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Organisationseinheit der BAM
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.
Gläser zeichnen sich durch eine breite und kontinuierlich abstimmbare chemische Zusammensetzung sowie einzigartige Formgebungstechniken aus, was sie oft zur Schlüsselkomponente moderner Hochtechnologien macht. Die Glasentwicklung ist jedoch oft noch zu kosten-, zeit- und energieintensiv. Der Einsatz von robotergestützten Schmelzsystemen, eingebettet in eine Ontologie-basierte digitale Umgebung, soll diese Probleme in Zukunft überwinden. Im Rahmen der BMBF Forschungsinitiative MaterialDigital unternimmt das Verbundprojekt GlasDigital „Datengetriebener Workflow für die beschleunigte Entwicklung von Glas“ erste Schritte in diese Richtung. Das Projektkonsortium, an dem das Fraunhofer ISC in Würzburg, die Friedrich-Schiller-Universität Jena (OSIM), die Technische Universität Clausthal (INW) und die Bundesanstalt für Materialforschung und -prüfung (BAM, Fachgruppe Glas) beteiligt sind, will alle wesentlichen Basiskomponenten für eine beschleunigte datengetriebene Glasentwicklung zusammenführen. Zu diesem Zweck wird ein robotergestütztes Hochdurchsatz-Glasschmelzsystem mit neuartigen Inline-Sensoren zur Prozessüberwachung, auf maschinellem Lernen (ML) basierenden adaptiven Algorithmen zur Prozessüberwachung und -optimierung, neuartigen Werkzeugen für die Hochdurchsatz-Glasanalyse sowie ML-basierten Algorithmen zum Glasdesign, Data Mining sowie Eigenschafts- und Prozessmodellierung ausgestattet. Der Vortrag gibt einen Überblick darüber, wie all diese Komponenten miteinander verzahnt sind, und veranschaulicht ihre Nutzbarkeit anhand einiger Beispiele.
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.
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.
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.
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.
Das Hochtemperatur-Laserprofilometer der BAM4 ermöglicht eine 3D-Formerkennung an keramischen Folien oder anderen flachen Objekten während thermischer Behandlungen wie zum Beispiel bei laufenden Entbinderungs- oder Sinterprozessen. Mit dem Lasertriangulationssensor werden das Höhenprofil, die lateralen und axialen Schwindungen und andere charakteristische Maße der Probe wie die Folienbreite und -dicke, Abstände zwischen spezifischen Merkmalen oder Krümmungen bestimmt. Somit können insbesondere auch Deformationen und Verwerfungen der Objekte sowie Schwindungsinhomogenitäten an strukturierten Objekten erkannt und mit dem Herstellungsprozess verknüpft werden.
Hydrogen gas diffusivity of fourteen glasses of the Na2O-Al2O3-SiO2 system are studied along the joins quartzalbite-jadeite-nepheline (Qz-Ab-Jd-Np, fully polymerized) and albite-sodium disilicate (Ab-Ds, depolymerized).
Density measurements show that ionic porosity decreases from 54.4% (Qz) to 51.5% (Np) and from 52.4% (Ab) to 50.2% (Ds). Hydrogen diffusivity D follows similar trends but at another scale. D at 523 K decreases from 4×10−12 to 3×10−14m2 s−1 (Qz-Np) and from 4×10−13 to 3×10−15m2 s−1 (Ab-Ds). Charge compensating Na+ acting as a filling agent in fully polymerized network structures leads to up to one order of Magnitude higher diffusivities as depolymerized glass structures of the same SiO2 content where Na+ takes the role of a
modifier ion. Temperature dependence of the diffusivity indicates that both the activation energy involved with the moving H2 molecule as well as the accessible volume in the structure contribute to this compositional trend.
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.
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.
The permeation of hydrogen gas was studied in meta-aluminous (tectosilicate) glass powders of Li2O×Al2O3×SiO2 (LAS), Na2O×Al2O3×SiO2 (NAS) and MgO×Al2O3×SiO2 (MAS) systems by pressure loading and vacuum extraction in the temperatures range 210–310 °C. With this method, both the solubility S and the diffusivity D were determined, while the permeability was given by the product SD. For all glasses, S was found to decrease with temperature, while D increased. Since the activation energy of diffusion of H2 molecules exceeded that of dissolution, permeation increased slightly with temperature. When extrapolated to standard conditions (25 °C), the permeability of tectosilicate glasses was found to be only 10-22–10-24 mol H2 (m s Pa)-1, which is 8–10 magnitudes lower than most polymers. Thin glass liners of these compositions are expected to be the most effective barrier for tanks of pressurised hydrogen.
Physical storage of gaseous hydrogen under high-pressure in glassy micro-containers such as spheres and capillaries is a promising concept for enhancing safety and the volumetric capacity of mobile hydrogen storage systems. As very low permeation through the container wall is required for storage of compressed hydrogen, development of glasses of minimal hydrogen permeability is needed. For this purpose, one has to understand better the dependence of hydrogen permeability on glass structure. The paper points out that minimizing the accessible free volume is as one strategy to minimize hydrogen permeability. Based on previously measured and comprehensive literature data, it is shown that permeation is independently controlled by ionic porosity and network modifier content. Thus, ionic porosity in modified and fully polymerized networks can be decreased equally to the lowest hydrogen permeability among the glasses under study. Applying this concept, a drop of up to 30,000 with respect to the permeation of hydrogen molecules through silica glass is attainable.
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.
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.