TY - CONF A1 - Busch, R. A1 - Tielemann, Christopher A1 - Reinsch, Stefan A1 - Patzig, C. A1 - Höche, T. A1 - Müller, Ralf T1 - Characterization of early crystallization stages in surface-crystallized diopside glass-ceramics N2 - Structure formation in glass-ceramics by means of surface crystallization is a challenging open question and remains elusive to definite answers. In several glass-ceramic systems, oriented crystal layers have been observed at the immediate surface, including diopside and some fresnoite systems. However, it is still open to debate, whether oriented surface crystallization is the result of oriented nucleation or growth selection effects. In the same vein, there is still discussion whether surface nucleation is governed by surface chemistry effects or by defects serving as active nucleation sites. In order to help answer these questions, annealing experiments at 850°C have been performed on a MgO·CaO·2SiO2 glass, leading to the crystallization of diopside at the surface. Different annealing durations and surface treatment protocols (i.a. lapping with diamond slurries between 16 µm and 1 µm grain size) have been applied. Particular focus has been put on earliest crystallization stages, with crystal sizes down to about 200 nm. The resultant microstructure has been analyzed by electron backscatter diffraction (EBSD) and two different kinds of textures have been observed, with the a- or b-axis being perpendicular to the sample surface and the c-axis lying in the sample plane. Even at shortest annealing durations, a clear texture was present in the samples. Additionally, selected samples have been investigated with energy-dispersive x-ray spectroscopy in the scanning transmission electron microscope (STEM-EDX). The diopside crystals have been found to exhibit distinguished submicron structure variations and the glass around the crystals was shown to be depleted of Mg. T2 - 93rd Annual Meeting of the German Society of Glass Technology in Conjunction with the Annual Meeting of French Union for Science and Glass Technology (USTV) CY - Nuremberg, Germany DA - 13.05.2019 KW - Glass KW - Crystallization KW - Diopside KW - EBSD KW - Orientation PY - 2019 AN - OPUS4-49296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scheffler, F. A1 - Tielemann, Christopher A1 - Busch, R. A1 - Kober, M. A1 - Müller, Ralf A1 - Brauer, D. S. T1 - Crystallization of glasses studied with PEEM N2 - A heat treated glass that formed crystals under controlled conditions can be a glass ceramic. A proper understanding of crystallization in glassy melts is needed yet still lacking. Involved processes include the mobility of Elements within the glass during heat treatment and the reorganization of atomic bonds during crystallization. This change in coordination number of certain elements is easily observable in bulk glass samples during heat treatment with XAS. Our plan was to monitor these reorganization processes in situ at the immediate surface during heat treatment with PEEM to get time and spatial resolved data. T2 - Joint Meeting of the Polish Synchrotron Radiation Society and SOLARIS Users CY - Online meeting DA - 09.09.2020 KW - Glass KW - Surface KW - Peem KW - Synchrotron PY - 2020 AN - OPUS4-51336 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kiefer, P. A1 - Balzer, R. A1 - Deubener, J. A1 - Behrens, H. A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Müller, Ralf T1 - Density, elastic constants and indentation hardness of hydrous soda-lime silica glasses JF - Journal of Non-Crystalline Solids N2 - The effect of structural water on density, elastic constants and microhardness of water-bearing soda-lime-silica glasses of up to 21.5 mol% total water is studied. It is found that the Poisson ratio and the water content are positively correlated, while density and the elastic moduli decrease with increasing water content. Vickers hardness decreases by approximately 27% from the dry to the most hydrous glass. For water fractions <3 mol%, the dependencies are non-linear reflecting the non-linear change in the concentrations of OH and H2O molecules dissolved, whereas for water fractions >3 mol% linear dependencies are found. To distinguish the effect of structural water and environmental water, indentations were performed in toluene, nitrogen gas and air. Timedependent softening was evident for testing dry glasses in humid atmospheres as well as for tests of hydrous glasses in dry atmospheres. This indicates that the response times of dissolved water species are effectively equal in both scenarios. KW - Elastic constants KW - Soda-lime-silica KW - Glass KW - Water content KW - Microhardness PY - 2019 DO - https://doi.org/10.1016/j.jnoncrysol.2019.119480 SN - 0022-3093 SN - 1873-4812 VL - 521 SP - 119480 PB - Elsevier B.V. AN - OPUS4-48758 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 - CONF A1 - Reinsch, Stefan T1 - Glass N2 - Überblick über die Arbeitsschwerpunkte des Fachbereichs 5.6 Glas und die Vielfalt des Werkstoffs Glas. An Hand der Vakuumheißgasextraktion (VHE) werden einige Beispiele u.a. zur Bestimmung des Wassergehalts oder des Diffusionskoeffizienten von Wasserstoff in Gläsern gezeigt. Zum Schluss erfolgt ein Ausblick auf die im nächsten Jahr zur Verfügung stehende robotergestützte Glasscreening Anlage. N2 - Overview about the key activities of division 5.6 glass and the diversity of the material glass. For the vacuum hot extraction method (VHE-MS) some examples are presented e. g. for the measurement of water content or the determination of diffusion coefficient of hydrogen in glasses. Finally, an outlook is shown on the robot controlled glass screening device which will be available next year. T2 - BAM - IFW Workshop CY - Berlin, Germany DA - 25.11.2019 KW - Glass KW - Glass screening device KW - Vacuum hot extraction PY - 2019 AN - OPUS4-50452 LA - eng 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 - 93rd Annual Meeting German Soc Glass Technol in conjunction with annual meeting French Union for Sci and Glass technol CY - Nuremberg, Germany DA - 13.05.2019 KW - Blähen KW - Glass KW - Kristallisation KW - Sintern PY - 2019 AN - OPUS4-50433 LA - eng 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 - JOUR A1 - Welter, T. A1 - Müller, Ralf A1 - Deubener, J. A1 - Marzok, Ulrich A1 - Reinsch, Stefan T1 - Hydrogen Permeation Through Glass JF - Frontiers in Materials N2 - Physical storage of gaseous hydrogen under high-pressure in glassy micro-containers such as spheres and capillaries is a promising concept for enhancing safety and the volumetric capacity of mobile hydrogen storage systems. As very low permeation through the container wall is required for storage of compressed hydrogen, development of glasses of minimal hydrogen permeability is needed. For this purpose, one has to understand better the dependence of hydrogen permeability on glass structure. The paper points out that minimizing the accessible free volume is as one strategy to minimize hydrogen permeability. Based on previously measured and comprehensive literature data, it is shown that permeation is independently controlled by ionic porosity and network modifier content. Thus, ionic porosity in modified and fully polymerized networks can be decreased equally to the lowest hydrogen permeability among the glasses under study. Applying this concept, a drop of up to 30,000 with respect to the permeation of hydrogen molecules through silica glass is attainable. KW - Ionic porosity KW - hydrogen storage KW - Glass KW - Permeability KW - Solubility KW - Diffusivity PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513927 DO - https://doi.org/10.3389/fmats.2019.00342 VL - 6 SP - Article 342 AN - OPUS4-51392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tielemann, Christopher A1 - Reinsch, Stefan A1 - Maaß, Robert A1 - Deubener, J. A1 - Müller, Ralf T1 - Internal nucleation tendency and crystal surface energy obtained from bond energies and crystal lattice data JF - Journal of Non-Crystalline Solids: X N2 - We present an easy-to-apply method to predict structural trends in the internal nucleation tendency of oxide glasses. The approach is based on calculated crystal fracture surface energies derived from easily accessible diatomic bond energy and crystal lattice data. The applicability of the method is demonstrated on literature nucleation data for isochemically crystallizing oxide glasses. KW - Glass KW - Nucleation tendency KW - Fracture surface energy KW - Crystal lattice KW - Bond energy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548814 DO - https://doi.org/10.1016/j.nocx.2022.100093 SN - 2590-1591 VL - 14 SP - 1 EP - 5 PB - Elsevier B.V. AN - OPUS4-54881 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heuser, Lina A1 - Müller, Ralf A1 - Nofz, Marianne A1 - Deubener, J. T1 - Liquid phase sintering of alkali zinc borate glass-bearing silver pastes for applications in photovoltaics and microelectronics N2 - Liquid phase sintering of glass bearing silver pastes used in photovoltaics and microelectronics is poorly understood. In particular, the role of different network modifiers acting in the glass component and the question of the most suitable atmospheric oxygen level during sintering are still under considerable debate. To tackle these issues, low-melting and lead-free X2O-ZnO-B2O3 glasses with X = Li, Na, K and Rb (LZB, NZB, KZB and RZB) were prepared. Infrared spectroscopy showed that the glass structure was similar to each other, while an increase of tetrahedrally coordinated boron with increasing field strength of the alkali was evident. In turn, the glass transition temperature (from differential thermal analysis) increased in the order: RZB (449 °C) < KZB (460 °C) < NZB (465 °C) < LZB (472 °C). Powders of each glass were mixed with organics to receive silver-glass-pastes containing 30 vol% glass and these were subjected to heating microscopy in air. Although similar onset temperatures of sintering were recorded for Ag-NZB and Ag-LZB glass pastes, and for Ag-RZB paste and KZB-Ag-paste, respectively, differences in the crystallization behavior and final densification were observed between the former and the latter group. These were translated in terms of differences in silver dissolution and reprecipitation among the two groups. Further, running the experiments in nitrogen gas showed that sintering of all pastes was considerably hampered. The slow-down of the sinter kinetics was found to be in line with the assumed lower oxidation and dissolution of silver ions into the glass-forming liquid. T2 - 26th International Congress on Glass CY - Berlin, Germany DA - 03.07.2022 KW - Silver metallization paste KW - Sintering KW - Glass KW - Alkali zinc borate glasses KW - Viscosity KW - Structure PY - 2022 AN - OPUS4-55728 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 - CONF A1 - Deubener, J. A1 - Müller, Ralf A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Behrens, H. A1 - Balzer, R. A1 - Bauer, U. A1 - Kiefer, P. T1 - Micromechanical properties of hydrous oxide glasses N2 - Presentation of the results on structure and mechanical properties of water-bearing oxide glasses, which were found during the project at the locations Clausthal, Hanover and Berlin within the priority program SPP1594. T2 - 9th Otto Schott Colloquium CY - Jena, Germany DA - 09.09.2019 KW - Crack growth KW - Glass KW - Water content KW - Mechanical properties KW - IR PY - 2019 AN - OPUS4-50444 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scheffler, F. A1 - Fleck, M. A1 - Santiago, C. F. A1 - Brauer, D. S. A1 - Müller, Ralf T1 - Morphologies of Fresnoite surface crystals of BT0.75S glass under different atmospheric conditions N2 - Fresnoite glass-ceramics are characterized by piezoelectric, pyroelectric and non-linear optical properties. These properties can be adjusted by orienting the fresnoite crystals during crystallization. Crystallization begins at the surface. The first surface crystals are not oriented perpendicular and, therfore, produce a surface layer that has not the intended properties. To overcome this issue, the formation of fresnoite surface crystals at different atmospheric conditions was studied. T2 - 9th Int. Otto Schott Colloquium CY - Jena, Germany DA - 09.09.2019 KW - Glass KW - Surface crystallization KW - Crystal orientation PY - 2019 AN - OPUS4-50460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tielemann, Christopher A1 - Reinsch, Stefan A1 - Müller, Ralf T1 - Oriented Surface Crystallization N2 - Up to now, oriented surface crystallization phenomena are discussed controversially, and related studies are restricted to few glasses. For silicate glasses we found a good correlation between the calculated surface energy of crystal faces and oriented surface nucleation. Surface energies were estimated assuming that crystal surfaces resemble minimum energy crack paths along the given crystal plane. This concept was successfully applied by Rouxel in calculating fracture surface energies of glasses. Several oriented nucleation phenomena can be herby explained assuming that high energy crystal surfaces tend to be wetted by the melt. This would minimize the total interfacial energy of the nucleus. Furthermore, we will discuss the evolution of the microstructure and its effect on the preferred crystal orientation. T2 - 26th International Congress on Glass CY - Berlin, Germany DA - 03.07.2022 KW - Glass KW - Surface energy KW - Crystal orientation PY - 2022 AN - OPUS4-56074 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 - 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 - Tielemann, Christopher A1 - Busch, R. A1 - Reinsch, Stefan A1 - Patzig, C. A1 - Höche, T. A1 - Avramov, I. A1 - Müller, Ralf T1 - Oriented surface nucleation in diopside glass JF - Journal of Non-Crystalline Solids N2 - Es wird die Texturbildung in kristallisierendem Diopsidglas im Zusammenhang mit der Oberflächenbeschaffenheit der unbehandelten Probe untersucht. Zudem wird der diskutiert, dass es sich bei der Texturbildung in Gläsern höchstwahrscheinlich um ein Nukleationsphänomen handelt welches auf die richtungsabhängige Grenzflächenenergie der kristallisierenden Phase zurückzuführen ist. N2 - Oriented surface crystallization on polished diopside glass surfaces has been studied with scanning electron microscopy, electron backscatter diffraction, transmission electron microscopy and laser scanning microscopy. An orientation preference of [001] parallel to the glass surface was detected for separately growing diopside crystals even as small as 700 nm in size. This finding shows that crystal orientation occurs in the outermost surface layer without crystal-crystal interaction and indicates that the crystal orientation is a result of oriented nucleation. Depending on surface preparation, monomodal crystal orientation distributions with [100] perpendicular to the surface or bimodal distributions with [100] and [010] perpendicular to the glass Surface were detected. It was also shown that the degree of crystal orientation increases with decreasing Surface roughness. The observed orientation of diopside crystals could be explained in terms of the interfacial energies of different crystal faces. KW - Surface energy KW - Glass ceramic KW - Glass KW - EBSD KW - Diopsid PY - 2021 UR - https://www.sciencedirect.com/science/article/pii/S002230932100020X DO - https://doi.org/10.1016/j.jnoncrysol.2021.120661 SN - 0022-3093 VL - 562 PB - Elsevier B.V. AN - OPUS4-53073 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riechers, Birte A1 - Roed, L. A1 - Mehri, S. A1 - Ingebrigtsen, T. A1 - Hecksher, T. A1 - Dyre, J. A1 - Niss, K. T1 - Predicting nonlinear physical aging of glasses from equilibrium relaxation via the material time JF - Science advances N2 - The noncrystalline glassy state of matter plays a role in virtually all fields of materials science and offers complementary properties to those of the crystalline counterpart. The caveat of the glassy state is that it is out of equilibrium and therefore exhibits physical aging, i.e., material properties change over time. For half a century, the physical aging of glasses has been known to be described well by the material-time concept, although the existence of a material time has never been directly validated. We do this here by successfully predicting the aging of the molecular glass 4-vinyl-1,3-dioxolan-2-one from its linear relaxation behavior. This establishes the defining property of the material time. Via the fluctuation-dissipation theorem, our results imply that physical aging can be predicted from thermal-equilibrium fluctuation data, which is confirmed by computer simulations of a binary liquid mixture. KW - Physical aging KW - Equilibrium relaxation KW - Glass PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546015 DO - https://doi.org/10.1126/sciadv.abl9809 SN - 2375-2548 VL - 8 IS - 11 SP - 1 EP - 8 PB - American Association for the Advancement of Science CY - Washington, DC AN - OPUS4-54601 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Busch, R. A1 - Tielemann, Christopher A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Patzig, C. A1 - Krause, M. A1 - Höche, T. T1 - Sample preparation for analytical scanning electron microscopy using initial notch sectioning JF - Micron N2 - A novel method for broad ion beam based sample sectioning using the concept of initial notches is presented. An adapted sample geometry is utilized in order to create terraces with a well-define d step in erosion depth from the surface. The method consists of milling a notch into the surface, followed by glancing-angle ion beam erosion, which leads to preferential erosion at the notch due to increased local surface elevation. The process of terrace formation can be utilized in sample preparation for analytical scanning electron microscopy in order to get efficient access to the depth-dependent microstructure of a material. It is demonstrated that the method can be applied to both conducting and non-conducting specimens. Furthermore, experimental parameters influencing the preparation success are determined. Finally, as a proof-of-concept, an electron backscatter diffraction study on a surface crystallized diopside glass ceramic is performed, where the method is used to analyze orientation dependent crystal growth phenomena occurring during growth of surface crystals into the bulk. KW - 3D etching KW - Ion beam erosion Sectioning KW - EBSD KW - Sample preparation KW - Analytical scanning electron microscopy KW - SEM KW - Glass Ceramic KW - Glass KW - Diopsid PY - 2021 DO - https://doi.org/10.1016/j.micron.2021.103090 SN - 0968-4328 VL - 150 PB - Elsevier B.V. AN - OPUS4-53075 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Holzer, Marco A1 - Waurischk, Tina A1 - George, Janine A1 - Maaß, Robert A1 - Müller, Ralf T1 - Silicate glass fracture surface energy calculated from crystal structure and bond-energy data JF - Journal of Non-Crystalline Solids N2 - We present a novel method to predict the fracture surface energy, γ, of isochemically crystallizing silicate glasses using readily available crystallographic structure data of their crystalline counterpart and tabled diatomic chemical bond energies, D0. The method assumes that γ equals the fracture surface energy of the most likely cleavage plane of the crystal. Calculated values were in excellent agreement with those calculated from glass density, network connectivity and D0 data in earlier work. This finding demonstrates a remarkable equivalence between crystal cleavage planes and glass fracture surfaces. KW - Glass KW - Fracture surface energy KW - Toughness KW - Modeling KW - Mechanical properties PY - 2023 DO - https://doi.org/10.1016/j.jnoncrysol.2023.122679 SN - 0022-3093 VL - 622 SP - 1 EP - 6 PB - Elsevier B.V. AN - OPUS4-58767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -