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Synthesis of Tetramethylorthosilicate (TMOS) and Silica Nanopowder from the Waste Silicon Sludge
장희동,장한권,조국,길대섭,Jang, Hee-Dong,Chang, Han-Kwon,Cho, Kuk,Kil, Dae-Sup The Korean Institute of Resources Recycling 2007 資源 리싸이클링 Vol.16 No.5
폐실리콘 슬러지로부터 테트라메틸오쏘실리케이트(TMOS)와 실리카 나노분말을 제조하였다. 먼저, 실리카 나노분말의 전구체인 TMOS를 폐실리콘 슬러지로부터 촉매 화학반응에 의해 합성하였다. TMOS의 합성실험에서 반응온도가 $130^{\circ}C$ 이상에서는 반응시간이 5시간 경과 시 반응온도에 무관하게 100%의 반응율을 나타내었다. 그러나 $150^{\circ}C$ 이상에서는 초기 반응속도가 빨라졌다. 메탄올 주입속도를 0.8 ml/min에서 1.4 ml/min로 증가시에는 3시간 경과 후에는 반응율이 변화하지 않았다. 이와 같이 합성된 TMOS로부터 화염분무열분해법에 의해 실리카 나노분말을 제조하였다. 제조된 실리카 나노분말은 구형이며, 무응집 형태이었다. 평균입자 크기는 전구체의 주입속도 및 농도변화에 따라 9 nm에서 30 nm로 변화하였다. 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 $130^{\circ}C$. But the initial reaction rate became faster while the reaction temperature was higher than $150^{\circ}C$. As the methanol feedrate Increased from 0.8 ml/min to 1.4 ml/min, the yield of reaction was not varied after 3 hrs. 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.
특허(特許)와 논문(論文)으로 본 실리콘 슬러지의 재활용(再活用) 기술(技術) 동향(動向)
장희동,길대섭,장한권,조영주,조봉규,Jang, Hee-Dong,Kil, Dae-Sup,Chang, Han-Kwon,Cho, Young-Ju,Cho, Bong-Gyoo 한국자원리싸이클링학회 2012 資源 리싸이클링 Vol.21 No.4
반도체 및 태양광 산업에서는 반도체 소자 및 솔라셀을 제조하기 위하여 실리콘 웨이퍼가 사용되고 있다. 실리콘 웨이퍼는 실리콘 잉곳의 절단으로부터 만들어지며 이 공정에서 실리콘 슬러지가 발생한다. 반도체 소자의 사용처가 점점 증가함에 따라 실리콘 슬러지의 발생량 또한 증가하고 있는 실정이다. 최근 경제적인 측면과 효율성에 관한 측면에서 실리콘 슬러지의 재활용 기술이 폭넓게 연구되고 있다. 본 연구에서는 실리콘 슬러지의 재활용 기술에 대한 특허와 논문을 분석하였다. 분석범위는 1982년~2011년까지의 미국, EU, 일본, 한국의 등록/공개된 특허와 SCI 논문으로 제한하였다. 특허와 논문은 키워드를 사용하여 수집하였고, 기술의 정의에 의해 필터링하였다. 특허와 논문의 동향은 연도, 국가, 기업, 기술에 따라 분석하여 나타내었다. Silicon wafer for making semiconductor devices and solar cell is used in the semiconductor and solar industry, respectively. Silicon wafer is produced by cutting with silicon ingot and sludge contains silicon occurs from cutting process. Generation of silicon sludge is increasing on developing all industry sectors which have need of semiconductor device. These days it has been widely studied for the recycling technologies of the silicon sludge from view points of economy and efficiency. In this paper, patents and paper on the recycling technologies of the silicon sludge were analyzed. The range of search was limited in the open patents of USA (US), European Union (EU), Japan (JP), Korea (KR) and SCI journals from 1982 to 2011. Patents and journals were collected using key-words searching and filtered by filtering criteria. The trends of the patents and journals was analyzed by the years, countries, companies, and technologies.
장희동,윤호성 ( Hee Dong Jang,Ho Sung Yoon ) 한국공업화학회 1997 공업화학 Vol.8 No.6
유기금속화합물인 Tetraethylorthosilicate(TEOS)를 출발원료로 기상열분해법을 이용하여 초미립 실리카분말을 제조하였다. 반응온도, 가스유량, 반응물질의 농도, 및 반응물질의 예비가열온도가 초미립 실리카분말의 입자크기 특성에 미치는 영향을 조사하였다. 반응온도가 증가할수록 또한 체류시간이 감소할수록 생성분말의 입자크기가 작아지는 것을 알 수 있었다. 반응물농도가 증가할수록 입자크기가 증가하였고, 또한 반응물질의 예비가열온도가 증가하여도 입자크기는 큰 변화가 없음을 알 수 있었다. 본 연구조건에서 제조된 초미립 실리카분말의 평균 입자크기는 30∼58 nm이었다. Ultrafine silicon dioxide(SiO₂) powder was prepared from tetraethylorthosilicate(TEOS) by the gas-phase reaction. The effects of reaction temperature, flow rate of gas, TEOS concentration, and preheating temperature of reactants on the particle size were investigated. As the reaction temperature increased, average particle size of the silicone dioxide powder became smaller. Smaller particles were also obtained with decreasing the residence time of reactants in the reaction zone. Larger particles having narrow size distribution were produced with the high concentrations of the reactants. The effect of the preheating temperature was not considerable on the average particle size. The range of average particle size was from 30 nm to 58 nm depending on experimental conditions.
박제식,장희동,이철경,Park, Jesik,Jang, Hee Dong,Lee, Churl Kyoung 한국자원리싸이클링학회 2012 資源 리싸이클링 Vol.21 No.5
실리콘 웨이퍼공정에서 발생하는 실리콘 슬러지로부터 실리콘 및 탄화규소를 분리한 다음, 전해법으로 원소형태의 실리콘을 회수하는 연구를 수행하였다. 실리콘 슬러지의 주요 불순물은 절삭유, 금속불순물, 실리콘 및 실리콘 카바이드를 들 수 있다. 기계적 선별법으로 분리한 실리콘, 탄화실리콘 복합물을 $1000^{\circ}C$에 1시간동안 염화 배소하여 응축하고 회수한 사염화실리콘을 이온성액체인 $[Bmpy]Tf_2N$에 용해하여 전해액으로 사용하였다. 순환전위법으로부터 $[Bmpy]Tf_2N$의 안정한 전압구간과 사염화실리콘을 용해한 $[Bmpy]Tf_2N$ 전해액에서 실리콘의 환원으로 추정되는 환원피크를 얻을 수 있었다. 정전위법(-1.9 V vs. Pt-QRE)에서 1시간동안 금 전극 상에 전해한 다음, 전극표면을 XRD, SEM-EDS 및 XPS 분석을 통하여 실리콘이 원소형태로 전착되었음을 확인하였으며, 미량의 산소가 검출되는 것은 분석과정에서 시편이 공기 중에 노출되었기 때문으로 판단된다. As a recovery of elemental silicon from the sludge of Si wafer process, a process of mechanical separation-chlorine roasting-electrolysis has been suggested. The silicon sludge consisted of Si, SiC, machine oil, and metallic impurities. The oil and metal impurities was removed by mechanical separation. The Si-SiC mixture was converted to silicon chloride by chlorine roasting at $1000^{\circ}C$ for 1 hr and the silicon chloride was dissolved into an ionic liquid of $[Bmpy]Tf_2N$ as an electrolyte. Cyclic voltammetry results showed an wide voltage window of pure $[Bmpy]Tf_2N$ and a reduction peak of elemental Si from $[Bmpy]Tf_2N$ dissolved $SiCl_4$ on Au electrode, respectively. The silicon deposits could be prepared on the Au electrode by the potentiostatic electrolysis of -1.9 V vs. Pt-QRE. The elemental silicon uniformly electrodeposited was confirmed by various analytical techniques including XRD, FE-SEM with EDS, and XPS. Any impurity was not detected except trace oxygen contaminated during handling for analysis.
길대섭,장희동,장한권,조국,김선경,오경준,최진훈,Kil, Dae-Sup,Jang, Hee-Dong,Chang, Han-Kwon,Cho, Kuk,Kim, Sun-Kyung,Oh, Kyoung-Joon,Choi, Jin-Hoon 한국재료학회 2010 한국재료학회지 Vol.20 No.2
Surface modification of silica nanoparticles was investigated using an aerosol self assembly. Stearic acid was used as surface treating agent. A two-fluid jet nozzle was employed to generate an aerosol of the colloidal suspension, which contained 20 nm of silica nanoparticles, surface modifier, and ethyl alcohol. Powder properties such as morphology, specific surface area and pore size distribution were analyzed by SEM, BET and BJH methods, respectively. Surface properties of the silica power were analyzed by FT-IR. The OH bond of the $SiO_2$ surface was converted to a C-H bond. It was revealed that the hydrophilic surface changed to a hydrophobic one due to the aerosol self assembly. Morphology of the surface treated powder was nanostructured with lots of pores having an average diameter of around $2\;{\mu}m$. Depending on the stearic acid concentration (0.25 to 1.0 wt%), the pore size distribution of the particles and the degree of hydrophobicity ranged from 1.5 nm to 180 nm and 29.6% to 50.2%, respectively.