experiments. The results of these experiments showed that the levels of brittleness of the different concrete materials had a major impact on the failure mechanisms that they experienced during reinforcing bar pull-out. It was also clear that the specimen geometry and the casting method had a major impact on fiber orientation. The inclusion of fibers within concrete was also found to significantly improve strength and corrosion protection during reinforcing bar pull-out. T2 - 6th Conference on Industrial Computed Tomography CY - Wels, Austria DA - 09.02.2016 KW - Fiber KW - Reinforcing Bar KW - Computed Tomography KW - In-Situ KW - High-Performance Concrete PY - 2016 AN - OPUS4-35521 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -