Vanadium oxide synthesis

Chemistry of inorganic compounds – Oxygen or compound thereof – Metal containing

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C01G 3102

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044864000

ABSTRACT:
A process for preparing stoichiometric V.sub.6 O.sub.13 usable as the cathode active material in high energy density primary and secondary batteries comprises the steps of: (a) raising the temperature of ammonium metavanadate up to a temperature of from about 350.degree. C. to about 400.degree. C. over an approximately 2 hour time period in a dynamic atmosphere of nitrogen gas to thermally decompose the ammonium metavanadate into a nonstoichiometric V.sub.6 O.sub.13 product while evolving successively ammonia, water vapor and oxygen; (b) holding the nonstoichiometric V.sub.6 O.sub.13 product at said temperature of from about 350.degree. C. to about 400.degree. C. for about 4 hours in said dynamic atmosphere of nitrogen gas; (c) heating the nonstoichiometric V.sub.6 O.sub.13 product at a temperature of from about 400.degree. C. to about 500.degree. C. for from about 8 hours to about 12 hours in a dynamic atmosphere of a gaseous mixture having a composition giving an oxygen partial pressure equal to the oxygen partial pressure over stoichiometric V.sub.6 O.sub.13 at said temperature to form stoichiometric V.sub.6 O.sub.13 ; and (d) cooling the stoichiometric V.sub.6 O.sub.13 to room temperature in said dynamic atmosphere of said gaseous mixture.

REFERENCES:
Selim et al., "Thermochimica Acta", vol. 36, 1980, pp. 287-297.
Trau, "J. of Thermal Analysis", vol. 16, 1979, pp. 201-204.
Satava, "Coll. Czechoslov. Chem. Commun.", vol. 24, 1959, pp. 2172-2181.
D. W. Murphy et al., "Lithium Incorporation by V.sub.6 O.sub.13 and Related Vanadium (+4 +5) Oxide Cathode Materials", J. Electrochem. Soc., vol. 128, No. 10, pp. 2053 et seq., (Oct. 1981).
K. Wilhelmi et al., "A Refinement of the Crystal Structure of V.sub.6 O.sub.13 ", Acta Chem. Scand., vol. 25, No. 7, pp. 2675 et seq., (1971).
D. W. Murphy et al., "Vanadium Oxide Cathode Materials for Secondary Lithium Cells", J. Electrochem. Soc., vol. 126, No. 3, pp. 497 et seq. (Mar. 1979).

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