Resources Recycling (자원리싸이클링)

The Korean Institute of Resources Recycling (한국자원리싸이클링학회)
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Recovery of Silicon from Silicon Sludge by Electrolysis

실리콘 슬러지로부터 실리콘의 전해회수(電解回收)

  • Park, Jesik (School of Advanced Materials & System Eng., Kumoh National Institute of Technology) ;
  • Jang, Hee Dong (Nano-Materials Group, Korea Institute of Geoscience & Mineral Resources) ;
  • Lee, Churl Kyoung (School of Advanced Materials & System Eng., Kumoh National Institute of Technology)
  • 박제식 (금오공과대학교 신소재시스템공학부) ;
  • 장희동 (한국지질자원연구원 나노물질연구팀) ;
  • 이철경 (금오공과대학교 신소재시스템공학부)
  • Received : 2012.06.07
  • Accepted : 2012.08.06
  • Published : 2012.10.30
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Abstract

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.

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.

Keywords

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