廢실리콘슬러지로부터 TMOS 및 실리카 나노粉末 製造
Synthesis of Tetramethylorthosilicate(TMOS) and Silica Nanopowder from the Waste Silicon Sludge
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초록
폐실리콘 슬러지로부터 테트라메틸오쏘실리케이트(TMOS)와 실리카 나노분말을 제조하였다. 먼저, 실리카 나노분말의 전구체인 TMOS를 폐실리콘 슬러지로부터 촉매 화학반응에 의해 합성하였다. TMOS의 합성실험에서 반응온도가 130oC 이상에서는 반응시간이 5시간 경과 시 반응온도에 무관하게 100%의 반응율을 나타내었다. 그러나 150oC 이상에서는 초기 반응속도가 빨라졌다. 메탄올 주입속도를 0.8ml/min 에서 1.4ml/min로 증가시에는 3시간 경과 후에는 반응율이 변화하지 않았다. 이와 같이 합성된 TMOS로부터 화염분무열분해법에 의해 실리카 나노분말을 제조하였다. 제조된 실리카 나노분말은 구형이며, 무응집 형태이었다. 평균입자크기는 전구체의 주입속도 및 농도변화에 따라 9nm에서 30nm로 변화하였다.
Abstract
Tetramethylorthosilicate (TMOS) and silica nanopowder were synthesized from the waste silicon sludge containing 15% weight of silicon powder. TMOS, a precursor of silica nanopowder, was firstly prepared from the waste silicon sludge by catalytic chemical reaction. The maximum recovery of the TMOS was 100% after 5 hrs regardless of reaction temperature above 130oC. But the initial reaction rate became faster while the reaction temperature was higher than 150oC. As the methanol feedrate increased from 0.8ml/min to 1.4ml/min, the yield of reaction was not varied after 3hrs. Then, silica nanopowder was synthesized from the synthesized TMOS by flame spray pyrolysis. The morphology of as-prepared silica nanopowder was spherical and non-aggregated. The average particle diameters ranged from 9 nm to 30 nm and were in proportional to the precursor feed rate, and precursor concentration.
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