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US5028568A
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Niobium-doped titanium membranes
Assignee: Wisconsin Alumni Research Foundation
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Filing: 1989-07-05
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Granted: 1991-07-02
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Expires: 2009-07-05
Abstract
Abstract A metal oxide particulate membrane is made more electrically conductive, and thus more suitable for electrochemical cells by the incorporation into the membrane of a dopant element. The dopant is dissolved in an alcohol and then incorporated in the sol-gel process used to form the particulate metal oxide membrane. The invention is exemplified by a niobium doped titanium dioxide ceramic membrane which has good porosity while having a conductivity several orders of magnitude higher than a similar membrane made without incorporating the niobium dopant.
Inventors
- 👤 Marc A. Anderson
- 👤 Hirofumi Kikkawa
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 18:38
CPC Classifications
C; C04; C04B; C04B35/00; C04B35/01; C04B35/46; C04B38/00; C04B38/0045; C04B2111/00; C04B2111/00474; C04B2111/00793; C04B2111/00801
Claims Analysis
Total Claims: 20
Claim 1
Independent Claim
189 words
A method of making a metal oxide ceramic membrane with improved conductivity comprising the steps of: (a) dissolving in alcohol a quantity of a dopant element selected to have a valence value one different from the metal of the metal oxide ceramic; (b) combining with the dissolved dopant a quantity of a metal alkoxide selected to give a preselected ratio metal to dopant in excess of ten to one in the resultant membrane; (c) adding to the combination solution a limited amount of water and an acid in sufficient quantity to begin to peptize the metal oxide; (d) slowly adding an additional quantity of water to the combination solution; (e) heating the combination solution while stirring until a colloidal suspension is achieved; (f) separating water from the colloidal suspension until a gel is made; and (g) sintering the gel at a temperature of between about 200° C. and 600° C. into a unitary, durable, continuous porous ceramic membrane which then has incorporated into it the dopant element and which has an electrical conductivity of at least ten times higher than a porous ceramic membrane made without the dopant element.
Claim 2
Independent Claim
189 words
A method of making a metal oxide ceramic membrane with improved conductivity comprising the steps of: (a) dissolving in alcohol a quantity of a dopant element selected to have a valence value one different from the metal of the metal oxide ceramic; (b) combining with the dissolved dopant a quantity of a metal alkoxide selected to give a preselected ratio metal to dopant in excess of ten to one in the resultant membrane; (c) adding to the combination solution a limited amount of water and an acid in sufficient quantity to begin to peptize the metal oxide; (d) slowly adding an additional quantity of water to the combination solution; (e) heating the combination solution while stirring until a colloidal suspension is achieved; (f) separating water from the colloidal suspension until a gel is made; and (g) sintering the gel at a temperature of between about 200° C. and 600° C. into a unitary, durable, continuous porous ceramic membrane which then has incorporated into it the dopant element and which has an electrical conductivity of at least ten times higher than a porous ceramic membrane made without the dopant element.
Claim 3
Dependent Claim
35 words
The method of claim 1 wherein the metal alkoxide is in alcohol solution and wherein the alcohol in which the dopant is dissolved in a different alcohol from the alcohol in the metal alkoxide solution.
Claim 4
Dependent Claim
19 words
The method of claim 1 wherein the ratio of metal to dopant is between 100 and 10 to one.
Claim 5
Dependent Claim
14 words
The method of claim 1 wherein prior to step (c), the mixture is anhydrous.
Claim 6
Dependent Claim
18 words
The method of claim 1 wherein the sintering is at a temperature of 400 to 600 degrees C.
Claim 7
Dependent Claim
30 words
The method of claim 1 wherein the resultant membrane has conductivity at least one thousand times greater than the conductivity of a similar membrane prepared without the dopant being added.
Claim 8
Dependent Claim
21 words
The method of claim 1 wherein the dopant element has a valence value one more than the metal of the membrane.
Claim 9
Independent Claim
171 words
A method of making a niobium doped titanium ceramic membrane comprising the steps of: (a) dissolving in alcohol a quantity of a niobium slat; (b) adding to the dissolved niobium salt a quantity of a titanium alkoxide, the quantity selected to give a molar ratio of between 10 and 100 of titanium to niobium in the solution; (c) adding a limited amount of water and an acid to commence the peptizing of the titanium oxide molecules; (d) diluting the combination with additional water and stirring to ensure complete mixing; (e) heating the combination while stirring for a sufficient time for a colloidal suspension to form; (f) dewatering the colloidal suspension to make a gel; and (g) sintering the gel at a temperature of between about 200° C. and 600° C. to make a titanium oxide porous ceramic particulate membrane having a selected amount of niobium integrally incorporated into the membrane the membrane having an electrical conductivity of at least ten times higher than a porous ceramic membrane made without the niobium.
Claim 10
Independent Claim
171 words
A method of making a niobium doped titanium ceramic membrane comprising the steps of: (a) dissolving in alcohol a quantity of a niobium slat; (b) adding to the dissolved niobium salt a quantity of a titanium alkoxide, the quantity selected to give a molar ratio of between 10 and 100 of titanium to niobium in the solution; (c) adding a limited amount of water and an acid to commence the peptizing of the titanium oxide molecules; (d) diluting the combination with additional water and stirring to ensure complete mixing; (e) heating the combination while stirring for a sufficient time for a colloidal suspension to form; (f) dewatering the colloidal suspension to make a gel; and (g) sintering the gel at a temperature of between about 200° C. and 600° C. to make a titanium oxide porous ceramic particulate membrane having a selected amount of niobium integrally incorporated into the membrane the membrane having an electrical conductivity of at least ten times higher than a porous ceramic membrane made without the niobium.
Claim 11
Dependent Claim
34 words
The method of claim 8 wherein the titanium alkoxide is dissolved in alcohol and wherein the alcohol in which the niobium is dissolved is a different alcohol from the alcohol in the titanium alkoxide.
Claim 12
Dependent Claim
21 words
The method of claim 9 wherein the alcohol in which the niobium is dissolved is ethanol and the titanium is tetraisopropoxide.
Claim 13
Dependent Claim
14 words
The method of claim 8 wherein prior to step (c), the mixture is anhydrous.
Claim 14
Dependent Claim
11 words
The method of claim 8 wherein the acid is hydrochloric acid.
Claim 15
Dependent Claim
18 words
The method of claim 8 wherein the sintering is at a temperature of 400 and 600 degrees C.
Claim 16
Dependent Claim
32 words
The method of claim 8 wherein the resultant membrane has conductivity at least one thousand times greater than the conductivity of a titanium oxide ceramic membrane prepared without the niobium being added.
Claim 17
Dependent Claim
74 words
A novel composition of matter comprising a titanium oxide particulate porous ceramic membrane having integrally incorporated into its particles doping atoms of niobium in amount such that the ratio of titanium to niobium is between 100 and 10 to one, wherein the membrane has an electrical conductivity at least ten times higher than a titanium oxide particulate membrane without the niobium doping and a surface area in excess of 50 square meters per gram.
Claim 18
Dependent Claim
74 words
A novel composition of matter comprising a titanium oxide particulate porous ceramic membrane having integrally incorporated into its particles doping atoms of niobium in amount such that the ratio of titanium to niobium is between 100 and 10 to one, wherein the membrane has an electrical conductivity at least ten times higher than a titanium oxide particulate membrane without the niobium doping and a surface area in excess of 50 square meters per gram.
Claim 19
Dependent Claim
97 words
A porous particulate metal oxide ceramic membrane in which a dopant is integrally incorporated in the particles of the metal oxide sintered into the membrane, the dopant selected to have a valence value one different from the metal and present at a concentration of less than 10% of the metal of the metal oxide the electrical conductivity of the metal oxide ceramic membrane being at least ten times higher than the electrical conductivity of a metal oxide membrane without the dopant, the porous ceramic membrane having a surface area in excess of 50 square meters per gram.
Claim 20
Dependent Claim
97 words
A porous particulate metal oxide ceramic membrane in which a dopant is integrally incorporated in the particles of the metal oxide sintered into the membrane, the dopant selected to have a valence value one different from the metal and present at a concentration of less than 10% of the metal of the metal oxide the electrical conductivity of the metal oxide ceramic membrane being at least ten times higher than the electrical conductivity of a metal oxide membrane without the dopant, the porous ceramic membrane having a surface area in excess of 50 square meters per gram.
References Cited (Backward Citations)
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| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
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| 3.5 Years (Year 4) | 1994-07-01 | 1994-12-31 | 1995-07-02 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1998-07-01 | 1998-12-31 | 1999-07-02 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2002-07-01 | 2002-12-31 | 2003-07-02 | $7700.00 | Window Closed / Lapsed |