논문 상세보기
pp.620-625
A general synthetic method to make Fe3O4-δ (activated magnetite) is the reduction of Fe3O4 by H2 atmosphere. However, this process has an explosion risk. Therefore, we studied the process of synthesis of Fe3O4-δ depending on heat-treatment conditions using FeC2O4·2H2O in Ar atmosphere. The thermal decomposition characteristics of FeC2O4·2H2O and the δ-value of Fe3O4-δ were analyzed with TG/DTA in Ar atmosphere. β-FeC2O4·2H2O was synthesized by precipitation method using FeSO4·7H2O and (NH4)2C2O4·H2O. The concentration of the solution was 0.1 M and the equivalent ratio was 1.0. β-FeC2O4·2H2O was decomposed to H2O and FeC2O4 from 150˚C to 200˚C. FeC2O4 was decomposed to CO, CO2, and Fe3O4 from 200˚C to 250˚C. Single phase Fe3O4 was formed by the decomposition of β-FeC2O4·2H2O in Ar atmosphere. However, Fe3C, Fe and Fe4N were formed as minor phases when β-FeC2O4·2H2O was decomposed in N2 atmosphere. Then, Fe3O4 was reduced to Fe3O4-δ by decomposion of CO. The reduction of Fe3O4 to Fe3O4-δ progressed from 320˚C to 400˚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 δ-value of Fe3O4-δ was greatly influenced by the heat treatment temperature and the heating rate. However, Ar flow rate and holding time had a minor effect on δ-value.
