지르콘의 탄소열환원에 의한 ZrC/SiC의 합성

Preparation of ZrC/SiC by Carbothermal Reduction of Zircon

Ar 또는 $Ar/H_2$ 가스유통(100~500ml/min)하에서 $ZrSiO_4/C$계 및 $ZrSiO_4/Al/C$계로부터 ZrC/SiC 복합분체의 합성을 $1600^{\circ}C$ 온도범위 내에서 시도하고, 이의 생성기구, 생성속도 및 분체특성을 검토하였다. $ZrSiO_4/C$계에서는 $1400^{\circ}C$ 이상에서 $ZrO_2(s)$와 SiO(g)가 각각 탄소와 경쟁반응하여 ZrC 및 SiC를 생성하였다. ZrC생성을 위한 겉보기활성화에너지는 약 18.5kcal/mol($1400-1600^{\circ}C$)이었다. 한편 $ZrSiO_4/Al/C$계에서는 $1200^{\circ}C$ 이상에서 ZrO(g)가 Al(l, g) 및 탄소와 반응하여 ZrC를 생성하였으며, $1300^{\circ}C$ 이상에서는 SiO(g)가 Al(l, g) 및 탄소와 환원-탄화반응하여 SiC를 생성하였다. $1600^{\circ}C$, 5시간 반응으로 얻은 생성물은 평균입경 $21.8{\mu}m$을 갖는 분말로서 ZrC의 격자정수는 $4.679{\AA}$, 결정자크기는 $640{\AA}$이었으며 SiC의 격자정수는 $4.135{\AA}$, 결정자크기는 $540{\AA}$ 정도이었다.

The preparation of ZrC/SiC mixed powders from $ZrSiO_4/C$ and $ZrSiO_4/Al/C$ systems was attempted in the temperature range below $1600^{\circ}C$ under Ar or $Ar/H_2$ gas flow(100-500ml/min). The formation mechanism and kinetics of ZrC/SiC were suggested and the resultant powders were characterized. In $ZrSiO_4/C$ system, ZrC and SiC were formed by competitive reaction of $ZrO_2(s)$ and SiO(g) with carbon at temperature higher than $1400^{\circ}C$. The apparent activation energy for the formation of ZrC was approximately 18.5kcal/mol($1400-1600^{\circ}C$). In $ZrSiO_4/Al/C$ system, ZrC was formed by reaction of ZrO(g) with Al(l, g) and carbon at temperature higher than $1200^{\circ}C$, and SiC was formed by reduction-carbonization of SiO(g) with Al(l, g) and carbon at temperature higher than $1300^{\circ}C$. The products obtained at $1600^{\circ}C$ for 5h consisted of ZrC with lattice constant of $4.679{\AA}$ and crystallite size of $640{\AA}$, and SiC with lattice constant of $4.135{\AA}$ and crystallize size of $500{\AA}$. And also, the mean particle size was about $21.8{\mu}m$.