Surface modification of medical implants

• US 5,843,289 A
• Filed: 01/22/1996
• Issued: 12/01/1998
• Est. Priority Date: 01/22/1996
• Status: Expired due to Term

• Current Assignee: Etex Corporation (Zimmer Biomet Holdings, Inc.)
• Original Assignee: Etex Corporation (Zimmer Biomet Holdings, Inc.)
• Inventors: Lee, Dosuk D., Nagras, Atul
• Primary Examiner(s): Weisstuch, Aaron
• Application Number:
  US08/589,409
• Time in Patent Office: 1,044 Days
• Field of Search: 204/192.3, 204/192.32, 204/192.35, 156/643.1, 427/2.26, 216/67, 216/75-76
• US Class Current: 204/192.3
• CPC Class Codes: A61F 2/30767 Special external or bone-contacting surface, e.g. coating for improving bone ingrowth
• CPC Class Codes: A61F 2/3094 Designing or manufacturing processes
• CPC Class Codes: A61F 2002/3092 having an open-celled or open-pored structure
• CPC Class Codes: A61F 2002/30925 etched
• CPC Class Codes: A61F 2310/00023 Titanium or titanium-based alloys, e.g. Ti-Ni alloys
• CPC Class Codes: A61F 2310/00796 Coating or prosthesis-covering structure made of a phosphorus-containing compound, e.g. hydroxy(l)apatite
• CPC Class Codes: A61L 27/04 Metals or alloys
• CPC Class Codes: A61L 27/06 Titanium or titanium alloys
• CPC Class Codes: A61L 27/32 Phosphorus-containing materials, e.g. apatite
• CPC Class Codes: A61L 27/50 Materials characterised by their function or physical properties , e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
• CPC Class Codes: A61L 27/56 Porous materials, e.g. foams or sponges
• CPC Class Codes: C23C 8/36 using ionised gases, e.g. ionitriding
• CPC Class Codes: C23F 4/00 Processes for removing metallic material from surfaces, not provided for in group C23F1/00 or C23F3/00

Abstract

A method of obtaining a porous titanium surface suitable for medical implants is provided. The titanium surface is exposed to a plasma comprising a reactive plasma gas, the reactive plasma gas comprising an active etching species and a sputtering gas. The plasma conditions are effective to modify the titanium surface and provide surface porosity. The plasma conditions are effective to non-uniformly etch and sputter the titanium surface.

Claims

1. A method of making non-uniform titanium surface, comprising:

exposing a titanium surface to a first plasma effective to remove an oxide layer;

providing a second plasma comprising a reactive plasma gas, the reactive plasma gas comprising an active etching species and a sputtering ion, said second plasma effective, to remove titanium from the titanium surface and introduce surface porosity; and

exposing the titanium surface to the second plasma whereby a non-uniform surface is obtained.

3. The method of claim 1 or 2, wherein the active etching species comprises a chlorine or fluorine active species.

4. The method of claim 3, wherein the active chlorine or fluorine species is generated by introducing a chlorine- or fluorine-containing gas into the plasma.

5. The method of claim 4, wherein the chlorine- or fluorine-containing gas is selected from the group consisting of CF₄,cl₂, BCl₃, SF₆, CHF₃, CHCl₃, XeF₂, CCl₄, Freon 11, Freon 12, Freon 13, Freon 115 and mixtures thereof.

6. The method of claim 1 or 2, wherein the sputtering ion is generated by introduction of a species selected from the group of neon, argon, krypton, xenon, BCl₃, SF₆, and mixtures thereof into the plasma.

7. The method of claim 1 or 2, wherein plasma conditions are effective to redeposit sputtered species onto the titanium surface.

8. The method of claim 1 or 2, wherein plasma conditions are effective to sputter off oxygen adsorbed on the titanium surface during exposure of the surface to the plasma.

9. The method of claim 1 or 2, further comprising:

introducing a sputtering target into the plasma, said sputtering target comprising a masking element, such that the masking element is deposited onto the titanium surface during exposure of the surface to the reactive plasma gas.

10. The method of claim 1 or 2, wherein the reactive plasma gas further comprises a gas selected from the group consisting of helium, nitrogen, and oxygen.

11. The method of claim 1 or 2, wherein the titanium surface is selected from the group consisting of commercially pure titanium and titanium alloys.

12. The method of claim 11, wherein the plasma is effective to reactive etch the alloyed elements faster than titanium.

13. The method of claim 1 or 2, wherein the plasma comprises an RF plasma.

14. The method of claim 1 or 2, wherein a reactive plasma gas is obtained by operating a plasma power source in the range of about 100 KHz to about 2.45 GHz.

15. The method of claim 1 or 2, further comprising:

removing a passifying oxide layer prior to surface treatment of the work piece.

16. The method of claim 1 or 2, further comprising:

grit or sand blasting the titanium surface prior to exposure of the titanium surface to the plasma.

17. The method of claim 1 or 2, wherein the titanium surface to be treated is macroporous.

18. The method of claim 1 or 2, further comprising:

cleaning the surface with an oxygen plasma prior to exposure of the titanium surface to the plasma.

19. The method of claim 1 or 2, further comprising:

applying a hydroxyapatite coating to the surface treated work piece.

20. The method of claim 1 or 2, wherein the titanium surface is housed in a chamber maintained at a pressure in the range of about 5 to 100 millitorr.

2. A method of making a non-uniform titanium surface, comprising:

exposing a titanium surface to a first plasma effective to remove an oxide layer;

providing a second plasma comprising a reactive plasma gas, the reactive plasma gas comprising an active etching species and a sputtering ion, said second plasma effective to non-uniformly etch and non-uniformly sputter a titanium surface; and

exposing the titanium surface to the second plasma whereby a non-uniform surface is obtained.