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Synthesis of amorphous boron nitride from the molecular precursor ammonia-monochloroborane

Published online by Cambridge University Press:  31 January 2011

Douglas R. Ketchum ,
Allison L. DeGraffenreid ,
Philipp M. Niedenzu  and
Sheldon G. Shore
Douglas R. Ketchum
Affiliation:
Department of Chemistry, The Ohio State University, Columbus, Ohio 43210
Allison L. DeGraffenreid
Affiliation:
Department of Chemistry, The Ohio State University, Columbus, Ohio 43210
Philipp M. Niedenzu
Affiliation:
Department of Chemistry, The Ohio State University, Columbus, Ohio 43210
Sheldon G. Shore*
Affiliation:
Department of Chemistry, The Ohio State University, Columbus, Ohio 43210
*
a)Address all correspondence to this author.
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Abstract

Ammonia-monochloroborane, NH3BH2Cl, has been synthesized from the reaction of ammonia-borane with HCl in Et2O. Decomposition of the solid under NH3 to 600 °C produced amorphous BN in 97% yield. The 11B magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectrum of the amorphous BN is indicative of boron in the same environment as in hexagonal BN. Subsequent pyrolysis of the amorphous BN to 1000 °C produced turbostratic BN. Pyrolysis of NH3BH2Cl under vacuum to 1100 °C led to the formation of turbostratic BN as confirmed by x-ray diffraction (XRD) analysis. Gas evolution during this pyrolysis confirmed that the precursor loses H2 and HCl.

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Articles
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Journal of Materials Research , Volume 14 , Issue 5 , May 1999 , pp. 1934 - 1938
Copyright
Copyright © Materials Research Society 1999

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