US4567031A
Expired / Lapsed
US
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Process for preparing mixed metal oxides
Assignee: Combustion Engineering Inc
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Filing: 1983-12-27
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Granted: 1986-01-28
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Expires: 2003-12-27
Abstract
Abstract A process for preparing a mixed metal oxide, usable as the cathode or intercalation electrode in high energy density primary and secondary batteries, having the formula Li x M y O z where M is at least one metal selected from the group consisting of titanium, chromium, manganese, iron, cobalt and nickel, x is a number from about 0.1 to about 1.1, preferably from about 0.9 to about 1.1, y is a total number from about 1.1 to about 0.1, preferably from about 1.1 to about 0.9, respectively, and z is a number from about 1.9 to about 2.1, such as LiCoO 2 or [Li(Co 0 .5 Ni 0 .5) O 2 ], is comprised by preparing a mixed solution containing x moles of a soluble oxygen-containing salt of lithium and y total moles of soluble oxygen-containing salt(s) of the at least one metal M in a solvent therefor; concentrating the mixed solution; co-crystallizing a mixed salt of lithium and of the at least one metal M from the concentrated mixed solution; and calcining the co-crystallized mixed salt at a low temperature of from about 400° C. to about 500°C. for a short period of time of from about 1 hour to about 4 hours to form the mixed metal oxide.
Inventors
- 👤 Brian Riley
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-26 05:23
CPC Classifications
H; H01; H01M; H01M10/00; H01M10/05; H01M10/052; C; C01; C01G; C01G23/00; C01G23/003; C01G23/005; C01G37/00; C01G45/00; C01G45/12; C01G45/1221; C01G45/1228; C01G49/00; C01G49/0018; C01G49/0027; C01G51/00; C01G51/40; C01G51/42; C01G53/00; C01G53/40; C01G53/42; H01M4/00; H01M4/02; H01M4/36; H01M4/48; H01M4/52; H01M4/525; C01P; C01P2004/00; C01P2004/60; C01P2004/61; C01P2004/62; C01P2006/00; C01P2006/12; H01M4/485; H01M4/50; H01M4/505; Y; Y02; Y02E; Y02E60/00; Y02E60/10
Claims Analysis
Total Claims: 21
Claim 1
Independent Claim
155 words
A process for preparing a mixed metal oxide having the formula Li x M y O z where M is cobalt or cobalt and nickel, x is a number from about 0.1 to about 1.1, y is a total number from about 1.1 to about 0.l, respectively, and z is a number from about 1.9 to about 2.1 which comprises preparing a mixed solution containing x moles of a soluble oxygen-containing salt of lithium and y total moles of soluble oxygen-containing salt(s) of M in a solvent therefor, the soluble oxygen-containing salts being nitrates, oxalates or acetates; concentrating the mixed solution; co-crystallizing a mixed salt of lithium and of M from the concentrated mixed solution; and calcining the co-crystallized mixed salt at a low temperature of from about 400° C. to about 500° C. for a short period of time of from about 1 hour to about 4 hours to form the mixed metal oxide.
Claim 2
Dependent Claim
155 words
A process for preparing a mixed metal oxide having the formula Li x M y O z where M is cobalt or cobalt and nickel, x is a number from about 0.1 to about 1.1, y is a total number from about 1.1 to about 0.l, respectively, and z is a number from about 1.9 to about 2.1 which comprises preparing a mixed solution containing x moles of a soluble oxygen-containing salt of lithium and y total moles of soluble oxygen-containing salt(s) of M in a solvent therefor, the soluble oxygen-containing salts being nitrates, oxalates or acetates; concentrating the mixed solution; co-crystallizing a mixed salt of lithium and of M from the concentrated mixed solution; and calcining the co-crystallized mixed salt at a low temperature of from about 400° C. to about 500° C. for a short period of time of from about 1 hour to about 4 hours to form the mixed metal oxide.
Claim 3
Dependent Claim
30 words
A process according to claim 1, wherein x is a number from about 0.9 to about 1.1 and y is a total number from about 1.1 to about 0.9, respectively.
Claim 4
Dependent Claim
15 words
A process according to claim 1, wherein the mixed solution is concentrated by evaporating it.
Claim 5
Dependent Claim
16 words
A process according to claim 1, wherein the mixed solution is concentrated by vacuum distilling it.
Claim 6
Dependent Claim
23 words
A process according to claim 1, wherein the mixed salt is co-crystallized by rapidly freeze drying the concentrated mixed solution under a vacuum.
Claim 7
Dependent Claim
19 words
A process according to claim 1, wherein the mixed salt is co-crystallized by two-phase partitioning the concentrated mixed solution.
Claim 8
Dependent Claim
19 words
A process according to claim 1, wherein the mixed salt is co-crystallized by flash evaporating the concentrated mixed solution.
Claim 9
Dependent Claim
19 words
A process according to claim 1, wherein the mixed salt is co-crystallized by spray drying the concentrated mixed solution.
Claim 10
Dependent Claim
19 words
A process according to claim 1, wherein the mixed salt is co-crystallized by explosively dehydrating the concentrated mixed solution.
Claim 11
Dependent Claim
18 words
A process according to claim 1, wherein the co-crystallized mixed salt is calcined in a stream of air.
Claim 12
Dependent Claim
22 words
A process according to claim 1, wherein the co-crystallized mixed salt is calcined in a stream of carbon monoxide and carbon dioxide.
Claim 13
Dependent Claim
18 words
A process according to claim 1, wherein the soluble oxygen-containing salts are nitrates and the solvent is water.
Claim 14
Dependent Claim
18 words
A process according to claim 1, wherein the soluble oxygen-containing salts are oxalates and the solvent is water.
Claim 15
Dependent Claim
18 words
A process according to claim 1, wherein the soluble oxygen-containing salts are acetates and the solvent is water.
Claim 16
Dependent Claim
29 words
A process according to claim 1, wherein the mixed metal oxide has a high surface area of from about 20 m 2 /g to about 40 m 2 /g.
Claim 17
Dependent Claim
24 words
A process according to claim 1, wherein the mixed metal oxide has a small particle size of from about 0.1 μ to about 2μ.
Claim 18
Dependent Claim
103 words
A process for preparing a mixed metal oxide having the formula LiCoO 2 , which comprises preparing a mixed aqueous solution containing equimolar amounts of lithium nitrate and cobalt nitrate; concentrating the mixed solution by evaporating it; co-crystallizing an equimolar mixed lithium cobalt nitrate salt from the concentrated mixed solution by rapidly freeze drying the concentrated mixed solution; and calcining the co-crystallized mixed salt at a low temperature of from about 400° C. to about 500° C. for a short period of time of from about 1 hour to about 4 hours in a stream of air to form the mixed metal oxide.
Claim 19
Dependent Claim
103 words
A process for preparing a mixed metal oxide having the formula LiCoO 2 , which comprises preparing a mixed aqueous solution containing equimolar amounts of lithium nitrate and cobalt nitrate; concentrating the mixed solution by evaporating it; co-crystallizing an equimolar mixed lithium cobalt nitrate salt from the concentrated mixed solution by rapidly freeze drying the concentrated mixed solution; and calcining the co-crystallized mixed salt at a low temperature of from about 400° C. to about 500° C. for a short period of time of from about 1 hour to about 4 hours in a stream of air to form the mixed metal oxide.
Claim 20
Dependent Claim
113 words
A process for preparing a mixed metal oxide having the formula Li(Co 0 .5 Ni 0 .5)O 2 which comprises preparing a mixed aqueous solution containing one mole of lithium nitrate and one-half mole each of cobalt nitrate and nickel nitrate; concentrating the mixed solution by evaporating it; co-crystallizing a mixed lithium cobalt-nickel nitrate salt from the concentrated mixed solution by rapidly freeze drying the concentrated mixed solution; and calcining the co-crystallized mixed salt at a low temperature of from about 400° C. to about 500° C. for a short period of time of from about 1 hour to about 4 hours in a stream of air to form the mixed metal oxide.
Claim 21
Dependent Claim
113 words
A process for preparing a mixed metal oxide having the formula Li(Co 0 .5 Ni 0 .5)O 2 which comprises preparing a mixed aqueous solution containing one mole of lithium nitrate and one-half mole each of cobalt nitrate and nickel nitrate; concentrating the mixed solution by evaporating it; co-crystallizing a mixed lithium cobalt-nickel nitrate salt from the concentrated mixed solution by rapidly freeze drying the concentrated mixed solution; and calcining the co-crystallized mixed salt at a low temperature of from about 400° C. to about 500° C. for a short period of time of from about 1 hour to about 4 hours in a stream of air to form the mixed metal oxide.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1989-01-27 | 1989-07-29 | 1990-01-28 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1993-01-27 | 1993-07-29 | 1994-01-28 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1997-01-27 | 1997-07-29 | 1998-01-28 | $7700.00 | Window Closed / Lapsed |