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

作者：Schulz Stephan^*; Bauer Tillmann; Hoffbauer Wilfried; Guenne Joern Schmedt Auf Der; Doerr Markus; Marian Christel M; Assenmacher Wilfried

来源：Journal of Solid State Chemistry, 2008, 181(3): 530-538.

DOI：10.1016/j.jssc.2007.12.026

• single source precursor
• ammonolysis
• A1N
• solid state NMR

Ammonolysis of the monomeric, base-stabilized trisaminoalane Me(3)N-Al[N(H)Dipp)](3) (Dipp = 2,6-(i)Pr(2)-C(6)H(3)) yielded Al-N oligomers, which were characterized in detail by solid state NMR spectroscopy ((1)H, (13)C, (15)N, (27)Al) 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 NH(3) 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 ((15)N, (27)Al), 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.

• 出版日期2008-3