Method for plasma processing

• US 5,702,770 A
• Filed: 01/30/1996
• Issued: 12/30/1997
• Est. Priority Date: 01/30/1996
• Status: Expired due to Term

• Current Assignee: Becton, Dickinson & Co
• Original Assignee: Becton, Dickinson & Co
• Inventors: Martin, David Alan
• Primary Examiner(s): PIANALTO, BERNARD D
• Application Number:
  US08/593,975
• Time in Patent Office: 700 Days
• Field of Search: 427/574, 427/575, 427/579, 427/588, 427/569, 427/237, 427/238, 427/255.3, 427/296
• US Class Current: 427/475
• CPC Class Codes: B05D 1/62 Plasma-deposition of organic layers plasma deposition in general C23C14/00, C23C16/00
• CPC Class Codes: B05D 2201/02 Polymeric substrate
• CPC Class Codes: B05D 3/144 of polymeric substrates
• CPC Class Codes: B05D 7/227 of containers, cans or the like
• CPC Class Codes: C23C 16/045 Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
• CPC Class Codes: C23C 16/40 Oxides
• CPC Class Codes: C23C 16/402 Silicon dioxide
• CPC Class Codes: C23C 16/44 characterised by the method of coating C23C16/04 takes precedence
• CPC Class Codes: C23C 16/515 using pulsed discharges

Abstract

An apparatus and method for facilitating plasma processing and in particular chemical plasma enhanced vapor deposition, plasma polymerization or plasma treatment of barrier materials onto the interior surface of containers barrier materials are useful for providing an effective barrier against gas and/or water permeability in containers and for extending shelf-life of containers, especially plastic evacuated blood collection devices.

Claims

1. A method for applying a barrier film coating to the interior wall surface of a plastic substrate comprising:

(a) positioning a plastic substrate having an open end, a closed end, an exterior, an interior and an external and interior wall surface so that said open end is connected to a vacuum manifold system having a monomer supply source, an oxider supply source comprising air, oxygen or nitrous oxygen and a vacuum supply source;

(b) positioning the external wall surface of said plastic substrate with an electrode assembly;

(c) evacuating said interior of said substrate;

(d) delivering a monomer gas to said interior of said substrate;

(e) delivering oxygen to said interior of said substrate;

(f) delivering an alternating electrical current to said electrode; and

(g) ionizing said gases so as to form a plasma whereby a barrier film coating is applied to the interior wall surface of said substrate.

2. The method of claim 1 wherein said alternating current is a low frequency alternating current, radio frequency or microwave frequency.

3. The process of claim 1 wherein said substrate is blood collection tube.

4. The method of claim 1 wherein said oxidizer gas is delivered to said substrate at about 110 mTorr to about 200 mTorr.

5. The method of claim 1 wherein said monomer gas is delivered to said substrate at about 80 mTorr to about 190 mTorr.

6. The method of claim 1 wherein about 0.5 sccm to about 15 sccm of a monomer gas is delivered to said substrate.

7. The method of claim 1 wherein about 15 sccm to about 35 sccm of an oxidizer gas is delivered to said substrate.

8. The method of claim 1 wherein said substrate is evacuated from about 0.001 mTorr to about 100 mTorr.

9. The method of claim 1 wherein step (d) further includes a diluent gas.

10. The method of claim 9 wherein said diluent gas is an inert gas.

11. The method of claim 10 wherein said inert gas is helium, or argon.

12. The method of claim 10 wherein said non-reactive gas is nitrogen.

13. A method for applying a barrier film coating to the interior wall surface of a plastic substrate comprising:

(a) positioning a plastic article having an open end, a closed end and an external and interior wall surface so that said open end is connected to a vacuum manifold system having a monomer supply source, an oxidizer supply source and a vacuum supply source;

(b) positioning said exterior wall surface of said plastic article with an electrode assembly;

(c) evacuating said interior of said article to from about 0.001 mTorr to about 100 mTorr;

(d) delivering a monomer gas of HMDSO to said interior of said article from about 0.1 sccm to about 50 sccm and from about 80 mTorr to about 190 mTorr;

(e) delivering an oxidizer gas of air to said interior of said article from about 15 sccm to about 35 sccm and from about 110 mTorr to about 200 mTorr; and

(f) delivering a radio frequency power to said electrode of about 5 MHz to about 50 MHz and from about 15 Watts to about 40 Watts.

14. A method for applying a barrier film coating to the interior wall surface of a plastic substrate comprising:

(a) positioning a plastic article having an open end, a closed end, an exterior, an interior and an external and interior wall surface so that said open end is connected to a vacuum manifold system having a monomer supply source, an oxider supply source and a vacuum supply source;

(b) positioning the external wall surface of said plastic article with an electrode assembly;

(c) evacuating said interior of said article;

(d) delivering a monomer gas and an oxidizer gas to said interior of said article;

(e) delivering a radio frequency power to said electrode;

(f) ionizing said gases so as to form a plasma whereby a barrier film coating is applied to the interior wall surface of said container;

(g) stopping the radio frequency power in step (e); and

(h) repeating steps (e)-(f).

15. The method of claim 14 wherein step (d) further includes a diluent gas.

16. A method for applying a barrier film coating to the interior wall surface of a plastic substrate comprising:

(a) positioning a plastic article having an open end, a closed end, an exterior, an interior and an external and interior wall surface so that said open end is connected to a vacuum manifold system having a monomer supply source, an oxider supply source and a vacuum supply source;

(b) positioning the external wall surface of said plastic article with an electrode assembly;

(c) evacuating said interior of said article;

(d) delivering a monomer gas and an oxidizer gas to said interior of said article;

(e) delivering a radio frequency power to said electrode;

(f) ionizing said gases so as to form a plasma whereby a barrier film coating is applied to the interior wall surface of said container;

(g) stopping the delivery of gases in step (d); and

(h) repeating step (d).

17. The method of claim 16 wherein step (d) further includes a diluent gas.

18. A method for applying a barrier film coating to the interior wall surface of a plastic substrate comprising:

(a) positioning a plastic article having an open end, a closed end and an external and interior wall surface so that said open end is connected to a vacuum manifold system having a monomer supply source, an oxidizer supply source and a vacuum supply source;

(b) positioning said exterior wall surface of said plastic article with an electrode assembly;

(c) evacuating said interior of said article to from about 0.001 mTorr to about 100 mTorr;

(d) delivering a monomer gas of HMDSO to said interior of said article from about 0.1 sccm to about 50 sccm and from about 80 mTorr to about 190 mTorr;

(e) delivering an oxidizer gas of air to said interior of said article from about 15 sccm to about 35 sccm and from about 110 mTorr to about 200 mTorr;

(f) delivering a radio frequency power to said electrode of about 5 MHz to about 50 MHz and from about 5 Watts to about 40 Watts;

(g) stopping the delivery of gases in step (d);

(h) stopping the radio frequency power in step (e); and

(i) repeating steps (d)-(h).

19. The method of claim 18 wherein step (d) further includes a diluent gas.