초록
$K_2O-MgO-Al_2O_3$의 3성분계로부터 $K^+-{\beta}/{\beta}"-Al_2O_3$를 직접 고상반응법에 의하여 합성하였다. 합성시 초기조성, 합성온도, 합성시간 및 분쇄매체가 ${\beta}/{\beta}"-Al_2O_3$ 상형성 및 상관계에 미치는 영향에 대하여 분석하였으며 최대 분율의 ${\beta}"-Al_2O_3$ 상형성을 위한 최적 합성조건을 연구하였다. 조성범위로서 $K_2O$와 $Al_2O_3$상형성의 몰비를 1:5에서 1:6.2로, 안정화제로 사용된 MgO는 4.2 wt % 에서 6.3 wt % 사이에서 변화시켰으며 합성온도는 $1000^{\circ}C$에서 $1500^{\circ}C$까지 취하였다. ${\beta}/{\beta}"-Al_2O_3$상은 ${\alpha}-Al_2O_3$와 $KAlO_2$가 결합하는 $1000^{\circ}C$ 부근에서 형성되기 시작하여 점차 증가하다가 $1200^{\circ}C$ 부근에서 ${\alpha}-Al_2O_3$가 모두 사라지면서 균일화되었다. ${\beta}"-Al_2O_3$ 상분율은 $K_{1.67}Mg_{0.67}Al_{10.33}O_{17}$의 조성과 함께 $1300^{\circ}C$ 부근에서 최대값을 보였다. $1300^{\circ}C$ 이상의 합성 온도에서는 높은 potassium의 증기압에 따른 $K_2O$의 손실에 의하여 ${\beta}"-Al_2O_3$ 상분율이 감소하였으며 합성시간은 5시간 정도가 적당하였다. 분쇄 및 혼합을 위한 분산매체로는 증류수보다는 아세톤의 효과가 뛰어났다.
$K^+-{\beta}/{\beta}"-Al_2O_3$ in the ternary system $K_2O-MgO-Al_2O_3$ was directly synthesized by solid state reaction. The phase formation and phase relation were carefully investigated in relation to starting composition, calcining temperature and time, and dispersion medium. The optimal synthetic condition was also examined for the formation of ${\beta}"-Al_2O_3$ phase with a maximum fraction. As a composition range, the mole ratio of $K_2O$ to $Al_2O_3$ was changed from 1:5 to 1:6.2 and the amount of MgO used as a stabilizer was varied from 4.2 wt % to 6.3 wt %. The calcining temperature was selected between $1000^{\circ}C$ and $1500^{\circ}C$. At $1000^{\circ}C$, the ${\beta}/{\beta}"-Al_2O_3$ phases began to form resulted from the combining of ${\alpha}-Al_2O_3$ and $KAlO_2$ and increased with temperature rising. All of ${\alpha}-Al_2O_3$ phase disappeared to be homogenized to the ${\beta}/{\beta}"-Al_2O_3$ phase at $1200^{\circ}C$. Near the temperature at $1300^{\circ}C$, the fraction of ${\beta}"-Al_2O_3$ phase showed a maximum value with the composition of $K_{1.67}Mg_{0.67}Al_{10.33}O_{17}$. At temperatures above $1300^{\circ}C$, the fraction of ${\beta}"-Al_2O_3$ phase decreased gradually owing to $K_2O$ loss caused by a high potassium vapor pressure, and the appropriate calcining time was about 5 hours. Acetone was more effective than distilled water as a dispersion medium for milling and mixing.
