# US 8,784,864 B2 · Bone repair material and method for producing the same

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- Number: US 8,784,864 B2
- Document ID: US8784864B2
- Status: Granted
- Kind: B2
- Application number: 13/147,082
- Filed: 2010-01-29
- Published: 2011-11-24
- Granted: 2014-07-22
- Earliest claimed: 2009-01-30
- Assignees: Chubu University Educational Foundation; Osaka Yakin Kogyo Co., Ltd.; Avanced Medix Inc.
- Applicants: Tadashi Kokubo; Tomiharu Matsushita; Deepak K. Pattanayak
- Inventors: Tadashi Kokubo; Tomiharu Matsushita; Deepak K. Pattanayak
- Web page: https://patentgrep.com/patent/US8784864B2

## CPC

- A61F 2/30767: {Special external or bone-contacting surface, e.g. coating for improving bone ingrowth}
- A61L 27/06: Titanium or titanium alloys
- A61P 19/00: Drugs for skeletal disorders
- A61F 2002/30838: {Microstructures}
- A61F 2002/3084: {Nanostructures}
- A61F 2310/00023: Titanium or titanium-based alloys, e.g. Ti-Ni alloys
- A61F 2310/00616: Coating made of titanium oxide or hydroxides
- A61L 2400/18: Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
- A61L 2430/02: for reconstruction of bones; weight-bearing implants
- A61F: FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS (dental prosthetics A61C)
- A61L: METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES (preservation of bodies or disinfecting characterised by the agents employed A01N; preserving, e.g. sterilising, food or foodstuffs A23; preparations for medical, dental or toiletry purposes A61K)
- A61P: SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS

## Abstract

Bone repair materials are disclosed, from which ions are hardly eluted in living body and which are superior in apatite-forming ability and resistance to apatite peeling and have a scratch resistance high enough for practical use. The material comprises a substrate made of titanium or titanium alloys, and a surface layer, made substantially of titanium oxide, along the surface of the substrate. The substrate has on the surface thereof irregularities of from 1 nm to 10 μm in average in both width and depth. The layer has a zeta potential of +4.5 mV or more under an aqueous solution environment of pH 6 to 8, and a critical scratch resistance of 35 mN or more when vibration 100 μm in amplitude is added to a stylus with a spring constant of 200 g/mm on the surface layer and the stylus is moved at a rate of 10 mm/sec under a load increasing at a rate of 100 mN/min.

## Claims

### Claim 1

A bone repair material comprising:
a substrate made of titanium or titanium alloys, the substrate having on the surface thereof irregularities of from 1 nm to 10 μm in average in both width and depth; and
a surface layer along the surface of the substrate, the surface layer consisting essentially of titanium oxide and having a zeta potential of +4.5 mV or more under an aqueous solution environment of pH 6 to 8.

### Claim 2 (depends on 1)

The bone repair material according to claim 1, wherein the surface layer has a critical scratch resistance of 35 mN or more when vibration 100 μm in amplitude is added to a stylus with a spring constant of 200 g/mm on the surface layer and the stylus is moved at a rate of 10 mm/sec under a load increasing at a rate of 100 mN/min.

### Claim 3 (depends on 1)

The bone repair material according to claim 1, wherein the surface layer contains an acid group constituting an acid.

### Claim 4 (depends on 1)

A method for producing the bone repair material of claim 1, the method comprising the steps of:
preparing a substrate made of titanium or titanium alloys;
forming irregularities of from 1 nm to 10 μm in average in both width and depth on the surface of the substrate;
immersing the substrate in an acidic aqueous solution having a pH of 3 or less;
washing the substrate with water after the immersion; and thereafter
heating the substrate at a temperature of 450 to 750° C.

### Claim 5 (depends on 4)

The method according to claim 4, wherein the formation of the irregularities is conducted by an alkali treatment.

### Claim 6 (depends on 4)

The method according to claim 4, wherein the acidic aqueous solution is a solution selected from the group consisting of aqueous solutions of hydrochloric acid, sulfuric acid, nitric acid, fluoric acid, and mixed acid thereof.

### Claim 7 (depends on 4)

The method according to claim 4, wherein the formation of the irregularities is conducted by performing a treatment with an acidic aqueous solution that is the same as or different from the acidic aqueous solution.

### Claim 8 (depends on 4, 5, 6, 7)

The method according to any one of claims 4 to 7, wherein the washing time is from 10 seconds to 1 minute.