Journal of the Korean Magnetics Society (한국자기학회지)

The Korean Magnetics Society (한국자기학회)
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Study on Formation Mechanism of Iron Oxide Nanoparticles

산화철 나노입자의 형성 메커니즘에 대한 연구

  • Kim, Dong-Young (Department of Physics, Andong National University) ;
  • Yoon, Seok-Soo (Department of Physics, Andong National University) ;
  • Takahashi, Migaku (Department of Materials Science and Engineering, Chungnam National University, New Industry Creation Hatchery Center, Tohoku University)
  • Received : 2012.10.05
  • Accepted : 2012.10.19
  • Published : 2012.10.31
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Abstract

In order to analyze the formation mechanism of iron oxide nanoparticles, we measured the heat flow of $Fe(OL)_3$ precursor with temperature, and TEM images and AC susceptibility of aliquots samples sequentially taken from the reaction solution, respectively. The thermal decomposition of two OL-chain from $Fe(OL)_3$ produced the Fe-OL monomer, which were contributed to the formation of iron oxide nanoparticles. In the initial stage of nanoparticles formation, the small iron oxide nanoparticles had ${\gamma}-Fe_2O_3$ structure. However, as the iron oxide nanoparticles were rapidly growth, the iron oxide nanoparticles showed ${\gamma}-Fe_2O_3$-FeO core-shell structure which the FeO layer was formed on the surface of ${\gamma}-Fe_2O_3$ nanoparticles by insufficient oxygen supply from the reaction solution. These nanoparticles were transformed to $Fe_3O_4$ structure by oxidation during long aging time at high temperature. Finally, the $Fe_3O_4$ nanoparticles with high saturation magnetization and stable in the air could be easily synthesized by the thermal decomposition method.

본 연구에서는 $Fe(OL)_3$ 전구체가 고온에서 열분해 한 후 산화철 나노입자를 형성하는 메커니즘을 분석하기 위하여 전구체의 온도에 따른 열유속을 측정하였으며, 반응 과정에서 순차적으로 채취한 반응 원액의 TEM 및 교류 자화율을 측정 하였다. $Fe(OL)_3$는 고온에서 OL-chain 두 개가 순차적으로 분리되어 Fe-OL 단량체(monomer)가 되고, 이들이 산화철 나노입자 형성에 기여하게 된다. 또한 산화철 나노입자는 초기 성장 과정에서 ${\gamma}-Fe_2O_3$ 구조를 갖는 나노입자를 형성하지만, 나노 입자들이 급격히 성장할 때는 공급되는 산소량의 부족으로 인하여 FeO가 형성되어 ${\gamma}-Fe_2O_3$-FeO의 core-shell 구조를 갖는 나노입자들이 합성된다. 이러한 산화철 나노입자들을 고온에서 장시간 유지시키면 부족한 산소를 점차적으로 보충하여 $Fe_3O_4$ 구조를 갖는 나노입자로 변화한다. 따라서 포화자화량이 높고 공기 중에서 안정한 $Fe_3O_4$ 나노입자는 고온 열분해법을 이용하여 쉽게 제조할 수 있다.

Keywords

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