Preparation of Ultra-Low Thermal Expansion L$i_2$O-A$l_2$$O_3$-Si$O_2$ Glass-Ceramics by Sol-gel Technique

졸-겔 방법에 의한 $Li_2O-Al_2O_3-SiO_2$계 저열팽상성 결정화유리의 제조

  • Published : 1993.06.01

Abstract

Glass-ceramic monoliths with an ultra-low thermal expansion coefficient have been synthesized by the sol-gel technique using metal alkoxides as starting materials and dimethyl formamide as a drying control chemical additive. The ternary gels: $Li_2O\cdot Al_2O_3\cdot 2, 4 or $6SiO_2$ were obtained by hydrolysis and polycondensation reactions of metal alkoxides of silicon, aluminum and lithium. To produce cylindrical crack-free gel monoliths, excess water was used to the starting solutions and drying rates were controlled precisely to prevent cracking. In conversion process ,${\beta}$-eucryptite, $Li_2O\cdot Al_2O_3\cdot 3SiO_2$ and P-spodumene with ,${\beta}$-quartz solid solution phase were obtained by heating at the range of 750 ~$1000^{\circ}C$. Above $800^{\circ}C$, the ,${\beta}$-spodumene phase increased while ,${\beta}$-eucryptite phase decreased. The thermal expansion coefficient of the crystallized specimens were -15~ $+5{\times}{10^{-7}}/{\circ}C$ over the temperature range from room temperature to $600^{\circ}C$.

$Li_2O-Al_2O_3-SiO_3$계 결정화유리의 저온합성을 위하여 출방원료로서 각 해당 금속 알콕시드를 사용하였다. 알코올을 용매로 충분히 첨가하고, drying control chemical additive로 dimethy1 formamide를 적당량 첨가한 혼합용용액을 과잉의 물로 충분히 가수분해시킨 습윤겔을 저온으로 건고하여 균열이 없는 건조된 monolith겔을 합성하였다. 건조겔로부터 750-$950^{\circ}C$로 10시간 이상 소결하여 저열팽창성을 나타내는 ${\beta}$-eucrypytite(${\beta}$-quartz 고용체), $Li_2O\cdot Al_2O_3\cdot 3SiO_2$${\beta}$-spodumene등의결정상을 석출시켰다.

Keywords

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