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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.
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.
We present an experimental approach to study the three-dimensional microstructure of gas diffusion layer (GDL) materials under realistic compression conditions. A dedicated compression device was designed that allows for synchrotron-tomographic investigation of circular samples under well-defined compression conditions. The tomographic data provide the experimental basis for stochastic modeling of nonwoven GDL materials. A plain compression tool is used to study the fiber courses in the material at different compression stages. Transport relevant geometrical parameters, such as porosity, pore size, and tortuosity distributions, are exemplarily evaluated for a GDL sample in the uncompressed state and for a compression of 30 vol.%. To mimic the geometry of the flow-field, we employed a compression punch with an integrated channel-rib-profile. It turned out that the GDL material is homogeneously compressed under the ribs, however, much less compressed underneath the channel. GDL fibers extend far into the channel volume where they might interfere with the convective gas transport and the removal of liquid water from the cell.
Ultraschall-Transmissionsmessungen werden seit Jahrzehnten bei der Qualitätssicherung von Betonkonstruktionen eingesetzt. Aus den Wellengeschwindigkeiten lassen sich dynamische Elastizitätsmoduln und – nach lokaler Kalibrierung – auch Druckfestigkeiten ermitteln. Zudem ergeben sich Hinweise auf Risse und andere Materialschwächungen. Der Einsatz erfolgt vor allem im Labor oder an der Bauwerksoberfläche. Neuerdings werden auch Monitoringsysteme mit eingebetteten Sensoren auf Ultraschallbasis erfolgreich getestet. Die Talsperre Eibenstock dient als größte Sperre in Sachsen der Trinkwasserversorgung und dem Hochwasserschutz. Hier wurden während der Bauphase im Jahr 1979 im Fußbereich des Mauerkörpers Ultraschallsensoren eingebracht, die in Verbindung mit einem Messoszilloskop eine Überwachung der Erhärtung des Mauerbetons ermöglichten.
Der für die Sensorauswahl eingesetzte Messstellenumschalter wurde im September 2011 grundlegend instand gesetzt. Danach zeigte sich, dass die eingebetteten Sensoren selbst sowie die Verkabelung auch nach über fünfunddreißig Jahren in einwandfreiem Zustand sind. Eine nunmehr aufgelegte Messserie mit modernem Gerät von über einem Jahr mit ein- bis zweimonatigen Intervallen zeigte, dass die Wellengeschwindigkeit seit der Bauphase noch einmal um gut 10 % zugenommen hat, was für eine erhöhte Druckfestigkeit spricht. Innerhalb des Jahres zeigten sich auch bei Einsatz neuer, sehr sensibler Auswertemethoden (sog. Codawelleninterferometrie) nur geringfügige Schwankungen. Diese waren auch nicht zu erwarten, da sich die Füllhöhe zu den Messzeitpunkten nur gering unterschied, die Temperatur im Bauwerksinneren nur wenig schwankte und der Bauwerkszustand sehr gut ist.
Die Aussagen zur Betongüte sind direkt vergleichbar mit den früheren Mess- und Untersuchungsergebnissen an der Talsperre Gottleuba, die im gleichen Zeitraum errichtet wurde und ebenfalls mit einem Ultraschallsystem ausgerüstet war. Die Experimente zeigten, dass ein Einsatz von Ultraschallsystemen für die Bauwerksüberwachung auch über Jahrzehnte möglich ist. Dies war im vorliegenden Fall nie geplant, aber durch den Einsatz der Mitarbeiter vor Ort und der Herstellerfirma möglich. Bei zukünftigen Systemen ist eine langfristige Planung unter Einbeziehung aller Beteiligten sowie eine Einbindung in Überwachungs- und Wartungspläne notwendig, damit die qualitätsgesichert gewonnen Daten gewinnbringend genutzt werden können.
The Collaborative Research Center InPROMPT aims to establish a novel process concept for the hydroformylation of long-chained olefins, using a rhodium complex as catalyst in the presence of syngas. Recently, the hydroformylation in micro-emulsions, which allows for the efficient recycling of the expensive rhodium catalyst, was found to be feasible. However, the temperature and concentration sensitive multi-phase system demands a continuous observation of the reaction to achieve an operational and economically feasible plant operation. For that purpose, we tested the potential of both NMR and Raman spectroscopy for process control assistance. The lab-scale experiments were supported by sampling for off-line GC-analysis as reference analytics. The results of the NMR experiments will be part of another contribution.
Hydroformylation represents an important homogeneous catalyzed process, which is widely used within chemical industry. Usually applied with simple alkenes like Propene and Butene aldehydes obtained from alkenes >C6 are relevant intermediates in production of plasticizers, surfactants and polymers. Today the active catalyst species is often based on valuable Rhodium complexes in aqueous solution. This implies the problem of limited water solubility of the reactands, which is acceptable for short chain lengths, but states a problem in case of higher alkenes. Along with that efficient separation and recycling of the catalyst becomes more complicated. There are different approaches tackling this problem, e.g., by using of salt formation in the BASF process or downstream distillation within the Shell process