基于β-锂霞石负膨胀陶瓷填料的无铅低温封接玻璃结构性能研究

The Performance of Lead-free Low Temperature Sealed Glass Based on β-eucryptite Negative Expansion Ceramic Filler

陶瓷填料直接影响复合型低温封接玻璃的结构及性能,β-锂霞石是无铅低熔点封接玻璃优选填料之一。本文采用固相烧结法直接合成负膨胀卜锂霞石陶瓷材料,研究不同烧结工艺对其结构的影响,结果显示在1300℃二次重烧结可以获得致密的单相锂霞石结构,其膨胀系数为-70×10^-7K^-1,破碎后的多晶团聚颗粒可作为Bi2O3-ZnO-B2O3玻璃的负膨胀填料制备复合型低温封接玻璃。研究发现,随填料添加量增加,封接玻璃的膨胀系数降低,当添加量为10wt.%时,膨胀系数由113×10^-7K^-1降低至90×10^-7K^-1,且软化温度和流动性影响较小。此外,该β-锂霞石与基础玻璃具有很好的相容性,粘接界面致密无气孔且无可见微观裂纹,界面处无明显化学反应。本文为超低温无铅封接玻璃的制备提供给了一种较优的填料解决方案。

The structure and properties of composite sealing-glass are detennined partially by the ceramic filler,and the β-eucryptite is a preferred choice for the preparation of lead-free sealing glass.In this paper,the β-eucryptite ceramic was synthe sized by sintering,and the effect of the process on its structural properties was also studied.The results show that the secondary sintering process at 1300 ℃ could obtain dense and pure-phase β-eucryptite structure,and its coefficient of thermal expansion is -70×10^-7K^-1,which can be used as an expansion coefficient adjuster after being crushed in Bi2O3-ZnO-B2O3 glass.It was found that the expansion coefficient decreased with the increase of the filler content,and the expansion coefficient decreased from 113×10^-7K^-1 to 90×10^-7K^-1 when the addition amount was 10wt%,and the ceramic filler has little effect on glass softening point and liquidity.In addition,the β-eucryptite and the base glass have a good compatibility,there is no pore and no visible mi cro-cracks in the bonding interface.So,this paper provides a better filler solution for low melting sealing glass.