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

Journal Article · Sat Mar 15 00:00:00 EDT 2008 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/j.jssc.2007.12.026· OSTI ID:21043921

Schulz, Stephan ^[1]; Bauer, Tillmann; Hoffbauer, Wilfried ^[2]; Doerr, Markus; Marian, Christel M ^[3]; Assenmacher, Wilfried ^[4]

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1. Institute of Inorganic Chemistry, University of Duisburg-Essen, Universitaetsstrasse 5-7, 45141 Essen (Germany)
2. Institute of Inorganic Chemistry, University of Bonn, Gerhard-Domagk-Str. 1, 53121 Bonn (Germany)
3. Institute of Theoretical and Computational Chemistry, University of Duesseldorf, Universitaetsstr. 1, 40225 Duesseldorf (Germany)
4. Institute of Inorganic Chemistry, University of Bonn, Roemerstr. 164, 53117 Bonn (Germany)

Ammonolysis of the monomeric, base-stabilized trisaminoalane Me{sub 3}N-Al[N(H)Dipp)]{sub 3} (Dipp=2,6-{sup i}Pr{sub 2}-C{sub 6}H{sub 3}) yielded Al-N oligomers, which were characterized in detail by solid state NMR spectroscopy ({sup 1}H, {sup 13}C, {sup 15}N, {sup 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{sub 3} produced pure aluminum nitride (AlN). The role of the pyrolysis temperature and the influence of NH{sub 3} on the formation of crystalline materials were investigated. As-prepared AlN was characterized by solid state NMR spectroscopy ({sup 15}N, {sup 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. - Graphical abstract: Ammonolysis reactions of Me{sub 3}N-Al(NHDipp){sub 3} in liquid NH{sub 3} yielded Al-N oligomers, which can be transformed into nanocrystalline aluminum nitride particles under thermolysis conditions at 1000 deg. C. Theoretical calculations were performed in order to identify potential reaction intermediates.

• OSTI ID: 21043921
• Journal Information: Journal of Solid State Chemistry, Vol. 181, Issue 3; Other Information: DOI: 10.1016/j.jssc.2007.12.026; PII: S0022-4596(07)00550-6; Copyright (c) 2007 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA); ISSN 0022-4596
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
ALUMINIUM NITRIDES
AMMONIA
AMMONOLYSIS
CRYSTALS
DIFFERENTIAL THERMAL ANALYSIS
ENERGY-LOSS SPECTROSCOPY
NANOSTRUCTURES
NUCLEAR MAGNETIC RESONANCE
PYROLYSIS
REACTION INTERMEDIATES
STEADY FLOW
THERMAL GRAVIMETRIC ANALYSIS
TRANSMISSION ELECTRON MICROSCOPY
X-RAY DIFFRACTION