TY - CONF A1 - Wondraczek, L. A1 - Reinsch, Stefan A1 - Gaber, Martin A1 - Deubener, J. A1 - Müller, Ralf A1 - Komatsu, T. T1 - Nano-crystalline germanate glass-ceramics T2 - 78. Glastechnische Tagung CY - Nürnberg, Deutschland DA - 2004-06-07 PY - 2004 SP - 37 EP - 40 PB - Deutsche Glastechnische Gesellschaft CY - Offenbach AN - OPUS4-6953 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Ralf A1 - Gottschling, Peter A1 - Gaber, Martin T1 - Water concentration and diffusivity in silicates obtained by vacuum extraction KW - Silicate glasses and crystals KW - Water KW - Degassing KW - Diffusion coefficient PY - 2005 SN - 0927-4472 VL - 78 IS - 2 SP - 76 EP - 89 PB - Elsevier CY - Amsterdam AN - OPUS4-11836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Gaber, Martin A1 - Müller, Ralf T1 - Thermal induced release of hydrogen from fused silica T2 - 79. Glastechnische Tagung CY - Würzburg, Deutschland DA - 2005-05-23 PY - 2005 SN - 3-921089-43-3 SP - 4 pages PB - Deutsche Glastechnische Gesellschaft CY - Offenbach AN - OPUS4-11837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Heller, I. A1 - Behrens, H. A1 - Gaber, Martin A1 - Müller, Ralf T1 - Wasserdiffusion in Floatglas T2 - 79. Glastechnische Tagung CY - Würzburg, Deutschland DA - 2005-05-23 PY - 2005 SN - 3-921089-43-3 SP - 4 Seiten PB - Deutsche Glastechnische Gesellschaft CY - Offenbach AN - OPUS4-11838 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Moderne Anwendungen und thermische Eigenschaften von Silicatgläsern T2 - 2. Berlin-Brandenburger Seminar der Wissenschaftsglasbläser des Verbands Deutscher Glasbläser CY - Berlin, Germany DA - 2005-11-18 PY - 2005 AN - OPUS4-11789 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Gaber, Martin A1 - Deubener, J. A1 - Behrens, H. T1 - Viscosität und Wasserabgabeverhalten von Silicatgläsern T2 - Sitzung der Fachausschuss III der Deutschen Glastechnischen Gesellschaft (DGG) CY - Würzburg, Germany DA - 2005-10-12 PY - 2005 AN - OPUS4-11790 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Gaber, Martin T1 - Water concentration and diffusivity obtained by vacuum hot extraction T2 - Meeting 2005 des TC 14 der International Commision on Glass (ICG) CY - Parma, Italy DA - 2005-09-16 PY - 2005 AN - OPUS4-11791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Marzok, Ulrich A1 - Müller, Ralf A1 - Krauhausen, M. A1 - Burgstedt, F. A1 - Brode, W. T1 - Hochtemperatur shape screening keramischer Bauteile KW - Keramikherstellung KW - Sintern KW - Formmessung KW - Kontur KW - Lasermesstechnik PY - 2010 UR - http://edok01.tib.uni-hannover.de/edoks/e01fb12/685831345.pdf IS - Schlussbericht / Az: II D 5 - 25/06 SP - 1 EP - 54 CY - Berlin AN - OPUS4-28373 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Marzok, Ulrich A1 - Müller, Ralf A1 - Schadrack, Reinhard A1 - Krauhausen, M. A1 - Burgstedt, F. A1 - Brode, W. A1 - Reetz, R. T1 - High-temperature laser profilometry for ceramic tapes N2 - Advanced ceramics are promising key components for microsystems engineering, communication Technology and medical engineering. Driven by steadiiy increasing demands on dimensional accuracy of components and Integration density, sintering has to be controlled at an unprecedented degree of precision. Being most crucial for components of complex shape, graded or heterogeneous-composed parts like LTCC multilayers for microsystems, precise control of sintering has a decisive influence on the dimensional accuracy, mechanical integrity and reliability of sintered components. Thus, permanent or temporary shape distortions or warping during sintering may result from spatially heterogeneous microstructure and temperature distribution, e.g. during the co-firing process of green multilayer Stacks printed with metallization and other functional pastes. Whereas permanent warping can be easily measured after sintering, temporary warping during firing is more difficult to measure. Nonetheless, this effect may cause latent failures later, which often limit the applicability of ceramic components. PY - 2013 SN - 0173-9913 SN - 0196-6219 VL - 90 IS - 4 SP - E35 EP - E40 PB - Göller CY - Baden-Baden AN - OPUS4-28500 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Marzok, Ulrich A1 - Müller, Ralf A1 - Schadrack, Reinhard A1 - Krauhausen, M. A1 - Burgstedt, F. A1 - Brode, W. A1 - Reetz, R. T1 - Hochtemperatur-Laserprofilometrie an keramischen Bauteilen N2 - Hochleistungssinterwerkstoffe spielen eine wachsende Rolle in derzeitigen Schlüsseltechnologien wie der Mikrosystem-, Informations-, Kommunikations- und Medizintechnik. Dabei steigen die Anforderungen an die präzise Steuerung der Sinterung. Besonders für komplexe, gradierte oder heterogen zusammengesetzte Formkörper wie zum Beispiel keramische LTCC-Multilayer für die Mikrosystemtechnik hat die exakte Beherrschung dieses Prozessschrittes wesentlichen Einfluss auf die Maßhaltigkeit, mechanische Integrität und Zuverlässigkeit der gesinterten Bauteile. Bedingt durch die Heterogenität der mehrlagigen und mit Leit- und anderen Funktionspasten bedruckten Sinterkörper hinsichtlich ihrer sinterphysikalischen oder thermischen Eigenschaften können bleibende oder temporäre Verwerfungen beim Schrumpfungsprozess auftreten, wobei letztere unter Umständen Ursache latenter Fehler im späteren Bauteil sind. PY - 2013 SN - 0173-9913 SN - 0196-6219 VL - 90 IS - 3 SP - D19 EP - D24 PB - Göller CY - Baden-Baden AN - OPUS4-28013 LA - deu 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 - Nagamine, K. A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Honma, T. A1 - Komatsu, T. T1 - Crystallization behavior of lithium iron phosphate glass powders in different atmospheres N2 - Crystallization behavior in different atmospheres (air, Ar, and 7% H2/Ar) of lithium iron phosphate glass (33Li2O–33Fe2O3–1Nb2O5–33P2O5 (LFNP)) powders with different sizes of 2–1000 µm was examined. The crystallization peak temperature (Tp) in Ar and 7% H2/Ar decreased with decreasing the particle size of glass powders, but the value of Tp in air was independent of particle size. The crystallized glass obtained by heating to Tp showed the formation of the α-Li3Fe2(PO4)3 and LiFePO4 crystalline phases. Fe2O3 crystals were formed only in the inside of crystallized glass plates in the heating in air. The crystallization of LiFePO4 was largely enhanced in the particle size of <2 µm during the heating in Ar and 7% H2/Ar atmospheres. The main crystallization mechanism in LFNP glass was found to be surface crystallization. Significant shrinkages were observed for glass compacts (pellets) in the heating in 7% H2/Ar. These results suggest that controlling particle sizes and atmospheres enables the design the morphology of LiFePO4 crystals in LFNP glass. KW - DTA KW - Kristallisation KW - Phasenentwicklung KW - Unterschiedliche Atmosphären KW - Lithiumionen-Batterie PY - 2011 DO - https://doi.org/10.1111/j.1551-2916.2011.04579.x SN - 0002-7820 SN - 1551-2916 VL - 94 IS - 9 SP - 2890 EP - 2895 PB - Blackwell Publishing CY - Malden AN - OPUS4-24914 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Glas und Keramik für Schlüsseltechnologien - Prozessbegleitende Prüfverfahren und Simulation T2 - Sommerkolloquium 2012 des Instituts für Gesteinshüttenkunde des RWTH Aachen CY - Aachen, Germany DA - 2012-06-21 PY - 2012 AN - OPUS4-27421 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Eberstein, Markus A1 - Deubener, J. T1 - Sintering kinetcs of GMC with small rigid inclusions T2 - 10th. Int. Symp. Ceram. Mat. and Components for Energy and Environmental Applications CY - Dresden, Germany DA - 2012-05-20 PY - 2012 AN - OPUS4-27423 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Glaspulver - Processing, Effekte, Möglichkeiten T2 - 1. Fachtagung "Starkes Glas - Herausforderungen für zukünftige Glasanwendungen" CY - Weimar, Germany DA - 2012-05-07 PY - 2012 AN - OPUS4-27419 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Volatile Concentration and Mobility measured by VHE-MS T2 - International Conference on Materials Science CY - Ulaanbaatar, Mongolia DA - 2012-08-20 PY - 2012 AN - OPUS4-27420 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eberstein, Markus A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Rabe, Torsten A1 - Schiller, Wolfgang Arno A1 - Thiel, A. A1 - Deubener, J. T1 - Kinetic Modeling of LTCC-Shrinkage T2 - 3rd International Conference and Exhibition on Ceramic Interconnect and Ceramic Microsystems Technologies (CICMT 2007) CY - Denver, CO, USA DA - 2007-04-23 KW - LTCC KW - Glass matrix composites KW - Inclusions KW - Sintering kinetics KW - Modeling PY - 2007 SP - 1 EP - 8 PB - American Ceramic Soc. CY - Denver AN - OPUS4-14948 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Eberstein, Markus A1 - Deubener, J. A1 - Thiel, A. A1 - Schiller, Wolfgang Arno T1 - Effects of dispersed Al2O3 particles on sintering of LTCC T2 - 9th ESG Conf. with the Annual Meeting of the ICG Glass - The challenge for the 21st century CY - Trencín, Slovakia DA - 2008-06-22 PY - 2008 AN - OPUS4-16688 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Apel, E. A1 - Deubener, J. A1 - Bernard, A. A1 - Müller, Ralf A1 - Kappert, H. A1 - Rheinberger, V. A1 - Höland, W. T1 - Phenomena and mechanisms of crack propagation in glass-ceramics N2 - Lithium disilicate, leucite and apatite glass-ceramics have become state-of-the-art framework materials in the fabrication of all-ceramic dental restorative materials. The goal of this study was to examine the crack propagation behaviour of these three known glass-ceramic materials after they have been subjected to Vickers indentation and to characterize their crack opening profiles (δmeas vs. (a-r)). For this purpose, various methods of optical examination were employed. Optical microscopy investigations were performed to examine the crack phenomena at a macroscopic level, while high-resolution techniques, such as scanning electron microscopy (SEM) and atomic force microscopy (AFM), were employed to investigate the crack phenomena at a microscopic level. The crack patterns of the three glass-ceramics vary from fairly straightforward to more complex, depending on the amount of residual glass matrix present in the material. The high-strength lithium disilicate crystals feature a high degree of crosslinking, thereby preventing crack propagation. In this material, the crack propagates only through the residual glass phase, which constitutes 30%–40% by volume. Having a high glass content of more than 65% by volume, the leucite and apatite glass-ceramics show far more complex crack patterns. Cracks in the leucite glass-ceramic propagate through both the glass and crystal phase. The apatite glass-ceramic shows a similar crack behaviour as an inorganic–organic composite material containing nanoscale fillers, which are pulled out in the surroundings of the crack tip. The observed crack behaviour and the calculated View the MathML source values of the three types of glass-ceramics were compared to the Kkic values determined according to the SEVNB method. KW - Glass KW - Viscosity KW - Water content PY - 2008 DO - https://doi.org/10.1016/j.jmbbm.2007.11.005 SN - 1751-6161 VL - 1 IS - 4 SP - 313 EP - 325 PB - Elsevier CY - Amsterdam AN - OPUS4-18308 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Gaber, Martin A1 - Gottschling, Peter T1 - Water release from silicate glass powders T2 - 7. International Otto Schott Colloquium CY - Jena, Germany DA - 2002-07-09 PY - 2002 AN - OPUS4-6204 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Untersuchungen zur Sinterfahigkeit von Glaspulvern T2 - Physikalisches Kolloquium des Lehrnstuhls für Anorganische Chemie der Brandenburgischen Universität Cottbus CY - Cottbus, Germany DA - 2002-06-11 PY - 2002 AN - OPUS4-6205 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eberstein, Markus A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Rabe, Torsten A1 - Schiller, Wolfgang Arno A1 - Thiel, A. A1 - Deubener, J. T1 - Kinetic Modeling of LTCC Shrinkage: Effect of Alumina Content N2 - We studied sintering of LTCC-type glass matrix composites (GMCs) consisting of small glass and alumina particles of equal size. Primarily, crystals act as rigid inclusions, decelerating the densification rate. In later stages, they also dissolve, partially increasing the viscosity. Release of alumina finally induces crystallization of alumosilicates, which enables post-firing stability. To study both effects, two model GMCs were prepared: an α-Al2O3 + barium alumoborosilicate glass (BABS)–GMC, which shows neither significant dissolution nor crystallization, and an α-Al2O3 + calcium alumoborosilicate glass (CABS)–GMC, which dissolves readily and promotes crystallization. The kinetics of shrinkage for both GMC were modeled by utilizing Frenkel theory for the early stage and Mackenzie–Shuttleworth theory for the late stage, assuming that sintering is superimposed by the weighted contributions of triparticle glass–crystal clusters, their random occurrence (ideal mixing), and a shrinkage rate controlled by the GMC effective viscosity. In agreement with modeling, the experimental results showed that the shrinkage rate of BABS–GMC decreases progressively for crystal volume fractions Φ > 0.15. The attainable shrinkage is reduced by up to 8% for Φ = 0.45. For the CABS–GMC with Φ = 0.25, a reduction of Φ to 0.20 was evident due to partial α-Al2O3 dissolution. This effect was found able to increase the sintering temperature by ~50–60 K. KW - LTCC KW - Glas Matrix Composites KW - Inclusions KW - Sintering Kinetics KW - Modeling PY - 2007 SN - 1551-4897 VL - 4 IS - 4 SP - 173 EP - 180 CY - Washington, DC AN - OPUS4-16506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Eberstein, Markus A1 - Deubener, J. A1 - Thiel, A. A1 - Schiller, Wolfgang Arno ED - J.G. Heinrich, ED - C.G. Aneziris, T1 - Effect of dispersed Al2O3 particles on sintering of glass matrix composites T2 - 10th International Conference of the European Ceramic Society CY - Berlin DA - 2007-06-17 KW - LTCC KW - Glass matrix composites KW - Inclusions KW - Sintering kinetics KW - Modelling PY - 2007 SN - 3-87264-022-4 SP - 290 EP - 295 PB - Göller CY - Baden-Baden AN - OPUS4-17445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Deubener, J. T1 - Crystallization in multicomponent systems. Glasses for LTCC T2 - Meeting 2008 des TC7 der ICG am Rande der 9th ESG Conf. with the Annual Meeting of the ICG Glass-The challenge for the 21st century CY - Trencín, Slovakia DA - 2008-06-22 PY - 2008 AN - OPUS4-18106 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Eberstein, Markus A1 - Deubener, J. A1 - Thiel, A. A1 - Schiller, Wolfgang Arno T1 - Effects of dispersed Al2O3 particles on sintering of LTCC N2 - The sintering of Low Temperature Co-fired Ceramics prepared from alumoborosilicate glass- and Al2O3 powders of similar small particle size was studied by dilatometry, heating microscopy, microstructure analysis, glass- and effective viscosity measurements. The steric effect of Al3O3 inclusions was studied using a gnon-reactiveh model composite. With increasing Al3O3 volume fraction (Φ ≤ 0.45), sintering decelerates and its final stage shifts to higher temperature. The attainable shrinkage is reduced as Al2O3 particle clusters bearing residual pores become more frequent. The kinetics of sintering could be described formally superposing the weighed contributions of differentially sized and randomly composed glass-crystal particle clusters and assuming a sintering rate controlled by the effective matrix viscosity, which increases with Φ and with progressive wetting of Al2O3 particles during densification. The "reactive" model composite shows significant dissolution of Al2O3 into the glass, which has two opposed effects on sintering: reducing Φ and increasing glass viscosity. For the present case (Φ = 0.25), the latter effect dominates and sintering is retarded by Al2O3 dissolution. Crystallization of wollastonite starts after full densification. Dissolution of Al2O3 was found to promote the subsequent growth of anorthite. KW - LTCC KW - Glass matrix composites KW - Al2O3-inclusions KW - Sintering kinetics PY - 2005 SN - 1022-6680 SN - 1662-8985 VL - 39-40 SP - 375 EP - 380 PB - Trans Tech Publ. CY - Zurich AN - OPUS4-18441 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zietka, S. A1 - Deubener, J. A1 - Behrens, H. A1 - Müller, Ralf T1 - Glass transition and viscosity of hydrated silica glasses N2 - The viscosity of silica glasses with different water contents was measured by penetration of sapphire microspheres in the range from 1012-1014·7 Pas at ambient pressure. Commercial silica glasses were used together with hydrous silica glasses, which were prepared by melting glass powder plus water in an internally heated pressure vessel at 2-3 kbar and 1350-1450°C. The temperature dependence of the viscosity of silica glasses with total water contents Cw of 5·4×10-4, 7·0×10-4, 1·00×10-2, and 1·55×10-2(Cw in mass fractions) can be described by Arrhenius equations. From the results, the linear dependence of the T12 isokom (K) with the logarithm of the water content was determined as T12=192-409 logCw. The analysis of the compositional dependence of the T12 isokom in the H2O-Na2O-SiO2 system reveals a temperature depression of up to 200 K for mixed water- and sodium-bearing glasses compared to H2O-SiO2 and Na2O-SiO2 glasses with same molar silica content. From these findings we conclude that protons may contribute significantly to the mixed alkali effect in glasses. KW - Wassergehalt KW - Silicatgläser KW - Viskosität PY - 2007 SN - 1753-3562 SN - 0017-1050 SN - 0031-9090 SN - 1750-6697 VL - 48 IS - 6 SP - 380 EP - 387 PB - Society of Glass Technology CY - Sheffield AN - OPUS4-18396 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reinsch, Stefan A1 - Nascimento, M.L.F. A1 - Müller, Ralf A1 - Zanotto, E. D. T1 - Crystal growth kinetics in cordierite and diopside glasses in wide temperature ranges N2 - We measured and collected literature data for the crystal growth rate, u(T), of µ-cordierite (2MgO · 2Al2O3 · 5SiO2) and diopside (CaO · MgO · 2SiO2) in their isochemical glass forming melts. The data cover exceptionally wide temperature ranges, i.e. 800–1350 °C for cordierite and 750–1378 °C for diopside. The maximum of u(T) occurs at about 1250 °C for both systems. A smooth shoulder is observed around 970 °C for µ-cordierite. Based on measured and collected viscosity data, we fitted u(T) using standard crystal growth models. For diopside, the experimental u(T) fits well to the 2D surface nucleation model and also to the screw dislocation growth mechanism. However, the screw dislocation model yields parameters of more significant physical meaning. For cordierite, these two models also describe the experimental growth rates. However, the best fittings of u(T) including the observed shoulder, were attained for a combined mechanism, assuming that the melt/crystal interface growing from screw dislocations is additionally roughened by superimposed 2D surface nucleation at large undercoolings, starting at a temperature around the shoulder. The good fittings indicate that viscosity can be used to assess the transport mechanism that determines crystal growth in these two systems, from the melting point Tm down to about Tg, with no sign of a breakdown of the Stokes–Einstein/Eyring equation. KW - Crystal growth KW - Oxide glasses KW - Silicates KW - Kristallwachstumsgeschwindigkeit KW - Kinetik KW - Silikatgläser PY - 2008 DO - https://doi.org/10.1016/j.jnoncrysol.2008.09.007 SN - 0022-3093 VL - 354 IS - 52-54 SP - 5386 EP - 5394 PB - North-Holland Publ. Co. CY - Amsterdam AN - OPUS4-18383 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 - JOUR A1 - Müller, Ralf A1 - Eberstein, Markus A1 - Reinsch, Stefan A1 - Schiller, Wolfgang Arno A1 - Deubener, J. A1 - Thiel, A. T1 - Effect of rigid inclusions on sintering of low temperature co-fired ceramics KW - Sintering KW - Glass Matrix Composites KW - Rigid Inclusion KW - Effective Viscosity KW - Kinetic Modelling KW - LTCC PY - 2007 SN - 1753-3562 SN - 0017-1050 SN - 0031-9090 SN - 1750-6697 VL - 48 IS - 4 SP - 259 EP - 266 PB - Society of Glass Technology CY - Sheffield AN - OPUS4-16211 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Thiel, A. A1 - Eberstein, Markus A1 - Müller, Ralf A1 - Deubener, J. T1 - Viskosität von Glasmatrix-Kompositen mit partiell löslicher kristalliner Dispersphase T2 - 81. Glastechnische Tagung und 4. DGG-Symposium "Novel Optical Technologies" CY - Aachen, Deutschland DA - 2007-06-04 KW - Glasmatrixkomposite KW - Lösung KW - Sintern PY - 2007 SN - 978-3-921089-52-1 IS - CD-ROM SP - 1 EP - 8 PB - Deutsche Glastechnische Gesellschaft CY - Offenbach AN - OPUS4-16212 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Thiel, A. A1 - Eberstein, Markus A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Deubener, J. A1 - Schiller, Wolfgang Arno T1 - Viskosität von sinternden Glas/Kristallphasen-Kompositen T2 - 80. Glastechnische Tagung CY - Dresden, Deutschland DA - 2006-06-12 PY - 2006 SN - 3-921089-46-8 SP - 1(?) EP - 3(?) PB - Verl. d. Dt. Glastechn. Ges. CY - Offenbach AN - OPUS4-14045 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Eberstein, Markus A1 - Thiel, A. A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Deubener, J. A1 - Schiller, Wolfgang Arno T1 - Sinterkinetik von Glasmatrix-Kompositen mit reaktiver Dispersphase T2 - 80. Glastechnische Tagung CY - Dresden, Deutschland DA - 2006-06-12 PY - 2006 SN - 3-921089-46-8 SP - 4 Seiten PB - Verl. d. Dt. Glastechn. Ges. CY - Offenbach AN - OPUS4-14046 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Viscosity and degassing of hydrous silicate glasses T2 - 80. Glastechnische Tagung und 8th Int. Conference "Advances in Fusion and Processing of Glass" CY - Dresden, Germany DA - 2006-06-12 PY - 2006 AN - OPUS4-14259 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Reinsch, Stefan T1 - DMTA measurements on PTR glasses T2 - TC7, International Commission on Glass CY - Jena, Germany DA - 2006-07-23 PY - 2006 AN - OPUS4-14243 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Eberstein, Markus A1 - Thiel, A. A1 - Reinsch, Stefan A1 - Deubener, J. A1 - Schiller, Wolfgang Arno T1 - Sintering of glass matrix composites for LTCC applications T2 - 8th International Symposium Crystallization, American Ceramic Society CY - Jackson, WY, USA DA - 2006-09-24 PY - 2006 AN - OPUS4-14245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Reinsch, Stefan A1 - Meng, S. A1 - Eberstein, Markus A1 - Thiel, A. A1 - Müller, Ralf A1 - Deubener, J. T1 - Partial Solution of Dispersed alpha-Al2O3-Particles in Alumoborosilicate Glass T2 - 81. Glastechnische Tagung CY - Aachen, Deutschland DA - 2007-06-04 KW - Glasmatrixkomposite KW - Lösung KW - Sintern PY - 2007 SN - 978-3-921089-52-1 IS - CD-ROM SP - 1 EP - 5 PB - Deutsche Glastechnische Gesellschaft CY - Offenbach AN - OPUS4-16108 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Moraes, Flavia A1 - Müller, Wolfgang A1 - Frischat, G.H. A1 - Müller, Ralf T1 - Corrosion and crystallization at the inner surfaces of glass bricks N2 - Glass bricks are important transparent building materials. They are produced by joining two halves of glass pressings at 600–700 °C. During this production process alkali oxides evaporate and are redeposited at the cooler inner front surfaces of the bricks. This surface layer reacts with H2O and CO2 from the residual brick atmosphere, leading to the formation of an alkali-rich silicate-hydrate layer of ≥50 nm thickness, which could be evidenced leading to a reduced nano-hardness of similar thickness, and from which NaHCO3 crystals can finally grow. Climate chamber experiments (repeated cooling between at -8 and -14 °C and reheating to 0 to 15 °C) resulted in reversible NaHCO3 crystallization and redissolution, presumably influenced by water evaporation or condensation and driven by the NaHCO3 supersaturation of the silicate-hydrate layer. Depending on the time–temperature schedule, different crystal morphologies became visible in this closed system, e.g. isolated spherical crystals, crystals arranged in chains and in double-chains, respectively, which can limit already the transmittance of the glass bricks. When a crack occurs or the brick is opened, the hygroscopic NaHCO3 crystals take up more H2O from the ambient, react irreversibly with the glass surface, finally leading to a total loss of transmittance. KW - Chemical properties KW - Chemical durability KW - Corrosion KW - Crystallization KW - Crystal growth KW - Nucleation KW - Glasses KW - Mass spectroscopy KW - Mechanical properties KW - Hardness KW - Indentation KW - Microindentation KW - Microscopy KW - Optical microscopy KW - Scanning electron microscopy KW - Optical properties KW - Optical spectroscopy KW - Oxide glasses KW - Alkali silicates KW - Soda-lime-silica KW - Surfaces and interfaces PY - 2008 DO - https://doi.org/10.1016/j.jnoncrysol.2007.07.086 SN - 0022-3093 VL - 354 IS - 2-9 SP - 284 EP - 289 PB - North-Holland Publ. Co. CY - Amsterdam AN - OPUS4-16433 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schiller, Wolfgang Arno A1 - Müller, Ralf A1 - Rabe, Torsten ED - R. Clasen, ED - M. Herrmann, ED - Roosen, A. T1 - Über das Sintern von LTCC KW - LTCC KW - Komposite KW - Multilayer-Technik KW - Sintern KW - Simulation PY - 2007 SN - 0177-6983 VL - 21 IS - 1 SP - 41 EP - 46 PB - Göller CY - Baden-Baden AN - OPUS4-16428 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reinsch, Stefan A1 - Gaber, Martin A1 - Müller, Ralf A1 - Schiller, Wolfgang Arno T1 - Rate controlled debindering of glass ceramic composites N2 - Green compacts of ceramics, glass ceramic composites and sinter glass ceramics contain different amounts of organic materials added as pressing aids or binders. Before sintering, these organics have to burn out completely. In oxidising atmospheres, the debindering process is mostly exothermic and therefore difficult to control. This uncontrolled heat production due to locally enhanced debindering and respective gas release may cause damages in the green compact microstructure. Therefore, debindering is usually operated with very low heating rates (< 3 K/min) which requires long processing times of many hours. In this paper, we will show that it is possible to reduce the processing time for debindering dramatically by using the decomposition rate of the organic binder, detected by the weight loss of the sample, as a control factor of the furnace. T2 - 9th ESG (European Society of Glass) Conference with the Annual Meeting of the ICG Glass - "The challenge for the 21st century" CY - Trencin, Slovakia DA - 2008-06-22 KW - Debindering KW - Thermo gravimetry KW - Glass ceramic composites PY - 2005 SN - 1022-6680 SN - 1662-8985 VL - 39-40 SP - 583 EP - 586 PB - Trans Tech Publ. CY - Zurich AN - OPUS4-17840 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Deubener, J. A1 - Behrens, H. A1 - Müller, Ralf A1 - Zietka, S. A1 - Reinsch, Stefan T1 - Kinetic fragility of hydrous soda-lime-silica glasses N2 - The effect of hydration on the kinetic fragility of soda-lime-silica glasses was investigated by viscometry in the glass transition range. Water-bearing glasses were prepared from industrial float glass (FG) and a ternary model glass (NCS = 16Na2O 10CaO 74SiO2 in mol%) by bubbling steam through the melt at 1480 °C and up to 7 bar. Additionally, a sodium borosilicate glass (NBS = 16Na2O 10B2O3 74SiO2 in mol%) was hydrated under equal conditions. As detected by infrared spectroscopy water dissolves in the glasses exclusively as OH-groups. The hydration resulted in a total water content CW up to ~ 0.2 wt% for FG, NCS and NBS glasses. Kinetic fragility, expressed by the steepness index m, was determined from the temperature dependence of η at the glass transition. Viscosity data from previous studies on hydrous float glasses (CW > 1 wt%) were surveyed together with literature data on the (H2O)–Na2O–CaO–SiO2, (H2O)–Na2O–SiO2 and (H2O)–SiO2 systems to expand the range of water concentration and bulk composition. We could demonstrate that m decreases for all glasses although water is dissolved as OH and should depolymerize the network. An empirical equation of the general type m = a - b logCW where a, b are fitting parameters, enables m to be predicted, for each glass series as function of the water content CW. The enlarged data base shows that the parameter B of the Arrhenius viscosity-temperature relation decreases much stronger than the isokom temperature at the glass transition. KW - Soda-lime-silica KW - Fragility KW - Viscosity KW - Water in glass PY - 2008 DO - https://doi.org/10.1016/j.jnoncrysol.2008.04.021 SN - 0022-3093 VL - 354 IS - 42-44 SP - 4713 EP - 4718 PB - North-Holland Publ. Co. CY - Amsterdam AN - OPUS4-18187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Marzok, Ulrich A1 - Müller, Ralf A1 - Schadrack, Reinhard A1 - Krauhausen, M. A1 - Burgstedt, F. A1 - Brode, W. A1 - Reetz, R. ED - Kriegesmann, J. T1 - Hochtemperatur-Laserprofilometrie an keramischen Bauteilen N2 - Es wurde ein Gerät zur In-situ-Kontrolle des Sinterns keramischer Bauteile mit Hilfe der Hochtemperatur-Lasertriangulation aufgebaut. Durch Rotation der Probe und gleichzeitiger Positionierung des Laserabstandssensors erfolgt die dreidimensionale Erfassung der Topografie der Probenoberfläche. Derzeit können flache Proben mit den Maßen < 20 cm x 20 cm x 1 cm bis 1000 °C untersucht werden. Die örtliche Wiederholpräzision des verwendeten Lasersensors beträgt 10 µm bei 20 °C und 15 µm bei 1000 °C. Die lineare Positioniergenauigkeit des Sensors liegt bei 1 µm, die Winkelauflösung der Drehung des Probentellers beträgt 0,0025 °. Daten für ein 3D-Oberflächenprofil werden in etwa 2 bis 3 Minuten erzeugt. Spezielle Linienprofile erhält man bei einer Messzeit von wenigen Sekunden. N2 - A device was designed for the in situ monitoring of sintering of ceramic components using high-temperature laser triangulation. By simultaneous rotation of the sample and positioning of the laser distance sensor at the same time a three-dimensional detection of the topography of the sample surface could be achieved. Currently, flat samples with dimensions < 20 cm x 20 cm x 1 cm can be examined up to 1000 °C. The local repeatability precision of the laser sensor used is 10 µm at 20 °C and 15 µm at 1000 °C. The linear positioning accuracy of the sensor is 1 µm, the angular resolution of the rotation of the sample plate is 0.0025 °. Data for a 3D surface profile can be obtained in about 2 to 3 minutes. Specific line profiles can be received at a measurement time of a few seconds. PY - 2013 SN - 978-3-938595-00-8 VL - 135 IS - Kap. 6.3.1.0 PB - HvB-Verlag CY - Ellerau AN - OPUS4-28967 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Ralf A1 - Meszaros, Robert A1 - Peplinski, Burkhard A1 - Reinsch, Stefan A1 - Eberstein, Markus A1 - Schiller, Wolfgang Arno A1 - Deubener, J. T1 - Dissolution of alumina, sintering, and crystallization in glass ceramic composites for LTCC KW - LTCC KW - Sintering KW - Crystallization KW - Alumina dissolution KW - Rietveld analysis PY - 2009 DO - https://doi.org/10.1111/j.1551-2916.2009.03089.x SN - 0002-7820 SN - 1551-2916 VL - 92 IS - 8 SP - 1703 EP - 1708 PB - Blackwell Publishing CY - Malden AN - OPUS4-20676 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Reinsch, Stefan T1 - Sinterability of Glass Powders T2 - Status Seminar, Programm for Developing the Supporting System for Global Mulitidisciplinary Engineering Establishment CY - Nagaoka, Japan DA - 2010-07-29 PY - 2010 AN - OPUS4-22519 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Overall Crystallization Kinetics of Glass Powders T2 - Status Seminar, Programm for Developing the Supporting System for Global Mulitidisciplinary Engineering Establishment CY - Nagaoka, Japan DA - 2010-07-29 PY - 2010 AN - OPUS4-22520 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Eberstein, M. A1 - Deubener, J. T1 - Sinterkinetik von Glasmatrixkompositen für LTCC Anwendungen T2 - DKG - Symp. Simulation und Modellierung von Fertigungsprozesen CY - Erlangen, Germany DA - 2010-11-30 PY - 2010 AN - OPUS4-22521 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Nascimento, M.L.F. A1 - Zanotto, E. D. T1 - Crystal growth kinetics in cordierite and diopside glasses in wide temperature ranges T2 - Intern. Congr. on Glass ICG2010, Annual Meeting TC7, ICG CY - Bahia, Brazil DA - 2010-09-20 PY - 2010 AN - OPUS4-22522 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ried, Peter A1 - Gaber, Martin A1 - Beyer, Katrin A1 - Müller, Ralf A1 - Kipphardt, Heinrich A1 - Kannengießer, Thomas T1 - Thermo Analytic Investigation of Hydrogen Effusion Behavior - Sensor Evaluation and Calibration N2 - The well established carrier gas analysis (CGA) method was used to test different hydrogen detectors comprising a thermal conductivity detector (TCD) and a metal oxide semiconducting (MOx) sensor. The MOx sensor provides high hydrogen sensitivity and selectivity, whereas the TCD exhibits a much shorter response time and a linear hydrogen concentration dependency. Therefore, the TCD was used for quantitative hydrogen concentration measurements above 50?µmol/mol. The respective calibration was made using N2/H2 gas mixtures. Furthermore, the hydrogen content and degassing behaviour of titanium hydride (TiH2-x) was studied. This material turned out to be a potential candidate for a solid sample calibration. Vacuum hot extraction (VHE) coupled with a mass spectrometer (MS) was then calibrated with TiH2-x as transfer standard. The calibration was applied for the evaluation of the hydrogen content of austenitic steel samples (1.4301) and the comparison of CGA-TCD and VHE-MS. KW - Hydrogen KW - Steel KW - Vacuum hot extraction KW - Carrier gas analysis KW - Titanium hydride KW - Gas calibration PY - 2011 DO - https://doi.org/10.1002/srin.201000237 SN - 1611-3683 SN - 0177-4832 VL - 82 IS - 1 SP - 14 EP - 19 PB - Verl. Stahleisen CY - Düsseldorf AN - OPUS4-23202 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 - CHAP A1 - Müller, Ralf A1 - Reinsch, Stefan ED - Bansal, N. P. ED - Boccaccini, A.R. T1 - Viscous-phase silicate processing KW - Viskoses Sintern KW - Oberflächenkeimbildung KW - Glaspulver KW - Sintermodelle KW - Sinterglaskeramik KW - Glasmatrixkomposit PY - 2012 SN - 978-0-470-55344-2 IS - Chapter 3 SP - 75 EP - 144 PB - Wiley AN - OPUS4-27054 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Deubener, J. A1 - Behrens, H. T1 - Internal friction of hydrated soda-lime-silicate glasses N2 - The internal friction of hydrated soda-lime-silica glasses with total water content (CW ) up to 1.9 wt. % was studied by dynamic mechanical analysis (DMA) using temperature-frequency sweeps from 723 K to 273 K and from 1 s-1 to 50 s-1. Total water content and concentrations of H2O molecules (CH2O ) and OH groups (COH) in the DMA specimens were determined by infrared spectroscopy. For low water contents (CW ≈ COH < 0.25 wt. %) two discrete internal friction peaks below the glass transition (α relaxation) were assigned to the low-temperature motion of alkali ions (γ relaxation) and cooperative movements of dissimilar mobile species under participation of OH at higher temperature (βOH relaxation). For large water contents (CW > 1 wt. %), where significant amounts of molecular water are evident (CH2O > 0.15 wt. %), however, internal friction spectra change unexpectedly: the βOH peak heights saturate and a low temperature shoulder appears on the β-relaxation peak. This emerging relaxation mode (βH2O relaxation) was assigned to the motions of H2O molecules. βH2O relaxation was found to be faster than βOH but slower than γ relaxation. Activation energy of the different relaxation modes increased in the order γ < βH2O < βOH < α. KW - Internal friction KW - Glass KW - Water content PY - 2013 DO - https://doi.org/10.1063/1.4828740 SN - 0021-9606 SN - 1089-7690 VL - 139 SP - 174506-1 EP - 174506-6 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-29698 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 - TY - JOUR A1 - Blaeß, Carsten A1 - Müller, Ralf T1 - Sintering and foaming of bioactive glasses N2 - Sintering, crystallization, and foaming of 44.8SiO2–2.5P2O3–36.5CaO–6.6Na2O–6.6K2O–3.0CaF2 (F3) and 54.6SiO2–1.7P2O3–22.1CaO–6.0Na2O–7.9K2O–7.7MgO (13–93) bioactive glass powders milled in isopropanol and CO2 were studied via heating microscopy, differential thermal analysis, vacuum hot extraction (VHE), Infrared spectroscopy, and time-of-flight secondary ion mass spectrometry. Full densification was reached in any case and followed by significant foaming. VHE studies show that foaming is driven by carbon gases and carbonates were detected by Infrared spectroscopy to provide the major foaming source. Carbonates could be detected even after heating to 750◦C, which hints on a thermally very stable species or mechanical trapping. Otherwise, dark gray compact colors for milling in isopropanol indicate the presence of residual carbon as well. Its significant contribution to foaming, however, could not be proved and might be limited by the diffusivity of oxygen needed for carbon oxidation to carbon gas. KW - Bioactive Glass KW - Crystallization KW - Foaming KW - Sintering PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552454 DO - https://doi.org/10.1111/jace.18626 SN - 0002-7820 SP - 1 EP - 11 PB - Wiley online library AN - OPUS4-55245 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 - CONF A1 - Müller, Ralf T1 - GlasDigital - Datengetriebener Workflow für die beschleunigte Entwicklung von Glas N2 - Das Projekt GlasDigital im Rahmen der BMBF Initiative MaterialDigital wird vorgestellt. T2 - MatFo22 CY - Berlin, Germany DA - 14.11.2022 KW - Material Digital PY - 2022 AN - OPUS4-56282 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Chen, Y.-F. A1 - Contreras Jaimes, A. T1 - Datengetriebener Workflow für die beschleunigte Entwicklung von Glas (GlasDigital) N2 - Das Projekt GlasDigital wurde im allgemeinen vorgestellt, sowie die einzelnen Zwischenstände der verschiedenen Arbeitspakete aller Projektpartner präsentiert. Die allgemeine Porjektvorstellung ist auf deutsch. Die Zwischenstände der Arbeitsinhalte sind auf englisch. T2 - PMD Vollversammlung CY - Berlin, Germany DA - 03.11.2022 KW - Oxidglas KW - Robotische Glasschmelzanlage KW - ML KW - Ontologie KW - Digitaler Zwilling KW - Bildanalyse PY - 2022 AN - OPUS4-56491 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - GLAS DIGITAL - Datengetriebener Workflow für die beschleunigte Entwicklung von Glas N2 - Aktuelle Ergebnisse des Projektes GlasDigital werden kurz zusammenfassend und allgemein verständlich vorgestellt. T2 - MatFo 2022 CY - Cologne, Germany DA - 14.11.2022 KW - Oxidglas KW - robotische Glasschmelzanlage KW - Ontologie KW - ML KW - Digitaler Zwilling KW - Bildanalyse PY - 2022 AN - OPUS4-56492 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Agea-Blanco, Boris A1 - Blaeß, Carsten A1 - Reinsch, Stefan A1 - Behrens, H T1 - Sintering and Foaming of Silicate Glass Powders N2 - The lecture focuses on the mechanisms of non-desired gas bubble formation and foaming during the sintering of glass powder compacts. It is shown that foaming is driven by carbon gases and that carbonates, encapsulated in micropores or mechaniacally dissolved beneath the glass surface, provide the major foaming source. T2 - Sandanski Workshop Sinter crystallization 27th-29th September 2021 PROJECT “THEORY AND APPLICATIONS OF SINTER-CYSTALLIZATION” DN 19/7 CY - Online meeting DA - 27.10. 2021 KW - Sintering KW - Non-desired foaming PY - 2021 AN - OPUS4-53772 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 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 - 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 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 - Müller, Ralf A1 - Behrens, Harald A1 - Ageo-Blanco, Boris A1 - Reinsch, Stefan A1 - Wirth, Thomas T1 - Foaming Species and Trapping Mechanisms in Barium Silicate Glass Sealants N2 - Barium silicate glass powders 4 h milled in CO2 and Ar and sintered in air are studied with microscopy, total carbon analysis, differential thermal Analysis (DTA), vacuum hot extraction mass spectroscopy (VHE-MS), Fourier-transformed infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary-ion mass spectrometry (TOF-SIMS). Intensive foaming of powder compacts is evident, and VHE studies prove that foaming is predominantly caused by carbonaceous species for both milling gases. DTA Shows that the decomposition of BaCO3 particles mix-milled with glass powders occurs at similar temperatures as foaming of compacts. However, no carbonate at the glass surface could be detected by FTIR spectroscopy, XPS, and TOF-SIMS after heating to the temperature of sintering. Instead, CO2 molecules unable to rotate identified by FTIR spectroscopy after milling, probably trapped by mechanical dissolution into the glass bulk. Such a mechanism or microencapsulation in cracks and particle aggregates can explain the contribution of Ar to foaming after intense milling in Ar atmosphere. The amount of CO2 molecules and Ar, however, cannot fully explain the extent of foaming. Carbonates mechanically dissolved beneath the surface or encapsulated in cracks and micropores of particle aggregates are therefore probably the major foaming source. KW - Milling KW - Foaming KW - Glass powder KW - Sintering PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531227 DO - https://doi.org/10.1002/adem.202100445 SN - 1438-1656 VL - 24 IS - 6 SP - 2100445-1 EP - 2100445-13 AN - OPUS4-53122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Rouxel, T. A1 - Behrens, H. A1 - Deubener, J. A1 - Müller, Ralf T1 - Vacuum crack growth in alkali silicate glasses N2 - Crack growth velocity in alkali silicate glasses was measured in vacuum across 10 orders of magnitude with double cantilever beam technique. Measured and literature crack growth data were compared with calculated intrinsic fracture toughness data obtained from Young´s moduli and the theoretical fracture surface energy estimated from chemical bond energies. Data analysis reveals significant deviations from this intrinsic brittle fracture behavior. These deviations do not follow simple compositional trends. Two opposing processes may explain this finding: a decrease in the apparent fracture surface energy due to stress-induced chemical changes at the crack tip and its increase due to energy dissipation during fracture. KW - Silicate glass KW - Brittle fracture KW - Crack growth KW - Calculated intrinsic fracture toughness PY - 2021 DO - https://doi.org/10.1016/j.jnoncrysol.2021.121094 SN - 0022-3093 VL - 572 SP - 1 EP - 8 PB - Elsevier CY - Amsterdam AN - OPUS4-53144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heuser, Lina A1 - Nofz, Marianne A1 - Müller, Ralf A1 - Deubener, J. T1 - Silver dissolution and precipitation in an Na2O–ZnO–B2O3 metallization paste glass N2 - Thermally stimulated interactions between silver and glass, that is, silver dissolution as Ag+ and precipitation as Ag0 were studied in two glass series of molar target composition xAg2O–(19 − x)Na2O–28ZnO–53B2O3 with x = 0, 0.1, 0.5, 5 and (19Na2O–28ZnO–53B2O3)+yAg2O with y = 0.01, 0.05. These act as model for low-melting borate glasses being part of metallization pastes. The occurrence of metallic silver precipitates in melt-quenched glass ingots demonstrated that silver dissolved only in traces (< 0.01 mol%) in the glasses. The dissolved silver was detected by means of Raman spectroscopy and energy-dispersive X-ray spectroscopy. Increasing x in the batch could not lead to a significant increase of the silver ion fraction in the glass as possible in binary silver borate glasses. In situ observation of heated AgNO3 mixed with the base glass frit in a hot stage microscope showed that Ag0 precipitation occurs already at the solid state. At higher temperatures, small droplets of liquid silver were found to move freely within the melt, whereas coalescence caused a stepwise increase of their size. These results contribute to the understanding of formation of silver precipitates in metallization pastes described in the literature. KW - Silver metallization paste KW - Batch reactions KW - Borate KW - Glass forming melts KW - Glass manufacturing KW - Raman spectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559433 DO - https://doi.org/10.1111/ijag.16613 SN - 2041-1286 SP - 1 EP - 11 PB - Wiley Online Library AN - OPUS4-55943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heuser, Lina A1 - Nofz, Marianne A1 - Müller, Ralf T1 - Alkali and alkaline earth zinc and lead borate glasses: Sintering and crystallization N2 - Glasses in the systems Me2O-ZnO-B2O3 with Me = Li, Na, K, Rb (MeZB), Na2O-ZnO-CuO-B2O3 (NZCuB), CaO-ZnO-B2O3 (CaZB), and Li2O-PbO-B2O3 (LPbB) as a reference, were studied by differential thermal analysis, dilatometry, rotational viscometry, and heating microscopy. A decrease of viscosity and sintering range was found with decreasing number of fourfold coordinated boron. The viscosity of the alkali zinc borate glasses varies only slightly. LPbB and CaZB stand out by their reduced and increased viscosities, respectively. Sodium, potassium, and calcium zinc borate glasses possess a fragility above 76. All glasses were sintered to full density before crystallization. Mostly binary zinc borate phases govern crystallization. A ternary crystalline phase was detected only in the potassium containing sample. The Weinberg glass stability parameter ranges between 0.07 and 0.12. This is caused by the presence of several crystalline phases and varying melting points of even the same crystalline phase in different glass matrices. KW - Alkali zinc borate glasses KW - Lead borate glasses KW - Viscosity KW - Sintering KW - Crystallization KW - Fragility PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556128 DO - https://doi.org/10.1016/j.nocx.2022.100116 SN - 2590-1591 VL - 15 SP - 1 EP - 8 PB - Elsevier CY - Amsterdam AN - OPUS4-55612 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fest, Sarah Ute A1 - Reinsch, Stefan A1 - Müller, Ralf T1 - Milling, sintering and crystallization of 11BaO-25CaO-64SiO2 glass powder N2 - The crystallization of 11BaO-25CaO-64SiO2 mol% glass powders and related effects of glass powder milling have been studied by X-ray diffraction (XRD), light and scanning electron microscopy (SEM) and differential thermal analysis (DTA). Glass powders were made by ZrO2 crushing with subsequent sieving or sedimentation or alternatively made by milling with agate, corundum and tungsten carbide. Although surface crystallization was detectable during late sintering, all powders fully sintered. Wollastonite was found as primary crystal phase followed by cristobalite and sanbornite precipitation. The latter crystallization steps caused a second DTA-peak for fine powders. DTA-peak temperatures shifted to lower temperature with decreasing particle size in any case. No significant effects of milling materials on DTA-peak temperatures were evident. As an exception, however, milling in agate caused strongly decreased temperatures of the second DTA-peak. This observation can be explained by the progressive mechanical damaging, which results from the required prolonged milling time with agate due to its small materials density, and the fact that diamond made scratches did promote surface crystallization of cristobalite. The present study thus shows that even for glass powders with excellent sinterability, milling can affect microstructure evolution. KW - Glass KW - Crystallization KW - Powder preparation KW - SOFC PY - 2014 UR - http://onlinelibrary.wiley.com/doi/10.1111/ijag.12080/full DO - https://doi.org/10.1111/ijag.12080 SN - 2041-1286 SN - 2041-1294 VL - 5 IS - 3 SP - 236 EP - 247 PB - Wiley-Blackwell CY - Hoboken, NJ [u.a.] AN - OPUS4-30807 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ried, Peter A1 - Gaber, Martin A1 - Müller, Ralf A1 - Deubener, J. T1 - Hydrogen permeability of a barium-aluminoborosilicate glass - A methodical approach N2 - The H2 effusion from H2 saturated glass powders, H2 permeation through the wall of blown glass bulbs, and H2 permeation through the wall of glass capillaries were applied to evaluate the permeability of hydrogen gas in a barium-aluminoborosilicate (BABS) glass. To validate these methods, two commercial glasses (vitreous silica and borosilicate) were used as a reference. Permeation values obtained from the different experiments agreed within a factor of 3 or less. The H2 permeability of BABS glass at temperatures close to ambient was found to be at least 3 orders of magnitude below that of borosilicate and silica glasses. The powder method, which requires minimal sample preparation efforts, turned out to provide easy access to the measurement of H2 permeability of glasses down to P = 3.9 × 10- 21 mol s- 1 Pa- 1 m- 1. KW - Hydrogen gas KW - Permeability KW - Solubility KW - Diffusivity KW - Aluminoborosilicate glass PY - 2014 DO - https://doi.org/10.1016/j.jnoncrysol.2014.04.006 SN - 0022-3093 VL - 394-395 SP - 43 EP - 49 PB - North-Holland Publ. Co. CY - Amsterdam AN - OPUS4-30720 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Deubener, J. A1 - Krüger, S. T1 - Rate curve and induction time analysis of heterogeneous crystal nucleation in glass-ceramic systems T2 - 1st Joint Meeting of DGG - ACerS GOMD CY - Aachen, Germany DA - 2014-05-25 PY - 2014 AN - OPUS4-30850 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 - 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 - 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 - 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 - Eberstein, Markus A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Deubener, J. A1 - Schiller, Wolfgang Arno T1 - Sintering of glass matrix composites with small rigid inclusions KW - Glass ceramics KW - Inclusions KW - Sintering KW - Mixing KW - Powders KW - Solid-state reaction PY - 2009 DO - https://doi.org/10.1016/j.jeurceramsoc.2009.02.007 SN - 0955-2219 SN - 1873-619X VL - 29 IS - 12 SP - 2469 EP - 2479 PB - Elsevier CY - Oxford AN - OPUS4-19570 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Deubener, J. A1 - Bornhöft, H. A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Lumeau, J. A1 - Glebova, L.N. A1 - Glebov, L.B. T1 - Viscosity, relaxation and elastic properties of photo-thermo-refractive glass KW - Ultrasonic relaxation KW - Silicates KW - Rheology KW - Structural relaxation KW - Viscosity PY - 2009 DO - https://doi.org/10.1016/j.noncrysol.2008.10.002 SN - 0022-3093 VL - 355 SP - 126 EP - 131 PB - North-Holland Publ. Co. CY - Amsterdam AN - OPUS4-18671 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schiller, Wolfgang Arno A1 - Müller, Ralf A1 - Eberstein, Markus A1 - Reinsch, Stefan A1 - Rabe, Torsten T1 - Sintering of LTCC N2 - Low Temperature Co-fired Ceramic materials (LTCC) have attracted growing interest in recent years since they are promising candidates for highly integrated ceramic packaging. This paper surveys materials concepts of related glass ceramic composites (GCC) and discusses unsolved problems and challenges. The densification of GCC based on "viscous sintering" may be affected by steric effects and partial dissolution of dispersed crystal particles, crystallization and phase boundary reactions. KW - Sintering KW - Glass ceramic composites KW - Viscosity KW - Densification KW - Modelling PY - 2008 SN - 0173-9913 SN - 0196-6219 VL - 85 IS - 13 SP - 12 EP - 17 PB - Göller CY - Baden-Baden AN - OPUS4-19086 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Deubener, J. T1 - Dissolution of alumina in GMC for LTCC T2 - 8th Pacific Rim Conf. on Ceramic and Glass Technology CY - Vancouver, Canada DA - 2010-05-31 PY - 2010 AN - OPUS4-21416 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Glas an der Bundesanstalt für Materialforschung und -prüfung N2 - Im Vortrag wird ein kurzer Überblick über die BAM und die Aktivitäten zum Werkstoff Glas gegeben. T2 - 4. Glashüttentag der Jungen DGG vom 29.09.2016 bis 30.09.2016 in Berlin CY - Berlin, Germany DA - 29.09.2016 KW - Glas PY - 2016 AN - OPUS4-38331 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Sintering and crystallization of glass powders – effects, challenges and chances N2 - Chemical variability is a main strength of glass. Glass powders are therefore 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, even if it may not be obvious at first sight, a key component of advanced technologies. Manufacture and processing of initial glass powders often allow even more flexibility in materials design. At the same time, however, they can cause additional problems. The lecture illustrates possible consequences of glass powder processing upon glass crystallization and sintering as well as chances for targeted utilization. Simple kinetic models describing the effect of particle size distribution, surface crystallization and rigid inclusions on sintering as well effects of different milling and seeding on sinter crystallization are presented. T2 - Institutskolloquium CSIC CY - Madrid, Spain DA - 28.4.2016 KW - Glass KW - Powders KW - Sintering KW - Crystallization KW - SOFC KW - LTCC PY - 2016 AN - OPUS4-38333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Behrens, H. A1 - Deubener, J. T1 - Impact of structure and relaxation on fatigue and micromechanical properties of oxide glasses: the role of volatiles and bonding state N2 - As subcritical crack growth (SCCG) can reduce tensile strength of glasses by many orders of magnitude, the potential for improvement of fatigue behaviour is most intriguing in developing ultra-strong glasses. An essential bottleneck is the basic understanding of the numerous interplaying pressure-, temperature- and water-affected relaxation phenomena at the crack tip and related toughening strategies. Therefore, the present project aims to advance the basic understanding of structural relaxation effects and local properties caused by increased water concentration and tensile stresses at the crack tip as they are a key for structural toughening designs to develop SCCG-free glasses and glass surfaces. Our first studies give clear evidence that glass structure and dynamics is strongly modified upon hydration of glasses. These changes are highly related to the nature of network formers but are affected as well by the counter ions (network modifier). Results of the 1st project part suggest that structural relaxation below glass transition temperature, i.e. overlapping of short-range (beta) and long-range (alpha) interactions can contribute to SCCG in water-free environments and that structurally dissolved water in the glasses can have decisive impact on this effect. In the 2nd project stage specific glasses compositions will be investigated to gain an improved understanding on the relation of sub-Tg relaxation and inert SCCG as well as to shed light to the related effects of dissolved water and its speciation. These glasses cover a broader range of different glass topologies and binding partners, whereby the coupling of alpha and beta relaxations is varied systematically by alkali-, alkaline earth ions and water species concentrations. Preparation of hydrous glasses (up to 8 wt% water) will be performed by high pressure syntheses. Structure will be resolved by NMR, Raman and IR spectroscopy while structural relaxation is accessed in the temperature and frequency domain using dynamic mechanical spectroscopy and ultrasonic damping. We will focus on measurements of inert SCCG (region III) conducting experiments in vacuum and dry gas atmospheres using indentation techniques and stressing of glass specimens in DCB geometry. Experimental data on SCCG will be provided to SPP groups, which deals with fatigue in metallic glasses and vice versa we will test theoretical predictions of ab-initio simulations of partner within SPP 1594 in order to quantify the effect of water on the crack tip. In summa topological factors controlling the subcritical crack growth with respect to water will be identified from which structural toughening designs for highly fatigue resistant-glasses can be derived. N2 - Subkritisches Risswachstum (SCCG) kann die Zugfestigkeit von Glas um viele Größenordnungen erniedrigen. Deshalb birgt die Verbesserung des Ermüdungsverhaltens ein hohes Potential für das topologische Design hochfester Gläser. Ein diesbezüglicher Engpass ist das Verständnis der zahlreichen interagierenden druck-, temperatur- und wasserbeeinflussten Relaxationsphänomene an der Rissspitze und hieraus abgeleitete Verstärkungsstrategien. Ziel des Projekts ist es daher, das grundlegende Verständnis der Effekte, die infolge erhöhter Wasserkonzentrationen und Zugspannungen an der Rissspitze entstehen, zu vertiefen, da sie als ein Schlüssel für künftige strukturelle Designprinzipien zur Entwicklung schadenstoleranter Gläser und Glasoberflächen gelten. Unsere ersten Studien zeigen, dass die Struktur und Dynamik von Gläsern nach einer Hydration stark verändert sind. Diese Modifikationen sind mit der Art der Netzwerkbildner stark verknüpft, aber auch von ihren Gegenionen (Netzwerkwandler) abhängig. Die Ergebnisse des ersten Projektabschnitts legen nahe, dass strukturelle Relaxation unterhalb der Glasübergangstemperatur, d. h. ein Überlappen von kurz-reichweitigen (beta) und lang-reichweitigen (alpha) Wechselwirkungen, zum subkritisches Risswachstum in wasserfreien Umgebungen beitragen kann und, dass strukturell gelöstes Wasser in Gläsern sich entscheidend auf diese Effekt auswirken kann. Im zweiten Projektabschnitt werden daher spezielle Glaszusammensetzungen untersucht, die zu einem besseren Verständnis der Verbindung zwischen sub-Tg Relaxation und SCCG führen aber auch den Einfluss von gelöstem Wasser und dessen Speziation näher beleuchten. Diese Gläser weisen eine großen Breite an verschiedenen Topologien und Bindungspartnern auf, wobei die Kopplung von alpha und beta Relaxation durch Veränderungen in den Gehalten von Alkali-, Erdalkalionen und der Wasserspezies systematisch variiert wird. Die Präparation hydratisierter Gläser (bis zu 8 Ma.%) erfolgt mittels Hochdrucksynthesen. Die Glasstruktur wird durch NMR, Raman und IR Spektroskopie aufgeklärt während die Strukturrelaxation anhand dynamische mechanische Spektroskopie und Ultraschalldämpfung im Temperatur- und Frequenzraum erfasst wird. Im Fokus werden Messungen des inerten subkritischen Risswachstums (Region III) stehen, die Indenter-Experimente im Vakuum und trockenen Gasatmosphären sowie Verspannen von Glasproben in DCB Geometrie beinhalten. Experimentelle SCCG Daten werden Gruppen im Schwerpunktprogramm zur Verfügung stellen, die sich mit Ermüdung in metallischen Gläsern beschäftigen und im Gegenzug werden wir theoretische Vorhersagen aus ab initio Simulationen der Partner im SPP 1594 testen, um den Einfluss von Wasser auf die mechanischen Eigenschaften an der Rissspitze und deren Einfluss auf SCCG zu quantifizieren. In summa werden topologische Faktoren bezüglich Wasser, die SCCG kontrollieren, identifiziert, um daraus Designprinzipien für hoch ermüdungsresistente Gläser abzuleiten. T2 - Kolloquium des DFG-PP 1594 CY - Jena, Germany DA - 17.9.2015 KW - Glass KW - Fatigue PY - 2015 AN - OPUS4-38334 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Behrens, H. A1 - Deubener, J. A1 - Reinsch, Stefan A1 - Bauer, Ute A1 - Rößler, C. T1 - Impact of structure and relaxation on fatigue and micro-mechanical properties of oxide glasses: the role of volatiles and bonding state N2 - As subcritical crack growth (SCCG) can reduce tensile strength of glasses by many orders of magni-tude, the potential for improvement of fatigue behaviour is most intriguing in developing ultra-strong glasses. An essential bottleneck is the basic understanding of the numerous interplaying pressure-, temperature- and water-affected relaxation phenomena at the crack tip and related toughening strat-egies. Therefore, the present project aims to advance the basic understanding of structural relaxa-tion effects and local properties caused by increased water concentration and tensile stresses at the crack tip as they are a key for structural toughening designs to develop SCCG-free glasses and glass surfaces. Our first studies give clear evidence that glass structure and dynamics is strongly modified upon hy-dration of glasses. These changes are highly related to the nature of network formers but are affect-ed as well by the counter ions (network modifier). Results of the 1st project part suggest that struc-tural relaxation below glass transition temperature, i.e. overlapping of short-range (beta) and long-range (alpha) interactions can contribute to SCCG in water-free environments and that structurally dissolved water in the glasses can have decisive impact on this effect. In the 2nd project stage specific glasses compositions will be investigated to gain an improved un-derstanding on the relation of sub-Tg relaxation and inert SCCG as well as to shed light to the relat-ed effects of dissolved water and its speciation. These glasses cover a broader range of different glass topologies and binding partners, whereby the coupling of alpha and beta relaxations is varied systematically by alkali-, alkaline earth ions and water species concentrations. Preparation of hy-drous glasses (up to 8 wt% water) will be performed by high pressure syntheses. Structure will be resolved by NMR, Raman and IR spectroscopy while structural relaxation is accessed in the temper-ature and frequency domain using dynamic mechanical spectroscopy and ultrasonic damping. We will focus on measurements of inert SCCG (region III) conducting experiments in vacuum and dry gas atmospheres using indentation techniques and stressing of glass specimens in DCB geometry. Experimental data on SCCG will be provided to SPP groups, which deals with fatigue in metallic glasses and vice versa we will test theoretical predictions of ab-initio simulations of partner within SPP 1594 in order to quantify the effect of water on the crack tip. In summa topological factors con-trolling the subcritical crack growth with respect to water will be identified from which structural toughening designs for highly fatigue resistant-glasses can be derived. T2 - Kolloquium des DFG-PP 1593 Ultrastrong Glasses CY - Jena, Germany DA - 17.9.2015 KW - Glass KW - Fatigue PY - 2015 AN - OPUS4-38335 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Agea Blanco, Boris A1 - Reinsch, Stefan A1 - Müller, Ralf T1 - Sintering and foaming of barium silicate glass powder compacts N2 - The manufacture of sintered glasses and glass-ceramics, glass matrix composites, and glass-bounded ceramics or pastes is often affected by gas bubble formation. Against this background, we studied sintering and foaming of barium silicate glass powders used as SOFC sealants using different powder milling procedures. Sintering was measured by means of heating microscopy backed up by XPD, differential thermal analysis, vacuum hot extraction (VHE), and optical and electron microscopy. Foaming increased significantly as milling progressed. For moderately milled glass powders, subsequent storage in air could also promote foaming. Although the powder compacts were uniaxially pressed and sintered in air, the milling atmosphere significantly affected foaming. The strength of this effect increased in the order Ar ≈ N2 < air < CO2. Conformingly, VHE studies revealed that the pores of foamed samples predominantly encapsulated CO2, even for powders milled in Ar and N2. Results of this study thus indicate that foaming is caused by carbonaceous species trapped on the glass powder surface. Foaming could be substantially reduced by milling in water and 10 wt% HCl. KW - Glass powder KW - Sintering KW - Foaming KW - SOFC PY - 2016 UR - http://journal.frontiersin.org/article/10.3389/fmats.2016.00045/full?&utm_source=Email_to_authors_&utm_medium=Email&utm_content=T1_11.5e1_author&utm_campaign=Email_publication&field=&journalName=Frontiers_in_Materials&id=214488 DO - https://doi.org/10.3389/fmats.2016.00045 SN - 2296-8016 VL - 3 SP - Article 45, 1 EP - 10 AN - OPUS4-38303 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Marzok, Ulrich A1 - Reinsch, Stefan A1 - Gaber, Martin A1 - Welter, T. A1 - Deubener, J. T1 - Hydrogen permeability of glass measured by VHE-MS powder methods N2 - Glasses are can serve as exceptionally tight hydrogen barriers e.g. used for hydrogen storage in micro glass containers or cover glasses in micro electronic systems. Respective glass development, however, requires precise measurements of minimal hydrogen permeability, PH2. Recent studies showed that PH2 can be measured down to 2 10-21 mol s-1 Pa-1m-1 by means of Vacuum Hot Extraction (VHE) powder methods [1]. In this respect the isothermal gas release from glass powder particles is fitted in terms of classical diffusion models assuming spherical particles of uniform size thus obtaining the hydrogen diffusion coefficient, DH2. PH2 is then given by D H2 × S H2, where hydrogen solubility, SH2, is obtained from VHE studies of glass powders exposed to hydrogen atmosphere for different exposure time and hydrogen pressure. Measurements of minimal values of hydrogen permeability, however, require a careful evaluation and error discussion of this method. Against that background, we modeled hydrogen degassing during heating and subsequent isothermal annealing of glass powder particles of different shape and particle size distribution by means of COMSOL Multiphysics® [2] and verified related effects on DH2 obtained by the VHE powder method. T2 - SGT Centenary Conference, & ESG 2016 CY - Sheffield, UK DA - 4.9.2016 KW - Glass KW - Hydrogen KW - Permeability KW - Storage PY - 2016 AN - OPUS4-38307 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Marzok, Ulrich A1 - Reetz, R. A1 - Trunkhardt, M. T1 - High-temperature laser profilometry N2 - Advanced methods for 3D green density characterization like computed tomography and 3D FE sinter modeling can be utilized for increasing the reliability of sintered components. The experimental in situ observation of sintering, however, is currently restricted to silhouette methods, i.e. heating microscopy. For complex shaped samples, in situ shape screening during shrinkage would allow much better validation of 3D sinter simulation models. Further, by revealing temporary sinter warpage, 3D high-temperature shape screening allows to locate potential defects of complex sintered components. Against this background, BAM developed a testing device for in situ 3D high-temperature shape screening for ceramic and glass-ceramic tapes up to 1000°C [1-3]. Current work is focused on dropping this restriction in sample shape and temperature. The poster illustrates the current state of this work and possible applications of the method e.g. in detecting sinter warpage of metallized glass-ceramic LTCC tapes. T2 - SGT Centenary Conference, & ESG 2016 CY - Sheffield, UK DA - 04. 09. 2016 KW - Laser profilometry KW - 3D High-temperature shape screening KW - Sintering PY - 2016 AN - OPUS4-38320 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 - CONF A1 - Heunisch, Andreas A1 - Marzok, Ulrich A1 - Münchow, Marco A1 - Müller, Ralf A1 - Rabe, Torsten T1 - In situ characterization of the sintering behavior of LTCC laminates with embedded cavities by high temperature laser profilometry T2 - CICMT 2013 - IMAPS/ACerS 9th International conference and exhibition on ceramic interconnect and ceramic microsystems technologies CY - Orlando, FL, USA DA - 2013-04-23 KW - LTCC multilayer KW - Embedded cavities KW - High temperature laser profilometry KW - Low pressure lamination KW - Micro fluidics PY - 2013 DO - https://doi.org/10.4071/cicmt-tha44 SP - 275 EP - 282 AN - OPUS4-35077 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 - Blaeß, Carsten A1 - Müller, Ralf T1 - Master curve for viscous crack healing 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 - Müller, Ralf A1 - Marzok, Ulrich T1 - Hochtemperaturlaserprofilometrie (HTLP) N2 - Der Vortrag stellt die an der BAM neu entwickelte Methode der Hochtemperatur-Laserprofilometrie (HTLP) vor und illustriert Anwendungsmöglichkeieten T2 - Seminar Instrumentelle Analytik, Fakultät III Prozesswissenschaften, Lehrstuhl Keramik TU Berlin CY - TU Berlin, Germany DA - 17.2.2017 KW - Sintern KW - Hochtemperaturformerkennung PY - 2017 AN - OPUS4-44210 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Gaber, Martin A1 - Reinsch, Stefan T1 - Volatile concentration and mobility measured by VHE-MS N2 - Der Vortrag schildert die Funktionsweise und einige ausgewählte Anwendungsmöglichkeieten der Vakuum-Heißextraktion an der BAM. T2 - Seminar Instrumentelle Analytik, Fakultät III Prozesswissenschaften, Lehrstuhl Keramik TU Berlin CY - TU Berlin, Germany DA - 17.2.2017 KW - Gehalt volatiler Spezies KW - Heißextraktion PY - 2017 AN - OPUS4-44212 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Glasig-kristalline Werkstoffe für Schlüsseltechnologien - Prozessbegleitende Prüfung und Simulation N2 - Eigenschaftsprofile und Kennwertstreuungen keramischer und glaskeramischer Komponenten und Bauteile werden durch ihren Herstellungsprozess wesentlich mitbestimmt. Prozessbegleitende Prüf- und Simulationsmethoden gewinnen so wachsenden Einfluss auf die Erschließung neuer Applikationsfelder dieser Werkstoffe. Eine wichtige Rol¬le spielen hierbei oft thermokinetische Prozesse, die u. a. Wärmetransport- und Diffusionsvorgänge, Phasengrenzflächenreaktionen, das rheologische Verhalten heterogener Systeme sowie deren Gefügeevolution beim Sintern umfassen. Ziel des Vortrages ist es, diesen Trend anhand ausgewählter Bei-spiele aus der Arbeit des Fachbereichs Glas der BAM zu illustrieren. T2 - Deutsche Physikalische Gesellschaft, Vortragsreihe Gruppe 60+ der Physiker Berlin - Brandenburg CY - Berlin, Magnushaus, Germany DA - 5.4.17 KW - Prozessbegleitende Prüfung KW - LTCC PY - 2017 AN - OPUS4-44217 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Agea Blanco, Boris A1 - Reinsch, Stefan T1 - Sintering and foaming of barium silicate glass powders N2 - The manufacture of sintered glasses and glass-ceramics, glass Matrix composites and glass-bounded ceramics or pastes is often affected by gas bubble formation. Against this background, we studied sintering and foaming of barium silicate glass powders used as SOFC sealants using different powder milling scenarios. Sintering was measured by means of heating microscopy backed up by XPD, DTA, Vacuum Hot Extraction (VHE) and optical and electron microscopy. Foaming increased significantly as milling progressed. For moderately milled glass powders, subsequent storage in air could also promote foaming. Although the powder compacts were uniaxially pressed and sintered in air, the milling environment significantly affected foaming. The strength of this effect increased in the order Ar >> N2 < air < CO2. Conformingly, VHE studies revealed that the pores of aerated samples predominantly encapsulated CO2, even for powders milled in Ar and N2. Results of this study thus indicate that foaming is caused by carbonaceous species trapped on the glass powder surface. Foaming could be substantially reduced by milling in water and 10 wt% HCl. T2 - 12th Pacific Rim Conference on Ceramic and Glass Technology CY - Waikoloa, Hawaii, USA DA - 21.5.2017 KW - Sintering KW - Gas bubble formation KW - Foaming PY - 2017 AN - OPUS4-44220 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Körner, S. T1 - Dissolution and reprecipitation of silver in sintering silver-glass dispersions N2 - Electric contacts based on silver-glass dispersions are key components in optoelectronic microsystems and control modules for medical, information & communication and energy technology in our networked society. Driven by the complexity of modern production processes and ever shorter time-to-market requirements, the fast and specific development of tailored silver-glass dispersions has become a bottleneck of technology development. Nevertheless, the underlying mechanisms of silver dissolution, transport, and reprecipitation, and the resulting micro structure evolution during firing are poorly understood. The broad literature on the precipitation of colloidal silver particles and the related processes of silver dissolution and diffusion mostly refer to very small volume fractions of silver. Transferring these results to the sintering of glass-containing silver dispersions, is therefore highly questionable. In this case, silver dissolution, electrical contact between silver particles, transport and reprecipitation take place under special conditions. This includes short diffusion lengths (particle size < 10 μm), the presence of three-phase contacts silver - glass - sintering atmosphere, as well as silver reprecipitation at the sintering contacts as the driving force of silver transport. Here, a dynamic balance of the silver concentration can be expected to result from the ratio between silver dissolution and reprecipitation. The aim of the project is to gain basic insight into the mechanisms of dissolution, transport and reprecipitation of silver in sintering silver glass dispersions. In this context, the main focus is on gaining basic knowledge about the dissolution of metallic silver in low melting oxide glasses as the limiting factor of the sintering of silver-glass composites. In particular, we will strive to gain insight into the effect of the oxygen content of the sintering atmosphere, of the oxygen dissolved in the silver particles, of silver oxide on the surface of the silver powder, of the electric contact between the silver particles, as well as the basicity of the glass. Furthermore, we strive for insights into the silver mobility and the silver concentration that can be attained (silver solubility) in oxide glasses with a low melting point. Summing up all these aspects, a closed explanatory model for silver dissolution, transport and reprecipitation during the sintering of glass silver dispersions will be introduced. T2 - DFG Begutachtungskolloquium (PAK 949/1 und PAK 950/1) CY - Bonn, Germany DA - 07.03.2017 KW - Sintering KW - Silver KW - Glass KW - Solubility KW - Reprecipitation PY - 2017 AN - OPUS4-44227 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Körner, S. T1 - Dissolution and reprecipitation of silver in sintering silver-glass dispersions N2 - Electric contacts based on silver-glass dispersions are key components in optoelectronic microsystems and control modules for medical, information & communication and energy technology in our networked society. Driven by the complexity of modern production processes and ever shorter time-to-market requirements, the fast and specific development of tailored silver-glass dispersions has become a bottleneck of technology development. Nevertheless, the underlying mechanisms of silver dissolution, transport, and reprecipitation, and the resulting micro structure evolution during firing are poorly understood. The broad literature on the precipitation of colloidal silver particles and the related processes of silver dissolution and diffusion mostly refer to very small volume fractions of silver. Transferring these results to the sintering of glass-containing silver dispersions, is therefore highly questionable. In this case, silver dissolution, electrical contact between silver particles, transport and reprecipitation take place under special conditions. This includes short diffusion lengths (particle size < 10 μm), the presence of three-phase contacts silver - glass - sintering atmosphere, as well as silver reprecipitation at the sintering contacts as the driving force of silver transport. Here, a dynamic balance of the silver concentration can be expected to result from the ratio between silver dissolution and reprecipitation. The aim of the project is to gain basic insight into the mechanisms of dissolution, transport and reprecipitation of silver in sintering silver glass dispersions. In this context, the main focus is on gaining basic knowledge about the dissolution of metallic silver in low melting oxide glasses as the limiting factor of the sintering of silver-glass composites. In particular, we will strive to gain insight into the effect of the oxygen content of the sintering atmosphere, of the oxygen dissolved in the silver particles, of silver oxide on the surface of the silver powder, of the electric contact between the silver particles, as well as the basicity of the glass. Furthermore, we strive for insights into the silver mobility and the silver concentration that can be attained (silver solubility) in oxide glasses with a low melting point. Summing up all these aspects, a closed explanatory model for silver dissolution, transport and reprecipitation during the sintering of glass silver dispersions will be introduced. T2 - DFG Begutachtungskolloquium (PAK 949/1 und PAK 950/1) CY - Bonn, Germany DA - 07.03.2017 KW - Sintering KW - Silver KW - Glass KW - Solubility KW - Reprecipitation PY - 2017 AN - OPUS4-44228 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 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 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 - 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 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 - JOUR A1 - Kiefer, P. A1 - Maiwald, M. A1 - Deubener, J. A1 - Balzer, R. A1 - Behrens, H. A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Müller, Ralf T1 - Automated Analysis of Slow Crack Growth in Hydrous Soda-Lime Silicate Glasses N2 - To explore the impact of ambient and structural water on static fatigue, the initiation and growth of 3279 Vickers induced median radial cracks were automatically recorded and analyzed. We find that humidity is more efficient in initiating cracks and promoting their growth than water, which is dissolved in the glass structure. In particular for slow crack growth (< 3x10-6 m s-1), tests in dry nitrogen showed a considerable decrease in the crack growth exponent with increasing water content of the glasses. On the other hand, if tests were performed in humid air, the crack growth exponent was independent of the water content of the hydrous glasses, while stress intensity decreased slightly. These observations indicate that water promotes the processes at the crack-tip regardless of its origin. However, ambient water is more efficient. KW - Indentation fracture toughness KW - Slow crack growth KW - Automated analysis KW - Hydrous glass KW - Vickers indentation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513085 DO - https://doi.org/10.3389/fmats.2020.00268 VL - 7 SP - 268 AN - OPUS4-51308 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 - JOUR A1 - Waurischk, Tina A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Kiefer, P. A1 - Deubener, J. A1 - Balzer, R. A1 - Behrens, H. T1 - Crack Growth in Hydrous Soda-Lime Silicate Glass N2 - Stable crack growth was measured for nominal dry and water-bearing (6 wt%) soda-lime silicate glasses in double cantilever beam geometry and combined with DMA studies on the effects of dissolved water on internal friction and glass transition, respectively. In vacuum, a decreased slope of logarithmic crack growth velocity versus stress intensity factor is evident for the hydrous glass in line with an increase of b-relaxation intensity indicating more energy Dissipation during fracture. Further, inert crack growth in hydrous glass is found to be divided into sections of different slope, which indicates different water related crack propagation mechanism. In ambient air, a largely extended region II is observed for the hydrous glass, which indicates that crack growth is more sensitive to ambient water. KW - Internal friction KW - Soda-lime silicate glass KW - Water content KW - Stable crack growth KW - DCB geometry KW - Stress intensity factor PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506829 DO - https://doi.org/10.3389/fmats.2020.00066 VL - 7 SP - Articel 66 AN - OPUS4-50682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agea Blanco, Boris A1 - Blaess, C. A1 - Reinsch, Stefan A1 - Brauer, D. A1 - Müller, Ralf T1 - Sintering and foaming of barium and calcium silicate glass powders N2 - Sintering and foaming of barium and calcium silicate glass powder compacts have been studied for different powder milling. Sintering was measured by means of heating microscopy backed up by XRD, DTA, Vacuum Hot Extraction (VHE) and electron microscopy. Foaming intensity strongly increased with decreasing glass partiefe size. Although powder compacts were uniaxially pressed and sintered in ambient air, foaming was affected by the milling atmosphere and most intensive for milfing in C02. Conformingly, VHE studies revealed that foaming of fully sintered samples was mainly driven by C02, even for powders milled in technical air, Ar and N2. Prolonged storage of air milled barium silicate glass powders in ambient air before pressing and sintering caused further increase of foaming intensity. These findings indicate that carbonaceous species are preferentially trapped to or close beneath the powder surface during milling and later storage. The temperature range of C02 degassing from fully sintered barium and calcium silicate g/ass powder compacts fits the temperature ranges of decomposition of BaC03 and CaC03 mix-milled with the respective barium and calcium silicate glass powders. T2 - IMAPS/ACerS 11th International CICMT conference and exhibition CY - Dresden, Germany DA - 20.04.2015 KW - Sintering KW - Foaming KW - Silicate glass powders KW - Barium and calcium silicate plass powders KW - Degassing PY - 2015 SN - 978-1510804562 SP - 31 EP - 37 AN - OPUS4-35250 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 - Reinsch, Stefan A1 - Brauer, D. T1 - Sintering and Foaming of Barium and Calcium Silicate Glass Powders T2 - IMAPS/ACerS 11th International Conference and Exhibition on Ceramic Interconnect and Ceramic Microsystem Technologies (CICMT 2015) CY - Dresden, Germany DA - 2015-04-20 PY - 2015 AN - OPUS4-35197 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Blaeß, Carsten A1 - Agea Blanco, Boris A1 - Sojref, Regine A1 - Brauer, D. S. T1 - Sintering and foaming of barium and calcium silicate glass powders T2 - Crystallization 2015 CY - Nagaoka, Japan DA - 2015-10-11 PY - 2015 AN - OPUS4-35198 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -