Korean Chemical Engineering Research

The Korean Institute of Chemical Engineers (한국화학공학회)
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Synthesis Characteristics of ZnO Powder from Precursors Composed of Nitrate-Citrate Compounds

Nitrate-Citrate 혼합 전구체로부터 ZnO 입자의 합성반응 특성

  • Yang, Si Woo (Department of Chemical Engineering, Chungnam National University) ;
  • Lee, Seung Ho (Department of Chemical Engineering, Chungnam National University) ;
  • Lim, Dae Ho (Department of Chemical Engineering, Chungnam National University) ;
  • Yoo, Dong Jun (Department of Chemical Engineering, Chungnam National University) ;
  • Kang, Yong (Department of Chemical Engineering, Chungnam National University)
  • 양시우 (충남대학교 화학공학과) ;
  • 이승호 (충남대학교 화학공학과) ;
  • 임대호 (충남대학교 화학공학과) ;
  • 유동준 (충남대학교 화학공학과) ;
  • 강용 (충남대학교 화학공학과)
  • Received : 2015.12.14
  • Accepted : 2016.01.20
  • Published : 2016.06.01
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Abstract

Characteristics of self-propagating reaction for the preparation of ZnO powder from precursors composed of nitrate and citrate compounds were examined. The ratio of C/N was maintained in range of 0.7~0.8 to initiate the self-propagating reaction between the reducing citrate and oxidizing nitrate groups. The samples were decomposed thermally by using TGA. The sudden decomposition occurred in the range of X > 0.5 in a very short time with a very sharp decrease of mass, indicating that the self-propagating reaction would occur. Friedman, Ozawa-Flynn-Wall and Vyazovkin methods were employed to predict the activation energy, reaction order and frequency factor of the reaction rate in the rate determining step of X < 0.5 range. The activation energy increased with increasing fractional conversion in the range of 46~130 (kJ/min). The reaction order decreased in the range of 2.9~0.9, while the frequency factor increased in the range of 85~278 ($min^{-1}$), respectively, with increasing the rate of temperature increase.

Nitrate-citrate 혼합 전구체로부터 ZnO 입자 합성을 위한 자체진행 반응(Self-propagating reaction)의 특성을 고찰하였다. 질화물과 Citrate 그룹간의 자체진행 반응을 위해 탄소/질소 성분의 비는 0.7~0.8 수준으로 유지하였으며, 출발물질의 시료를 TGA방법에 의해 열분해하였다. 반응의 후반부인 반응 전환율이 0.5 이상에서 자체진행 반응의 특성을 나타내었으며 시료는 매우 짧은 시간에 많은 열을 방출하며 분해되었다. 반응의 전반부(X<0.5)가 전체반응의 율속단계로 나타났으며, 이 율속단계에서 반응의 특성을 Friedman, Ozawa-Flynn-Wall 그리고 Vyazovkin의 방법들을 사용하여 해석하였다. 율속단계에서 활성화 에너지는 46~130 (kJ/mol)의 범위로 반응 전환율이 증가함에 따라 증가하였으며, 반응차수는 2.9~0.9, 그리고 반응속도의 빈도인자(Frequency factor)는 85~278 ($min^{-1}$)의 범위에서 승온속도가 증가함에 따라 각각 전자는 감소하고 후자는 증가하였다.

Keywords

References

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