TY - CONF A1 - Reinsch, Stefan A1 - Müller, Ralf T1 - Surface-induced Crystallization of Glass 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. In this talk the state of the art on mechanisms of surface nucleation are summarized. On one hand, mechanical damaged surfaces show high nucleation activity, at which the nucleation occurs at convex tips and edges preferentially. On the other hand, solid foreign particles are dominant nucleation sites at low damaged surfaces. They enable nucleation at temperatures even far above Tg. The nucleation activity of the particles is substantially controlled by their thermal and chemical durability. But no systematic studies on initially oriented crystal growth or nucleation from defined active nucleation sites have been pursued, so far. Therefore, the main objective of a just started project is to advance the 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. As a first attempt we focused on possible reorientation of separately growing surface crystals during early crystal growth. First results show clear evidence that separately growing crystals can reorient themselves as they are going to impinge each other. T2 - Glasforum der Deutschen Glastechnischen Gesellschaft (DGG) CY - Würzburg, Germany DA - 11.06.2018 KW - Crystallization KW - Silicate Glasses KW - Surface Nucleation PY - 2018 AN - OPUS4-45593 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Bestimmung der Partikelgrößenverteilung mittels Zentrifugen-Sedimentationsverfahren nach ISO 13318-2 (Küvette) N2 - Im Vortrag werden das Messprinzip des Zentrifugen-Sedimentationsverfahrens erläutert und die Anforderungen der zugrundeliegenden Normen diskutiert. Es schließen sich umfangreiche Ausführungen zur praktischen Durchführung der Messung, insbesondere auch zu den vorbereitenden Arbeiten, sowie zur Auswertung der Rohdaten an. Nach einem Vergleich der Ergebnisse mit anderen Messverfahren, wird das Verfahren in einer Zusammenfassung bewertet. T2 - Rheologie und Stabilität von dispersen Systemen CY - Potsdam, Germany DA - 14.04.2018 KW - Partikelgrößenverteilung KW - Analytische Zentrifuge PY - 2018 AN - OPUS4-45098 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas A1 - Trappe, Volker A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Evolution of CFRP stress cracks observed by in situ X-ray refractive imaging N2 - Modern air-liners and rotor blades of wind turbines are basically made of fiber reinforced plastics (FRP). Their failure heavily impairs the serviceability and the operational safety. Consequently, knowledge of the failure behavior under static and cyclic loads is of great interest to estimate the operational strength and to compare the performance of different materials. Ideally, the damage evolution under operational load is determined with in-situ non-destructive testing techniques. Here, we report on in-situ synchrotron X-ray imaging of tensile stress induced cracks in carbon fiber reinforced plastics (CFRP) due to inter fiber failure. An in-house designed compact-tensile testing machine with a load range up to 15 kN was integrated into the beam path. Since conventional radiographs do not reveal sufficient contrast to distinct cracks due to inter fiber failure and micro cracking from fiber bundles, the Diffraction Enhanced Imaging technique (DEI) is applied in order to separate primary and scattered (refracted) radiation by means of an analyzer crystal. In the laboratory, scanning X-ray refraction topography of CFRP has been applied long before but it comes along with several disadvantages: the long total measuring time hampers real time (in-situ) measurements and the required small beam size hinders end-to-end imaging. The introduced technique overcomes both drawbacks. Imaging and tensile test rig are run unsynchronized at the greatest possible frame rate (0.7 s-1 at 28.8 µm pixel size) and smallest possible strain rate (5.5∙10-4 s-1). For 0°/90° non-crimped fabrics (ncf) the first inter fiber cracks occurred at 380 MPa (strain 0.7 %). Prior to failure at about 760 MPa (strain 2.0 %) we observe the evolution of a nearly equidistant 1 mm grid of cracks running across the entire sample in the fully damaged state before total failure. T2 - 41st Risø International Symposium on Materials Science - Materials and Design for Next Generation Wind Turbine Blades CY - Online meeting DA - 07.09.2020 KW - X-ray refraction KW - Diffraction Enhanced Imaging KW - Carbon Fiber Reinforced Plastics KW - In situ tensile test KW - Crack evolution PY - 2020 AN - OPUS4-51223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Busch, Richard A1 - Müller, Ralf A1 - Patzig, Christian A1 - Höche, Thomas A1 - Reinsch, Stefan A1 - Tielemann, Christopher T1 - Surface Initiated Structure Formation in Glass Ceramics N2 - A summery of previous research regarding surface crystallization is given as well as results regarding thecurrent DFG project are presented. T2 - XRM Workshop CY - Halle, Germany DA - 03.03.2020 KW - Glass KW - Surface KW - XRM PY - 2020 AN - OPUS4-51337 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra A1 - Lindemann, Franziska A1 - Hodoroaba, Vasile-Dan T1 - Nano Powder - a Challenge for Granulometry N2 - If the particle size decreases, the ratio of surface area to volume increases considerably. This provides benefits for all surface-driven processes that run faster or at lower temperatures than larger particles. However, handling and characterization of the nanopowders are much more difficult. Particularly polydisperse powders with irregular shape, as grinding products, represent a challenge. Granulometry in the submicron and nanoscale often leads to incorrect results without knowledge of particle morphology. This presentation demonstrates potentials of using the volume-specific surface area (SV or VSSA) in the granulometric characterization of nanopowders, for instance, correlations between the volume-specific surface area and the median particle size are discussed considering the particle morphology and the model of the logarithmic normal distribution. Moreover, the presentation deals with the optimal dispersion of nanopowders during sample preparation. Indirect ultrasound device with defined cooling was developed to prevent both contamination by sonotrode abrasion and sample changes by heat. Successful granulometric characterization of nanopowders demands both improved dispersion technology and very often an effective combination of two or more measurement methods. T2 - Jahrestagung der Deutschen Keramischen Gesellschaft CY - Leoben, Austria DA - 06.05.2019 KW - Nano screening KW - VSSA KW - Nano particle KW - Particle size PY - 2019 AN - OPUS4-47976 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Bestimmung der Partikelgrößenverteilung mittels Zentrifugen-Sedimentationsverfahren nach ISO 13318-2 (Küvette) N2 - Im Vortrag werden das Messprinzip des Zentrifugen-Sedimentationsverfahrens erläutert und die Anforderungen der zugrundeliegenden Normen diskutiert. Es schließen sich umfangreiche Ausführungen zur praktischen Durchführung der Messung, insbesondere auch zu den vorbereitenden Arbeiten, sowie zur Auswertung der Rohdaten an. Nach einem Vergleich der Ergebnisse mit anderen Messverfahren, wird das Verfahren in einer Zusammenfassung bewertet. T2 - Rheologie und Stabilität von dispersen Systemen CY - Potsdam, Germany DA - 03.06.2019 KW - Nanomaterial KW - Partikelgrößenverteilung KW - Analytische Zentrifuge PY - 2019 AN - OPUS4-48286 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Agea-Blanco, Boris A1 - Blaeß, Carsten A1 - Waurischk, Tina T1 - Sintering and foaming of silicate glass powders N2 - Glass powders are promising candidates for manufacturing a broad diversity of sintered materials like sintered glass-ceramics, glass matrix composites, glass bonded ceramics or pastes. Powder processing, however, can substantially affect sinterability, e.g. by promoting surface crystallization. On the other hand, densification can be hindered by gas bubble formation for slow crystallizing glass powders. Against this background, we studied sintering and foaming of silicate glass powders with different crystallization tendency for wet milling and dry milling in air, Ar, N2, and CO2 by means of heating microscopy, DTA, Vacuum Hot Extraction (VHE), SEM, IR spectroscopy, XPS, and ToF-SIMS. In any case, foaming activity increased significantly with progressive milling. For moderately milled glass powders, subsequent storage in air could also promote foaming. Contrarily, foaming could be substantially reduced by milling in water and 10 wt% HCl. Although all powder compacts were uniaxially pressed and sintered in air, foaming was significantly affected by different milling atmosphere and was found most pronounced for milling in CO2 atmosphere. Conformingly, VHE studies revealed that foaming is mainly driven by carbonaceous species, even for powders milled in other gases. Current results of this study thus indicate that foaming is caused by carbonaceous species trapped on the glass powder surface. T2 - IMAPS/ACerS 15th International Conference and Exhibition on Ceramic Interconnect and Ceramic Microsystems Technologies (CICMT 2019) CY - Shanghai, China DA - 16.04.2019 KW - Glass powder KW - Sintering KW - Foaming PY - 2019 AN - OPUS4-48196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reinsch, Stefan A1 - Tielemann, Christopher A1 - Busch, R. A1 - Patzig, C. A1 - Müller, Ralf A1 - Höche, T. T1 - Oriented surface crystallization in 18BaO·22CaO·60SiO2 and MgO·CaO·2SiO2 glasses N2 - Up to now, oriented surface crystallization phenomena are discussed controversially, and related studies are restricted to few glasses. The vast majority of previous work does not consider possible effects of surface preparation and surrounding atmosphere. Moreover, very few observations of surface crystal orientation were made on separately grown crystals. The aim of our project is to advance the basic understanding of oriented surface crystallization, e.g. whether preferred orientation of surface crystals results from oriented nucleation or reorientation mechanisms during early crystal growth. In both cases, crystal orientation may reflect the orientation of the glass surface or that of anisotropic active surface nucleation sites. Therefore, we focus on orientation of surface crystals separately growing under controlled conditions. First results on diopside (MgCaSi2O6) and walstromite (BaCa2Si3O9) crystals growing from 18BaO·22CaO·60SiO2 and MgO·CaO·2SiO2 glass surfaces, respectively, indicate that different orientation mechanisms may occur. Neighbored walstromite crystals were found to gradually reorient themselves when they are going to impinge each other during stepwise isothermal treatments (log η = 4,5 Pa*s) of polished glass samples. Nevertheless, no preferred crystal orientation was evident for separate crystals. For diopside crystals growing from polished glass surfaces (1 μm diamond lapping foil), strong preferred orientation was observed for 3.5 to 85 min annealing at 850 °C. Electron Backscatter Diffraction (EBSD) studies showed that the c-axis of surface crystals is oriented parallel to the glass surface and that separated diopside crystals as small as 600 nm are already oriented. Studies on glass surfaces, polished with diamond lapping foils starting from 16 μm down to 1 μm grain, revealed that crystal orientation may scatter arround this preferential orientation and that this scatter progressively decreases with decreasing polishing grain size. T2 - 93rd Annual Meeting of the German Society of Glass Technology (DGG) in conjunction with the French Union for Science and Glass Technology (USTV) Annual Meeting CY - Nuremberg, Germany DA - 13.05.2019 KW - Surface crystallization KW - Orientation KW - Glass KW - Diopside PY - 2019 AN - OPUS4-48198 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schilling, Markus A1 - Niebergall, Ute A1 - Böhning, Martin T1 - Addressing ESC using FNCT enhanced by optical fracture surface analysis N2 - During their lifetime, polymer components subjected to mechanical loads and environmental influences show a loss of their mechanical properties required for their specific applications. In this respect, the craze-crack damage mechanism slow crack growth (SCG) is relevant for PE-HD components used in high-performance applications such as pipes and containers for the storage and transport of dangerous goods. SCG is considered to be the major failure mechanism in polyolefins and it typically occurs suddenly and unexpectedly. Due to the fields of application, SCG is a safety relevant issue. To test for the resistance of PE-HD pipe and container materials against SCG, the full-notch creep test (FNCT) is widely applied in Europe. In this study, SCG phenomena in PE-HD are investigated in detail based on an improved FNCT, especially including the consideration of the influence of environmental liquids effecting the damage mechanism. Using an enhanced fracture surface and a crack propagation analysis with imaging techniques such as light microscopy (LM), laser scanning microscopy (LSM), X-ray computed tomography (CT-scan) and scanning electron microscopy (SEM), detailed data concerning SCG are obtained. The combined application of FNCT and such imaging techniques is explicitly advantageous and recommended to gain important information on damage occurring to PE-HD induced by mechanical stress and the influence of environmental liquids, which is essential within the Fourth Industry Revolution. T2 - PPS Europe-Africa 2019 Regional Conference (PPS 2019) CY - Pretoria, South Africa DA - 18.11.2019 KW - Polyethylene, PE-HD KW - Full-Notch Creep Test (FNCT) KW - Fracture surface analysis KW - Slow crack growth KW - Environmental stress cracking KW - Laser Scanning Microscopy (LSM) KW - Scanning Electron Microscopy (SEM) PY - 2019 AN - OPUS4-50939 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ghafafian, Carineh A1 - Popiela, Bartosz A1 - Trappe, Volker T1 - Damage Mechanisms of Scarf Joint Repairs for Wind Turbine Rotor Blade Shell Applications N2 - Wind turbine rotor blades, made of fiber reinforced polymers (FRP), often fail before their projected 20-year lifespan, largely due to defects that originate during manufacturing and are propagated by operational fatigue and environmental conditions. The cost-intensive replacement outcomes lead to a high loss of earnings, and are one of the inhibitors of wind turbine production [1]. A potential repair alternative is to locally patch these areas of the blades with adhesively bonded structural repairs. However, the effects of such repair methods of the outer shell region on the structural integrity of the rotor blades are still largely unknown, and are thus investigated in this project. The shell components of rotor blades are made of FRP composite material sandwiching a lightweight core, often a rigid foam or Balsa wood. The repair methods involve replacing the lost load path with a new material that is joined to the parent structure [2]. Repairs in this project focus on the scarf method, which allow for a smoother load distribution across the joint, aiming to study the damage mechanism of glass FRP scarf repairs for wind turbine blade shell applications. Namely, the source and path of the damage initiation and propagation, role of the interface between parent and patch material, and the role of the fiber orientation mismatch at this interface are examined. Biaxial ±45° and 0/90° FRP specimens are produced with the vacuum-assisted resin infusion (VARI) process using E-glass non-crimp fabric. The patch layers are then joined using VARI with a scarf ratio of 1:50, using glass FRP fabric with half the areal weight of the parent side to allow for better drapability. The methods and practices in specimen production are based on common industry practice in rotor blade shell manufacturing and repairs. The specimens are tested under uniaxial tensile load, during which they are periodically monitored for damage onset. A comparison of the ±45° and 0/90° specimens allows for an understanding of the role of a highly mismatching fiber orientation in the transition zone between parent and patch material on the failure mechanism of the scarf joint. Although failure in both orientations begins as delamination at the joint edge, the difference in the mechanisms at play in the two different specimen types leads ultimately to different fracture paths. Namely, in the inter fiber failure mechanism of the ±45° specimens, the higher interlaminar strength compared to the intralaminar strength of the laminate leads to intralaminar failure of the ±45° scarf joint specimens. Alternatively, the competition in the 0/90° specimens lies between the interlaminar strength and fiber failure strength, and here we experience failure primarily across the scarf joint length. The scarf joint in the 0/90° specimens disrupts the continuity of the load-carrying 0° layers, directing the failure path to remain primarily along the scarf joint. Experimental results are compared to finite element analyses of scarf patch repairs on glass FRP sandwich specimens with the same respective layup orientations, where the damage initiation regions are identified and correlated to fiber orientation, serving as a bridge to future work which will experimentally examine the scarf repair patches on sandwich shell specimens. T2 - Joint Event: ICCS23 - 23rd International Conference on Composite Structures & MECHCOMP6 - 6th International Conference on Mechanics of Composites CY - Online meeting DA - 01.09.2020 KW - Wind turbine blade shells KW - Glass fiber reinforced polymers KW - Scarf repairs PY - 2020 AN - OPUS4-51175 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -