Stepwise conversion of a single source precursor into crystalline AlN by transamination reaction

摘要

Ammonolysis of the monomeric, base-stabilized trisaminoalane Me3N-Al[N(H)Dipp)](3) (Dipp = 2,6-Pr-i(2)-C6H3) yielded Al-N oligomers, which were characterized in detail by solid state NMR spectroscopy (H-1, C-13, N-15, Al-27) and TGA/DTA. Pyrolysis of as-prepared oligomers at different temperatures in an argon steam yielded carbon-containing black solids, whereas pyrolysis under a steady flow of NH3 produced pure aluminum nitride (A1N). The role of the pyrolysis temperature and the influence of NH3 on the formation of crystalline materials were investigated. As-prepared A1N was characterized by solid state NMR spectroscopy (N-15, Al-27), X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron energy loss spectroscopy (EELS). Theoretical calculations were performed in order to identify potential reaction intermediates. (C) 2007 Elsevier Inc. All rights reserved.