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Fundamental understanding of crack healing in glassy crystalline materials is very important for solid oxide fuel cell (SOFC) sealants, since cracks caused by sealing or thermal cycling still remain a substantial bottleneck in developing durable SOFC.
Previous studies on soda lime silicate glass [Sin14] showed that crack healing is driven by viscous flow and that healing progress is proportional to time t and inverse viscosity η. This finding would allow to present healing data of a given glass for different temperatures in a master curve healing progress versus t/η. Such master curves would be a helpful tool in understanding crack healing kinetics.
Against this background, crack healing in non-crystallizing sodium calcium silicate (NCS) and sodium borosilicate glasses (NBS) have been studied. Moreover, to evaluate the influence of micro structure in crystallized glass on crack healing process, glass matrix composites (GMC) were prepared from NCS and zirconia as inert ceramic filler material mimicking a partially crystalline micro structure. By this way, the micro structure can be kept constant during crack healing. Cracks were generated by Vickers indention and healed isothermally at different temperatures. Crack healing progress was monitored by optical and electron microscopy. Results show that the above mentioned proportionality actually applies for the studied glasses for which such a master curve could be obtained. In comparison to a non-crystallized glass, the effective viscosity of GMC is increased by the rigid filler content. This effect substantially retards crack broadening during later healing stages, which often ends up in large pores. On the other hand, local viscous crack healing is still possible in larger glassy regions. This behavior seems to be very interesting for crack healing optimized micro structures.
Crack healing in glasses
(2017)
Fundamental understanding of crack healing in glassy crystalline materials is very important for many applications, especially for solid oxide fuel cells (SOFC) sealants since cracks caused by mechanical stress or thermal cycling still remain a substantial bottleneck in developing durable SOFC. Previous studies on soda lime silicate glass published by Singh showed that crack healing is driven by viscous flow. There he postulated that the healing progress is proportional to time, t, and the inverse viscosity. This finding would allow to present for a given glass data of crack healing measured at different temperatures in a master curve, if the healing progress is plotted versus t/η. Such master curves would be a helpful tool in understanding crack healing kinetics. To verify the applicability of such master curves, crack healing in non-crystallizing soda-lime-silicate (NCS) and sodium-borosilicate glasses (NBS) was studied. Cracks were generated by Vickers indention and healed isothermally at different temperatures. Crack healing progress was monitored by optical and electron microscopy. The results show that the above mentioned proportionalities applies to the two glasses. In both cases the afore developed master curve could be obtained.
Partially crystalline glasses are predominantly used as solid oxide fuel cell (SOFC) sealants due to their superior long term durability. However, cracks caused by thermal cycling still remain a substantial bottleneck in developing durable SOFC sealants inasmuch as, in contrast to crystal free glasses, large crystal volume fractions can retard healing. Hence, the basic understanding of crack healing in glassy crystalline materials and the effects of micro structure are important for finding optimum micro structures for both, durability and crack healing.
For studying these effects, several model glass matrix composites (GMC), for which simultaneous crystal growth and crack healing can be excluded, have been synthesized. Sodium calcium silicate glass – zirconia GMC turned out to provide sufficiently homogeneous, dense and durable model GMC for our studies. The microstructure of this GMC shows large crystal free glassy regions embedded in network of finely dispersed ZrO2 nanoscale crystals. Whereas the glassy regions allow easy local crack healing, the network of dispersed crystals increases the effective viscosity on a global scale. This effect substantially retards crack broadening during later healing stages, which often ends up in large pores. Therefore, this type of microstructure seems to be an interesting candidate for crack healing optimized sealants.
Fundamental understanding of crack healing in glassy crystalline materials is very important for many applications, especially for sealing solid oxide fuel cells (SOFC) since cracks caused by sealing or thermal cycling still remain a substantial bottleneck in developing durable SOFC.
Previous studies on soda lime silicate glass [Sin14] showed that crack healing is driven by viscous flow and that healing progress is proportional to time t and inverse viscosity η. This finding would allow to present healing data of a given glass for different temperatures in a master curve healing progress versus t/η. Such master curves would be a helpful tool in understanding crack healing kinetics.
Against this background, crack healing in non-crystallizing sodium calcium silicate (NCS) and sodium borosilicate glasses (NBS) have been studied. Moreover, to evaluate the influence of micros structure in crystallized glass on crack healing process, glass matrix composites (GMC) where prepared out of NCS and zirconia as inert ceramic filler material mimicking a partially crystalline micro structure. Cracks were generated by Vickers indention and healed isothermally at different temperatures. Crack healing progress was monitored by optical and electron microscopy. Results show that the above mentioned proportionality actually applies for the studied glasses for which such a master curve could be obtained. In comparison to a non-crystallized glass, the effective viscosity of GMC is increased by rigid filler content. This effect substantially retards crack broadening during later healing stages, which often ends up in large pores. On the other hand, local viscous crack healing is still possible in larger glassy regions. This behavior seems to be very interesting for crack healing optimized sealants.
Partially crystalline glasses are predominantly used as solid oxide fuel cell (SOFC) sealants due to their superior long term durability. However, cracks caused by thermal cycling still remain a substantial bottleneck in developing durable SOFC sealants inasmuch as, in contrast to crystal free glasses, large crystal volume fractions can retard healing. Hence, the basic understanding of crack healing in glassy crystalline materials and the effects of micro structure are important for finding optimum micro structures for both, durability and crack healing.
For studying these effects, several model glass matrix composites (GMC), for which simultaneous crystal growth and crack healing can be excluded, have been synthesized. Sodium calcium silicate glass – zirconia GMC turned out to provide sufficiently homogeneous, dense and durable model GMC for our studies. The microstructure of this GMC shows large crystal free glassy regions embedded in network of finely dispersed ZrO2 nanoscale crystals. Whereas the glassy regions allow easy local crack healing, the network of dispersed crystals increases the effective viscosity on a global scale. This effect substantially retards crack broadening during later healing stages, which often ends up in large pores. Therefore, this type of microstructure seems to be an interesting candidate for crack healing optimized sealants.
Fundamental understanding of crack healing in glassy crystalline materials is very important for many applications, especially for solid oxide fuel cells (SOFC) sealants since cracks caused by mechanical stress or thermal cycling still remain a substantial bottleneck in developing durable SOFC.
Previous studies on soda lime silicate glass published by Singh showed that crack healing is driven by viscous flow. He postulated that the healing progress is proportional to time, t, and the inverse viscosity. For a given glass, this finding would allow to present data of crack healing measured at different temperatures in a master curve, if the healing progress is plotted versus t/. Such master curves would be a helpful tool in understanding crack healing kinetics.
To verify the applicability of such master curves, crack healing in non-crystallizing soda-lime-silicate (NCS) and sodium-borosilicate glasses (NBS) was studied. Cracks were generated by Vickers indention and healed isothermally at different temperatures. Crack healing progress was monitored by optical and electron microscopy. The results show that the above mentioned proportionality applies to the two glasses and the afore developed master curve could be obtained in both cases.
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.
Bioglass® 45S5 is mainly used clinically as powders, granules or pastes instead of sintered compacts. This is due to the inherent problem of crystallization during the sintering, which results in poor mechanical properties and reduced bioactivity. Recently, new bioactive glasses with improved crystallization stability have been developed as promising candidates for manufacturing of sintered powder compacts for bone regeneration, which combine improved sintering behavior with bioactivity. Compared with the well-known Bioglass® 45S5 (SiO2-P2O5-CaO-Na2O) the calcium/alkali oxide ratio was increased, sodium oxide was partially replaced by potassium oxide and up to 3 mol% calcium fluoride were added, in order to stabilize the glass against crystallization. The aim of this study was to investigate the sintering and crystallization behavior of these new bioactive glasses.
Sintering and crystallization were characterized by heating microscopy, XRD, FTIR, SEM, and DTA. The results show that a sintered density of 88-99 % is achieved in contrast to only 57-67% for Bioglass® 45S5. In addition, FTIR and XRD analyses show that Bioglass® 45S5 crystallized during sintering while for the new glasses no crystalline phases are detected. The thermal properties of all glasses were studied by DTA measurements, and the influence of grain size was characterized. These studies showed that full densification can be attained for particle size < 32 µm, whereas coarser particles progressively increase residual porosity. Observed foaming phenomena, are strongly retarded by crystallization of beta-HAp.