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US5609633A
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Titanium-based bone-bonding composites having inverted concentration gradients of alkali and titanium ions in a surface layer
Assignee: Sagawa Printing Co Ltd
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Filing: 1994-11-09
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Granted: 1997-03-11
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Expires: 2014-11-09
Abstract
Abstract A bone substitute, which provides both the fracture toughness of titanium or titanium alloys and the bioactivity of apatite, wherein titanium or titanium alloys and apatite are tightly adhered, is produced by soaking a substrate of titanium or titanium alloy in an alkaline solution to form a layer comprising amorphous alkali titanate, followed by the heating of the said substrate up to at most the titanium or titanium alloy transition temperature so as to form a stabilized amorphous alkali titanate layer and a sufficient concentration gradient of alkali and titanium ions to permit the growth of apatite thereon from solutions containing apatite-containing ions.
Inventors
- 👤 Tadashi Kokubo
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 18:55
CPC Classifications
A; A61; A61L; A61L27/00; A61L27/28; A61L27/30; A61L27/306; A61F; A61F2/00; A61F2/02; A61F2/28; A61L27/02; A61L27/04; A61L27/06; A61L27/32; A61F2310/00; A61F2310/00389; A61F2310/00592; A61F2310/00796; A61L2430/00; A61L2430/02
Claims Analysis
Total Claims: 16
Claim 1
Independent Claim
223 words
A bone repairing material comprising a substrate of titanium or a titanium alloy and on the surface of the substrate a primary surface layer comprising a titanium oxide phase and an amorphous phase of alkali titanate, said primary surface layer thereby forming an interface between said substrate and primary surface layer, said primary surface layer having an interior and an outer surface, said primary surface layer comprising a titanium oxide phase and an amorphous phase of alkali titanate, said primary surface layer having been treated so as to provide a layer comprising amorphous alkali titanate phase and a sufficient concentration gradient of alkali and titanium ions to permit apatite from natural or simulated body fluid to be grown thereon and wherein the concentration of titanium oxide phase in the primary surface layer gradually decreases from the layer interior towards the outer surface, while the concentration of the total alkali ions in the primary surface layer gradually increases from the layer interior towards the outer surface, and wherein said interface between said substrate and said primary surface layer and boundaries of the phases within the surface layer are tightly bonded, said primary surface layer having been heated in a gas comprising oxygen to from about 300° C. to not more than the titanium or titanium alloy transition temperature, for about 1 to 24 hours.
Claim 2
Dependent Claim
223 words
A bone repairing material comprising a substrate of titanium or a titanium alloy and on the surface of the substrate a primary surface layer comprising a titanium oxide phase and an amorphous phase of alkali titanate, said primary surface layer thereby forming an interface between said substrate and primary surface layer, said primary surface layer having an interior and an outer surface, said primary surface layer comprising a titanium oxide phase and an amorphous phase of alkali titanate, said primary surface layer having been treated so as to provide a layer comprising amorphous alkali titanate phase and a sufficient concentration gradient of alkali and titanium ions to permit apatite from natural or simulated body fluid to be grown thereon and wherein the concentration of titanium oxide phase in the primary surface layer gradually decreases from the layer interior towards the outer surface, while the concentration of the total alkali ions in the primary surface layer gradually increases from the layer interior towards the outer surface, and wherein said interface between said substrate and said primary surface layer and boundaries of the phases within the surface layer are tightly bonded, said primary surface layer having been heated in a gas comprising oxygen to from about 300° C. to not more than the titanium or titanium alloy transition temperature, for about 1 to 24 hours.
Claim 3
Dependent Claim
20 words
A material according to claim 1, further comprising a layer of apatite on top of the said primary surface layer.
Claim 4
Dependent Claim
19 words
A material according to claim 1, wherein the thickness of the primary surface layer is 0.1 to 10 μm.
Claim 5
Dependent Claim
19 words
A material according to claim 2, wherein the thickness of the primary surface layer is 0.1 to 10 μm.
Claim 6
Dependent Claim
18 words
A material according to claim 2, wherein the thickness of the apatite layer is at least 1 μm.
Claim 7
Independent Claim
228 words
A method of producing a material useful as a bone substitute comprising heating a substrate of titanium or titanium alloy and on the surface of the substrate a primary surface layer comprising a titanium oxide phase and an amorphous phase of alkali titanate, said primary surface layer thereby forming an interface between said substrate and primary surface layer, said primary surface layer having an interior and an outer surface, said primary surface layer comprising a titanium oxide phase and an amorphous phase of alkali titanate, said primary surface layer having been treated so as to provide a layer comprising amorphous alkali titanate and a sufficient concentration gradient of alkali and titanium ions to permit apatite from natural or simulated body fluid to be grown thereon and wherein the concentration of titanium oxide phase in the primary surface layer gradually decreases from the layer interior towards the outer surface, while the concentration of the total alkali ions in the primary surface layer gradually increases from the layer interior towards the outer surface, and wherein said interface between said substrate and said primary surface layer and boundaries of the phases within the surface layer are tightly bonded, said heating being conducted in a gas comprising oxygen to a temperature from about 300° C. to not more than the titanium or titanium alloy transition temperature, for about 1 to 24 hours.
Claim 8
Independent Claim
228 words
A method of producing a material useful as a bone substitute comprising heating a substrate of titanium or titanium alloy and on the surface of the substrate a primary surface layer comprising a titanium oxide phase and an amorphous phase of alkali titanate, said primary surface layer thereby forming an interface between said substrate and primary surface layer, said primary surface layer having an interior and an outer surface, said primary surface layer comprising a titanium oxide phase and an amorphous phase of alkali titanate, said primary surface layer having been treated so as to provide a layer comprising amorphous alkali titanate and a sufficient concentration gradient of alkali and titanium ions to permit apatite from natural or simulated body fluid to be grown thereon and wherein the concentration of titanium oxide phase in the primary surface layer gradually decreases from the layer interior towards the outer surface, while the concentration of the total alkali ions in the primary surface layer gradually increases from the layer interior towards the outer surface, and wherein said interface between said substrate and said primary surface layer and boundaries of the phases within the surface layer are tightly bonded, said heating being conducted in a gas comprising oxygen to a temperature from about 300° C. to not more than the titanium or titanium alloy transition temperature, for about 1 to 24 hours.
Claim 9
Dependent Claim
29 words
A method according to claim 6, further comprising soaking the resultant product in an aqueous solution comprising calcium and phosphorous in a concentration level of, at least, apatite solubility.
Claim 10
Dependent Claim
46 words
A method according to claim 6, wherein the amorphous alkali titanate phase was formed by soaking the titanium or titanium alloy in an alkaline solution containing at least one of: sodium ions Na + , potassium ions K + , and calcium ions Ca 2+ .
Claim 11
Dependent Claim
16 words
A method according to claim 6, wherein the heating temperature is from 300° to 800° C.
Claim 12
Dependent Claim
16 words
A method according to claim 6, wherein the heating temperature is from 550° to 650° C.
Claim 13
Dependent Claim
15 words
A method according to claim 9, wherein the heating is conducted for about 1-24 hours.
Claim 14
Dependent Claim
15 words
A method according to claim 10, wherein the heating is conducted for about 1-24 hours.
Claim 15
Dependent Claim
16 words
A material according to claim 1, wherein the heating temperature is from 300° to 800° C.
Claim 16
Dependent Claim
16 words
A material according to claim 1, wherein the heating temperature is from 550° to 650° C.
References Cited (Backward Citations)
US4801300A
Cited
US4965088A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 2000-03-10 | 2000-09-09 | 2001-03-11 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2004-03-10 | 2004-09-09 | 2005-03-11 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2008-03-10 | 2008-09-09 | 2009-03-11 | $7700.00 | Window Closed / Lapsed |