TY - CONF A1 - Müller, Ralf T1 - Sintering and Crystallization of Glass Powders (invited) T2 - 3rd GlaCERCo Network-wide Workshop CY - Erlangen, Germany DA - 2014-10-08 PY - 2014 AN - OPUS4-30855 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Glas und Keramik für Schlüsseltechnologien - Prozessbegleitende Prüfung und Simulation T2 - Sommerkolloquium des GHI der RWTH CY - Aachen, Germany DA - 2012-06-21 PY - 2012 AN - OPUS4-30854 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Glaspulver - Processing, Effekte, Möglichkeiten T2 - Festkolloquium der Universität des Saarlandes CY - Saarbrücken, Germany DA - 2013-03-23 PY - 2013 AN - OPUS4-30853 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - GlasDigital: Data-driven workflow for accelerated glass development N2 - lasses stand out by their wide and continuously tunable chemical composition and large variety of unique shaping techniques making them a key component of modern high technologies. Glass development, however, is still often too cost-, time- and energy-intensive. The use of robotic melting systems embedded in an ontology-based digital environment is intended to overcome these problems in future. As part of the German research initiative MaterialDigital, the joint project GlasDigital takes first steps in this direction. The project consortium involves the Fraunhofer ISC in Würzburg, the Friedrich Schiller University Jena (OSIM), the Clausthal University of Technology (INW), and the Federal Institute for Materials Research and Testing (BAM, Division Glasses) and aims to combine all main basic components required for accelerated data driven glass development. For this purpose, a robotic high throughput glass melting system is equipped with novel inline sensors for process monitoring, machine learning (ML)-based, adaptive algorithms for process monitoring and optimization, novel tools for high throughput glass analysis and ML-based algorithms for glass design, including software tools for data mining as well as property and process modelling. The talk gives an overview how all these tools are interconnected and illustrates their usability with some examples. T2 - HVG-DGG Fachausschuss I CY - Jena, Germany DA - 03.11.2023 KW - Glass KW - Robotic melting KW - Ontologie KW - Simulation KW - Workflow KW - Data Space PY - 2023 AN - OPUS4-60383 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chen, Ya‐Fan A1 - Arendt, Felix A1 - Bornhöft, Hansjörg A1 - de Camargo, Andréa S. S. A1 - Deubener, Joachim A1 - Diegeler, Andreas A1 - Gogula, Shravya A1 - Contreras Jaimes, Altair T. A1 - Kempf, Sebastian A1 - Kilo, Martin A1 - Limbach, René A1 - Müller, Ralf A1 - Niebergall, Rick A1 - Pan, Zhiwen A1 - Puppe, Frank A1 - Reinsch, Stefan A1 - Schottner, Gerhard A1 - Stier, Simon A1 - Waurischk, Tina A1 - Wondraczek, Lothar A1 - Sierka, Marek T1 - Ontology‐Based Digital Infrastructure for Data‐Driven Glass Development N2 - The development of new glasses is often hampered by inefficient trial‐and‐error approaches. The traditional glass manufacturing process is not only time‐consuming, but also difficult to reproduce with inevitable variations in process parameters. These challenges are addressed by implementing an ontology‐based digital infrastructure coupled with a robotic melting system. This system facilitates high‐throughput glass synthesis and ensures the collection of consistent process data. In addition, the digital infrastructure includes machine learning models for predicting glass properties and a tool for extracting patent information. Current glass databases have significant gaps in the relationships between compositions, process parameters, and properties due to inconsistent studies and nonconforming units. In addition, process parameters are often omitted, and even original literature references provide limited information. By continuously expanding the database with consistent, high‐quality data, it is aimed to fill these gaps and accelerate the glass development process. KW - Digitalisation KW - Data-driven glass development KW - Ontology PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625844 DO - https://doi.org/10.1002/adem.202401560 SN - 1527-2648 SP - 1 EP - 12 PB - Wiley VHC-Verlag AN - OPUS4-62584 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Blaeß, Carsten A1 - Müller, Ralf T1 - Fast crack healing in glass-matrix composites with rigid filler percolation frameworks N2 - To ensure the durability of solid oxide fuel cell sealants, the understanding of the microstructural influence on viscous crack healing is essential. To this end, the effect of microstructure with respect to the spatial distribution of filler particles on viscous crack healing was studied with confocal laser scanning microscopy in glass-matrix composites (GMCs) made by mix-milling and sintering of sodalime magnesium silicate glass and Φ ≈ 6 vol% ZrO2 chemically inert rigid filler particles. This way, no change in Φ occurred during the crack healing treatments studied on Vickers indentation-induced radial cracks in polished GMC surfaces. Different microstructures were mimicked using different ZrO2 particle sizes for mix-milling. Unlike coarse ZrO2 particles, similar in size to the glass particle, fine ZrO2 particles, much smaller than the glass particles, form a rigid percolation framework (RPF) of ZrO2 filler particles around the former glass particles or glass particle agglomerates. For this RPF microstructure, crack healing was observed more readily as crack healing retardation phenomena like large-scale crack widening and crack tip rounding were strongly reduced, whereas narrow cracks could still heal locally within the glassy regions. KW - Crack healing KW - Glass matrix composite KW - Rigid percolation frameworks KW - Vickers indentation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625921 DO - https://doi.org/10.1111/jace.20386 SN - 0002-7820 SP - 1 EP - 10 PB - Wiley AN - OPUS4-62592 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Balzer, R. A1 - Behrens, H. A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Kiefer, P. A1 - Deubener, J. A1 - Fechtelkord, M. T1 - Water in Alkali Aluminosilicate Glasses N2 - To understand the influence of water and alkalis on aluminosilicate glasses, three polymerized glasses with varying ratios of Na/K were synthesized [(22. 5-x)Na2O-xK2O-22.5 Al2O3-55 SiO2 with x = 0, 7.5, and 11.25]. Subsequently, these glasses were hydrated (up to 8 wt% H2O) in an internally heated gas pressure vessel. The density of hydrous glasses linearly decreased with water content above 1 wt%, consistent with the partial molar volume of H2O of 12 cm3/mol. Near-infrared spectroscopy revealed that hydroxyl groups are the dominant species at water content of <4 wt%, and molecular water becomes dominating at water content of >5 wt%. The fraction of OH is particularly high in the pure Na-bearing glass compared to the mixed alkali glasses. 27Al magic angle spinning-NMR spectroscopy shows that aluminum is exclusively fourfold coordinated with some variations in the local geometry. It appears that the local structure around Al becomes more ordered with increasing K/Na ratio. The incorporation of H2O reinforces this effect. The differential thermal analysis of hydrous glasses shows a significant mass loss in the range of glass transition already during the first upscan, implying the high mobility of water in the glasses. This observation can be explained by the open structure of the aluminosilicate network and by the low dissociation enthalpy of H2O in the glasses (≈ 8 kJ/mol). The effect of the dissolved H2O on the glass transition temperature is less pronounced than for other aluminosilicate glasses, probably because of the large fraction of Al in the glasses. KW - NMR spectroscopy KW - Alkali aluminosilicate glasses KW - Water speciation KW - Glass transition KW - Infrared spectroscopy PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509497 DO - https://doi.org/10.3389/fmats.2020.00085 VL - 7 SP - 85 AN - OPUS4-50949 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Brita A1 - Rurack, Knut A1 - Müller, Ralf A1 - Jancke, Harald T1 - Untersuchungen zur Alterung von Kieselsolen und -gelen T2 - 11. Arbeitstagung des AK Nichtkristalline und Partiellkristalline Strukturen CY - Wolfersdorf, Deutschland DA - 2003-09-08 PY - 2003 UR - http://www2.uni-jena.de/chemie/DGK-AK4/VOR_03/Unger.pdf SP - 1(?) EP - 10(?) AN - OPUS4-3119 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut A1 - Unger, Brita A1 - Müller, Ralf A1 - Resch-Genger, Ute T1 - SiO2-Gele als Matrices für Fluoreszenzmarker T2 - 75. Glastechnische Tagung CY - Wernigerode, Deutschland DA - 2001-05-21 PY - 2001 SP - 8 EP - 11 PB - DGG, Deutsche Glastechnische Gesellschaft e.V. CY - Frankfurt/M. AN - OPUS4-2084 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Brita A1 - Rurack, Knut A1 - Müller, Ralf A1 - Jancke, Harald A1 - Resch-Genger, Ute T1 - Microscopic vs. macroscopic structural evolution of SiO2 sols and gels employing a tailor-made fluorescent reporter dye N2 - The short- and long-term structural evolution and aging of sol–gel materials prepared under mild conditions are studied by fluorometry, dynamic light scattering (DLS), 29Si NMR and gravimetry. In combination with the first, a newly developed donor–acceptor-substituted fluorescent probe with two acidophilic sites of different strength and topology is introduced. Its performance in detecting changes in parameters such as polarity, proticity, and pore volume on the microscopic scale is compared to two other dyes and to the macroscopic changes revealed by DLS, NMR and gravimetry. At early stages of the sol–gel process, fluorometry, DLS and NMR reveal similar changes which are typical of the structural evolution of SiO2 sols having different synthesis parameters. During later times of sol aging, DLS and NMR reflect the growth of the network and indicate that all sols approach similar structural equilibria. Fluorometry supports these findings by signalling a gradual decrease in mobile species with high proton activity. The formation of the spanning cluster upon gelation is strongly evident only from DLS results while the local environment of the fluorophore remains largely unchanged. However, the fluorescent dye is able to report microscopic changes even during long-term aging. Drying of the gels with a pronounced contraction of solvated pores is readily observable by fluorometry and gravimetry. During the late reaction stages, the fluorescence properties of the tailor-made dye are still sensitive toward the environment. PY - 2005 DO - https://doi.org/10.1039/b501622c SN - 0959-9428 SN - 1364-5501 VL - 15 IS - 30 SP - 3069 EP - 3083 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-10378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winkel, A. A1 - Meszaros, R. A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Travitzky, N. A1 - Fey, T. A1 - Greil, P. A1 - Wondraczek, L. T1 - Sintering of 3D-printed glass/HAp composites N2 - We report the sintering of 3D-printed composites of 13-93 bioactive glass and hydroxyapatite (HAp) powders. The sintering process is characterized on conventionally produced powder compacts with varying HAp content. A numeric approximation of the densification kinetics is then obtained on the basis of Frenkel, Mackenzie–Shuttleworth, and Einstein–Roscoe models, and optimized sintering conditions for 3D-printed structures are derived. Fully isotropic sintering of complex cellular composites is obtained by continuous heating to 750°C at a rate of 2 K/min for a HAp content of 40 wt%. The approach can readily be generalized for printing and sintering of similar glass-ceramic composites. KW - Sintering glass composit bio material PY - 2012 DO - https://doi.org/10.1111/j.1551-2916.2012.05368.x SN - 0002-7820 SN - 1551-2916 VL - 95 IS - 11 SP - 3387 EP - 3393 PB - Blackwell Publishing CY - Malden AN - OPUS4-27053 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut A1 - Unger, Brita A1 - Müller, Ralf A1 - Jancke, Harald A1 - Resch-Genger, Ute T1 - Die Strukturentwicklung von SiO2 Solen und Gelen im Vergleich mikroskopischer und makroskopischer Untersuchungsmethoden T2 - 77. Glastechnische Tagung CY - Leipzig, Deutschland DA - 2003-05-26 PY - 2003 VL - 77 SP - 101 EP - 104 PB - DGG CY - Offenbach AN - OPUS4-3121 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Brita A1 - Rurack, Knut A1 - Müller, Ralf A1 - Resch-Genger, Ute A1 - Buttke, K. T1 - Effects of the Sol-Gel Processing on the Fluorescence Properties of Laser Dyes in Tetraethoxysilane Derived Matrices N2 - Two fluorescent dyes were incorporated into sol-gel derived SiO2 matrices. The dye was added to SiO2 precursors of different degrees of pre-condensation and the spectroscopic properties of the immobilized dye were measured at various aging and drying stages of the resulting gels. The significant influence of the processing parameters on the spectroscopic properties is manifested in the relative intensity of a second red shifted emission band (550–560 nm), which was observed besides the typical coumarin emission band (495 nm). The appearance of this long wavelength emission might be attributed to dye aggregation or to other reactions with the ambient matrix forced by micro porosity phenomena. KW - Sol-gel KW - Precursor chemistry KW - Fluorescence properties KW - Optical solids PY - 2000 DO - https://doi.org/10.1023/A:1008768318418 SN - 0928-0707 SN - 1573-4846 VL - 19 SP - 799 EP - 802 PB - Kluwer Academic Publ. CY - Dordrecht AN - OPUS4-1080 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eichelbaum, M. A1 - Rademann, K. A1 - Müller, Ralf A1 - Radtke, Martin A1 - Görner, Wolf T1 - Zur Chemie des Goldes in Silicatgläsern: Untersuchungen zum nicht-thermisch aktivierten Wachstum von Goldclustern KW - Glas KW - Goldcluster KW - Nanophotonik PY - 2005 DO - https://doi.org/10.1002/ange.200502174 SN - 0044-8249 SN - 0932-2140 SN - 1521-3757 VL - 117 IS - 48 SP - 8118 EP - 8122 PB - Wiley-VCH CY - Weinheim AN - OPUS4-7691 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eichelbaum, M. A1 - Rademann, K. A1 - Weigel, W. A1 - Löchel, B. A1 - Radtke, Martin A1 - Müller, Ralf T1 - Gold-Ruby Glass in a New Light: On the Microstructuring of Optical Glasses with Synchrotron Radiation KW - Nanoparticles KW - Glasses KW - Synchrotron radiation KW - X-ray lithography KW - Surface plasmon resonance KW - Luminescence PY - 2007 SN - 0017-1557 VL - 40 IS - 4 SP - 1 EP - 5 CY - London AN - OPUS4-16432 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Waurischk, Tina A1 - Deubener, J. A1 - Müller, Ralf T1 - Internal friction and energy dissipation during fracture in silicate glasses N2 - To obtain a deeper insight into the nature of energy dissipation during fracture, the internal friction of 13 borosilicate, aluminosilicate, soda-lime, and lead-containing glasses, for which inert crack growth data are known, was measured using dynamic mechanical thermal analysis. For asymmetrically bent glass beams, the loss tangent, tan δ, was determined between 0.2 and 50 Hz at temperatures between 273 K and the glass transition temperature, Tg. It was found that the area under the tan δ vs T·Tg−1 curve correlates with the crack growth exponent, n, in the empirical v = v0·KIn relation between crack growth velocity, v, and stress intensity, KI, which indicates that n correlates with the degree of energy dissipation of sub-Tg relaxation phenomena. KW - Glass KW - Internal friction KW - Crack growth PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-651371 DO - https://doi.org/10.1063/5.0255432 SN - 0021-9606 VL - 162 IS - 19 SP - 1 EP - 9 PB - AIP Publishing AN - OPUS4-65137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pan, Z. A1 - Waurischk, Tina A1 - Duval, A. A1 - Müller, Ralf A1 - Deubener, J. A1 - Krishnan, N. M. A. A1 - Wondraczek, K. A1 - Wondraczek, L. T1 - Precise Real‐Time Measurement of Liquid Viscosity Using Digital Video Data N2 - Quantitative knowledge of liquid viscosity is of fundamental importance in many areas of materials synthesis and processing. However, the determination of viscosity often relies on specialized experimental equipment, offline experimentation, or invasive procedures, in particular when required in extreme conditions such as at high temperature, high pressure, and in confined or corrosive environments. Here, this study proposes and validates a fast and simple method that mimics the intuitive perception of liquid flow within a quantitative framework. For this, this study employs digital video observation to derive quantitative values of the shear viscosity of liquids, with high precision and rapid acquisition rates. The technique involves capturing liquid dynamics after minor mechanical stimulation. Processed imaging data are indexed by similarity and referenced to a digital database generated with a finite element model, from which values of viscosity are obtained in line. The approach is tested on water at room temperature and on a high‐temperature glass melt. Covering a viscosity range of four orders of magnitude, both yield convincing agreement with tabulated reference data at low computational cost. KW - Glass KW - Liquid Viscosity KW - Digital Video Data KW - Finite Element Method PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-651363 DO - https://doi.org/10.1002/aisy.202500297 SN - 2640-4567 VL - 7 IS - 12 SP - 1 EP - 12 PB - Wiley VHC-Verlag AN - OPUS4-65136 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Eichelbaum, M. A1 - Rademann, K. A1 - Müller, Ralf A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Görner, Wolf T1 - Vom Atom zum Nanodraht: Kontrolliertes Wachstum von Edelmetall-Nanokristalliten in Kalk-Natron-Silikatglas T2 - 79. Glastechnische Tagung CY - Würzburg, Deutschland DA - 2005-05-23 KW - Glas KW - Metallnanocluster KW - Optische Eigenschaften PY - 2005 SN - 3-921089-43-3 SP - 15 Seiten PB - Deutsche Glastechnische Gesellschaft CY - Offenbach AN - OPUS4-7558 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Prewitz, Marc A1 - Müller, Ralf A1 - Marotzke, Christian A1 - Holtappels, Kai T1 - Characterization of glass capillary storage modules considering permeability and mechanical stress via finite elements N2 - Glass capillaries are potential candidates for long term hydrogen storage under high pressure. Burst pressure strongly drops with surface damaging, a polymer coating is needed. The aim is to study stress distribution within single coated glass capillaries sealed to metal fittings T2 - 88. Glastechnische Tagung DGG – ACerS GOMD 2014 CY - Aachen, Germany DA - 25.05.2014 KW - Burst test KW - Hydrogen storage KW - Polymer coating PY - 2014 AN - OPUS4-35784 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 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 - Welter, T. A1 - Marzok, Ulrich A1 - Deubener, J. A1 - Reinsch, Stefan A1 - Müller, Ralf T1 - Hydrogen diffusivity in sodium aluminosilicate glasses N2 - Hydrogen gas diffusivity of fourteen glasses of the Na2O-Al2O3-SiO2 system are studied along the joins quartzalbite-jadeite-nepheline (Qz-Ab-Jd-Np, fully polymerized) and albite-sodium disilicate (Ab-Ds, depolymerized). Density measurements show that ionic porosity decreases from 54.4% (Qz) to 51.5% (Np) and from 52.4% (Ab) to 50.2% (Ds). Hydrogen diffusivity D follows similar trends but at another scale. D at 523 K decreases from 4×10−12 to 3×10−14m2 s−1 (Qz-Np) and from 4×10−13 to 3×10−15m2 s−1 (Ab-Ds). Charge compensating Na+ acting as a filling agent in fully polymerized network structures leads to up to one order of Magnitude higher diffusivities as depolymerized glass structures of the same SiO2 content where Na+ takes the role of a modifier ion. Temperature dependence of the diffusivity indicates that both the activation energy involved with the moving H2 molecule as well as the accessible volume in the structure contribute to this compositional trend. KW - Aluminosilicate glasses KW - Hydrogen diffusivity KW - Ionic porosity PY - 2019 DO - https://doi.org/10.1016/j.jnoncrysol.2019.119502 VL - 521 SP - 119502 PB - Elsevier B.V. AN - OPUS4-50392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kiefer, P. A1 - Deubener, J. A1 - Müller, Ralf A1 - Behrens, H. T1 - Statistical analysis of propagation rates of indentation-induced radial cracks N2 - Due to the stochastic nature of crack nucleation by Vickers indentation, a statistical analysis of propagation rates of 185 radial cracks was performed. Crack growth was observed directly using a video camera with high Image acquisition rate. It is found that propagation rates are controlled by the environmental reactions at the crack-tip shortly after their initiation (< 1 s). Calibration of the stress intensity KI showed that the residual stress factor χ and the exponent n of the equation KI==χPc−n (with P==load and c==crack length) are broadly distributed among the 185 analyzed cracks, ranging from 10−16 to 104 and from 0.1 to 5, respectively. For the most frequent crack, the equation KI==0.052Pc−1.47 holds. The results show that correlations of indentation-induced crack length to stress intensity necessitate the use of statistical significant data that are calibrated by the environmental reactions at the crack-tip. KW - Stress intensity factor KW - Vickers indentation KW - Subcritical crack growth KW - Soda-lime-silica glass PY - 2019 DO - https://doi.org/10.1016/j.jnoncrysol.2019.119739 VL - 527 SP - 119739 PB - Elsevier B.V. AN - OPUS4-50393 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 - Dynamic Mechanical Analysis (DMA): Viscoelasticity N2 - Der Vortrag gibt einen Überblick über die am FB 56 der BAM betriebene Dynamisch-Mechanische Analyse mit dem Schwerpunkt auf Anwendungen für Glas N2 - The talk presents an overview over the method of Dynamic Mechanical Analysis used at the BAM division 5.6 Glass mainly focussed on glasses. T2 - Seminar Instrumentelle Analytik, Fakultät III Prozesswissenschaften, Lehrstuhl Keramik TU Berlin CY - Berlin, Germany DA - 25.01.2019 KW - Dynamisch Mechanische Analyse KW - Dynamic mechanical analysis KW - Glas PY - 2019 AN - OPUS4-50436 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Vacuum hot extraction: Detection of volatiles N2 - Der Vortrag gibt einen Überblick über die Möglichkete und Grenzen der Methode der Vakuum-Heiß-Extraktion an der BAM T2 - Seminar Instrumentelle Analytik, Fakultät III Prozesswissenschaften, Lehrstuhl Keramik TU Berlin CY - Berlin, Germany DA - 25.01.2019 KW - Heißgasextraktion KW - Glas PY - 2019 AN - OPUS4-50434 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Balzer, R. A1 - Behrens, H. A1 - Schuth, S. A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Fechtelkord, M. A1 - Deubener, J. T1 - The influence of H2O and SiO2 on the structure of silicoborate glasses N2 - To understand the impact of dissolved water on structure and properties, four boron-rich glasses of molar compositions 15-x Na2O x CaO 15 SiO2 70 B2O3 (with x=0, 7.5, 10) and 10 Na2O 15 SiO2 75 B2O3 were prepared and subsequently hydrated (up to 8 wt% H2O). Density measurements show a non-linear trend upon hydration implying large structural changes in particular at water contents<2 wt%. Near-infrared spectroscopy shows hydroxyl groups are the dominant species in all glasses upon the entire range of water content. Molecular H2O is detectable only at total water contents>2 wt%. 11B MAS NMR spectra show that the abundance of BO4 species is mainly controlled by ratio of (Na2O+CaO)/B2O3 while incorporation of water plays a minor role. Compared to borate glasses, the efficiency of formation of BO4 tetrahedra is favored by crosslinking of the network by SiO4-units. The glass transition temperatures, determined by differential thermal analysis, decreases continuously with water content due to breakage of B-O-B bonds by hydrolysis. However, compared to Silicates and aluminosilicates, the effect of dissolved water is less pronounced which can be explained by weaker B-O-B bonds in comparison to Si-O-Si bonds. KW - High pressure KW - Water speciation KW - Silicoborate glasses KW - Infrared spectroscopy KW - NMR spectroscopy PY - 2019 DO - https://doi.org/10.1016/j.jnoncrysol.2019.05.030 VL - 519 SP - 38 EP - 51 PB - Elsevier B.V. AN - OPUS4-48748 LA - eng 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 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 - Waurischk, Tina A1 - Müller, Ralf T1 - Subcritical crack growth in hydrous soda-lime silicate glass N2 - Glass strength and fatigue is limited by surface cracks. As subcritical crack growth (SCCG) is governed by ambient humidity, stress corrosion at the crack tip is widely accepted to be the underlying mechanism. However, as water is known to have decisive effect on glass properties and can rapidly enter the crack tip near glass region, SCCG could be affected by such water related phenomena. We tried to mimic these effects studying water dissolution and speciation, mechanical properties, and SCCG in water-bearing glasses. For this purpose, glasses up to 8 wt% water have been prepared by means of high-pressure melting of glass powder - water mixtures. As part of this effort, SCCG in dry and hydrous commercial micros¬cope slide glass (CW = 6 wt%) was studied in double cantilever beam (DCB) geometry and sub-Tg relaxation was measured by Dynamic Mechanical Analysis (DMA). For SCCG in ambient air (24% r.h.), SCCG was promoted by the presence of 6wt% bulk water with respect to the dry glass. On the other hand, stress intensity values, KI, required to cause slow crack growth (v < 10-6 ms-1) resemble literature findings for float glass of similar composition in liquid water, which might represent the maximum possible promoting effect of ambient water on SCCG. For SCCG in vacuum (10-3 mbar), dissolved bulk water causes even more pronounced effects. Most strikingly, it strongly decreases the slope of the log v(KI)-curve, which is a measure of dissipated energy during fracture. A strong increase of sub-Tg relaxation with increasing water content was confirmed by DMA. As a consequence, slow crack growth occurs at KI values as measured in the dry glass whereas fast crack growth occurs at much larger KI than that of the dry glass. Kinks and shoulders shown by the inert log v(KI)-curve indicate that bulk water does not simply affect bulk mechanical properties. T2 - 9th Otto Schott Colloquium CY - Jena, Germany DA - 09.09.2019 KW - Internal friction KW - Soda-lime silicate glass KW - Crack growth KW - Water content KW - DCB PY - 2019 AN - OPUS4-49534 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Akatsuka, C. A1 - Honma, T. A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Tanaka, S. A1 - Komatsu, T. T1 - Surface crystallization and gas bubble formation during conventional heat treatment in Na2MnP2O7 glass N2 - The crystallization behavior of sodium ion conductive Na2MnP2O7 glass was examined to clarify the crystallization mechanism. The formation of thermodynamically metastable phase, layered Na2MnP2O7, at the surface of the glass occurred. Heat treatment at 430 °C for 3 h lead to surface crystals of Na2MnP2O7 oriented with the (101) direction perpendicular to the sample surface. As the heat treatment temperature increased, the glass-ceramic samples deformed, and the presence numerous micro bubbles due to dissolved water was detected. KW - Glass-ceramic KW - Crystallization KW - Sodium ion batteries KW - Bubble formation KW - Phosphate PY - 2019 DO - https://doi.org/10.1016/j.jnoncrysol.2019.01.030 VL - 510 SP - 36 EP - 41 PB - Elsevier B.V. AN - OPUS4-49618 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Blaeß, Carsten A1 - Müller, Ralf A1 - Poologasundarampilai, G. A1 - Brauer, D. S. T1 - Sintering and concomitant crystallization of bioactive glasses N2 - The sintering of bioactive glasses allows for the preparation of complex structures, such as three‐dimensional porous scaffolds. Such 3D constructs are particularly interesting for clinical applications of bioactive glasses in bone regeneration, as the scaffolds can act as a guide for in‐growing bone cells, allowing for good Integration with existing and newly formed tissue while the scaffold slowly degrades. Owing to the pronounced tendency of many bioactive glasses to crystallize upon heat treatment, 3D scaffolds have not been much exploited commercially. Here, we investigate the influence of crystallization on the sintering behavior of several bioactive glasses. In a series of mixed‐alkali glasses an increased CaO/alkali metal oxide Ratio improved sintering compared to Bioglass 45S5, where dense sintering was inhibited. Addition of small amounts of calcium fluoride helped to keep melting and sintering temperatures low. Unlike glass 13‐93, these new glasses crystallized during sintering but this did not prevent densification. Variation in bioactive glass particle size allowed for fine‐tuning the microporosity resulting from the sintering process. KW - Bioactive glass KW - Crystallization KW - Scaffolds KW - Sintering PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-485458 DO - https://doi.org/10.1111/ijag.13477 SN - 2041-1286 VL - 10 IS - 4 SP - 449 EP - 462 PB - Wiley AN - OPUS4-48545 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 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 - JOUR A1 - Holzer, Marco A1 - Johansen, Sidsel M. A1 - Christensen, Johan F.S. A1 - Smedskjaer, Morten M. A1 - Cicconi, Maria Rita A1 - de Ligny, Dominique A1 - Müller, Ralf A1 - de Camargo, Andrea S.S. A1 - Maaß, Robert T1 - Direct connection between secondary relaxation mode and fracture toughness in alkali-aluminosilicate glasses N2 - Oxide glasses are intrinsically brittle, lacking sufficient atomic-scale mechanisms that can relax mechanical stresses in the vicinity of a propagating crack. As a result, fracture is typically well-captured by considering local bond rupture at the crack tip. Here we demonstrate that barrier energies related to the low-temperature 𝛾-relaxation mode in alkali-aluminosilicate glasses are inversely related to the fracture toughness measured via standardized three-point bending fracture experiments. This holds true for both a series with varying cations (Li, Na, K) and one with varying Li concentration. The structural rationale for this finding is gained via Raman spectroscopy. The findings suggest that a fundamental structural relaxation mode measured on bulk specimens can serve as an effective guideline for fracture toughness of oxide glasses. Data for additional silicate glasses support this conclusion. KW - Fracture toughness KW - Oxide glass KW - Mechanical properties KW - Alkali-aluminosilicate glasses KW - Internal friction PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-651540 DO - https://doi.org/10.1016/j.mtadv.2025.100669 SN - 2590-0498 VL - 29 SP - 1 EP - 10 PB - Elsevier Ltd. CY - Amsterdam, Niederlande AN - OPUS4-65154 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 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 - TY - JOUR A1 - Wirth, Cynthia A1 - Müller, Ralf A1 - Günster, Jens A1 - Mühler, T. A1 - Görke, R. A1 - Heinrich, J.G. T1 - Submicrometer silica spheres generated by laser fuming N2 - The production of agglomerate-free SiO2 particles exhibiting a monomodal distribution of particle sizes of around 300 nm by means of direct laser fuming of micrometric SiO2 powders has been successfully demonstrated. With a 12 kW cw CO2 laser system, a production rate of up to 1 kilogram powder per hour was achieved. Almost ideal spherical amorphous SiO2 particles in a broad particle size distribution between 10 nm and several 100 nm (d50 ≈ 300 nm) were synthesized. Several observations suggest weak agglomeration forces between the particles. A temperature reduction of 200 °C for sintering powder compacts was observed. KW - Laser KW - SiO2 KW - Nanopowder PY - 2013 DO - https://doi.org/10.4416/JCST2012-00033 SN - 2190-9385 N1 - Geburtsname von Wirth, Cynthia: Gomes, C. M. - Birth name of Wirth, Cynthia: Gomes, C. M. VL - 4 IS - 1 SP - 11 EP - 18 PB - Göller CY - Baden-Baden AN - OPUS4-31423 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 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 - JOUR A1 - Zocca, Andrea A1 - Wirth, Cynthia A1 - Bernardo, E. A1 - Müller, Ralf A1 - Günster, Jens A1 - Colombo, P. T1 - LAS glass-ceramic scaffolds by three-dimensional printing N2 - Highly porous (>60% open porosity) glass–ceramic scaffolds with remarkable mechanical properties (compression strength of ~15 MPa) were produced by indirect 3D printing. Precursor glass powders were printed into 3D ordered structures and then heat treated to sinter and develop crystalline phases. The final glass–ceramic contained a β-spodumene solid solution together with a secondary phase of lithium disilicate. The precision of the printed geometry and the density of the struts in the scaffold depended on several processing parameters (e.g. powder size and flowability, layer thickness) and were improved by increasing the binder saturation and drying time. Two types of powders with different particle size distribution (PSD) and flowability were used. Powders with a larger PSD, could be processed within a wider range of printing parameters due to their good flowability; however, the printing precision and the struts density were lower compared to the scaffolds printed using the powder in a smaller average PSD. KW - Glass ceramics KW - Porosity KW - Shaping KW - Strength KW - Additive manufacturing PY - 2013 DO - https://doi.org/10.1016/j.jeurceramsoc.2012.12.012 SN - 0955-2219 SN - 1873-619X N1 - Geburtsname von Wirth, Cynthia: Gomes, C. M. - Birth name of Wirth, Cynthia: Gomes, C. M. VL - 33 IS - 9 SP - 1525 EP - 1533 PB - Elsevier CY - Oxford AN - OPUS4-28284 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peplinski, Burkhard A1 - Adam, Christian A1 - Adamczyk, Burkart A1 - Müller, Ralf A1 - Michaelis, Matthias A1 - Krahl, T. A1 - Emmerling, Franziska T1 - Nanocrystalline and stacking-disordered beta-cristobalite AlPO4: the now deciphered main constituent of a municipal sewage sludge ash from a full-scale incineration facility N2 - For the first time evidence is provided that a nanocrystalline and stacking-disordered, chemically stabilized β-cristobalite form of AlPO4 occurs in a sewage sludge ash (SSA). This proof is based on a combined X-ray powder diffraction and X-ray fluorescence investigation of an SSA produced at a large-scale fluidized bed incineration facility serving a catching area with a population of 2 million. The structural and chemical characterization was carried out on 'as received' SSA samples as well as on solid residues remaining after leaching this SSA in sodium hydroxide solution. Thus, it was ascertained that the observed nanocrystalline and stacking-disordered cristobalite-like component belongs to the aluminum phosphate component of this SSA, rather than to its silicon dioxide component. In addition, a direct proof is presented that the chemically stabilized β-cristobalite form of AlPO4 does crystallize from X-ray amorphous precursors under conditions that mimic the huge heating rate and short retention time (just seconds at T ≈ 850°C), typical for fluidized bed incinerators. KW - Aluminum phosphate KW - Chemical stabilization of high-temperature forms KW - Cristobalite form KW - Stacking disorder KW - Incinerator ash KW - Sewage sludge ash PY - 2015 DO - https://doi.org/10.1017/S0885715614001213 SN - 0885-7156 VL - 30 IS - Supplement S 1 SP - S31 EP - S35 PB - JCPDS CY - Swarthmore, Pa. AN - OPUS4-33435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peplinski, Burkhard A1 - Adam, Christian A1 - Adamczyk, Burkart A1 - Müller, Ralf A1 - Schadrack, Reinhard A1 - Michaelis, Matthias A1 - Emmerling, Franziska A1 - Reuther, H. A1 - Menzel, Michael T1 - Evidence of formation of the tridymite form of AlPO4 in some municipal sewage sludge ashes N2 - Evidence is provided that the tridymite component observed in the X-ray diffraction patterns of some sewage sludge ashes (SSAs) should not be interpreted as the tridymite modification of SiO2 but as the tridymite form of AlPO4. This proof is based on a combined X-ray Powder Diffraction (XRD), X-ray fluorescence (XRF) and Mossbauer spectroscopy investigation of two SSAs produced at two fluidized bed incineration facilities, located in different municipalities and operated differently. The structural and chemical characterization was carried out on the 'as received' SSA samples as well as on the residues of these two SSAs pretreated by leaching in citric acid. In addition, direct proof is presented that the tridymite form of AlPO4 does crystallize from X-ray amorphous precursors under conditions that mimic the huge heating rate and short retention time (just seconds at T ≈ 850 °C) typical for fluidized bed incinerators. KW - Aluminium phosphate KW - Ash KW - Fly ash KW - Incinerator ash KW - Sewage sludge ash KW - Tridymite form PY - 2013 DO - https://doi.org/10.1017/S0885715613000869 SN - 0885-7156 VL - 28 IS - S2 SP - S425 EP - S435 PB - JCPDS CY - Swarthmore, Pa. AN - OPUS4-29703 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -