Electrochemical grafting of carbon fibers with aliphatic amines for improved composite strength

Patent metadata

Field	Value
Publication number	US-11225754-B2
Application number	US-201816604595-A
Country	US
Kind code	B2
Filing date	Apr 11, 2018
Priority date	May 26, 2017
Publication date	Jan 18, 2022
Grant date	Jan 18, 2022

Abstract

The surface of a carbon fiber is electrochemically treated by a method to form nitrogen containing groups on the surface of the carbon fiber. The method comprises contacting a carbon fiber surface with an aqueous solution comprised of a non-cyclic aliphatic amine and water soluble inorganic hydroxide with said aqueous solution having a pH of at least 9. A positive electrical bias is then applied to the carbon fibers in the aqueous solution relative to another electrode in contact with the aqueous solution, wherein the positive electrical bias is at a voltage above the oxidation potential of water. The treated carbon fibers are useful for making epoxy reinforced carbon fiber composites.

First claim

The invention claimed is:

1. A method of treating the surface a carbon fiber comprising;
(i) contacting a carbon fiber surface with an aqueous solution comprised of a non-cyclic aliphatic amine and water soluble inorganic hydroxide and said aqueous solution having a pH of at least 9, and
(ii) applying a positive electrical bias to the carbon fibers in the aqueous solution relative to another electrode in contact with the aqueous solution, wherein the positive electrical bias is at a voltage above the oxidation potential of water.

2. The method of claim 1 , wherein the pH is at least 11.

3. The method of claim 1 , wherein the non-cyclic aliphatic amine is represented by:

wherein X is C, N, or O, Y is C or N, m is 0 to 200, n is 0 to 200, p is 0 to 10 and q is 1 to 3.

4. The method of claim 3 , wherein the non-cyclic aliphatic amine is selected from the group consisting of hexamethylenediamine, 2,2′ethylenedioxy-bis(ethylamine), diethylenetriamine, triethylenetetramine, and combination thereof.

5. The method of claim 1 , wherein the voltage is at least 0.6 V to about 1.2 V relative to a saturated Ag/AgCl reference electrode.

6. The method of claim 1 , wherein the non-cyclic aliphatic amine is present in the aqueous solution at a concentration of 0.1 millimolar to 100 millimolar.

7. The method of claim 6 , wherein the concentration of the non-cyclic aliphatic amine is from 10 to 30 millimolar.

8. The method of claim 1 , wherein water soluble inorganic hydroxide is potassium hydroxide, sodium hydroxide or combination thereof.

9. The method of claim 1 , wherein the water soluble inorganic hydroxide is present in the aqueous solution at a concentration of 10 millimolar to 1000 millimolar.

10. The method of claim 9 , wherein the concentration of the water soluble inorganic hydroxide is 50 to 150 millimolar.

11. The method of claim 1 , wherein the applying of the positive electrical bias is performed at a constant current.

12. The method of claim 10 , wherein the current is from 1 to 100 milliamps per gram of carbon fiber.

13. The method of claim 12 , wherein the method is performed for a residence time in the aqueous solution from 1 second to 200 seconds.

14. A carbon fiber treated by the method of claim 1 .

15. An epoxy fiber reinforced composite comprising a cured epoxy resin matrix having therein carbon fibers of claim 14 , wherein the carbon fibers comprise greater than 50% by volume of said composite.

Assignees

• Dow Global Technologies Llc

Inventors

• Lowe Michael A
• Baumer Richard

Classifications

• D06M13/513

  with at least one carbon-silicon bond · CPC title

• D06M2101/40

  Fibres of carbon · CPC title

• D06M10/08

  Organic compounds · CPC title

• D06M15/6436

  containing amino groups · CPC title

• D06M13/328 Primary

  the amino group being bound to an acyclic or cycloaliphatic carbon atom · CPC title