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Ammonolysis of niobium(V) bromide

Journal Article · · Inorg. Chem.; (United States)
DOI:https://doi.org/10.1021/ic00256a030· OSTI ID:6802926

Niobium nitrides and carbonitrides are materials with desirable properties such as hardness, thermal stability, and particularly, in the case of cubic forms, superconductivity. The ammonolysis of niobium halides provides a synthetic route to the nitride. This has been previously examined by Fowles and Pollard, who found, through tensimetric determinations, that the initial ammonolytic reaction leads to the ammonia-soluble derivative NbCl/sub 3/(NH/sub 2/)/sub 2/. Evaporation of the ammonia left a solid residue that, upon thermal treatment, produced NbN. Additional work by Allbutt and Fowles showed that long-term ammonolysis leads to an insoluble residue having a formula corresponding to NbBr(NH/sub 2/)/sub 2/NH. (The structure of a similar tantalum analogue has been recently established.) More recent developments in this area include the work of Sinitsyna, who performed dry ammonolysis reactions between the niobium halides and an excess of the corresponding ammonium halide to produce niobium halide nitrides, NbNX/sub 2/. Finally, Grebtsova et al. studied the thermal conversion of the ammonolysis residue of NbCl/sub 5/ into NbN by a variety of techniques. The present work was undertaken to better characterize the ammonolytic intermediates as well as the thermal decomposition products and also to explore the use of these intermediates in the preparation of derivatives that could be converted into carbonitrides similar to previous work in the titanium system.

Research Organization:
Oak Ridge National Lab., TN
DOE Contract Number:
AC05-84OR21400
OSTI ID:
6802926
Journal Information:
Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 26:9; ISSN INOCA
Country of Publication:
United States
Language:
English