TY - JOUR A1 - Prewitz, M. A1 - Gaber, M. A1 - Müller, Ralf A1 - Marotzke, C. A1 - Holtappels, Kai T1 - Polymer coated glass capillaries and structures for high-pressure hydrogen storage: Permeability and hydrogen tightness JF - International journal of hydrogen energy N2 - The hydrogen tightness of high-pressure hydrogen storage is a Basic criterion for long-term storage. The H2 permeation coefficients of epoxy resin and a glass lacquer were determined to enable the geometric optimization of a glass capillary storage. It was found that the curing conditions have no significant influence on the H2 permeation coefficient of resin. The H2 permeation coefficient of epoxy resin is only about three orders of Magnitude greater than that of borosilicate glass. This suggests that the initial pressure of 700 bar takes about 2.5 years to be halved in capillary array storage. Therefore, a high-pressure hydrogen storage tank based on glass capillaries is ideally suited for long-term storage in mobile applications. KW - Permeability KW - Glass capillaries KW - Coating KW - Hydrogen storage KW - Long-term calculation KW - Epoxy resin PY - 2018 DO - https://doi.org/10.1016/j.ijhydene.2017.12.092 SN - 0360-3199 VL - 43 IS - 11 SP - 5637 EP - 5644 PB - Elsevier AN - OPUS4-44327 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Blaeß, Carsten A1 - Müller, Ralf T1 - Master curve for viscous crack healing JF - Materials Letters N2 - A novel method to generalize kinetic data of viscous crack healing in glasses is proposed. The method assumes that crack healing progress is proportional to the healing time, t, and indirect proportional to viscosity, n. This way, crack length and crack width data, normalized to the initial crack length and plotted versus t/n, allow to compare crack healing progress for different cracks and healing temperatures in a master curve. Crack healing experiments conducted in this study demonstrate the applicability of this method for a commercial microscope slide glass. KW - Crack healing KW - Glass KW - Master curve KW - Vickers indentation PY - 2018 DO - https://doi.org/10.1016/j.matlet.2017.12.082 SN - 0167-577X SN - 1873-4979 VL - 216 SP - 110 EP - 112 PB - Elsevier AN - OPUS4-44300 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scheuerlein, C. A1 - Finn, Monika A1 - Meyer, Christian A1 - Lackner, F. A1 - Savary, F. A1 - Rehmer, Birgit T1 - Thermomechanical Behavior of the HL-LHC 11 Tesla Nb3Sn Magnet Coil Constituents During Reaction Heat Treatment JF - IEEE Transactions on applied superconductivity N2 - The knowledge of the temperature-induced changes of the superconductor volume and of the thermomechanical behavior of the different coil and tooling materials is required for predicting the coil geometry and the stress distribution in the coil after the Nb3Sn reaction heat treatment. In this paper, we have measured the Young’s and shear moduli of the HL-LHC 11 T Nb3Sn dipole magnet coil and reaction tool constituents during in situ heat cycles with the dynamic resonance method. The thermal expansion behaviors of the coil components and of a free standing Nb3Sn wire were compared based on dilation experiments. KW - Superconducting magnet KW - Young`s modulus KW - Thermal expansion KW - Stress-strain-behavior PY - 2018 DO - https://doi.org/10.1109/TASC.2018.2792485 SN - 1051-8223 SN - 1558-2515 VL - 28 IS - 3 SP - 4003806 - 1 EP - 4003806 - 6 PB - IEEE Council on Superconductivity CY - New York AN - OPUS4-44020 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wisniewski, W. A1 - Thieme, C. A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Groß-Barsnick, S.-M. A1 - Rüssel, C. T1 - Oriented surface nucleation and crystal growth in a 18BaO·22CaO·60SiO2 mol% glass used for SOFC seals JF - CrystEngComm N2 - A glass of the composition 37BaO·16CaO·47SiO2 wt% produced on an industrial scale is crystallized at 970 °C for times ranging from 15 min to 2 h. The crystallization at the immediate surface as well as the crystal growth into the bulk are analyzed using scanning electron microscopy (SEM) including energy dispersive X-ray spectroscopy (EDXS) and electron backscatter diffraction (EBSD) as well as X-ray diffraction in the Θ–2Θ setup (XRD). The immediate surface shows the oriented nucleation of walstromite as well as the formation of wollastonite and an unknown phase of the composition BaCaSi3O8. All three phases also grow into the bulk where walstromite ultimately dominates the kinetic selection and grows throughout the bulk due to a lack of bulk nucleation. Walstromite shows systematic orientation changes as well as twinning during growth. A critical analysis of the XRD-patterns acquired from various crystallized samples indicates that their evaluation is problematic and that phases detected by XRD in this system should be verified by another method such as EDXS. KW - Glass KW - Surface nucleation KW - Orientation KW - EBSD PY - 2018 DO - https://doi.org/10.1039/c7ce02008b VL - 20 IS - 6 SP - 787 EP - 795 PB - Royal Society of Chemistry AN - OPUS4-44405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Agea Blanco, Boris A1 - Meyer, Christian A1 - Müller, Ralf A1 - Günster, Jens T1 - Sand erosion of solar glass: Specific energy uptake, total transmittance, and module efficiency JF - International Journal of Energy Research N2 - Surface roughness, R Z , normal transmittance, Τ N , total transmittance, Τ T , and photovoltaic (PV) module efficiency, η S , were measured for commercial solar glass plates and PV test modules identically sandblasted with different loads of quartz sand (200 – 400 μ m), impact inclination angles, and sand particle speed. Measured data are presented versus the specific energy uptake during sand blasting, E (J/m2). Cracks, adhering particles, and scratch ‐ like textures probably caused by plastic flow phenomena could be observed after sand blasting. Their characteristic size was much smaller than that of sand particles. After blasting and subsequent cleaning, the glass surface was still covered with adhering glass particles. These particles, cracks, and scratch ‐ like textures could not be removed by cleaning. For sand blasting with α = 30° inclination angle and E = 30 000 J/m2, normal transmittance, total transmittance, and relative module efficiency decreased by 29%, 2% and ∽ 2%, respectively. This finding indicates that diffusive transmission of light substantially contributes to PV module efficiency and that the module efficiency decrease caused by sand erosion can be better estimated from total than by normal transmittance measurements. KW - Transmittance KW - Efficiency KW - Photovoltaic modules KW - Roughness KW - Sand blasting PY - 2018 DO - https://doi.org/10.1002/er.3930 SN - 1099-114X SN - 0363-907X VL - 42 IS - 3 SP - 1298 EP - 1307 PB - Wiley & Sons, Ltd. AN - OPUS4-44157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 - Blaeß, Carsten A1 - Müller, Ralf A1 - Feldmann, Ines A1 - Brauer, D.S. T1 - Sintering ability of fluoride-containing bioactive glass powder N2 - Sintered bioactive glass scaffolds of defined shape and porosity, e.g. made via additive manufacturing, must provide sufficient bioactivity and sinterability. As higher bioactivity is often linked to high corrosion and crystallization tendency, a certain compromise between sintering ability and bioactivity is therefore required. Groh et al. developed a fluoride-containing bioactive glass (F3), which allows fiber drawing and shows a bioactivity well comparable to that of Bioglass®45S5. To study whether and to what extent the sinterability of F3 glass powder is controlled by particle size, coarse and fine F3 glass powders (300-310µm and 0-32µm) were prepared by crushing, sieving and milling. Sintering, degassing and phase transformation during heating were studied with heating microscopy, vacuum hot extraction (VHE), DTA, XRD, and SEM. For the coarse glass powder, sintering proceeds slowly and is limited by surface crystallization of primary Na2CaSi2O6 crystals. Although the crystallization onset of Na2CaSi2O6 is shifted to lower temperature, full densification is attained for the fine powder. This finding indicate that certain porosity might be tuned via particle size variation. Above 900°C, intensive foaming is evident for the fine powder. VHE studies revealed that carbon species are the main foaming source. T2 - 92. Glastechnische Tagung CY - Bayreuth, Germany DA - 28.05.2018 KW - Sintering KW - Bioactive glass KW - Crystallization PY - 2018 AN - OPUS4-45568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Behrens, H. A1 - Bauer, U. A1 - Reinsch, Stefan A1 - Kiefer, P. A1 - Müller, Ralf A1 - Deubener, J. T1 - Structural relaxation mechanisms in hydrous sodium borosilicate glasses JF - Journal of Non-Crystalline Solids N2 - Borosilicate glasses (16Na2O–10B2O3–74SiO2, NBS) with water contents up to 22 mol% H2O were prepared to study the effect of water on structural relaxation using DTA, viscometry and internal friction measurements. The results show that the glass transition temperature Tg of DTA and the isokom temperature T12, of viscometry are in excellent agreement, confirming the equivalence of enthalpy and viscous relaxation for NBS glass. Combining Tg data with water speciation data demonstrates that OH groups are mainly responsible for the decrease of Tg with increasing hydration, while molecular water plays only a minor role. Internal friction spectra at 7.125 Hz confirm the decisive influence of water on mechanical relaxation. The temperature range of α-relaxation (glass transition) strongly decreases while two β-relaxation peaks (sub-Tg) progressively appear with increasing water content. A high temperature β-relaxation peak, attributed to the presence of OH groups, shifts from 670 to 450 K as total water content increases from 0.01 to 5 wt%. A low temperature β-relaxation peak, attributed to molecular water, appears at 380 K and 330 K in glasses containing 3 and 5 wt% H2O, respectively. These findings suggest that relaxation mechanism of different hydrous species at low temperature may contribute to fatigue of stressed glasses. KW - Borosilicate glass KW - Water KW - Relaxation KW - Internal friction KW - Glass transition PY - 2018 DO - https://doi.org/10.1016/j.jnoncrysol.2018.05.025 VL - 497 SP - 30 EP - 39 PB - Elsevier B.V. AN - OPUS4-45608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waurischk, Tina A1 - Müller, Ralf A1 - Behrens, H. A1 - Deubener, J. A1 - Balzer, R. A1 - Kiefer, P. T1 - The influence of water as volatile on crack propagation in soda-lime silicate glass N2 - The talk was given at the Spring School of the SPP1594 in Hannover and summarizes the actual findings about crack growth in water bearing soda-lime silicate glass and a comparison to other oxide glasses. T2 - Spring School des SPP1594 CY - Hannover, Germany DA - 06.03.2018 KW - DCB KW - Soda-lime silicate glass KW - Crack growth KW - Vickers KW - Water speciation PY - 2018 AN - OPUS4-45699 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waurischk, Tina A1 - Kiefer, P. A1 - Balzer, R. A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Deubener, J. A1 - Behrens, H. T1 - Wasser und Risswachstum in Silicatgläsern N2 - Die Festigkeit von Gläsern wird durch die Oberflächenqualität beeinflusst. Kommt es neben dem Auftreten von Defekten zusätzlich zum Risswachstum ausgehend hiervon, wird die Festigkeit minimiert. Das Wachstum hängt dabei maßgeblich von der Luftfeuchtigkeit ab. Dieses Ermüdungsverhalten von Gläsern besser zu verstehen und dabei die Mechanismen und den Einfluss von im Volumen eingebauten Wasser auf das unterkritische Risswachstum zu untersuchen, ist Ziel der Arbeiten. Als Teilprojekt im Rahmen des DFG Schwerpunktprogramms SPP 1594 „Ultrastrong glasses“ soll der Einfluss des im Volumen eingebauten Wassers auf die Rissspitze untersucht werden. Zusammen mit der Leibniz Universität Hannover und der TU Clausthal werden hierfür hochwasserhaltige Gläser (bis zu 8 Gew%) bei 8 kbar über die Flüssigphase synthetisiert, die makroskopisch den hohen Wasseranteil nachstellen. Die Charakterisierung erfolgt hinsichtlich des Wassereinbaus, der mechanischen Eigenschaften und des Risswachstums. Die Arbeiten in Berlin beziehen sich hierbei auf die Messungen des unterkritischen Risswachstums in Luft und Vakuum, sowie Verlustwinkelmessungen. Erste Ergebnisse zeigen Unterschiede im korrosionsbeeinflussten (langsames) und inerten (schnelles und im Vakuum stattfindendes) Risswachstumsverhalten der untersuchten Gläsern. Die Rissgeschwindigkeit beim Übergang vom korrosionsbeeinflussten zum inerten Risswachstum ist hin¬gegen für alle Gläser ähnlich und folglich ein kinetisch durch den äußeren Wassertransport an die Rissspitze bestimmter Prozess. Der Widerstand gegen Risswachstum steigt mit Tg und zusätzlich kann anhand der Verlustwinkelmessungen ein Zusammenhang zwischen der Netzwerk- und der β-Relaxation ermittelt werden. Je höher der Wassergehalt im Glas ist, desto niedriger wird Tg und einfacher das Risswachstum, welches sich durch längere Risse kennzeichnet. Besonders stark tritt dieser Effekt bei einem Überschuss an molekularem Wasser auf. T2 - 1. Fachsymposium der Glasapparatebauer CY - Munich, Germany DA - 19.04.2018 KW - Wasser KW - Risswachstum KW - Glas KW - Vickers KW - DCB PY - 2018 AN - OPUS4-45701 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waurischk, Tina A1 - Balzer, R. A1 - Kiefer, P. A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Behrens, H. A1 - Deubener, J. T1 - Sub-critical crack growth in silicate glass N2 - Premature failure of glass under load is caused by sub-critical crack growth (SCCG) originate from microscopic flaws at the surface. While SCCG is related to the humidity of the ambient atmosphere, leading to stress corrosion phenomena at the crack tip, the detailed mechanism and the effect of different network formers are still not fully understood. For more clarity, various soda silicate glasses with a second network former were investigated by double cantilever beam technique: Na2O*Al2O3*SiO2 (NAS), Na2O*B2O3*SiO2 (NBS), Na2O*PbO*SiO2 (NPbS). Three effects on the crack growth velocity, v, versus stress intensity, KI, curves were found out. The slope in region I, which is limited by corrosion, increases in the order NAS < NBS ≲ NPbS. The velocity range of region II reflecting the transition between corrosion effected and inert crack growth (region III), varies within one order of magnitude between the glasses. The KI region of inert crack growth strongly scatters between 0.4 and 0.9 MPam1/2. For comparison, crack growth at different humidity in commercial soda lime silicate glass (NCS) was measured. T2 - 92nd Annual Meeting of the German Society of Glass Technology in Conjunction with the Annual Meetings of the Czech Glass Society & the Slovak Glass Society CY - Bayreuth, Germany DA - 28.05.2018 KW - Risswachstum KW - DCB KW - Glas PY - 2018 AN - OPUS4-45702 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kiefer, P. A1 - Deubener, J. A1 - Waurischk, Tina A1 - Balzer, R. A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Behrens, H. T1 - Statistical analysis of Vickers induced subcritical crack growth in soda-lime silicate glasses N2 - Studies on Vickers induced subcritical crack growth are controversially discussed since the stresses that drive the crack growth are distributed three dimensionally within the material and cannot be retraced by available methods. Hence, empirical approaches are used to calculate mechanical material parameters such as the stress intensity factor KI. However, the results of these approaches show large deviations from those measured by standardized techniques such as double cantilever beam (DCB) or double cleavage drilled compression (DCDC). Yet, small specimen sizes and low specimen quantities can prevent the execution of DCB and DCDC measurements. Here we present an approach that is based on a statistical analysis of Vickers induced radial cracks. For this purpose more than 150 single radial cracks were analyzed. The cracks were generated in a commercial soda-lime silicate glass. The experiments were performed in a glovebox purged with dry nitrogen gas to minimize the influence of atmospheric water on crack growth. The temporally resolved evolution of the radial cracks was monitored in-situ using an inverted microscope equipped with a camera system directly below the Vickers indenter. An automated image analysis software was used to determine the crack length over time. The data show that the crack propagation and thereby the crack velocities are not uniformly but statistically distributed. These findings allow, using the statistical mean value of the distributions in combination with DCB data, a precise formulation of KI for each measured crack length. T2 - 92nd Annual Meeting of the German Society of Glass Technology in Conjunction with the Annual Meetings of the Czech Glass Society & the Slovak Glass Society CY - Bayreuth, Germany DA - 28.05.2018 KW - Crack growth KW - Soda-lime silicate glass KW - Vickers PY - 2018 AN - OPUS4-45703 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kiefer, P. A1 - Deubener, J. A1 - Waurischk, Tina A1 - Balzer, R. A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Behrens, H. T1 - Subcritical crack growth in water bearing soda-lime silicate glasses N2 - The presence of water in the surrounding atmosphere of a propagating crack has a major influence on the subcritical crack growth. While these external phenomena are well understood, there is still a lack of knowledge on the influence of structurally bound water on crack propagation. Thus, our recent study aims on the analysis of crack propagation in water bearing soda-lime silicate glasses with up to 8 wt.% water. The samples were synthesized in an internally heated pressure vessel at 0.5 GPa. Since this preparation route limits the sample sizes, standard test geometries allowing for the determination of stress intensity factors, such as double cantilever beam, are not feasible. Thus, radial cracks in the hydrous glasses were initiated by Vickers indentation and crack growth was simultaneously captured with a camera system. An automated image analysis algorithm was used for the analysis of the crack length of each single video frame. To minimize influences by atmospheric water, all experiments were conducted in a glovebox purged with dry N2. About 150 cracks per glass composition were analyzed to provide statistical significance of the Vickers-induced SCCG. The results show that structurally bound water has a major influence on SCCG by means of crack lengths, growth rates and time of crack initiation. T2 - 92nd Annual Meeting of the German Society of Glass Technology in Conjunction with the Annual Meetings of the Czech Glass Society & the Slovak Glass Society CY - Bayreuth, Germany DA - 28.05.2018 KW - Water speciation KW - Soda-lime silicate glass KW - Crack growth KW - Vickers PY - 2018 AN - OPUS4-45704 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kiefer, P. A1 - Balzer, R. A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Behrens, H. A1 - Deubener, J. T1 - Statistical analysis of subcritical crack growth in water bearing soda-lime silicate glasses N2 - The talk was given at the PNCS-ESG 2018 in Saint Malo and summarizes the actual findings about Vickers induced crack growth in water bearing soda-lime silicate glasses. T2 - 15th International Conference on the Physics of Non-Crystalline Solids & 14th European Society of Glass Conference CY - Saint Malo, France DA - 09.07.2018 KW - Water speciation KW - Vickers KW - Crack growth KW - Soda-lime silicate glass PY - 2018 AN - OPUS4-45707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Gaber, M. T1 - VACUUM HOT EXTRACTION (VHE-MS): Concentration, diffusion and degassing of volatiles N2 - Der Vortrag gibt eine Einführung in die Methode der Vakuumheißextraktion und beschreibt die Anwendungsmöglichkeiten der an der BAMN betriebenen Anlage. T2 - Seminar Instrumentelle Analytik, Fakultät III Prozesswissenschaften, Lehrstuhl Keramik TU Berlin CY - TU Berlin, Germany DA - 26.1.2018 KW - Gasabgabe KW - Diffusion KW - Gasgehalt PY - 2018 AN - OPUS4-45665 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Gaber, M. A1 - Reinsch, Stefan T1 - Thermal Analysis and Relaxation Phenomena in Oxide Glasses N2 - Wasser beeinflusst empfindlich eine Vielzahl von thermisch aktivierten Relaxationsphänomenen in Gläsern wie die Spannungsrelaxation, das unterkritische Risswachstum, innere Reibung, Viskosität, Sinterverhalten und Kristallisation. Thermische Methoden können dabei wesentliche Beiträge zum Verständnis dieser Phänomene liefern. Der Vortrag gibt einen Überblick über die Möglichkeiten der VakuumHeißExtraktion (VHE) zur Untersuchung des Wassergehalts, des Wasserabgabeverhaltens und der Wassermobilität sowie über den Einfluss des Wassers auf die innere Reibung (DMA). N2 - Dissolved water decisively influences numerous thermally activated relaxation phenomena in glasses like stress relaxation, sub-critical crack growth, internal friction, viscosity, sintering, and crystallization. Thermoanalytical methods can essentially help for better understanding of these phenomena. The lecture introduces the Vacuum Hot Extraction method (VHE) and illustrates its possibilities for measuring water content, degassing and mobility. As another thermoanalytical method, the Dynamic Mechanical Themoanalysis (DMA), allowing to study the effect of dissolved water on the internal friction in glasses, is introduced. T2 - Spring school DFG SPP 1594 CY - Hannover, Germany DA - 06.03.2018 KW - Wasser KW - Silicatglas KW - Relaxationsphänomene KW - Relaxation KW - Thermoanalytical Methods KW - Glass KW - Dissolved water PY - 2018 AN - OPUS4-45668 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Deubener, J. A1 - Behrens, H. T1 - Wasser in Silicatglas N2 - Der Vortrag gibt einen Überblick über den Stand des Wissens zum strukturellen Einbau von Wasser in Silicat- und Boratgläsern, den Einfluss des gelösten Wassers auf deren Viskosität sowie zu den strukturellen Vorstellungen zum Wassertransport. T2 - 1. Fachsymposium der Glasapparatebauer CY - Munich, Germany DA - 19.04.2018 KW - Wasser KW - Glass KW - Struktur PY - 2018 AN - OPUS4-45669 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Glass Sintering with Concurrent Crystallization and Foaming N2 - Glass powders are promising candidates for manufacturing a broad diversity of sintered materials like sintered glass-ceramics, glass matrix composites or glass bonded ceramics with tailored mechanical, thermal, electrical and optical properties and complex shape. Its wide and precise adjustability makes this class of materials a key component for advanced technologies. Processing of glass or composite powders often allow even more flexibility in materials design. At the same time, however, processing can have substantial effects on the glass powder surface and sinterability. Thus, mechanical damage and surface contamination can strongly enhance surface crystallization, which may retard or even fully prevent densification. Whereas sintering and concurrent crystallization have been widely studied, partially as cooperative effort of the TC7 of the ICG, and although glass powder sintering is predominantly applied for glasses of low crystallization tendency, sintering is also limited by gas bubble formation or foaming. The latter phenomenon is much less understood and can occur even for slow crystallizing glass powders. The lecture illustrates possible consequences of glass powder processing on glass sintering, crystallization and foaming. T2 - 7th Int Congress on Ceramics, Symposium Frontiers of Glass Science CY - Iguacu, Brazil DA - 17.06.2018 KW - Glass KW - Powder KW - Sintering KW - Foaming PY - 2018 AN - OPUS4-45670 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian A1 - Goedecke, Caroline A1 - Sojref, Regine T1 - Transformation of the antidiabetic drug metformin N2 - For years there have been more and more reports on the presence of drugs in the aquatic environment. Due to the demographic change, the consumption of pharmaceuticals has risen sharply. After taking the drugs, they are partly metabolized in the human body. However, the metabolism is not complete so that both the metabolites and non-metabolized amounts of the parent compounds are excreted. These compounds reach the waste water and afterwards the sewage treatment plants. In sewage treatment plants transformation products can be formed by the oxidative conditions during wastewater treatment processes. The transformation products may have a higher toxicity than the actual environmental pollutants and are often only partly removed during the waste water treatment. Since a lot of these compounds are still unknown, the transformation products are not detected by target analysis used in sewage treatment plants and are often released undetected in the aquatic ecosystems. The released substances may be subject to additional transformation processes in the environment. Pharmaceuticals produced in high amounts can be already detected in the μg/L range in water bodies worldwide. Metformin and its major transformation product guanylurea are one of the main representatives. Metformin is the drug of choice for treating type 2 diabetes. The drug therapy for diabetes mellitus has increased significantly in recent years. In the year 2015 1500 tons of metformin were prescribed in Germany (for statutory insured persons). Metformin is not metabolized in the human body and is excreted unchanged therefore concentrations between 57 μg/L and 129 μg/L are found in German waste water treatment plants influents. In this work the transformation of the antidiabetic drug metformin is investigated. The degradation of metformin is initialize by commercial water treatment techniques like UV-radiation or noncommercial techniques like heterogenous photocatalysis based on titanium dioxide. The degradation of metformin and resulting transformation products are analyzed by LC-MS/MS and LC-HRMS. T2 - SPEA 10 CY - Almeria, Spain DA - 04.06.2018 KW - Metformin KW - Photocatalysis PY - 2018 AN - OPUS4-47030 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waurischk, Tina A1 - Balzer, R. A1 - Kiefer, P. A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Behrens, H. A1 - Deubener, J. T1 - Sub-critical crack growth in silicate glasses N2 - Environmental conditions are known to influence sub-critical crack growth (SCCG) that are released from microscopic flaws at the glass surface, leading to stress corrosion phenomena at the crack tip. The processes at the crack-tip are complex and water has been identified as a key component governing SCCG at low crack velocities (region I). In particular, the influence of humidity accelerating crack propagation is well studied for industrial soda-lime silicate glasses, which are practically free (< 1000 ppm) of dissolved water. To shed light on the corrosion process, the situation at the crack-tip is reversed in the present study as dissolved water in larger fractions is present in the glass and crack propagation is triggered in dry environment. For this purpose, water-bearing silicate glasses of up to 8 wt% total water were synthesized in an internally heated pressure vessel at 0.5 GPa and compared to dry glasses of standard glass manufacturing. SCCG was measured using the double cantilever beam technique and by Vickers indentation. For dry glasses, three trends in the crack growth velocity versus stress intensity curve were found. The slope in region I limited by environmental corrosion increases in the order sodium aluminosilicate < sodium borosilicate ≲ sodium lead silicate. The velocity range of region II reflecting the transition between corrosion affected and inert crack growth (region III), varies within one order of magnitude among the glasses. The KI region of inert crack growth strongly scatters between 0.4 and 0.9 MPam1/2. For hydrous glasses, it is found that those of low Tg are more prone to SCCG. As water strongly decreases Tg, it promotes SCCG. First results indicate that molecular water has a dominating influence on SCCG. T2 - ICG Annual Meeting 2018 CY - Yokohama, Japan DA - 23.09.2018 KW - DCB KW - Glass KW - Crack growth KW - Water speciation PY - 2018 AN - OPUS4-47164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Welter, T. A1 - Deubener, J. A1 - Reinsch, Stefan A1 - Marzok, Ulrich A1 - Müller, Ralf T1 - Glass structures with low H2-diffusity N2 - Effective hydrogen storage capacities are prerequisite for an efficient energy provision using fuel cells. Since glass has low intrinsic hydrogen permeability, it is a promising material for hydrogen storage containers as well as hydrogen diffusion barriers. Previous studies on oxidic glasses suggest a correlation between the glass composition and hydrogen permeation that was derived mainly from silica glass. In the present study, we concentrate on the relationship between thermodynamic (i.e., configurational entropy) and topologic (i.e., free volume, network polymerization) parameters. Experimental data were gathered well below the glass transition temperature, excluding significant effects caused by structural relaxation and chemical dissolution of hydrogen. The results of seven analysed glasses on the SiO2-NaAlO2 joint showed that the hydrogen permeability in fully polymerized glasses cannot solely be derived from the total free volume of the glass structure. Hence, evidence is provided that the size distribution of free volume contributes to hydrogen solubility and diffusion. Additionally, the results indicate that the configurational heat capacity ΔCp at Tg affects the hydrogen permeability of the investigated glasses. T2 - 92. Glastechnische Tagung der DGG CY - Bayreuth, Germany DA - 28.05.2018 KW - Hydrogen permeability KW - Atomic packing factor KW - Glass composition KW - Diffusion coefficient PY - 2018 AN - OPUS4-45900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Welter, T. A1 - Marzok, Ulrich A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Deubener, J. T1 - Silicate glass structures with low hydrogen permeability N2 - Efficient energy provision using fuel cells requires effective hydrogen storage capacities. Glass is a material of low intrinsic hydrogen permeability and is therefore a promising material for hydrogen storage containers or diffusion barriers. Pioneer work on oxidic glasses seems to indicate a correlation between glass composition and hydrogen 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) glass parameters. Experiments were performed well below the glass transition temperature, which excludes significant structural relaxation and chemical dissolution of hydrogen. The compositional dependence of seven glasses on the SiO2-NaAlO2 join pointed out that in fully polymerized glasses the H2 permeability cannot be solely derived from the total free volume of the glass structure. Hence, evidence is provided that the size distribution of free volume contributes to hydrogen diffusion and solubility. Additionally, results indicate that hydrogen permeability of the glasses is affected by the configurational heat capacity ΔCp at Tg. T2 - 15th International Conference on the Physics of Non-Crystalline Solids & 14th European Society of Glass Conference CY - Saint Malo, France DA - 09.07.2018 KW - Diffusion coefficient KW - 3D glass structure model KW - Glass composition KW - Hydrogen permeation PY - 2018 AN - OPUS4-45911 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Deubener, J. A1 - Allix, M. A1 - Davis, M.J. A1 - Duran, A. A1 - Höche, T. A1 - Honma, T. A1 - Komatsu, T. A1 - Krüger, S. A1 - Mitra, I. A1 - Müller, Ralf A1 - Nakane, S. A1 - Pascual, M.J. A1 - Schmelzer, J.W. A1 - Zanotto, E.D. A1 - Zhou, S. T1 - Updated definition of glass-ceramics JF - Journal of Non-Crystalline Solids N2 - Glass-ceramics are noted for their unusual combination of properties and manifold commercialized products for consumer and specialized markets. Evolution of novel glass and ceramic processing routes, a plethora of new compositions, and unique exotic nano- and microstructures over the past 60 years led us to review the Definition of glass-ceramics. Well-established and emerging processing methods, such as co-firing, additive manufacturing, and laser patterning are analyzed concerning the core requirements of processing glass-ceramics and the Performance of the final products. In this communication, we propose a revised, updated definition of glass-ceramics, which reads “Glass-ceramics are inorganic, non-metallic materials prepared by controlled crystallization of glasses via different processing methods. They contain at least one type of functional crystalline phase and a residual glass. The volume fraction crystallized may vary from ppm to almost 100%”. KW - Glass-ceramics definition PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-464711 DO - https://doi.org/10.1016/j.jnoncrysol.2018.01.033 SN - 0022-3093 SN - 1873-4812 VL - 501 SP - 3 EP - 10 PB - Elsevier B.V. AN - OPUS4-46471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kotaka, M. A1 - Honma, T. A1 - Komatsu, T. A1 - Shinozaki, K. A1 - Affatigato, M. A1 - Müller, Ralf T1 - Control of self-powdering phenomenon in ferroelastic β′-Gd2(MoO4)3 crystallization in boro-tellurite glasses JF - Journal of Non-Crystalline Solids N2 - Glasses with compositions of 21Gd2O3-63MoO3-(16-x)B2O3-xTeO2 (mol%) (x= 0, 2, 4, 8) were prepared using a conventional melt quenching technique, and the crystallization behavior of ferroelastic β′-Gd2 MoO4)3 Crystals was examined to clarify the mechanism of self-powdering phenomenon and to design bulk crystallized glasses. It was found that the self-powdering phenomenon appeared significantly during the crystallization at temperatures near the crystallization peak temperature, but the phenomenon is suppressed in the crystallization at temperatures much higher than the glass transition temperature. It was also found that the substitution of TeO2 for B2O3 in the base glasses suppresses the self-powdering phenomenon and consequently bulk crystallized glasses were obtained in the glass with x=8 mol%. The densities at room temperature of the base glasses are d =4.755–4.906 g/cm3, being much higher than the value of d=4.555 g/cm3 for β′-Gd2(MoO4)3 crystal. It is proposed that the stresses in the inside of crystals induced by large density differences (i.e., large molar volume differences) between the glassy phase and crystals might be relaxed effectively in the glasses containing TeO2 with weak TeeO bonds and fragile character. KW - Glass crystallization stress PY - 2018 DO - https://doi.org/10.1016/j.jnoncrysol.2017.12.006 SN - 0022-3093 SN - 1873-4812 VL - 501 SP - 85 EP - 92 PB - Elsevier B.V. AN - OPUS4-46472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Agea Blanco, Boris A1 - Blaeß, Carsten A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Behrens, H. T1 - Sintering and foaming of silicate N2 - Glass powders are promising candidates for manufacturing a broad diversity of sintered materials like sintered glass-ceramics, glass matrix composites or glass bonded ceramics with properties and complex shape. 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 - ICG Annual Meeting 2018 CY - Yokohama, Japan DA - 23.09.2018 KW - Foaming KW - Glass KW - Powder KW - Sintering PY - 2018 AN - OPUS4-46474 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Marzok, U. T1 - Hochtemperatur Laserprofilometrie (HTLP) N2 - Der Vortrag gibt einen Überblick über Funktionsweise und Anwendungsmöglichkeiten der an der BAM entwickelten Messmethode der Hochtemperatur-Laserprofilomtrie T2 - Seminar Instrumentelle Analytik, Fakultät III Prozesswissenschaften, Lehrstuhl Keramik TU Berlin CY - TU Berlin, Germany DA - 26.01.2018 KW - Sinterung KW - Hochtemperatur KW - Formerkennung PY - 2018 AN - OPUS4-46475 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waurischk, Tina A1 - Balzer, R. A1 - Kiefer, P. A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Behrens, H. A1 - Deubener, J. T1 - The influence of volatile constituents on mechanical properties of glasses N2 - Im Rahmen des Young Researcher Day des SPP1594 wurden die bisherigen Inhalte der Projekte zusammengefasst und vorgetragen. T2 - Annual Meeting and Young Researcher Day CY - Jena, Germany DA - 11.09.2018 KW - Glass KW - Crack growth KW - Vickers KW - DCB KW - Water speciation PY - 2018 AN - OPUS4-46728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Nofz, Marianne T1 - High temperature coatings (Book review) T2 - Materials and Corrosion N2 - All in all, practicing professionals as well as researchers can read this book with pleasure and great benefit. It presents a comprehensive collection of data and practical examples manifested in about 100 graphs, 80 schemes of processes and devices, a manifold of images showing the microstructure of alloys or details of components and several phase diagrams. Tables containing data on commercially available coatings, alloys, compositions of corrosive salts, function of constituents of coatings add further important pieces of information. Thus, this book is a valuable source of information for anyone engaged in work with or research on high temperature coatings. KW - Coating KW - High temperature PY - 2018 DO - https://doi.org/10.1002/maco.201870104 SN - 0947-5117 VL - 69 IS - 10 SP - 1490 EP - 1490 PB - Wiley‐VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-46749 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tielemann, Christopher A1 - Kirzdörfer, Adrian A1 - Reinsch, Stefan A1 - Müller, Ralf T1 - First hints on reorientation of surface crystals N2 - Up to now, the mechanisms of surface nucleation and surface-induced texture formation are far from being understood. Very few observations of crystal orientation were focused on separately growing surface crystals. In conclusion, no systematic studies on initially oriented crystal growth or nucleation from defined active surface nucleation sites exists. Therefore, the main objective of this just is to advance the basic understanding of the mechanisms of surface-induced microstructure formation in glass ceramics. As a first attempt, we focus on reorientation of separately growing surface crystals during their early growth. T2 - 92nd Annual Meeting of the German Society of Glass Technology in Conjunction with the Annual Meetings of the Czech Glass Society & the Slovak Glass Society CY - Bayreuth, Germany DA - 28. Mai 2018 KW - Glass KW - Crystallization KW - BCS PY - 2018 AN - OPUS4-47536 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nofz, Marianne A1 - Dörfel, Ilona A1 - Sojref, Regine A1 - Wollschläger, Nicole A1 - Mosquera Feijoo, Maria A1 - Schulz, Wencke A1 - Kranzmann, Axel T1 - Thin Sol-Gel Alumina Coating as Protection of a 9% Cr Steel Against Flue Gas Corrosion at 650 °C JF - Oxidation of Metals N2 - Samples of sol-gel alumina coated and uncoated P92 steel were exposed to flue gas at 650 °C for 300 h. As result of this treatment a 50 µm thick bi-layered oxide scale had formed on the surface of the uncoated sample. Below the scale a 40 µm thick inner oxidation zone was detected. In contrast, the porous, micron thick alumina coating enabled the formation of a chromium oxide scale with a thickness of some nanometers at the interface between steel substrate and coating. In this case high temperature corrosion of the steel was prevented so far. KW - Steel KW - Oxide coatings KW - High-temperature corrosion KW - TEM KW - SEM PY - 2018 DO - https://doi.org/10.1007/s11085-017-9799-0 SN - 0030-770X SN - 1573-4889 VL - 89 IS - 3-4 SP - 453 EP - 470 PB - Springer AN - OPUS4-44472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wollschläger, Nicole A1 - Nofz, Marianne A1 - Dörfel, Ilona A1 - Schulz, Wencke A1 - Sojref, Regine A1 - Kranzmann, Axel T1 - Exposition of sol-gel alumina-coated P92 steel to flue gas: Time-resolved microstructure evolution, defect tolerance, and repairing of the coating JF - Materials and Corrosion N2 - Technically relevant P92 steel (9% Cr) was coated with a micron-thick porous alumina layer prepared by sol-gel technique and treated with flue gas (60 CO2-30 H2O-2 O2-1 SO2-7 N2 (mole fraction in %)) at 650 ° to mimic an oxyfuelcombustion process. Local defects in the coating were marked using focused ion beam (FIB) technique and were inspected after exposition to hot flue gas atmosphere at 300, 800, and 1300 h, respectively. Local defects like agglomerated alumina sol particles tend to spall off from the coating uncovering the underlying dense chromia scale. Re-coating was found to restore the protection ability from oxidation when repeatedly treated with hot flue gas. Cracks and voids did not promote the local oxidation due to the formation of crystalline Mn/S/O species within and on top of the coating. The protective character of the steel-coating system is a result of (i) the fast formation of a dense chromia scale at the surface of sol-gel alumina-coated P92 steel bars in combination with (ii) the porous alumina coating acting as diffusion barrier, but also as diffusion partner in addition with (iii) fast Mn outward diffusion capturing the S species from flue gas. KW - Alumina coatings KW - Oxyfuel KW - Steel P92 KW - High temperature corrosion PY - 2018 DO - https://doi.org/10.1002/maco.201709712 SN - 1521-4176 SN - 0947-5117 SN - 0043-2822 VL - 69 IS - 4 SP - 492 EP - 502 PB - Wiley-VCH Verlag GmbH&Co. KGaA CY - Weinheim AN - OPUS4-45300 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Schmidt, Wolfram A1 - Ramirez Caro, Alejandra A1 - Sojref, Regine A1 - Mota Gassó, Berta ED - Greim, M. ED - Kusterle, W. ED - Teubert, O. T1 - Contribution of the coarse aggregates to rheology - effects of flow coefficient, particle size distribution, and volume fraction T2 - Rheologische Messungen an Baustoffen 2018 N2 - In order to observe the effect of the aggregate phases between 2 mm and 16 mm without overlap with rheological effects induced by the cement hy-dration and without interactions with a threshold fine sand particle size that affects both, paste and aggregates, rheological experiments were conducted on a limestone filler based paste mixed with aggregates up to 16 mm. Vari-ous aggregate fractions were blended and mixed with the replacement paste in different volumetric ratios. The dry aggregates’ flow coefficients were determined and compared to yield stress and plastic viscosity values at different aggregate volume fractions. The results indicated that the flow coefficient is not a suitable parameter to predict the performance of the aggregates in the paste. It was shown that the yield stress of pastes is largely determined by the blend of different aggregate fractions, while the plastic viscosity to large extend depends upon the coars-est aggregate fraction. Based on the results, ideal aggregate composition ranges for minimised yield stress are presented. For the plastic viscosity no such grading curves to achieve minimum values could be found, but high viscosity curves are identified. KW - Rheology KW - Flow Coefficient KW - Particle Size Distribution KW - Volume Fraction KW - Cement KW - Concrete KW - Reference Material KW - Limestone Filler PY - 2018 SN - 978-3-7469-1878-5 SP - 96 EP - 108 PB - tredition GmbH CY - Hamburg AN - OPUS4-44434 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -