This work proposes four different glass formulas derived from the SiO 2 -Li 2 O-K 2 O-Al 2 O 3 system to investigate the effect of glass composition on their crystal formations and properties. Glass LD1 was SiO 2 -Li 2 O-K 2 O-Al 2 O 3 system with the addition of P 2 O 5 and CaF 2 as nucleating agents. In Glass LD2, a slight amount of MgO was mixed in order to increase the viscosity of the melting glass. Finally, the important factor of Si : Li ratio was increased in Glasses LD3 and LD4 with compositions otherwise the same as LD1 and LD2. The results found that P 2 O 5 and CaF 2 served as a nucleating site for lithium phosphate and fluorapatite to encourage heterogenous nucleation and produce a fine-grained interlocking microstructure of lithium disilicate glass ceramics. MgO content in this system seemed to increase the viscosity of the melting glass and thermal expansion coefficient including the chemical solubility. Increasing the Si : Li ratio in glass compositions resulted in the change of the microstructure of Li 2 Si 2 O 5 crystals.
Barium-free glass-ceramic sealants for the planar solid oxide fuel cell (pSOFC) have attracted considerable attention to avoid the crystallization of the high coefficient of thermal expansion (CTE) BaCrO4; reaction product at the interface between barium-containing glass-ceramic sealants and Crofer22 APU interconnect, which decreases the long-term mechanical stability of the sealant. In this study, Barium-free glass-ceramic sealants in the CaO-MgO-B2O3-Al2O3-SiO2 system with varying amounts of Bi2O3 from 0 to 10 wt. % were prepared by conventional melting and their thermal properties were investigated. The glass transition temperature (Tg), dilatometric softening temperature, and coefficient of thermal expansion (CTE) were determined by a dilatometer. The Tg, onset of crystallization (Tx) and crystallization temperature (Tc) were obtained from DTA. Results of phase analysis by X–ray diffraction of glasses after thermal treatment at 900 oC for 2 h indicated that the major phase of all glasses was diopside (MgCaSi2O6) and minor phases were åkermanite (Ca2MgSi2O7) and forsterite (Mg2SiO4). The Tg of the fabricated glasses tended to decrease with increasing Bi2O3 content while the CTE of glasses increased after the thermal treatment and was in the range of requirement for SOFC sealant.
This work proposes three different glass formula derived from the SiO2-Li2O-K2O-Al2O3 system to investigate the effect of glass compositions on their crystal formation and mechanical properties. Glass LD_1 was SiO2-Li2O-K2O-Al2O3 system with adding P2O5 and CaF2 as nucleating agents. In Glass LD_2, a few amount of MgO was mixed to improve the viscosity of the glass. Finally, an important factor of Si:Li ratio was increased in Glass LD_3. Glass batches were melted at 1500°C and cast into a graphite mold which was annealed at 400-500°C before heat treatment at 700, 750, 800 and 850°C.
XRD results can be indexed Li2Si2O5, Li2SiO3, Ca5(PO4)3F and SiO2 as an early crystallization when heat treated at 700°C. After heat treatment at 750-850°C, the intensity of SiO2 disappeared and the peaks associated to Li3PO4 appeared; meanwhile, Li2Si2O5 increased in intensity. Adding MgO resulted in decreasing the viscosity of the glass with no significant effects on the formation of lithium disilicate. By increasing Si:Li ratio, the peak of SiO2 more obviously observed. SEM results revealed the development of microstructure from plate-like to interlocking rod-shaped crystals in all glasses. The highest indentation fracture toughness and biaxial flexural strength found in all glass ceramics heat treatment at 800°C because the finest microstructure observed at this temperature, except LD_3 heat treated at 850°C, which obtained the finest microstructure. LD_1 heat treated at 850°C presented the best chemical solubility 59 μg/cm2.
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