• Korean Journal of Materials Research
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• v.22 no.11
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• pp.620-625
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• 2012

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.

• Elastomers and Composites
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• v.21 no.1
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• pp.13-19
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• 1986

The effects of several vulcanizing accelerators on the determination of kinetic parameters of natural rubber vulcanizate was studied by DSC. Kinetic parameters were determined by means of the calculation procedures of Borchardt-Daniels and Oscillating Disk Rheometer (ODR) cure curve analysis, using both DSC exothermal thermogram and ODR cure curve. In order to examine the credibility in the DSC method the same compound which was und for DSC method was used for the comparison with the results of ODR data. Upon this method, kinetic rate constant (k), and Arrehenius parameter (Ea, ko, n) have been determined for rubber compounds via a new method using DSC thermogram and ODR cure curve. In the comparison of DSC and ODR results, kinetic parameters has shown good agreements between two results. Consequently, from the present studies, it is shown that the DSC thermoanalytical method can provide an alternate new method of kinetic study of rubber vulcanization.