Journal of the Korean Chemical Society (대한화학회지)

Korean Chemical Society (대한화학회)
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In-situ Fourier Transform Infrared Spectroscopic Study during Thermolysis of Trimethylaluminum and its Adduct

Trimethylaluminum (TMA), $NH_3$ 및 TMA :$NH_3$Adduct의 열분해 반응에 대한 in-situ FTIR 분광학적 연구

  • Hyang Sook Kim (Solid State Chemsitry Lab., Korea Research Institute of Chemical Technology) ;
  • Seong Han Kim (Solid State Chemsitry Lab., Korea Research Institute of Chemical Technology) ;
  • Jin Soo Hwang (Solid State Chemsitry Lab., Korea Research Institute of Chemical Technology) ;
  • Joong Gill Choi (Department of Chemistry, Yonsei University) ;
  • Paul Joe Chong (Solid State Chemsitry Lab., Korea Research Institute of Chemical Technology)
  • 김향숙 (한국화학연구원 고체화학실) ;
  • 김성한 (한국화학연구원 고체화학실) ;
  • 황진수 (한국화학연구원 고체화학연구실) ;
  • 최중길 (연세대학교 이과대학 화학과) ;
  • 정필조 (한국화학연구원 고체화학실)
  • Published : 1993.12.20
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Abstract

The thermal decomposition of trimethylaluminum (TMA) with ammonia has been investigated by in-situ Fourier transform infrared spectroscopy. The spectroscopic reaction cell, which permits heating interna lly up to 1100$^{\circ}C$, consists of stainless-steel hexagonal-port chamber containing two NaCl windows installed in parallel. In this work, the stoichiometric reaction between TMA and $NH_3$ is found to be completed immediately after mixing. FTIR spectra observed in the range of temperature 25∼1100$^{\circ}C$ show that TMA and TMA : $NH_3$ adduct decompose into methane as a predominant product around 500$^{\circ}C$. The assignments of the IR bands due to the gaseous TMA, $NH_3$ and TMA : $NH_3$ adduct are attempted on the basis of the published data. Furthermore, the decomposition of TMA can be described as a first-order reaction. Kinetic data about the decompositon of TMA and TMA : $NH_3$adduct will also be discussed.

TMA와 $NH_3$와의 기상 열분해 반응을 in-situ FTIR 분광법으로 관찰하였다. 사용한 spectroscopic reaction cell은 stainless-steel제로 자체 제작한 hexagonal-port chamber로서 2개의 NaCl window를 평행하게 설치하여 1100$^{\circ}C$까지 가열할 수 있으며 또한 이와 같은 높은 온도에서 분광분석이 가능하였다. TMA와 $NH_3$는 혼합 즉시 반응하여 TMA:$NH_3$adduct를 생성하였으며, 500$^{\circ}C$에서그 adduct가 완전분해됨을 FTIR로 확인하였다. TMA와 TMA:$NH_3$adduct의 열분해는 주생성물로$CH_4$을 방출하였다. 기상의 TMA,$NH_3$ 및 TMA:$NH_3$ adduct에 대하여 상온에서 관찰한 IR band들은 문헌값과 대조하여 assign하였다. TMA의 열분해에 대한 kinetic data로부터 이 반응이 1차식으로 일어남을 알 수 있었다.

Keywords

References

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