# US 9,050,389 B2 · Medical implant comprising a biodegradable magnesium-based alloy and method for its manufacture

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- Number: US 9,050,389 B2
- Document ID: US9050389B2
- Status: Granted
- Kind: B2
- Application number: 13/331,683
- Filed: 2011-12-20
- Published: 2012-06-21
- Granted: 2015-06-09
- Earliest claimed: 2010-12-21
- Assignees: DePuy Synthes Products, Inc.
- Applicants: Peter Kurze; Thomas Imwinkelried; Stefan Beck; Dora Banerjee; Tamara Schwarz
- Inventors: Peter Kurze; Thomas Imwinkelried; Stefan Beck; Dora Banerjee; Tamara Schwarz
- Web page: https://patentgrep.com/patent/US9050389B2

## CPC

- A61L 27/047: {Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06}
- A61B 17/80: Cortical plates {, i.e. bone plates; Instruments for holding or positioning cortical plates, or for compressing bones attached to cortical plates}
- A61B 17/864: {hollow, e.g. with socket or cannulated}
- A61L 27/306: {Other specific inorganic materials not covered by A61L27/303 - A61L27/32}
- A61L 27/58: Materials at least partially resorbable by the body
- A61L 31/022: {Metals or alloys}
- A61L 31/082: {Inorganic materials}
- A61L 31/148: {Materials at least partially resorbable by the body}
- C01F 5/24: Magnesium carbonates
- A61F 2310/00425: Coating made of magnesium or of Mg-based alloys
- A61L 27/303: {Carbon}
- 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
- Y10T 428/265: 1 mil or less
- Y10T 428/31678: Of metal
- 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)
- A61B: DIAGNOSIS; SURGERY; IDENTIFICATION (usefulness limited to only animals A61D)
- C01F: COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts of peroxyacids C01B15/00; sulfides or polysulfides of magnesium, calcium, strontium, or barium C01B17/42; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds other than ammonia or cyanogen containing nitrogen and non-metals and optionally metals C01B21/082; amides or imides of silicon C01B21/087}; metal {imides or} amides C01B21/092, {C01B21/0923}; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanic acid C01C3/14; salts of cyanamide C01C3/16; thiocyanates C01C3/20; {double sulfates of magnesium with sodium or potassium C01D5/12; with other alkali metals C01D15/00, C01D17/00})
- 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)
- Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION

## Abstract

A medical implant comprises a biodegradable magnesium-based alloy of which at least a part of its surface layer comprises a magnesium carbonate. A method for the manufacture of a biocompatible, corrosion-inhibiting protective surface layer on a medical implant comprising a magnesium-based alloy, comprises: providing an implant comprising a magnesium-based alloy to be coated; placing the implant into a reactor chamber; exposing at least part of the surface of said implant to an atmosphere comprising humid carbon dioxide to produce a coating on the surface of the implant comprising a magnesium carbonate of the formula x MgCO3.y Mg (OH)2, whereby x+y=1; removing the implant from the reactor chamber; and drying the surface of the implant.

## Claims

### Claim 1

A method for the manufacture of a biocompatible, corrosion-inhibiting protective surface layer on a medical implant comprising a magnesium-based alloy, the method comprising:
placing an implant comprising a magnesium-based alloy into a reactor chamber;
exposing at least part of a surface of said implant to an atmosphere comprising humid carbon dioxide, wherein the concentration of the carbon dioxide is at least 50%, and wherein the atmosphere is modified by the addition of gaseous hydrocarbons comprising methane or propane, to produce a coating on the surface of the implant comprising a magnesium carbonate of the formula x MgCO3 .y Mg (OH)2, whereby x+y=1;
removing the implant from the reactor chamber; and
drying the surface of the implant.

### Claim 2 (depends on 1)

The method according to claim 1, wherein the atmosphere has a relative humidity of at least 30%.

### Claim 3 (depends on 2)

The method according to claim 2, wherein said relative humidity is 100%.

### Claim 4 (depends on 2)

The method according to claim 2, wherein the temperature in said reactor chamber is in the range of 10° C. to 50° C.

### Claim 5 (depends on 2)

The method according to claim 2, wherein the temperature in said reactor chamber is in the range of 20° C. to 30° C.

### Claim 6 (depends on 2)

The method according to claim 2, wherein said relative humidity is at least about 90%.

### Claim 7 (depends on 1)

The method according to claim 1, wherein the concentration of carbon dioxide is at least about 90%.

### Claim 8 (depends on 1)

The method according to claim 1, wherein the gaseous hydrocarbons are added in an amount of less than 10% of the total gas content.

### Claim 9 (depends on 1)

The method according to claim 1, wherein the atmosphere is activated by heating up the atmosphere without heating up the implant.

### Claim 10 (depends on 9)

The method according to claim 9, wherein the atmosphere is activated by heating up the atmosphere using microwaves.

### Claim 11 (depends on 1)

The method according to claim 1, wherein the pressure in said reactor exceeds atmospheric pressure.

### Claim 12 (depends on 11)

The method according to claim 11, wherein the pressure in said reactor chamber is in the range of about 5 to about 60 bar.

### Claim 13 (depends on 1)

The method according to claim 1, wherein water is added to the reactor chamber before placing the implant into the reactor chamber.

### Claim 14 (depends on 1)

The method according to claim 1, wherein the pressure in said reactor corresponds essentially to atmospheric pressure.

### Claim 15 (depends on 1)

The method according to claim 1, wherein said magnesium-based implant is coated over a time period lasting about 24 hours to about 720 hours.

### Claim 16 (depends on 1)

The method according to claim 1, wherein said drying is effected at 80° C. to 130° C.

### Claim 17 (depends on 1)

The method according to claim 1 further comprising:
treating the surface of the implant with supercritical carbon dioxide prior to exposing at least part of the surface of the implant to the atmosphere.

### Claim 18 (depends on 1)

The method according to claim 1, wherein said drying is effected for about 10 minutes to about 30 minutes.

### Claim 19

A method for the manufacture of a biocompatible, corrosion-inhibiting protective surface layer on a medical implant comprising a magnesium-based alloy, the method comprising:
placing an implant comprising a magnesium-based alloy into a reactor chamber wherein the pressure in said reactor exceeds atmospheric pressure;
exposing at least part of a surface of said implant to an atmosphere comprising humid carbon dioxide to produce a coating on the surface of the implant comprising a magnesium carbonate of the formula x MgCO3 .y Mg (OH)2, whereby x +y =1;
removing the implant from the reactor chamber; and
drying the surface of the implant.

### Claim 20 (depends on 19)

The method according to claim 19, wherein the atmosphere has a relative humidity of at least 30%.

### Claim 21 (depends on 20)

The method according to claim 20, wherein the atmosphere is modified by the addition of hydrogen gas and/or gaseous hydrocarbons.

### Claim 22 (depends on 21)

The method according to claim 21, wherein the gaseous hydrocarbons comprise methane or propane.

### Claim 23 (depends on 21)

The method according to claim 21, wherein the hydrogen gas and/or gaseous hydrocarbons are added in an amount of less than 10% of the total gas content.

### Claim 24 (depends on 20)

The method according to claim 20, wherein said relative humidity is 100%.

### Claim 25 (depends on 20)

The method according to claim 20, wherein the temperature in said reactor chamber is in the range of 10° C. to 50° C.

### Claim 26 (depends on 20)

The method according to claim 20, wherein the temperature in said reactor chamber is in the range of 20° C. to 30° C.

### Claim 27 (depends on 20)

The method according to claim 20, wherein said relative humidity is at least about 90%.

### Claim 28 (depends on 19)

The method according to claim 19, wherein the concentration of the carbon dioxide is at least 50%.

### Claim 29 (depends on 28)

The method according to claim 28, wherein the concentration of the carbon dioxide is at least about 90%.

### Claim 30 (depends on 19)

The method according to claim 19, wherein the atmosphere is activated by heating up the atmosphere without heating up the implant.

### Claim 31 (depends on 30)

The method according to claim 30, wherein the atmosphere is activated by heating up the atmosphere using microwaves.

### Claim 32 (depends on 19)

The method according to claim 19, wherein the pressure in said reactor chamber is in the range of about 5 to about 60 bar.

### Claim 33 (depends on 19)

The method according to claim 19, wherein water is added to the reactor chamber before placing the implant into the reactor chamber.

### Claim 34 (depends on 19)

The method according to claim 19, wherein said magnesium-based implant is coated over a time period lasting about 24 hours to about 720 hours.

### Claim 35 (depends on 19)

The method according to claim 19, wherein said drying is effected at 80° C. to 130° C.

### Claim 36 (depends on 19)

The method according to claim 19 further comprising:
treating the surface of the implant with supercritical carbon dioxide prior to exposing at least part of the surface of the implant to the atmosphere.

### Claim 37 (depends on 19)

The method according to claim 19, wherein said drying is effected for about 10 minutes to about 30 minutes.
