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Title: Synthesis of tungsten nitrides and carbide nitrides

Abstract

Efforts to prepare the unknown, metastable tungsten(VI) nitride WN{sub 2} have proceeded with various reactions of WNCl{sub 3} conducted under mild conditions. Reactions of WNCl{sub 3} with Zn{sub 3}N{sub 2} in sealed tubes at 400{degrees}C frequently failed because of explosions. Under careful management of composition of the reaction mixture and temperature programming, however, the reactions were successfully completed to provide amorphous W{sub 3}N{sub 5}. Annealing of the latter at 800{degrees}C in a sealed silica tube resulted in decomposition into a mixture of W and hexagonal WN, as well as growth by chemical transport of a few crystals of the new nitride carbide WN{sub 2}C, based upon single crystal x-ray structure analysis. Reaction of WNCl{sub 3} with Ca{sub 3}N{sub 2} in acetonitrile at 80{degrees}C results in a precursor which can be converted at 500{degrees}C into the new metastable cubic-WN with the rock salt structure. The explosive azido precursor WN(N{sub 3}){sub 3}{sm_bullet}xCH{sub 3}CN can be obtained by reaction of WNCl{sub 3} with NaN{sub 3} in acetonitrile at 20{degrees}C, and successfully converted to nitrido products in situ. Some reactions of WN(N{sub 3}){sub 3}{sm_bullet}xCH{sub 3}CN will be discussed.

Authors:
;  [1]
  1. Ames Lab., IA (United States)
Publication Date:
OSTI Identifier:
560227
Report Number(s):
CONF-970443-
TRN: 97:005895-0203
Resource Type:
Conference
Resource Relation:
Conference: 213. national meeting of the American Chemical Society, San Francisco, CA (United States), 13-17 Apr 1997; Other Information: PBD: 1997; Related Information: Is Part Of 213th ACS national meeting; PB: 2904 p.
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; ACETONITRILE; ANNEALING; PRECURSOR; TUNGSTEN NITRIDES; SYNTHESIS; TUNGSTEN CHLORIDES; NITROGEN CHLORIDES; CRYSTAL STRUCTURE

Citation Formats

Zhang, Zhihong, and McCarley, R E. Synthesis of tungsten nitrides and carbide nitrides. United States: N. p., 1997. Web.
Zhang, Zhihong, & McCarley, R E. Synthesis of tungsten nitrides and carbide nitrides. United States.
Zhang, Zhihong, and McCarley, R E. Wed . "Synthesis of tungsten nitrides and carbide nitrides". United States.
@article{osti_560227,
title = {Synthesis of tungsten nitrides and carbide nitrides},
author = {Zhang, Zhihong and McCarley, R E},
abstractNote = {Efforts to prepare the unknown, metastable tungsten(VI) nitride WN{sub 2} have proceeded with various reactions of WNCl{sub 3} conducted under mild conditions. Reactions of WNCl{sub 3} with Zn{sub 3}N{sub 2} in sealed tubes at 400{degrees}C frequently failed because of explosions. Under careful management of composition of the reaction mixture and temperature programming, however, the reactions were successfully completed to provide amorphous W{sub 3}N{sub 5}. Annealing of the latter at 800{degrees}C in a sealed silica tube resulted in decomposition into a mixture of W and hexagonal WN, as well as growth by chemical transport of a few crystals of the new nitride carbide WN{sub 2}C, based upon single crystal x-ray structure analysis. Reaction of WNCl{sub 3} with Ca{sub 3}N{sub 2} in acetonitrile at 80{degrees}C results in a precursor which can be converted at 500{degrees}C into the new metastable cubic-WN with the rock salt structure. The explosive azido precursor WN(N{sub 3}){sub 3}{sm_bullet}xCH{sub 3}CN can be obtained by reaction of WNCl{sub 3} with NaN{sub 3} in acetonitrile at 20{degrees}C, and successfully converted to nitrido products in situ. Some reactions of WN(N{sub 3}){sub 3}{sm_bullet}xCH{sub 3}CN will be discussed.},
doi = {},
journal = {},
number = ,
volume = ,
place = {United States},
year = {1997},
month = {12}
}

Conference:
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