Journal of the Korean Ceramic Society (한국세라믹학회지)

The Korean Ceramic Society (한국세라믹학회)
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Synthesis of Aluminum Nitride Powers and Whiskers from a (NH4)[Al(edta)]·2H2O Complex under a Flow of Nitrogen

질소 분위기에서 (NH4)[Al(edta)]·2H2O 착물으로부터 질화알루미늄 분말 및 휘스커의 합성

  • Jung, Woo-Sik (School of Chemical Engineering and Technology, College of Engineering, Yeungnam University)
  • 정우식 (영남대학교 응용화학공학부)
  • Published : 2002.01.01
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Abstract

Aluminum nitride (AlN) powders and whiskers were synthesized by a modified carbothermal reduction and nitridation where a ($NH_4)[Al(ethylenediaminetetraacetate)]{\cdot}2H_2O$ complex is used as precursor. The AlN powders were obtained by calcining the complex without mixing any carbon source under a flow of nitrogen in the temperature range 1200∼1500$^{\circ}$C and then burning out the residual carbon. The nitridation process was investigated by $^{27}Al$ magic-angle spinning (MAS) unclear magnetic resonance, infrared spectroscopy and X-ray diffraction. The complex is pyrolyzed, converted to ${\rho}$- and ${\gamma}$- alumina and then nitridated to AlN without ${\gamma}-{\alpha}$ alumina transition. The morphology of ${\gamma}$-alumina, when it was converted to AlN, was retained, strongly indicating that ${\gamma}$-alumina is converted to AlN through solid-state $AlO_xN_y$, not through gaseous intermediates such as aluminum and aluminaum suboxides. AlN whiskers were obtained, when a (0001) sapphire was used as a catalyst.

전구체로 ($NH_4)[Al(ethylenediaminetetraacetate)]{\cdot}2H_2O$ 착물을 이용한 수정된 열탄소환원질화법으로 질화알루미늄(AlN) 분말과 휘스커를 합성하였다. 이 분말은 질소분위기에서 별도의 환원용 탄소를 혼합하지 않고 1200$^{\circ}$C에서 1500$^{\circ}$C까지의 온도에서 하소시킨 다름 잔류탄소를 태워 버림으로써 얻어졌다. 이 질화과정을 Al-27 마법각 스핀 핵자기공명, 적외선 분광법 및 X-선 회절법으로 연구했다. 전구체 착물은 열분해되어 ${\rho}$-알루미나와 ${\gamma}$-알루미나로 되었다가 ${\gamma}-{\alpha}$알루미나 전이없이 AlN으로 바뀌었다. ${\gamma}$-알루미나가 AlN으로 바뀌면서 분말의 형상이 유지되는 것으로 보아 이 변환과정에서의 중간체는 알루미늄이나 aluminum suboxides와 같은 기체상이 아니고, 고체상의 $AlO_xN_y$임을 알 수 있다. (0001) 사파이어를 이용하면 AlN 휘스커를 합성할 수 있다.

Keywords

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