IP Library Granted Patent US 9,991,521
Granted Patent B2
US 9,991,521 · App. 14/396,001 · Granted Jun 5, 2018

Method for dispersing particles in perfluorinated polymer ionomer

View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 9,991,521
App. No.
14/396,001
Granted
Jun 5, 2018
Kind
B2
Abstract

A method for preparing dispersing particles in perfluorinated polymer ionomer includes combining particles and a perfluorinated ionomer precursor in a mixture, and converting the perfluorinated ionomer precursor to a perfluorinated proton-conducting ionomer in the presence of the particles.

Claims (27)

1. A method for dispersing particles in perfluorinated polymer ionomer, the method comprising:

combining the particles and a perfluorinated ionomer precursor having an equivalent weight less than 700 g/mol in a mixture;

dispersing the particles and coating the particles with a uniform, nano-thick coat of the perfluorinated ionomer precursor; and

treating the perfluorinated ionomer precursor with a cross-linking agent in a basic solution comprising at least one tertiary amine base, thereby converting the perfluorinated ionomer precursor to a cross-linked perfluorinated proton-conducting ionomer in the presence of the particles, the cross-linked perfluorinated proton-conducting ionomer having an equivalent weight ranging from 280 q/mol to 700 g/mol and being insoluble in water;

wherein the perfluorinated ionomer precursor comprises perfluorinated carbon-carbon linear backbone chains and perfluorinated pendent side chains extending off of the perfluorinated carbon-carbon linear backbone chains, and the perfluorinated pendent side chains terminate with a —SO 2 X group, where each X is independently selected from the group consisting of fluorine (F), chlorine (Cl) and amine (NH 2 ),

wherein the cross-linking agent has the formula H 2 NSO 2 —Rf—SO 2 NH 2 , wherein, Rf is branched or unbranched perfluoroalkyl or perfluoropolyether group comprising 1-10 carbon atoms and 0-4 oxygen atoms.

2. The method as recited in claim 1 , wherein the perfluorinated ionomer precursor has a dry weight of 5%-100%, by weight, of the particles.

3. The method as recited in claim 1 , wherein the perfluorinated ionomer precursor has a dry weight of 30%-70%, by weight, of the particles.

4. The method as recited in claim 1 , wherein the perfluorinated proton-conducting ionomer surrounds the particles.

5. The method as recited in claim 1 , wherein the combining of the particles and the perfluorinated ionomer precursor includes dissolving the perfluorinated ionomer precursor in at least one solvent.

6. The method as recited in claim 5 , wherein the coating further comprises removing at least one solvent.

7. The method as recited in claim 6 , including applying the particles that are coated with the cross-linked perfluorinated proton-conducting ionomer onto a substrate.

8. The method as recited in claim 7 , wherein the cross-linking includes forming at least one sulfonimide group, —SO 2 —NH—SO 2 —, to covalently link two perfluorinated pendent side chains of the perfluorinated ionomer precursor that is coated on the particles.

9. The method as recited in claim 6 , including applying the particles that are coated with the perfluorinated ionomer precursor onto a substrate and then treating the perfluorinated ionomer precursor to form the cross-linked perfluorinated proton-conducting ionomer.

10. The method as recited in claim 1 , wherein the combining of the particles and the perfluorinated ionomer precursor includes providing at least one monomer of the perfluorinated ionomer precursor and mixing the at least one monomer with the particles.

11. The method as recited in claim 10 , including polymerizing the at least one monomer to produce the perfluorinated ionomer precursor in the presence of the particles.

12. The method as recited in claim 11 , including treating the perfluorinated ionomer precursor on the particles to form the cross-linked perfluorinated proton-conducting ionomer.

13. The method as recited in claim 1 , wherein the particles include nano-particles, and the nano-particles include at least one noble metal.

14. The method as recited in claim 13 , wherein the nano-particles are further disposed on a support selected from the group consisting of porous carbon, metal oxide and combinations thereof.

15. A method for dispersing particles in perfluorinated polymer ionomer, the method comprising:

(a) combining noble metal catalyst particles and a perfluorinated ionomer precursor having an equivalent weight less than 700 g/mol in a mixture to coat the noble metal catalyst particles with the perfluorinated ionomer precursor;

(b) applying the noble metal catalyst particles that are coated with the perfluorinated ionomer precursor from step (a) onto a polymeric substrate; and

(c) after step (b), treating the perfluorinated ionomer precursor with a cross-linking agent in basic solution comprising at least one tertiary amine base, thereby converting the perfluorinated ionomer precursor to a cross-linked perfluorinated proton-conducting ionomer having an equivalent weight ranging from 280 g/mol to 700 g/mol and being insoluble in water;

wherein the perfluorinated ionomer precursor comprises perfluorinated carbon-carbon linear backbone chains and perfluorinated pendent side chains extending off of the perfluorinated carbon-carbon linear backbone chains, and the perfluorinated pendent side chains terminate with a —SO 2 X group, where each X is independently selected from the group consisting of fluorine (F), chlorine (Cl) and amine (NH 2 ),

wherein the combining includes dispersing the particles and coating the particles with a uniform, nano-thick coat of the perfluorinated ionomer precursor

wherein the cross-linking agent has the formula H 2 NSO 2 —Rf—SO 2 NH 2 , wherein, Rf is branched or unbranched perfluoroalkyl or perfluoropolyether group comprising 1-10 carbon atoms and 0-4 oxygen atoms.

16. The method as recited in claim 15 , wherein the polymeric substrate is perfluorinated sulfonic acid.

Assignments (5)
CORRECTIVE ASSIGNMENT TO CORRECT THE ASSIGNEE ADDRESS PREVIOUSLY RECORDED AT REEL: 035728 FRAME: 0905. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT. Recorded Aug 24, 2015
From: BALLARD POWER SYSTEMS INC.
To: AUDI AG
Reel/Frame 036481/0803 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 19, 2015
From: BALLARD POWER SYSTEMS INC.
To: AUDI AG
Reel/Frame 035728/0905 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 17, 2014
From: UNITED TECHNOLOGIES CORPORATION
To: BALLARD POWER SYSTEMS INC.
Reel/Frame 034190/0298 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 13, 2014
From: UTC POWER CORPORATION
To: UNITED TECHNOLOGIES CORPORATION
Reel/Frame 034164/0189 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 11, 2014
From: YANG, ZHIWEI; GUMMALLA, MALLIKA
To: UTC POWER CORPORATION
Reel/Frame 034149/0475 →