Preparation of copper alkoxides and sol/gel precursors of superconducting ceramics

Claim 1

A method for the preparation of high purity copper (II) alkoxides comprising: (a) reacting an alkali metal with an anhydrous, deoxygenated alcohol and recovering from the resulting reaction product an anhydrous, deoxygenated alcoholic alkali metal alkoxide solution; (b) admixing anhydrous copper (II) fluoride with the alkali metal alkoxide solution; (c) heating said mixture to a temperature of between from about ambient temperature and about 10° C. below the boiling point of the alcohol for between about 0.25 hour and about 8 hours to form a solution of alkali metal fluoride and copper (II) alkoxide; (d) ammoniating said alkali metal fluoride and copper (II) solution with anhydrous ammonia to form a saturated ammoniacal alcoholic solution of ammoniacal copper (II) alkoxide in solution and an alkali metal fluoride precipitate; and (e) recovering an alkali metal free ammoniacal copper (II) alkoxide solution.

Claim 2

A method for the preparation of high purity copper (II) alkoxides comprising: (a) reacting an alkali metal with an anhydrous, deoxygenated alcohol and recovering from the resulting reaction product an anhydrous, deoxygenated alcoholic alkali metal alkoxide solution; (b) admixing anhydrous copper (II) fluoride with the alkali metal alkoxide solution; (c) heating said mixture to a temperature of between from about ambient temperature and about 10° C. below the boiling point of the alcohol for between about 0.25 hour and about 8 hours to form a solution of alkali metal fluoride and copper (II) alkoxide; (d) ammoniating said alkali metal fluoride and copper (II) solution with anhydrous ammonia to form a saturated ammoniacal alcoholic solution of ammoniacal copper (II) alkoxide in solution and an alkali metal fluoride precipitate; and (e) recovering an alkali metal free ammoniacal copper (II) alkoxide solution.

Claim 7

A method for the preparation of a homogeneous sol/gel useful in the preparation of superconducting ceramics comprising: (a) reacting an alkali metal with an anhydrous deoxygenated alcohol and recovering from the resulting reaction product an anhydrous, deoxygenated alcoholic alkali metal alkoxide solution; (b) admixing anhydrous copper (II) fluoride with the alkali metal alkoxide solution; (c) heating said mixture to a temperature of between about ambient temperature and about 10° below the boiling point of the alcohol for between about 0.25 hour and about 8 hours to form a solution of alkali metal fluoride and a copper (II) alkoxide; (d) ammoniating said alkali metal fluoride and copper (II) alkoxide solution with anhydrous ammonia to form a saturated ammoniacal alcoholic solution of ammoniacal copper (II) alkoxide in solution and an alkali metal fluoride precipitate; (e) recovering an alkali metal free ammoniacal copper (II) alkoxide solution; (f) hydrating said ammoniacal copper (II) alkoxide solution by the addition of 2 moles of triply distilled deionized water for each such mole of ammoniacal copper (II) alkoxide present in said solution and stirring said water containing solution for a time in the range of about 0.5 hour to about 2 hours; (g) adding a solution of barium alkoxide in excess alcohol, at a temperature of at least 55° C., to the ammoniacal copper (II) alkoxide solution obtained in (f), said amount of barium added being about 2/3 the amount, on a molar basis, of copper present and stirring the resulting barium-copper containing solution at a temperature from about 60° C. to about 70° C. for a time in the range of about 0.5 hour to about 2.0 hours; (h) adding a lanthanide series metal alkoxide solution to the solution resulting from (g), the amount of lanthanide metal added being about 1/3, on a molar basis, the amount of copper present in (g) and heating the resulting lanthanide metal-barium-copper solution at a temperature in the range of about 50° C. to about 60° C. for a time in the range of about 8 hours to about 16 hours; and (i) concentrating and ageing the lanthanide metal-barium-copper solution to produce a sol/gel.

Claim 8

A method for the preparation of a homogeneous sol/gel useful in the preparation of superconducting ceramics comprising: (a) reacting an alkali metal with an anhydrous deoxygenated alcohol and recovering from the resulting reaction product an anhydrous, deoxygenated alcoholic alkali metal alkoxide solution; (b) admixing anhydrous copper (II) fluoride with the alkali metal alkoxide solution; (c) heating said mixture to a temperature of between about ambient temperature and about 10° below the boiling point of the alcohol for between about 0.25 hour and about 8 hours to form a solution of alkali metal fluoride and a copper (II) alkoxide; (d) ammoniating said alkali metal fluoride and copper (II) alkoxide solution with anhydrous ammonia to form a saturated ammoniacal alcoholic solution of ammoniacal copper (II) alkoxide in solution and an alkali metal fluoride precipitate; (e) recovering an alkali metal free ammoniacal copper (II) alkoxide solution; (f) hydrating said ammoniacal copper (II) alkoxide solution by the addition of 2 moles of triply distilled deionized water for each such mole of ammoniacal copper (II) alkoxide present in said solution and stirring said water containing solution for a time in the range of about 0.5 hour to about 2 hours; (g) adding a solution of barium alkoxide in excess alcohol, at a temperature of at least 55° C., to the ammoniacal copper (II) alkoxide solution obtained in (f), said amount of barium added being about 2/3 the amount, on a molar basis, of copper present and stirring the resulting barium-copper containing solution at a temperature from about 60° C. to about 70° C. for a time in the range of about 0.5 hour to about 2.0 hours; (h) adding a lanthanide series metal alkoxide solution to the solution resulting from (g), the amount of lanthanide metal added being about 1/3, on a molar basis, the amount of copper present in (g) and heating the resulting lanthanide metal-barium-copper solution at a temperature in the range of about 50° C. to about 60° C. for a time in the range of about 8 hours to about 16 hours; and (i) concentrating and ageing the lanthanide metal-barium-copper solution to produce a sol/gel.