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반도체급 삼염화실란 중의 극미량 인의 분광광도법적 정량
김동권,한명완,김희영,Dong Kwon Kim,Myoung Wan Han,Hee Young Kim 대한화학회 1992 대한화학회지 Vol.36 No.2
고순도 삼염화실란(TCS) 중의 미량 인(P) 불순물 농도를 흡착 분리 방법을 이용하여 분광광도법적으로 측정하는 방법을 제안하였다. TCS 중의 미량 불순물인 P 염화물을 보다 안정한 $POCl_3$로 산화시킨 다음, ethanol 용매에 잘 녹으며$POCl_3$와 안정된 부가화합물 complex를 형성하는 물질로서$AlCl_3$를 선택하여 분리해 내었다. 이러한 흡착을 이용한 농축 분리 방법을 통해 분석 도중에 실리카 겔 및 기포의 생성을 방지할 수 있었는데, 반도체급 TCS 중의 P 농도는 ${\pm}$ 17% 표준편차 범위내에서 5.32${\mi}g/l$로 측정되었다. 이와같이 $AlCl_3$로 P 화합물을 제거시킨 정제된 TCS 중의 P 농도는 0.15${\mi}g/l$이하로 측정되어 $AlCl_3$의 우수한 흡착 성능이 습식분석에 효과적으로 이용될 수 있음을 확인할 수 있다. 또한 TCS 정제 중 P 불순물 제거에 효과적인 것으로 알려진 다른 흡착 물질의 성능도 본 측정 방법으로 비교 분석하였다. A procedure for spectrophotometric determination of traces of phosphorus(P) in high-purity trichlorosilane(TCS) is proposed using an adsorptive separation. $PCl_3$, which is a dominant P impurity within TCS, is first oxidized by oxygen to a stable form as $POCl_3$. $AlCl_3$ is selected as an adsorbent which forms a thermally stable complex with $POCl_3$ in TCS and can be well dissolved in aqueous ethanol solution. The proposed adsorptive separation method is free from the formation of silica gel and gas bubbles during the colorimetric analysis of TCS. The method reveals that the P concentration in a semiconductor-grade TCS is 5.32 ${\mi}g/l$ within the standard deviation of ${\pm}$ 17%. On the other hand, the P concentration of the purified TCS which is separated from the $AlCl_3$${\cdot}$$POCl_3$ complex is reduced to be less than 0.15 ${\mi}g/l$, showing the efficient applicability of $AlCl_3$ to the wet chemical analysis. The proposed method is also tested to verify the effectiveness of other well-known adsorbents.
김동권,이정민,이보성 ( Dong Kwon Kim,Jung Min Lee,Bo Sung Rhee ) 한국화학공학회 1991 Korean Chemical Engineering Research(HWAHAK KONGHA Vol.29 No.2
Granulation is an operating process for solid treating in which powdered material grows into spherical granules of some sizes on a rotating disc by adding a certain amount of an appropriate binder and spraying water continuously. In this research a mathematical model for predicting the sizes growing granules with time was proposed and its applicability was examined through a series of experiments. Adhesion coefficient D increased as the feed rate(F) of powdered graphite decreased and when feed rate(F) was fixed, the D values increased as the spraying rate of water(W) and rpm(N) of the disc increased. An empirical correlation between adhesion coefficient D and operating variables was obtained as follows, D=0.560×10^(-3)((W/F)^(3.90)N^(1.50) Finally, the theoretical results of D from the proposed mathematical model were in good agreement with those from experiments and so the assumed model may well be applicable to other systems of spherical growing ball.
반도체급 삼염화실란중의 극미량 붕소의 분광 광도법적 측정
김동권,김희영,Dong Kwon Kim,Hee Young Kim 대한화학회 1991 대한화학회지 Vol.35 No.5
흡착 분리 방법을 이용하여 고순도 삼염화실란(TCS) 중의 미량 붕소 농도를 분광광도법적으로 측정하는 방법을 제안하였다. TCS중의 붕소 화합물과 복합체를 잘 형성하고 황산-quinalizarin계 발색 시약에 잘 녹으며 측정시 간섭 효과를 나타내지 않는 Lewis 염기성 물질로 NaCl이 선택되었다. 이러한 흡착 분리 방법을 통해 TCS분석 도중에 실리카겔 및 기포가 생성되는 문제를 방지할 수 있었는데, 반도체급 TCS중의 붕소 농도는 ${\pm}$20%의 표준편차 범위내에서 6.1 ${\mu}$g/l로 측정되었다. 반면 NaCl로 붕소화합물을 제거시킨 정제된 TCS 중의 붕소 농도는 0.2 ${\mu}$g/l이어서 NaCl의 우수한 흡착 성능을 확인할 수 있었다. 또한 NaCl이 TCS 정제 중 붕소 제거에 효과적임을 다른 잘 알려진 흡착제들과 비교 분석하였다. A procedure for spectrophotometric determination of traces of boron in high-purity trichlorosilane (TCS) is proposed utilizing an adsorptive separation. NaCl is chosen as an Lewis base adsorbent which forms a complex with boron compounds in TCS, and is well dissolved in sulfuric acid-quinalizarin color-forming agent without causing an interference in colorimetric measurements. The proposed adsorptive separation method is free from the formation of silica gel and gas bubbles during the analysis of TCS. The method reveals that the boron concentration in a semiconductor grade TCS is 6.1 ${\mu}$g/l within the standard deviation of ${\pm}$20%. On the other hand, the boron concentration of the purified TCS which is separated from NaCl-boron compounds complex is reduced to 0.2 ${\mu}$g/l, showing the efficient applicability of NaCl to the adsorptive separation. The effectiveness of NaCl for the removal of boron in TCS purification is also described in comparison with other well-known adsorbents.
중공 원형 소재로부터 다각형 튜브 제품의 평금형 전방 압출에 대한 최종단계의 상계해석
김동권,조종래,배원병,Kim, Dong Kwon,Cho, Jong Rae,Bae, Won Byong 한국정밀공학회 1995 한국정밀공학회지 Vol.12 No.11
In this study, a deformation model for the regular polygonal-shaped tubes from hollow-cylindrical billets is proposed and a kinematically admissible velocity field is obtained from this deformation model. The final stage upper-bound extrusion load and the average extruded length are determined by minimizing the total power consumption with respect to chosen parameters. Experiments have been carried out with hard solder billets at room temperature. The theoretical predictions of the extrusion load are in good agreements with the experimental results and there is generally reasonable agreement in average extruded height between theory and experiment.