반도체 웨이퍼 제조 공정 중 발생하는 질산, 불산, 초산으로 구성된 혼합폐산을 재활용하기 위한 연구를 수행하였다. 초기에 $NaNO_3$와 Si powder를 사용하여 불산을 $Na_2SiF_6$로 침전시켜 불소화합물을 제조하였고, 이 때 혼산 중 불산의 농도는 초기 127g/L에서 0.5g/L로 낮아져 불산 회수율은 99.5%였다. $Na_2SiF_6$ 제조 후 남은 혼산의 질산과 초산의 농도는 각각 502g/L, 117g/L였고, 이 혼산에 NaOH를 투입하여 pH=4로 맞춘 후 -440 mmHg, $95^{circ}C$에서 증발농축을 하여 초산 분리 회수하였다. 회수된 초산의 농도는 약 15%였고, 회수율은 85.3% 이상이었다. 또한, 농축여액을 $20^{circ}C$까지 냉각하여 $NaNO_3$ 결정을 석출시킴으로 질산나트륨을 제조하였고, 그 회수율은 약 93%이상이었다. 제조된 $Na_2SiF_6$와 $NaNO_3$를 $90^{circ}C$에서 건조시킨 후, XRD 분석한 결과, 순수 $Na_2SiF_6$와 $NaNO_3$만 합성된 것을 확인하였고, 그 순도는 각각 약 97%, 98%로 시판용과 유사하였다.
We researched separation of mixed waste acids with HF, $CH_3COOH$, $HNO_3$ that were produced during a semiconductor wafer process to recycle these acids. At first, we manufactured the fluoride compound in form of $Na_2SiF_6$ by precipitating HF using $NaNO_3$ and Si powder. The concentration of HF was reduced from the initial concentration of 127 g/L to 0.5 g/L with an HF recovery ratio of 99.5%. After the manufacture of $Na_2SiF_6$, the concentration of $HNO_3$ and $CH_3COOH$ demonstrated 502 g/L and 117 g/L respectively. Following these findings we added NaOH in this $CH_3COOH/HNO_3$ mixed acid in order to obtain pH=4. Next we separated the $CH_3COOH$ and recoverd it through the use of vaccum evaporation at -440 mmHg, $95^{circ}C$. The concentration of the recovered $CH_3COOH$ was approximately 15% and the recovery ratio of $CH_3COOH$ was over 85%. We precipitated the $NaNO_3$ by cooling the concentrated solution to $20^{circ}C$ with a $HNO_3$ recovery ratio of over 93%. We confirmed that only $Na_2SiF_6$ and $NaNO_3$ were manufactured by XRD analysis after drying these precipitants at $90^{circ}C$. The precipitants demonstrated a purity of approximately 97% and 98% respectively. Therefore, the purity of the precipitants proved to be similar to that of commercial products.
