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기상반응에 의한 초미립 무기분말 제조시 입자성장 모델연구 - 초미립 철분말 제조에의 응용 -
박균영,오의경,김선근,장희동 ( Kyun Young Park,Eui Kyung Oh,Sun Geon Kim,Hee Dong Jang ) 한국화학공학회 1996 Korean Chemical Engineering Research(HWAHAK KONGHA Vol.34 No.4
Presented is a model for the prediction of the particle size distribution of inorganic powders made by the gasphase reaction. The assumption used in previous models that a monomer forms a nucleus is eliminated; the model incorporates the determination of the number of monomers required to form a nucleus and the nucleation rate based on the classical theory. The present model was applied to a manufacture of ultrafine iron powders by hydrogen reduction of FeCl₂ vapor. The average particle size of the iron powder predicted by the model was one half to two thirds of the experimental value. For a reaction temperature of 900℃, the model could fit the experimental diameter by using the surface tension of iron 1.283 times as high as that in the literature. The model prediction agrees well with experimental observation in the trend of particle size increasing with the feed rate of FeCl₂. The model, however, showed a deviation from experimental observations on the effects of the reaction temperature and of the preheating temperature on the particle size. Further investigation needs to be followed to correct the model.
박균영 ( Kyun Young Park ),이미선 ( Mi Sun Lee ),김민철 ( Min Cheol Kim ),이찬희 ( Chan Hee Lee ),박회경 ( Hoey Kyung Park ),강태원 ( Tae Won Kang ),정해성 ( Hae Seong Jeong ),한경아 ( Kyoung Ah Han ),허원회 ( Weon Hoe Huh ),유지 한국화학공학회 2013 Korean Chemical Engineering Research(HWAHAK KONGHA Vol.51 No.3
The chlorination of a metallurgical-grade silicon was carried out in a fluidized bed reactor, 25 mm in diameter. The flow rate of the chlorine admitted into the reactor was 0.2 L/min and that of the carrier nitrogen was 0.8~1.0 L/ min. The reactor temperature was maintained at 450℃ and the temperature of the coolant at the SiCl4 condenser was at -5℃. The SiCl4 yield increased with increasing the mole fraction of chlorine in the feed gas, exhibiting 28% at the mole fraction of 0.2. Further increase of the chlorine mole fraction was not attempted in a worry that the reactor might be failed due to the high exothermicity of the reaction. The production of SiCl4 from silicon by fluidized bed chlorination was demonstrated on a laboratory scale, which is a stepping stone for future studies under more severe conditions toward industrial application.
실리콘 웨이퍼 절단공정(切斷工程)에서 발생(發生)하는 실리콘 카바이드 슬러지로부터 철(鐵), 실리콘 제거(除去)
박회경,고봉환,박균영,강태원,장희동,Park, Hoey Kyung,Go, Bong Hwan,Park, Kyun Young,Kang, Tae Won,Jang, Hee Dong 한국자원리싸이클링학회 2013 資源 리싸이클링 Vol.22 No.2
실리콘 슬러지로부터 원심분리에 의해 1 단계로 실리콘(Si)을 분리 한 후 남게 되는 실리콘 카바이드(SiC) 농축물 내에 포함되어 있는 철과 잔존하는 실리콘을 추가적으로 제거함으로써 실리콘 카바이드의 순도를 향상 시킬 수 있는 가능성을 탐색해 보았다. 실리콘 카바이드 농축물을 대상으로 하여 염산(HCl)/수산화나트륨(NaOH)에 의한 액상 침출법과 염소 가스에 의한 기상 염소화법을 비교해 보았다. 실리콘 카바이드 농축물을 1 M 염산 수용액에서 $80^{\circ}C$에서 1 시간 동안 침출시킴으로써 회수된 실리콘 카바이드에 잔류하는 철의 농도를 49 ppm 까지 제거하였으며, 1 M 수산화나트륨 수용액에서 $50^{\circ}C$에서 1 시간 동안 침출시킴으로써 실리콘 카바이드 내 잔류하는 실리콘의 농도를 860 ppm 까지 제거하였다. 기상 염소화 반응은 직경 2.4 cm, 길이 32 cm의 전기로에 의해 가열되는 알루미나 튜브의 중심에 실리콘 카바이드 농축물을 위치시키고, 질소와 염소의 혼합가스를 흘려보내는 방식에 의해 이루어졌는데, 반응온도 $500^{\circ}C$, 반응시간 4 시간, 가스유량 300 cc/min, 염소 몰분율 10%의 조건 하에서 실리콘 카바이드 내 철과 실리콘의 잔류 농도를 48 ppm과 405 ppm 까지 낮출 수 있었다. In the present study, the possibility of recovering and recycling the silicon carbide(SiC) from a silicon sludge by removing Fe and Si impurities was investigated. Si and SiC were separated from the silicon sludge using centrifugation. The separated SiC concentrate consisted of Fe, Si and SiC, in which Fe and Si were removed to recover the pure SiC. Leaching with acid/alkali solution was compared with the vapor-phase chlorination. The Fe concentration removed in the SiC was 49 ppm, and it was separated by leaching with 1 M HCl solution at $80^{\circ}C$ for 1 h. The Si concentration removed in the SiC was 860 ppm, and it was separated by leaching with 1M NaOH solution at $50^{\circ}C$ for 1 h. The SiC concentrate was chlorinated in a tubular reactor, 2.4 cm in diameter and 32 cm in length. The boat filled with SiC concentrate was located at the midpoint of the alumina tube, then, the chlorine and nitrogen gas mixture was introduced. The Fe and Si concentration removed in the SiC were 48 ppm and 405 ppm, respectively, at $500^{\circ}C$ reactor temperature, 4 h reaction time, 300 cc/min gas flow rate, and 10% $Cl_2$ gas mole fraction.
염화알미늄 증기의 부분가수분해를 통한 알파 알루미나 나노입자 제조
박회경 ( Hoey Kyung Park ),유연석 ( Youn Sug Yoo ),박균영 ( Kyun Young Park ),정경열 ( Kyeong Youl Jung ) 한국화학공학회 2011 Korean Chemical Engineering Research(HWAHAK KONGHA Vol.49 No.5
Spherical alumina precursors represented by (AlO)x(Cl)y(OH)z, 30~200 nm in particle diameter, were prepared by partial hydrolysis of AlCl3 vapor in a 500 ml reactor. Investigated on the particle morphology and size were the effects of the reaction time, the stirring speed and the reaction temperature. The particle morphology and size was insensitive to the reaction time in the range 20 to 300 s. The variation of the stirring speed from 0 to 300 and 800 rpm showed that the particle size was the largest at 0 rpm. As the temperature was varied from 180 to 190, 200, 140 °C, the particle size showed a maximum at 190 ˚C. By calcination of the as-produced particles at 1,200 °C for 6h with a heating rate of 10 °C/min, α-alumina particles 45 nm in surface area equivalent diameter were obtained. The particle shape after calcination turned wormlike due to sintering between neighboring particles. A rapid calcination at 1400 °C for 0.5 h with a higher heating rate of 50 °C/min reduced the sintering considerably. An addition of SiCl4 or TMCTS(2,4,6,8-tetramethylcyclosiloxane) to the AlCl3 reduced the sintering effectively in the calcination step; however, peaks of γ or mullite phase appeared. An addition of AlF3 to the particles obtained from the hydrolysis resulted in a hexagonal disc shaped alumina particles.