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Effects of Heat Treatment Conditions of FeC2O4·2H2O on the Formation of Fe3O4-δ

FeC2O4·2H2O의 열처리 조건이 Fe3O4-δ 형성에 미치는 영향

  • Oh, Kyoung-Hwan (Department of Materials Science and Engineering, Chungnam National University) ;
  • Park, Won-Shik (Department of Materials Science and Engineering, Chungnam National University) ;
  • Rhee, Sang-In (Dept. of Mechanical Design, Daeduk College) ;
  • Suhr, Dong-Soo (Department of Materials Science and Engineering, Chungnam National University)
  • Received : 2012.10.08
  • Accepted : 2012.10.31
  • Published : 2012.11.27

Abstract

A general synthetic method to make $Fe_3O_{4-{\delta}}$ (activated magnetite) is the reduction of $Fe_3O_4$ by $H_2$ atmosphere. However, this process has an explosion risk. Therefore, we studied the process of synthesis of $Fe_3O_{4-{\delta}}$ depending on heat-treatment conditions using $FeC_2O_4{\cdot}2H_2O$ in Ar atmosphere. The thermal decomposition characteristics of $FeC_2O_4{\cdot}2H_2O$ and the ${\delta}$-value of $Fe_3O_{4-{\delta}}$ were analyzed with TG/DTA in Ar atmosphere. ${\beta}-FeC_2O_4{\cdot}2H_2O$ was synthesized by precipitation method using $FeSO_4{\cdot}7H_2O$ and $(NH_4)_2C_2O_4{\cdot}H_2O$. The concentration of the solution was 0.1 M and the equivalent ratio was 1.0. ${\beta}-FeC_2O_4{\cdot}2H_2O$ was decomposed to $H_2O$ and $FeC_2O$4 from $150^{\circ}C$ to $200^{\circ}C$. $FeC_2O4$ was decomposed to CO, $CO_2$, and $Fe_3O_4$ from $200^{\circ}C$ to $250^{\circ}C$. Single phase $Fe_3O_4$ was formed by the decomposition of ${\beta}-FeC_2O_4{\cdot}2H_2O$ in Ar atmosphere. However, $Fe_3C$, Fe and $Fe_4N$ were formed as minor phases when ${\beta}-FeC_2O_4{\cdot}2H_2O$ was decomposed in $N_2$ atmosphere. Then, $Fe_3O_4$ was reduced to $Fe_3O_{4-{\delta}}$ by decomposion of CO. The reduction of $Fe_3O_4$ to $Fe_3O_{4-{\delta}}$ progressed from $320^{\circ}C$ to $400^{\circ}C$; the reaction was exothermic. The degree of exothermal reaction was varied with heat treatment temperature, heating rate, Ar flow rate, and holding time. The ${\delta}$-value of $Fe_3O_{4-{\delta}}$ was greatly influenced by the heat treatment temperature and the heating rate. However, Ar flow rate and holding time had a minor effect on ${\delta}$-value.

Acknowledgement

Supported by : 한국연구재단

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