Process for obtaining tissue-protective implants prepared from titanium or a titanium-base microalloy

• US 5,354,390 A
• Filed: 03/31/1993
• Issued: 10/11/1994
• Est. Priority Date: 04/10/1992
• Status: Expired due to Fees

• Current Assignee: TAVKOZLESI KUTATO INTEZET 65
• Original Assignee: Tavkozlesi Kutato Intezet
• Inventors: Haszmann, Karoly, Vargha, Kalman, Juhasz, Imre, Szabo, Gyorgy, Kovacs, Lajos
• Primary Examiner(s): Roy, Upendra
• Application Number:
  US08/041,441
• Time in Patent Office: 559 Days
• Field of Search: 427/2, 205/318, 205/322, 148/518, 148/269, 623/16
• US Class Current: 148/518
• CPC Class Codes: A61C 8/0015 being a conversion layer, e.g. oxide layer
• 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: A61L 27/06 Titanium or titanium alloys
• CPC Class Codes: C25D 11/26 of refractory metals or alloys based thereon

Abstract

The invention relates to a new process for obtaining tissue-protective devices of bone surgery implants prepared from a medical-purity metal, titanium and/or a titanium-base microalloy containing at least 98% by weight of titanium, by establishing a biocompatible (tissue-protective) coating on the metal surface by anodic oxidation after degreasing and chemical or electrochemical etching, which comprises carrying out the anodic oxidation of the etched implant surfaces in an aqueous solution of a phosphate concentration lower than 20% by weight with a current density of 2 to 50 mA/cm² until reaching a voltage of at least 105 V, then, after washing to ion-free, heat-treating the thus-oxidized implants at a temperature between 120° C. and 750° C. for 5 to 120 minutes, and repeating once or twice the anodic oxidation and heat-treatment with the phosphate concentration, current density and temperature values as given above for the first step.

Claims

1. A process for obtaining tissue-protective devices of bone surgery, especially cheek bone, mandible and common surgery, implants prepared from a medical-purity metal, titanium and/or a titanium-base microalloy containing at least 98% by weight of titanium, by establishing a bio-compatible (tissue-protective) coating on the metal surface of the implant by anodic oxidation after degreasing and chemical or electrochemical etching, which comprises carrying out the anodic oxidation of the implant surface in an aqueous solution of a phosphate concentration lower than 20% by weight with a current density of 2 to 50 mA/cm² until reaching a voltage of at least 105 V, then, after washing to ion-free, heat-treating the implants at a temperature between 120°

C. and 750°

C. for 5 to 120 minutes, and repeating once or twice the anodic oxidation and heat-treatment with the phosphate concentration, current density and temperature values as given above for the first step.

2. A process as claimed in claim 1, which comprises using a primary, secondary or tertiary orthophosphate and/or methyl ethyl phosphate as phosphate-containing bath.

3. A process as claimed in claim 1, which comprises using an aqueous solution containing 3 to 7% by weight of disodium hydrogen phosphate as aqueous solution.

4. A process as claimed in claim 1, which comprises carrying out the heat-treatment of the implants for 5 to 120 minutes.

5. A process as claimed in claim 1, which comprises carrying out the anodic oxidation with a current density of 15 to 25 mA/cm² until reaching a voltage of 105 to 125 V.

6. A process as claimed in claim 1, which comprises carrying out the heat-treatment at a temperature of 300°

to 450°

C.

7. A process as claimed in claim 1, which comprises carrying out the heat-treatment at a temperature of 680°

to 740°

C. under vacuum.

8. A process as claimed in claim 2, which comprises using ammonium, potassium or sodium orthophosphate as primary orthophosphate.

9. A process as claimed in claim 5, which comprises carrying out the heat-treatment for 40 to 60 minutes.