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Nowadays, the use of bioactive glasses is established for bone regeneration; however glasses are used mostly as powders, granules or in a paste. Sintered scaffolds are not used clinically, because of the inherent problem of crystallization during the sintering process, resulting in poor mechanical properties and reduced bioactivity. Therefore it was the aim to design new bioactive glasses, which combine improved processing and sintering 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 8 mol% calcium fluoride were added, in order to stabilize the glass against crystallization.
The sintering behavior of the new glasses was characterized by heating microscopy and compared to that of Bioglass® 45S5. Results show that the new glasses achieve a sintered density of 88-99 % in contrast to only 57-67% for Bioglass® 45S5. In addition, FTIR and XRD analyses show that Bioglass® 45S5 crystallizes during sintering while for the new glasses no crystalline phases were detected. The thermal properties of all glasses were studied by DTA and DSC measurements, and the influence of grain size was characterized. These studies showed an increase of sintering temperature and final porosity with increasing particle size. The structure of sintered compacts during and after sintering was examined using light and electron microscopy (SEM).
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.
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.