기계적합금화에 의한 Fe/Al2O3 및 Fe/TiO2계 나노복합분말의 제조
Synthesis of Fe/Al2O3 and Fe/TiO2 nanocomposite powder by mechanical alloying
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초록
본 연구에서는 Fe/Al2O3 및 Fe/TiO2계 나노복합분말을 제조하기 위하여 실온 기계적 합금화법(MA)을 적용하였 다. 합금계는 Fe3O4-M(M = Al, Ti)이고 여기서 순금속 Al 및 Ti은 고상반응 시 환원제로서 선택하였다. Fe3O4-순금속의 혼합 분말을 각각 25시간 및 75시간 MA 처리한 결과 Fe/Al2O3 및 Fe/TiO2 나노복합분말이 얻어졌으며, 이것은 나노결정립의 α-Fe 기지에 Al2O3 및 TiO2가 각각 미세하게 분산된 나노복합분말임을 알 수 있었다. 또한 Fe3O4-Al계에서 보다 짧은 반응 시간에 복합분말이 생성되는 것은 Fe3O4의 Al에 의한 환원반응 시 큰 반응열에 기인하는 것으로 사료된다. MA법으로 제조 된 Fe/TiO2 복합분말의 X선 회절분석으로부터 α-Fe 결정립 크기는 30 nm 임을 알 수 있었다. 또한 MA 과정 중 시료의 자 기 측정으로부터 Fe3O4의 순금속 Al 및 Ti에 의한 고상환원반응 과정을 자세히 관찰할 수 있었다.
Abstract
Nanocomposite formation of metal-metal oxide systems by mechanical alloying (MA) has been investigated at room temperature. The systems we chose are the Fe3O4-M (M = Al, Ti), where pure metals are used as reducing agent. It is found that Fe/Al2O3 and Fe/TiO2 nanocomposite powders in which Al2O3 and TiO2 are dispersed in α-Fe matrix with nano-sized grains are obtained by MA of Fe3O4 with Al and Ti for 25 and 75 hours, respectively. It is suggested that the shorter MA time for the nanocomposite formation in Fe/Al2O3 is due to a large negative heat associated with the chemical reduction of magnetite by aluminum. X-ray diffraction results show that the average grain size of α-Fe in Fe/TiO2 nanocomposite powders is in the range of 30 nm. The change in magnetic properties also reflects the details of the solidstate reduction of magnetite by pure metals during MA.
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