IP Library Granted Patent US 11,585,771
Granted Patent B2
US 11,585,771 · App. 17/677,716 · Granted Feb 21, 2023

Metal nanoparticle-decorated nanotubes for gas sensing

Inventors: Gabriel Iftime (Dublin, CA); Clinton Smith (San Francisco, CA); David Eric Schwartz (San Carlos, CA); Yong Zhang (Millbrae, CA); Vedasri Vedharathinam (Sunnyvale, CA)
Assignee: Palo Alto Research Center Incorporated
G01N27/04B01J20/0225B01J20/205B01J20/3204B01J20/327G01N27/126G01N27/127G01N33/0009B22F1/102B22F2999/00B82Y15/00B82Y30/00B82Y40/00C22C2026/002
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 11,585,771
App. No.
17/677,716
Granted
Feb 21, 2023
Kind
B2
Abstract

Disclosed herein are methods of producing metal nanoparticle-decorated carbon nanotubes. The methods include forming a reaction mixture by combining a first solution with a second solution, wherein the first solution comprises polymer-coated metal nanoparticles comprising metallic nanoparticles coated with a polymer, and wherein the second solution comprises carbon nanotubes. The methods also include heating the reaction mixture to a temperature greater than a glass transition temperature of the polymer for a time sufficient to cause the polymer-coated metal nanoparticles to bind to the carbon nanotubes forming the metal nanoparticle-decorated carbon nanotubes.

Claims (28)

1. A method of producing metal nanoparticle-decorated carbon nanotubes, the method comprising:

forming a reaction mixture by combining a first solution with a second solution, wherein the first solution comprises polymer-coated metal nanoparticles comprising metallic nanoparticles coated with a polymer, and wherein the second solution comprises carbon nanotubes; and

heating the reaction mixture to a temperature greater than a glass transition temperature of the polymer for a time sufficient to cause the polymer-coated metal nanoparticles to bind to the carbon nanotubes forming the metal nanoparticle-decorated carbon nanotubes.

2. The method of claim 1 , wherein the polymer-coated metal nanoparticles are fully-formed prior to forming the reaction mixture.

3. The method of claim 2 , wherein the polymer-coated metal nanoparticles are non-covalently bound to the carbon nanotubes.

4. The method of claim 1 , wherein an average degree of functionalization of the carbon nanotubes with carboxylic acid groups and/or hydroxyl groups is less than 3 wt % based on a total weight of the carbon nanotubes.

5. The method of claim 1 , further comprising:

dispersing the metal nanoparticle-decorated carbon nanotubes in a non-aqueous solvent-based ink.

6. The method of claim 1 , wherein the polymer-coated-metal nanoparticles are coated with a hydrophobic polymer layer.

7. The method of claim 1 , wherein the carbon nanotubes are substantially free of carboxylic acid functional groups and hydroxyl functional groups.

8. A method of producing metal nanoparticle-decorated carbon nanotubes, the method comprising:

forming polymer-coated metal nanoparticles by dispersing a polymer and a salt precursor of a metal into a solvent, reducing the metal salt precursor of the metal with a reducing reagent;

forming a reaction mixture by combining a first solution with a second solution, wherein the first solution comprises polymer-coated metal nanoparticles comprising metallic nanoparticles coated with a polymer, and wherein the second solution comprises carbon nanotubes; and

heating the reaction mixture to a temperature greater than a glass transition temperature of the polymer for a time sufficient to cause the polymer-coated metal nanoparticles to bind to the carbon nanotubes forming the metal nanoparticle-decorated carbon nanotubes.

9. The method of claim 8 , wherein an average degree of functionalization of the carbon nanotubes with carboxylic acid groups and/or hydroxyl groups is less than 3 wt % based on a total weight of the carbon nanotubes.

10. The method of claim 8 , wherein the solvent is both a solvent and a reducing reagent.

11. The method of claim 9 , wherein the solvent and a reducing reagent is ethylene glycol.

12. The method of claim 8 , further involving heating of the solution of polymer and a salt precursor of a metal into the solvent.

13. The method of claim 8 , further involving removal of excess of un-bound polymer onto the polymer-coated nanoparticles by washing with a first solvent, separation and redispersion of the polymer-coated nanoparticles into a second solvent to form a polymer-coated nanoparticle dispersion that is free of unbound polymer, (i.e., does not contain unbound polymer).

14. The method of claim 8 , wherein the carbon nanotubes are selected from a group of single wall and multi-wall carbon nanotubes.

15. The method of claim 8 , wherein the diameter of the metallic core of the polymer coated metal nanoparticles decorated carbon nanotubes is comprised in a range from 1 nm to 20 nm.

16. The method of claim 8 , wherein the diameter of the metallic core of the polymer coated metal nanoparticles decorated carbon nanotubes is comprised in a range from 1 nm to 20 nm and the carbon nanotubes are single wall carbon nanotubes.

17. A method of producing metal alloy nanoparticle-decorated carbon nanotubes, the method comprising:

forming polymer-coated metal nanoparticles by dispersing a polymer and a mixture of two or more salt precursors of metals into a solvent, reducing the mixture of metal salt precursors with a reducing reagent forming polymer coated alloy metal nanoparticles containing two or more metals;

forming a reaction mixture by combining a first solution with a second solution, wherein the first solution comprises polymer-coated metal nanoparticles comprising metallic nanoparticles coated with a polymer, and wherein the second solution comprises carbon nanotubes; and

heating the reaction mixture to a temperature greater than a glass transition temperature of the polymer for a time sufficient to cause the polymer-coated metal nanoparticles to bind to the carbon nanotubes forming the metal nanoparticle-decorated carbon nanotubes.

18. The method of claim 17 , wherein the salt precursors of the polymer-coated metal alloy nanoparticles is selected from a group of metal ions that after reduction process form metals selected from a group of palladium, iridium, rhodium, platinum, and gold.

19. The method of claim 17 , wherein an average degree of functionalization of the carbon nanotubes with carboxylic acid groups and/or hydroxyl groups is less than 3 wt % based on a total weight of the carbon nanotubes.

Assignments (9)
SECOND LIEN NOTES PATENT SECURITY AGREEMENT Recorded Jul 2, 2025
From: XEROX CORPORATION
To: U.S. BANK TRUST COMPANY, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
Reel/Frame 071785/0550 →
FIRST LIEN NOTES PATENT SECURITY AGREEMENT Recorded Apr 11, 2025
From: XEROX CORPORATION
To: U.S. BANK TRUST COMPANY, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
Reel/Frame 070824/0001 →
TERMINATION AND RELEASE OF SECURITY INTEREST IN PATENTS RECORDED AT RF 064760/0389 Recorded Feb 13, 2024
From: CITIBANK, N.A., AS COLLATERAL AGENT
To: XEROX CORPORATION
Reel/Frame 068261/0001 →
SECURITY INTEREST Recorded Feb 13, 2024
From: XEROX CORPORATION
To: CITIBANK, N.A., AS COLLATERAL AGENT
Reel/Frame 066741/0001 →
SECURITY INTEREST Recorded Nov 20, 2023
From: XEROX CORPORATION
To: JEFFERIES FINANCE LLC, AS COLLATERAL AGENT
Reel/Frame 065628/0019 →
CORRECTIVE ASSIGNMENT TO CORRECT THE REMOVAL OF US PATENTS 9356603, 10026651, 10626048 AND INCLUSION OF US PATENT 7167871 PREVIOUSLY RECORDED ON REEL 064038 FRAME 0001. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT. Recorded Jun 28, 2023
From: PALO ALTO RESEARCH CENTER INCORPORATED
To: XEROX CORPORATION
Reel/Frame 064161/0001 →
SECURITY INTEREST Recorded Jun 22, 2023
From: XEROX CORPORATION
To: CITIBANK, N.A., AS COLLATERAL AGENT
Reel/Frame 064760/0389 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 20, 2023
From: PALO ALTO RESEARCH CENTER INCORPORATED
To: XEROX CORPORATION
Reel/Frame 064038/0001 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 9, 2023
From: IFTIME, GABRIEL; SMITH, CLINTON; SCHWARTZ, DAVID ERIC; ZHANG, YONG; VEDHARATHINAM, VEDASRI
To: PALO ALTO RESEARCH CENTER INCORPORATED
Reel/Frame 062313/0412 →
Continuity (3)
Division 16996239 · Aug 18, 2020
Division 15582172 · Apr 28, 2017
Related Publication 20220178859A1 · Jun 9, 2022