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Title: The preparation and characterization of high surface area transition metal nitrides

Abstract

This study is concerned with the synthesis of high-surface-area molybdenum and vanadium nitrides by the reaction of oxide and ammonium oxide precursors with ammonia. The reactions have been followed using thermogravimetric analysis (TGA) and high temperature X-Ray diffraction (XRD) to determine reaction intermediates, while the development of surface area was investigated by interrupting the TGA experiments and measuring the surface area using the BET method. Molybdenum trioxide and ammonium paramolybdate react to form high surface area Mo{sub 2}N and a mixture of MoN and Mo{sub 2}N, respectively. Diammonium molybdate reacts with ammonia to form low surface area MoN. Each compound reacts through a different pathway to form a common MoO{sub x}N{sub 1-x} oxynitride intermediate, which subsequently reacts to form the nitride product. The nitride phase formed is determined by the temperature at which the oxynitride reacts, while the structure of the oxynitride precursor influences the ultimate surface area. The reactions of V{sub 2}O{sub 5}, VO{sub 2}, V{sub 2}O{sub 3}, and NH{sub 4}VO{sub 3} with ammonia all produce low surface area vanadium oxynitrides at 750C. Each reaction proceeds through a series of lower vanadium oxide intermediates. In all reaction, V{sub 2}O{sub 3} is the precursor to the oxynitride. The use ofmore » hydrogen bronzes of molybdenum trioxide and vanadium pentoxide as starting materials lowers the reaction temperatures, but does not alter the nitridification reaction networks. In the case of molybdenum trioxide, however, insertion of hydrogen eliminates the formation of molybdenum dioxide which is a by-product of the reaction of MoO{sub 3} with ammonia.« less

Authors:
Publication Date:
Research Org.:
California Univ., Berkeley, CA (USA)
OSTI Identifier:
7022477
Resource Type:
Miscellaneous
Resource Relation:
Other Information: Thesis (Ph. D.)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; MOLYBDENUM NITRIDES; CHEMICAL PREPARATION; VANADIUM NITRIDES; AMMONIA; AMMONIUM COMPOUNDS; CHEMICAL PROPERTIES; CHEMICAL REACTION KINETICS; CHEMICAL REACTIONS; HYDROGEN; MOLYBDENUM OXIDES; OXIDES; REACTION INTERMEDIATES; SURFACE AREA; SURFACE PROPERTIES; THERMAL GRAVIMETRIC ANALYSIS; VANADIUM OXIDES; X-RAY DIFFRACTION; CHALCOGENIDES; CHEMICAL ANALYSIS; COHERENT SCATTERING; DIFFRACTION; ELEMENTS; GRAVIMETRIC ANALYSIS; HYDRIDES; HYDROGEN COMPOUNDS; KINETICS; MOLYBDENUM COMPOUNDS; NITRIDES; NITROGEN COMPOUNDS; NITROGEN HYDRIDES; NONMETALS; OXYGEN COMPOUNDS; PNICTIDES; QUANTITATIVE CHEMICAL ANALYSIS; REACTION KINETICS; REFRACTORY METAL COMPOUNDS; SCATTERING; SYNTHESIS; THERMAL ANALYSIS; TRANSITION ELEMENT COMPOUNDS; VANADIUM COMPOUNDS; 400201* - Chemical & Physicochemical Properties

Citation Formats

Jaggers, C H. The preparation and characterization of high surface area transition metal nitrides. United States: N. p., 1988. Web.
Jaggers, C H. The preparation and characterization of high surface area transition metal nitrides. United States.
Jaggers, C H. Fri . "The preparation and characterization of high surface area transition metal nitrides". United States.
@article{osti_7022477,
title = {The preparation and characterization of high surface area transition metal nitrides},
author = {Jaggers, C H},
abstractNote = {This study is concerned with the synthesis of high-surface-area molybdenum and vanadium nitrides by the reaction of oxide and ammonium oxide precursors with ammonia. The reactions have been followed using thermogravimetric analysis (TGA) and high temperature X-Ray diffraction (XRD) to determine reaction intermediates, while the development of surface area was investigated by interrupting the TGA experiments and measuring the surface area using the BET method. Molybdenum trioxide and ammonium paramolybdate react to form high surface area Mo{sub 2}N and a mixture of MoN and Mo{sub 2}N, respectively. Diammonium molybdate reacts with ammonia to form low surface area MoN. Each compound reacts through a different pathway to form a common MoO{sub x}N{sub 1-x} oxynitride intermediate, which subsequently reacts to form the nitride product. The nitride phase formed is determined by the temperature at which the oxynitride reacts, while the structure of the oxynitride precursor influences the ultimate surface area. The reactions of V{sub 2}O{sub 5}, VO{sub 2}, V{sub 2}O{sub 3}, and NH{sub 4}VO{sub 3} with ammonia all produce low surface area vanadium oxynitrides at 750C. Each reaction proceeds through a series of lower vanadium oxide intermediates. In all reaction, V{sub 2}O{sub 3} is the precursor to the oxynitride. The use of hydrogen bronzes of molybdenum trioxide and vanadium pentoxide as starting materials lowers the reaction temperatures, but does not alter the nitridification reaction networks. In the case of molybdenum trioxide, however, insertion of hydrogen eliminates the formation of molybdenum dioxide which is a by-product of the reaction of MoO{sub 3} with ammonia.},
doi = {},
journal = {},
number = ,
volume = ,
place = {United States},
year = {1988},
month = {1}
}

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