IP Library Granted Patent US 7,695,974
Granted Patent B2
US 7,695,974 · App. 12/021,675 · Granted Apr 13, 2010

Method for imaging the ionomer spatial distribution in fuel cell electrodes

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Quick Facts
Patent No.
US 7,695,974
App. No.
12/021,675
Granted
Apr 13, 2010
Kind
B2
Abstract

A method for evaluating the spatial distribution of an ionomer in a fuel cell MEA. The method includes embedding the MEA in an epoxy, and then slicing thin sections from the MEA. The sliced sections are then exposed to a titanium tetrachloride vapor that stains the epoxy. The stained sections are then viewed with, for example, a transmission electron microscope (TEM) where the lighter regions in the TEM image show the ionomer distribution.

Claims (26)

1. A method for evaluating the spatial distribution of an ionomer in a membrane electrode assembly (MEA), wherein the MEA includes electrodes that have an ionomer, said method comprising:

embedding the MEA in a support material;

slicing thin sections of the MEA;

exposing the MEA sections to a staining material, wherein the staining material is titanium tetrachloride, that stains the support material in the MEA, but does not stain the ionomer, including the electrode ionomer; and

viewing the MEA sections to identify the non-stained ionomer regions in the MEA sections.

2. The method according to claim 1 wherein exposing the MEA sections to titanium chloride includes exposing the MEA sections to a titanium tetrachloride vapor for a predetermined period of time.

3. The method according to claim 2 wherein exposing the MEA sections to titanium chloride vapor includes exposing the MEA sections to the titanium tetrachloride vapor for a period of one to two minutes.

4. The method according to claim 1 wherein exposing the MEA sections to titanium tetrachioride includes staining the support material with titanium in the titanium tetrachioride and leaving the ionomer in the MEA unstained.

5. The method according to claim 1 wherein slicing thin sections of the MEA includes using a microtome machine to slice the MEA.

6. The method according to claim 5 further comprising allowing the MEA slices to float on water in the microtome machine for a predetermined period of time.

7. The method according to claim 1 wherein embedding the MEA in a support material includes embedding the MEA in an epoxy.

8. The method according to claim 7 wherein embedding the MEA in an epoxy includes dripping the epoxy on the MEA in a vacuum environment and then exposing the MEA to pressure so that the epoxy is forced into pores in the MEA.

9. The method according to claim 1 wherein viewing the MEA sections includes using a transmission electron microscope.

10. The method according to claim 1 further comprising partially drying the MEA slices before they are exposed to the staining material.

11. A method for evaluating the spatial distribution of an ionomer in a membrane electrode assembly (MEA), wherein the MEA includes electrodes that have an ionomer, said method comprising:

embedding the MEA in a support material;

slicing thin sections of the MEA;

exposing the sliced MEA sections to a titanium tetrachloride vapor for a predetermined period of time so that the epoxy is stained with titanium in the titanium tetrachloride and the ionomer in the MEA is unstained, including the electrode ionomer; and

viewing the MEA sections with a transmission electron microscope to identify the non-stained ionomer regions in the MEA sections.

12. The method according to claim 11 wherein exposing the MEA sections to titanium tetrachioride vapor includes exposing the MEA sections to the titanium tetrachloride vapor for a period of one to two minutes.

13. The method according to claim 11 wherein slicing thin sections of the MEA includes using a microtome machine to slice the MEA.

14. The method according to claim 13 further comprising allowing the MEA slices to float on water in the microtome machine for a predetermined period of time.

15. The method according to claim 14 further comprising partially dying the MEA slices before they are exposed to the titanium tetrachloride vapor.

16. A method for evaluating the spatial distribution of an ionomer in a membrane electrode assembly (MEA), wherein the MEA includes electrodes that have an ionomer, said method comprising:

exposing the MEA to a staining material, wherein the staining material is titanium tetrachloride, that stains all of the materials in the MEA except the ionomer, including the electrode ionomer; and

viewing the MEA to identify the non-stained ionomer regions in the MEA.

Assignments (12)
RELEASE OF SECURITY INTEREST Recorded Nov 7, 2014
From: WILMINGTON TRUST COMPANY
To: GM GLOBAL TECHNOLOGY OPERATIONS LLC
Reel/Frame 034185/0587 →
CHANGE OF NAME Recorded Feb 10, 2011
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: GM GLOBAL TECHNOLOGY OPERATIONS LLC
Reel/Frame 025781/0211 →
SECURITY AGREEMENT Recorded Nov 8, 2010
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: WILMINGTON TRUST COMPANY
Reel/Frame 025324/0475 →
RELEASE OF SECURITY INTEREST Recorded Nov 5, 2010
From: UAW RETIREE MEDICAL BENEFITS TRUST
To: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
Reel/Frame 025315/0001 →
RELEASE OF SECURITY INTEREST Recorded Nov 4, 2010
From: UNITED STATES DEPARTMENT OF THE TREASURY
To: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
Reel/Frame 025245/0780 →
SECURITY AGREEMENT Recorded Aug 28, 2009
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: UAW RETIREE MEDICAL BENEFITS TRUST
Reel/Frame 023162/0187 →
SECURITY AGREEMENT Recorded Aug 27, 2009
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: UNITED STATES DEPARTMENT OF THE TREASURY
Reel/Frame 023156/0215 →
RELEASE OF SECURITY INTEREST Recorded Aug 21, 2009
From: CITICORP USA, INC. AS AGENT FOR BANK PRIORITY SECURED PARTIES; CITICORP USA, INC. AS AGENT FOR HEDGE PRIORITY SECURED PARTIES
To: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
Reel/Frame 023155/0880 →
RELEASE OF SECURITY INTEREST Recorded Aug 20, 2009
From: UNITED STATES DEPARTMENT OF THE TREASURY
To: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
Reel/Frame 023124/0670 →
SECURITY AGREEMENT Recorded Apr 16, 2009
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: CITICORP USA, INC. AS AGENT FOR BANK PRIORITY SECURED PARTIES; CITICORP USA, INC. AS AGENT FOR HEDGE PRIORITY SECURED PARTIES
Reel/Frame 022554/0479 →
SECURITY AGREEMENT Recorded Feb 3, 2009
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: UNITED STATES DEPARTMENT OF THE TREASURY
Reel/Frame 022195/0334 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 29, 2008
From: BALOGH, MICHAEL P.; HAYES, FREDERICK A.
To: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
Reel/Frame 020433/0332 →