Titanium plasma nitriding intensified by thermionic emission source

• US 5,334,264 A
• Filed: 06/30/1992
• Issued: 08/02/1994
• Est. Priority Date: 06/30/1992
• Status: Expired due to Fees

• Current Assignee: Board of Supervisors of Louisiana State University Agricultural & Mechanical College (Louisiana State University System)
• Original Assignee: Board of Supervisors of Louisiana State University Agricultural & Mechanical College (Louisiana State University System)
• Inventors: Meletis, Efstathios I.
• Primary Examiner(s): ROY, UPENDRA
• Application Number:
  US07/906,929
• Time in Patent Office: 763 Days
• Field of Search: 148/222, 148/421, 427/570, 437/16, 437/18
• US Class Current: 148/222
• CPC Class Codes: C23C 8/24 Nitriding
• CPC Class Codes: C23C 8/36 using ionised gases, e.g. ionitriding

Abstract

The present invention relates to ion nitriding of pure titanium or titanium-containing alloys at low pressure by intensifying the glow discharge.

Plasma intensification was produced by thermionic emission in conjunction with a triode glow discharge system. Effective ion nitriding can be achieved by employing the present invention at relatively low temperatures (480° C.) and with significantly enhanced compound layer growth kinetics compared to the conventional nitriding techniques. Processed Ti and Ti-6Al-4V developed a surface layer of TiN followed by a Ti₂ N layer and an interstitial nitrogen diffusion zone. Processed specimens showed a three fold increase in surface hardness. Surface roughness was found to be a function of the degree of plasma intensification. Processing of Ti-6Al-4V resulted in a higher wear, corrosion and wear-corrosion resistance. The present invention indicates that ion nitriding with intensified glow discharge has a great potential as a surface modification method for Ti and Ti alloys. Materials nitriding by the present invention having the properties defined above are suitable for use as orthopaedic implant devices as well as other applications of titanium and titanium alloys requiring resistance to wear and corrosion.

Claims

1. In a process for nitriding the surface of titanium or a titanium-containing alloy for providing a hard surface layer material with enhanced wear and corrosion resistance by plasma nitriding, the improvement comprising combining a thermionic emission source with a plasma nitriding glow discharge source whereby the glow discharge is intensified.

2. The process of claim 1 wherein the titanium is essentially pure.

3. The process of claim 1 wherein the titanium is alloyed with other elements, such alloys falling into categories of α

, β and

α

-β

types.

4. The process of claim 1 wherein the titanium is present in conjunction with other materials.

5. The process of claim 1 wherein the nitriding of the surface of titanium or a titanium-containing alloy is conducted at a temperature from about 300°

C. to about 600°

C.

6. The process of claim 1 wherein the nitriding of the surface of titanium or a titanium-containing alloy is conducted at a pressure of about 5 to about 250 mTorr.

7. The process of claim 1 wherein a surface layer of TiN followed by Ti₂ N layer and interstitial nitrogen diffusion layer are formed in the titanium or titanium-containing alloy.

8. The process of claim 1 wherein the glow discharge source is a positively charged electrode, a RF source or a magnetic fluid.

9. The process of claim 1 wherein the glow discharge source is operated at an applied voltage of about 1 to about 3KeV.

10. The process according to claim 1 wherein the glow discharge source had a current flux density from about 0.5 to about 4 mA/cm².

11. The process of claim 1 wherein nitriding of the surface of titanium or a titanium containing alloy occurs in a period of time from about 1 to about 20 hrs.

12. The process of claim 1 wherein the nitriding occurs under an inert gas atmosphere.

13. The process of claim 3 wherein the titanium-containing alloy is Ti-6Al-4V.

14. The process of claim 7 wherein the nitriding introduces nitrogen into the surface of titanium or a titanium-containing alloy to a depth from about 20 to about 90 μ

m.

15. The process according to claim 10 wherein the current flux density is 3.13 mA/cm².

16. The process of claim 12 wherein the inert gas atmosphere is selected from the group consisting of essentially pure He, Ne, Ar, N₂ and mixtures thereof.

17. The process of claim 14 wherein the nitriding introduces nitrogen into the surface of titanium or a titanium-containing alloy to a depth of about 50 μ

.

18. The process of claim 16 wherein the atmosphere is a Ar-N₂ mixture.

19. The process of claim 18 wherein the Ar to N₂ ratio is from 1:

1 ranging to pure N₂.

20. The process of claim 19 wherein the Ar to N₂ ratio is 3:

1.