IP Library Granted Patent US 9,093,685
Granted Patent B2
US 9,093,685 · App. 12/321,466 · Granted Jul 28, 2015

Methods of making membrane electrode assemblies

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Quick Facts
Patent No.
US 9,093,685
App. No.
12/321,466
Granted
Jul 28, 2015
Kind
B2
Abstract

Method of making a membrane electrode assembly comprising: providing a membrane comprising a perfluorinated sulfonic acid; providing a first transfer substrate; applying to a surface of the first transfer substrate a first ink, said first ink comprising an ionomer and a catalyst; applying to the first ink a suitable non-aqueous swelling agent; forming an assembly comprising: the membrane; and the first transfer substrate, wherein the surface of the first transfer substrate comprising the first ink and the non-aqueous swelling agent is disposed upon one surface of the membrane; and heating the assembly at a temperature of 150° C. or less and at a pressure of from about 250 kPa to about 3000 kPa or less for a time suitable to allow substantially complete transfer of the first ink and the second ink to the membrane; and cooling the assembly to room temperature and removing the first transfer substrate and the second transfer substrate.

Claims (56)

1. A method of making a membrane electrode assembly, the method comprising steps of:

applying a first ink to a surface of a first transfer substrate, the first ink comprising a protonated ionomer and a catalyst;

drying the applied first ink by baking;

applying to the dried first ink a suitable non-aqueous swelling agent selected from the group consisting of n-propanol, 1,5-pentanediol, and dimethyl acetamide;

forming an assembly of the first transfer substrate and a membrane by contacting a first surface of the membrane with the first ink via the applied swelling agent, the membrane comprising a protonated perfluorinated sulfonic acid;

hot-pressing the assembly at a temperature in a range from about 30° C. to about 90° C. and at a pressure of from about 250 kPa to about 3000 kPa for a length of time resulting in substantially complete transfer the first ink to the membrane;

cooling the hot-pressed assembly to room temperature; and

removing the first transfer substrate.

2. The method of claim 1 , further comprising:

applying a second ink to a surface of a second transfer substrate, the second ink comprising a protonated ionomer and a catalyst;

drying the applied second ink by baking;

applying to the dried second ink a suitable non-aqueous swelling agent selected from the group consisting of n-propanol, 1,5-pentanediol, and dimethyl acetamide;

prior to said hot-pressing, forming the assembly to also comprise the second transfer substrate by contacting an opposing second surface of the membrane with the second ink via the applied non-aqueous swelling agent; and

after said hot-pressing, also removing the second transfer substrate after cooling the assembly to room temperature.

3. The method of claim 2 , further comprising applying a releasing agent to the first transfer substrate, the second transfer substrate, or both.

4. The method of claim 2 , wherein the non-aqueous swelling agent applied to each of the dried first and second inks is n-propanol and the hot-pressing temperature is 30° C.

5. The method of claim 2 , wherein the non-aqueous swelling agent applied to each of the dried first and second inks is dimethyl acetamide and the hot-pressing temperature is 70° C.

6. The method of claim 2 , wherein the non-aqueous swelling agent applied to each of the dried first and second inks is 1,5-pentanediol and the hot-pressing temperature is 90° C.

7. The method of claim 2 , wherein one of the first and second inks is a cathode ink and the other of the first and second inks is an anode ink.

8. The method of claim 1 , wherein the non-aqueous swelling agent is n-propanol and the hot-pressing temperature is about 30° C.

9. The method of claim 1 , wherein the non-aqueous swelling agent is 1,5-pentanediol and the hot-pressing temperature is about 90° C.

10. The method of claim 1 , wherein the non-aqueous swelling agent is dimethyl acetamide and the hot-pressing temperature is 70° C.

11. The method of claim 1 , wherein the hot-pressing time is about 6 minutes.

12. The method of claim 1 , wherein the hot-pressing pressure is about 500 kPa to about 3000 kPa.

13. A method of making a membrane electrode assembly, the method comprising steps of:

applying a first ink to a surface of a first transfer substrate, the first ink comprising an ionomer salt and a catalyst;

drying the applied first ink by baking;

applying to the dried first ink a suitable non-aqueous swelling agent selected from the group consisting of n-propanol, 1,5-pentanediol, acetone, dimethyl acetamide, and N-methyl pyrrolidone;

forming an assembly of the first transfer substrate and a membrane by contacting a first surface of the membrane with the first ink via the applied non-aqueous swelling agent, the membrane comprising a salt of perfluorinated sulfonic acid;

hot-pressing the assembly at a temperature in a range from about 30° C. to about 125° C. and at a pressure of from about 250 kPa to about 3000 kPa for a length of time resulting in substantially complete transfer the first ink to the membrane;

cooling the hot-pressed assembly to room temperature; and

removing the first transfer substrate.

14. The method of claim 13 , further comprising:

applying a second ink to a surface of a second transfer substrate, the second ink comprising an ionomer salt and a catalyst;

drying the applied second ink by baking;

applying to the dried second ink a suitable non-aqueous swelling agent selected from the group consisting of n-propanol, 1,5-pentanediol, acetone, dimethyl acetamide, and N-methyl pyrrolidone;

prior to said hot-pressing, forming the assembly to also comprise the second transfer substrate by contacting an opposing second surface of the membrane with the second ink via the applied swelling agent; and

after said hot-pressing, also removing the second transfer substrate after cooling the assembly to room temperature.

15. The method of claim 14 , wherein the non-aqueous swelling agent applied to each of the dried first and second inks is n-propanol and the temperature is 40° C.

16. The method of claim 14 , wherein the non-aqueous swelling agent applied to each of the dried first and second inks is 1,5-pentanediol and the hot-pressing temperature is 100° C.

17. The method of claim 14 , wherein the non-aqueous swelling agent applied to each of the dried first and second inks is acetone and the hot-pressing temperature is 30° C.

18. The method of claim 14 , wherein the non-aqueous swelling agent applied to each of the dried first and second inks is dimethyl acetamide and the hot-pressing temperature is 30° C.

19. The method of claim 14 , wherein the non-aqueous swelling agent applied to each of the dried first and second inks is N-methyl pyrrolidone and the hot-pressing temperature is 125° C.

20. The method of claim 14 , wherein one of the first and second inks is a cathode ink and the other of the first and second inks is an anode ink.

21. The method of claim 14 , further comprising applying a releasing agent to the first transfer substrate, the second transfer substrate, or both.

22. The method of claim 13 , wherein the non-aqueous swelling agent is acetone and the hot-pressing temperature is from about 30° C. to about 50° C.

23. The method of claim 13 , wherein the salt of the perfluorinated sulfonic is a sodium salt, a potassium salt, or combinations thereof.

24. The method of claim 13 , wherein the non-aqueous swelling agent is n-propanol and the hot-pressing temperature is from about 30° C. to about 50° C.

25. The method of claim 13 , wherein the non-aqueous swelling agent is n-propanol and the hot-pressing temperature is about 40° C.

26. The method of claim 13 , wherein the non-aqueous swelling agent is 1,5-pentanediol and the hot-pressing temperature is from about 80° C. to about 120° C.

27. The method of claim 13 , wherein the non-aqueous swelling agent is 1,5-pentanediol and the hot-pressing temperature is 100° C.

28. The method of claim 13 , wherein the non-aqueous swelling agent is acetone and the hot-pressing temperature is 30° C.

29. The method of claim 13 , wherein the non-aqueous swelling agent is dimethyl acetamide and the hot-pressing temperature is 30° C.

30. The method of claim 13 , wherein the non-aqueous swelling agent is N-methyl pyrrolidone and the hot-pressing temperature is 125° C.

31. The method of claim 13 , wherein the hot-pressing time is in a range from about 6-10 minutes.

32. The method of claim 13 , wherein the hot-pressing pressure is about 1000 kPa.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 7, 2018
From: LOS ALAMOS NATIONAL SECURITY, LLC
To: TRIAD NATIONAL SECURITY, LLC
Reel/Frame 047447/0001 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 12, 2009
From: KIM, YU SEUNG; LEE, KWAN-SOO; ROCKWARD, TOMMY Q.T.
To: LOS ALAMOS NATIONAL SECURITY, LLC
Reel/Frame 022691/0201 →
CONFIRMATORY LICENSE Recorded Mar 19, 2009
From: LOS ALAMOS NATIONAL SECURITY
To: ENERGY, U.S. DEPARTMENT OF
Reel/Frame 022421/0905 →