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Diluted Synthesis of Manocrystalline CeO2 by Mechanical Milling

희석혼합체의 기계적 분쇄에 의한 나노 CeO2의 합성

  • Lim, Geon-Ja (Nano-Materials Research Center, Korea Institute of Science and Technology) ;
  • Kim, Tae-Eun (Nano-Materials Research Center, Korea Institute of Science and Technology) ;
  • Lee, Jong-Ho (Nano-Materials Research Center, Korea Institute of Science and Technology) ;
  • Lee, Hae-Weon (Nano-Materials Research Center, Korea Institute of Science and Technology) ;
  • Rhee, Dong-Joo (Nano fluid Technologies Co., Ltd.) ;
  • Hyun, Sang-Hoon (Department of Ceramic Engineering, Yonsei University)
  • 임건자 (한국과학기술연구원 나노재료연구센타) ;
  • 김태은 (한국과학기술연구원 나노재료연구센타) ;
  • 이종호 (한국과학기술연구원 나노재료연구센타) ;
  • 이해원 (한국과학기술연구원 나노재료연구센타) ;
  • 이동주 ((주) 나노플루이드) ;
  • 현상훈 (연세대학교 세라믹공학과)
  • Published : 2002.01.01

Abstract

The nanocrystalline $CeO_2$ was synthesized by mechanical milling and subsequent heat-treatment with the mixture of $Ce(OH)_4$ precursor and diluent, NaCl. Using deionized water, the diluent, NaCl, in the mixture has been easily dissolved out. Diffusion barrier was provided by the diluent during heat-treatment, which suppressed not only the coarsening of primary particle but also the agglormeration between the particles. Crystallite and aggregate size of $CeO_2$ depended on the concentration of diluent, temperature and time of heat-treatment; increased with the temperature and time increases. In case the mixture was heat-treated at high than $600^{\circ}C$, however, the crystallite size was saturated near 20 nm, which was supposed to be due to the densification of diluent.

산화물의 금속 전구체인 $Ce(OH)_4$를 희석제인 NaCl과 함께 기계적으로 분쇄하여 나노 크기의 일차입자를 제조하고, 분쇄한 전구체 분말은 희석제와 함께 열처리를 하여 나노 결정립의 $CeO_2$를 합성하였다. 희석제는 전구체의 분쇄시 분말의 재응집을 억제하여 분쇄효율을 증진시켰을 뿐만 아니라 열처리 중에는 일차입자 성장과 응집을 억제하여 열처리 온도와 시간에 따라 일차입자의 크기 뿐만 아니라 응집체으 크기도 제어할 수 있었다. 열처리 중 희석제는 고온에서 전구체 표면에서 치밀화 되어 일차입자 성장과 응집체 형성의 확산장벽으로 작용하는 것으로 판단되며 열처리 후 증류수에 쉽게 용해되어 $CeO_2$ 나노 입자 제조에 효과적이었다. 일차입자와 응집체의 크기 및 결정성은 희석제의 농도, 열처리 온도와 시간에 의존하는 것으로 확인 되었다.

Keywords

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