IP Library Granted Patent US 7,749,479
Granted Patent B2
US 7,749,479 · App. 11/562,867 · Granted Jul 6, 2010

Carbon fibers having improved strength and modulus and an associated method and apparatus for preparing same

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Quick Facts
Patent No.
US 7,749,479
App. No.
11/562,867
Granted
Jul 6, 2010
Kind
B2
Abstract

The invention is directed to carbon fibers having high tensile strength and modulus of elasticity. The invention also provides a method and apparatus for making the carbon fibers. The method comprises advancing a precursor fiber through an oxidation oven wherein the fiber is subjected to controlled stretching in an oxidizing atmosphere in which tension loads are distributed amongst a plurality of passes through the oxidation oven, which permits higher cumulative stretches to be achieved. The method also includes subjecting the fiber to controlled stretching in two or more of the passes that is sufficient to cause the fiber to undergo one or more transitions in each of the two or more passes. The invention is also directed to an oxidation oven having a plurality of cooperating drive rolls in series that can be driven independently of each other so that the amount of stretch applied to the oven in each of the plurality of passes can be independently controlled.

Claims (23)

1. A carbon fiber having a tensile strength of at least 950 ksi and modulus of elasticity of at least 45 Msi, the carbon fiber having an atomic force microscopy surface image that is characterized by the presence of a plurality of striations of low phase angle domains and a plurality of striations of high phase angle domains that extend across the surface of the carbon fiber, wherein the carbon fiber has an average phase angle depth of 5 nanometers or greater.

2. The carbon fiber according to claim 1 , wherein the carbon fiber has a tensile strength of at least 975 ksi and modulus of elasticity of at least 47 Msi.

3. The carbon fiber according to claim 1 , wherein the carbon fiber has a tensile strength of at least 1000 ksi and modulus of elasticity of at least 50 Msi.

4. The carbon fiber according to claim 1 , wherein the carbon fiber has an average phase angle depth of 8 nanometers or greater.

5. The carbon fiber according to claim 1 , wherein the carbon fiber has a roughness having a Root Mean Square Roughness (Rq) value of about 2 or greater.

6. A carbon fiber having a tensile strength of at least 1000 ksi and modulus of elasticity of at least 50 Msi, and wherein the carbon fiber has a crystallite width value L a of about 4 nm or greater and a resistivity value of about 14 μΩm or greater.

7. The carbon fiber of claim 6 , wherein the carbon fiber has a radial uniformity RU value of about 50 or greater.

8. The carbon fiber of claim 6 , wherein the carbon fiber has an average phase angle depth of 8 nanometers or greater.

9. The carbon fiber of claim 6 , wherein the carbon fiber has an RD value of about 0.05 or less.

10. A carbon fiber having an atomic force microscopy surface image that is characterized by the presence of a plurality of striations of low phase angle domains and a plurality of striations of high phase angle domains that extend across the surface of the carbon fiber, and wherein the carbon fiber has a crystallite width value L a of about 4 nm or greater.

11. The carbon fiber according to claim 10 , wherein the fiber further has Root Mean Square Roughness (Rq) value of about 2 or greater.

12. The carbon fiber according to claim 10 , wherein the fiber further has Root Mean Square Roughness (Rq) value of about 4 or greater.

13. The carbon fiber according to claim 10 , wherein the fiber has a modulus of elasticity of at least 50 Msi, a resistivity of at least 13 μΩm or greater, and a crystallite width value L a of about 4 nm or greater.

14. The carbon fiber according to claim 13 , wherein the carbon fiber has an average phase angle depth of 8 nanometers or greater.

15. A carbon fiber that is prepared by:

stabilizing a carbon fiber precursor polymer by exposing the fiber to an oxidizing atmosphere at an elevated temperature in multiple passes to produce an oxidized fiber;

subjecting the fiber in at least two of the passes to a % stretch that is between 10 and 30%;

passing the oxidized fiber through a furnace at a temperature between about 400 and 800° C.; and

carbonizing the fiber by passing the fiber through a furnace having a temperature that is between about 1300 and 1500° C., wherein the carbon fiber has a tensile strength of at least 1000 ksi and a modulus of elasticity of at least 50 Msi.

16. The carbon fiber of claim 15 wherein the fiber has an atomic force microscopy surface image that is characterized by the presence of a plurality of striations of low phase angle domains and a plurality of striations of high phase angle domains that extend across the surface of the carbon fiber.

17. The carbon fiber of claim 15 , wherein the carbon fiber has a crystallite width value L a of about 4 nm or greater and a resistivity value of about 14 μΩm or greater.

18. The carbon fiber of claim 15 , wherein the carbon fiber has an average phase angle depth of 5 nanometers or greater.

19. The carbon fiber of claim 15 , wherein the carbon fiber has a roughness having a Root Mean Square Roughness (Rq) value of about 2 or greater.

Assignments (12)
RELEASE OF SECURITY INTEREST Recorded Oct 2, 2014
From: CITIZENS BANK, NATIONAL ASSOCIATION
To: HEXCEL CORPORATION; HEXCEL HOLDINGS LUXEMBOURG S.À.R.L.
Reel/Frame 033887/0199 →
TERMINATION OF SECURITY INTEREST IN PATENTS Recorded Sep 24, 2014
From: CITIZENS BANK, NATIONAL ASSOCIATION (F/K/A RBS CITIZENS, N.A.)
To: HEXCEL CORPORATION
Reel/Frame 033813/0565 →
RELEASE OF SECURITY INTEREST Recorded Sep 3, 2013
From: BANK OF AMERICA, N.A.
To: HEXCEL CORPORATION
Reel/Frame 031140/0729 →
SECURITY AGREEMENT Recorded Jul 1, 2013
From: HEXCEL CORPORATION; HEXCEL HOLDINGS LUXEMBOURG S.A.R.L.
To: RBS CITIZENS, N.A., AS ADMINISTRATIVE AGENT
Reel/Frame 030724/0287 →
SECURITY INTEREST Recorded Jan 30, 2012
From: HEXCEL CORPORATION
To: BANK OF AMERICA, N.A., AS ADMINISTRATIVE AGENT
Reel/Frame 027810/0301 →
SECURITY AGREEMENT IP SUPPLEMENT Recorded Jul 15, 2011
From: HEXCEL CORPORATION
To: BANK OF AMERICA, N.A., AS ADMINISTRATIVE AGENT
Reel/Frame 026596/0948 →
SECURITY AGREEMENT Recorded Aug 20, 2010
From: HEXCEL CORPORATION
To: BANK OF AMERICA, N.A.
Reel/Frame 024864/0016 →
RELEASE OF SECURITY INTEREST Recorded Aug 20, 2010
From: DEUTSCHE BANK TRUST COMPANY AMERICAS
To: HEXCEL CORPORATION
Reel/Frame 024864/0040 →
GRANT OF PATENT SECURITY INTEREST Recorded May 21, 2009
From: HEXCEL CORPORATION
To: DEUTSCHE BANK TRUST COMPANY AMERICAS, AS ADMINISTRATIVE AGENT
Reel/Frame 022722/0240 →
RELEASE OF PATENT SECURITY INTEREST Recorded May 21, 2009
From: DEUTSCHE BANK TRUST COMPANY AMERICAS, AS ADMINISTRATIVE AGENT
To: HEXCEL CORPORATION; HEXCEL REINFORCEMENTS CORP.
Reel/Frame 022722/0301 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 20, 2007
From: LEON Y LEON, CARLOS A.
To: HEXCEL CORPORATION
Reel/Frame 019033/0434 →
GRANT OF PATENT SECURITY INTEREST (IP SUPPLEMENT NO. 7) Recorded Mar 1, 2007
From: HEXCEL CORPORATION
To: DEUTSCHE BANK TRUST COMPANY AMERICAS, AS ADMINISTRATIVE AGENT
Reel/Frame 018948/0637 →