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Synthesis of Iron Nanopowder from FeCl3 Solution by Chemical Reduction Method for Recycling of Spent Neodymium Magnet

네오디뮴 폐자석 재활용을 위한 화학환원법을 이용한 철 나노 분말 제조

  • Ha, Yonghwang (Department of Resources Recycling and Environmental Engineering, Jungwon University) ;
  • Gang, Ryun-Ji (Department of Resources Recycling and Environmental Engineering, Jungwon University) ;
  • Choi, Seung-Hoon (Department of Environmental & Chemical Engineering, Seonam University) ;
  • Yoon, Ho-Sung (Korea Institute of Geoscience and Mineral Resources) ;
  • Ahn, Jong-Gwan (Department of Resources Recycling and Environmental Engineering, Jungwon University)
  • 하용황 (중원대학교 자원순환환경공학과) ;
  • 강윤지 (중원대학교 자원순환환경공학과) ;
  • 최승훈 (서남대학교 환경화학공학과) ;
  • 윤호성 (한국지질자원연구원) ;
  • 안종관 (중원대학교 자원순환환경공학과)
  • Received : 2012.11.13
  • Accepted : 2012.12.06
  • Published : 2012.12.31

Abstract

Recycling process of iron should be developed for efficient recovery of neodymium(Nd), rare metal, from acid-leaching solution of neodymium magnet. In this study, $FeCl_3$ solution as iron source was used for synthesis of iron nanoparticle with the condition of various factors, etc, reductant, surfactant. $Na_4O_7P_2$ and polyvinylpyrrolidone(PVP) as surfactants, $NaBH_4$ as reductant, and palladium chloride($PdCl_2$) as a nucleation seed were used. Iron powder was analyzed with instruments of XRD, SEM and PSA for measuring shape and size. Iron nanoparticles were made at the ratio of 1 : 5(Fe (III) : $NaBH_4$) after 30 min of reduction time. Size and shape of iron particles synthesized were round-form and 50 nm ~ 100 nm size. Zeta-potential of iron at the 100 mg/L of $Na_4O_7P_2$ was negative value, which is good for dispersion of metal particle. When $Na_4O_7P_2$(100 mg/L), PVP($FeCl_3$ : PVP = 1 : 4, w/w) and Pd($FeCl_3$ : $PdCl_2$ = 1 : 0.001, w/w) were used, iron nanoparticles which are round-shape, well-dispersed, near 100 nm-sized can be made.

네오디뮴 폐자석 침출액으로부터 희유금속인 네오디뮴을 회수하기 위해서는 네오디뮴과 같이 침출되는 철의 부가가치를 높이는 연구가 필요하다. 본 연구에서는 네오디뮴과 같이 침출되는 철의 유용자원화를 위한 기초연구로 철 나노분말 제조하는 실험을 수행하였다. 본 연구는 $FeCl_3$ 용액을 철 분말 원료로, 분산제는 $Na_4O_7P_2$와 Polyvinylpyrrolidone를 이용하였고, 환원제로는 $NaBH_4$, 철 나노분말 핵생성 촉진제 시드(seed)로 염화팔라듐을 사용하였다. 제조한 철 나노분말을 XRD, 전자현미경(SEM) 및 PSA 등을 이용하여 분말의 형상 및 크기 등을 분석하였다. 철과 $NaBH_4$의 농도비가 1 : 5이며, 반응시간이 30분 이상인 경우에서 철 분말이 제조되었으며, 이때 철 분말은 구형이었으며, 입도는 약 50 nm ~ 100 nm 크기였다. 분산제 $Na_4O_7P_2$의 경우 100 mg/L에서 철이온의 제타포텐셜이 음의 값을 가지므로 100 mg/L로 일정하게 하고, PVP와 Pd의 농도를 다양하게 하였을 경우, $FeCl_3$와 PVP와 Pd의 질량비 1 : 4 및 1 : 0.001에서, 분산이 양호하고, 입도 100 nm 크기인 철 나노분말을 합성하였다.

Keywords

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