IP Library Granted Patent US 10,370,306
Granted Patent B2
US 10,370,306 · App. 13/797,448 · Granted Aug 6, 2019

Polymer composite having dispersed transition metal oxide particles

Inventors: David L. Reid (Orlando, FL); Sudipta Seal (Orlando, FL); Eric Petersen (College Station, TX); Robert Draper (Orlando, FL)
Assignees: University of Central Florida Research Foundation, Inc.; Texas A&M University System
C06B45/105C06B23/007C06B45/10C08F136/06C08J3/205
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Quick Facts
Patent No.
US 10,370,306
App. No.
13/797,448
Granted
Aug 6, 2019
Kind
B2
Abstract

A method of forming polymer composites having transition metal oxide nanoparticles dispersed therein includes mixing a transition metal oxide precursor including at least one transition metal, a polymer as a binder, a solvent for the polymer, and water to form a first solution including polymer-transition metal complexes. The polymer-transition metal complexes are hydrolyzed to produce a plurality of transition metal oxide nanoparticles, wherein water is added in the mixing in a stoichiometric excess for the hydrolyzing. The solvent and residual of the water remaining after the hydrolyzing are removed. A polymer composite including a plurality of transition metal oxide nanoparticles dispersed in the polymer results after the removing, where some of the polymer is chemically conjugated to a surface of the transition metal oxide nanoparticles.

Claims (32)

1. A composition of matter, comprising:

a polymer providing a liquid or a solid continuous phase with fuel particles in said continuous phase, and

a plurality of crystalline transition metal oxide nanoparticles dispersed in said polymer, wherein some of said polymer is chemically conjugated to a surface of said plurality of crystalline transition metal oxide nanoparticles;

wherein said crystalline transition metal oxide nanoparticles are unagglomerated, and wherein said crystalline transition metal oxide nanoparticles are homogeneously dispersed in said polymer.

2. The composition of matter of claim 1 , wherein said polymer provides OH functionality.

3. The composition of matter of claim 1 , wherein said crystalline transition metal oxide nanoparticles comprise titania.

4. The composition of matter of claim 1 , wherein said polymer comprises hydroxyl-terminated polybutadiene (HTPB) or polybutadiene acrylonitrile (PBAN).

5. The composition of matter of claim 1 , further comprising an oxidizer in said continuous phase.

6. The composition of matter of claim 1 , wherein said transition metal oxide nanoparticles have a size range of 1 nm to 3 nm in diameter.

7. A method of forming polymer composites comprising a composition of matter of claim 1 , the method comprising:

mixing a transition metal oxide precursor including at least one transition metal, a polymer as a binder, a solvent for said polymer, and water to form a first solution including polymer-transition metal complexes;

hydrolyzing said polymer-transition metal complexes to produce a plurality of transition metal oxide nanoparticles, wherein said water is added in said mixing in a stoichiometric excess for said hydrolyzing, and

removing said solvent and water remaining after hydrolyzing, resulting in a polymer composite having a plurality of crystalline transition metal oxide nanoparticles dispersed in said polymer, and wherein some of said polymer is chemically conjugated to a surface of said crystalline transition metal oxide nanoparticles wherein said crystalline transition metal oxide nanoparticles are unagglomerated and are homogeneously dispersed in said polymer.

8. The method of claim 7 , wherein said polymer provides OH functionality or COOH functionality.

9. The method of claim 7 , wherein said transition metal comprises titanium.

10. The method of claim 7 , combining said transition metal oxide precursor with a chelating agent, before said mixing and wherein said mixing comprises adding said transition metal oxide precursor combined with said chelating agent to a solution of said polymer, said solvent, and said water to form said first solution.

11. The method of claim 7 , wherein said hydrolyzing is performed at a temperature below 100° C.

12. The method of claim 7 , wherein said solvent comprises a non-polar solvent, further comprising adding a hydroxide comprising material to said first solution, and wherein said removing includes removal of said hydroxide comprising material.

13. The method of claim 7 , further comprising adding a surfactant to said first solution, wherein said first solution after said mixing provides a single phase inverse microemulsion.

14. The method of claim 13 , combining said transition metal oxide precursor with a chelating agent, before said mixing and wherein said mixing comprises adding said transition metal oxide precursor combined with said chelating agent to a solution of said polymer, said solvent, and said water to form said first solution including said single phase inverse microemulsion.

15. A composition of matter, comprising:

a polymer providing a liquid or a solid continuous phase, and

a plurality of crystalline transition metal oxide nanoparticles dispersed in said polymer, wherein said transition metal oxide nanoparticles have a size range of 1 nm to 3 nm in diameter, and wherein some of said polymer is chemically conjugated to a surface of said plurality of crystalline transition metal oxide nanoparticles;

wherein said crystalline transition metal oxide nanoparticles are unagglomerated, and wherein said crystalline transition metal oxide nanoparticles are homogeneously dispersed in said polymer.

16. The composition of matter of claim 15 , wherein said polymer provides OH functionality.

17. The composition of matter of claim 15 , wherein said crystalline transition metal oxide nanoparticles comprise titania.

18. The composition of matter of claim 15 , further comprising fuel particles in said continuous phase.

19. The composition of matter of claim 15 , further comprising an oxidizer in said continuous phase.

20. A method of forming polymer composites comprising the composition of matter of claim 15 , the method comprising:

mixing a transition metal oxide precursor including at least one transition metal, a polymer as a binder, a solvent for said polymer, and water to form a first solution including polymer-transition metal complexes;

hydrolyzing said polymer-transition metal complexes to produce a plurality of transition metal oxide nanoparticles, wherein said water is added in said mixing in a stoichiometric excess for said hydrolyzing, and

removing said solvent and water remaining after hydrolyzing, resulting in a polymer composite having a plurality of crystalline transition metal oxide nanoparticles dispersed in said polymer, and wherein some of said polymer is chemically conjugated to a surface of said crystalline transition metal oxide nanoparticles, wherein said crystalline transition metal oxide nanoparticles are unagglomerated and are homogeneously dispersed in said polymer.

Assignments (5)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 23, 2022
From: ALLEN, TYLER W.; KREITZ, KEVIN R.; JOHNSON, MITCHELL T.
To: THE TEXAS A&M UNIVERSITY SYSTEM
Reel/Frame 060291/0296 →
CONFIRMATORY LICENSE Recorded Jan 25, 2018
From: TEXAS A&M UNIVERSITY SYSTEM
To: NIH - DEITR
Reel/Frame 044724/0467 →
CONFIRMATORY LICENSE Recorded Dec 14, 2017
From: TEXAS ENGINEERING EXPERIMENT STATION
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 044872/0418 →
CORRECTIVE ASSIGNMENT TO CORRECT THE ASSIGNEE DATA PREVIOUSLY RECORDED AT REEL: 030572 FRAME: 0535. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT. Recorded Mar 25, 2016
From: UNIVERSITY OF CENTRAL FLORIDA RESEARCH FOUNDATION, INC.
To: THE TEXAS A&M UNIVERSITY SYSTEM
Reel/Frame 038260/0216 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 6, 2013
From: REID, DAVID L.; SEAL, SUDIPTA; PETERSEN, ERIC; DRAPER, ROBERT
To: UNIVERSITY OF CENTRAL FLORIDA RESEARCH FOUNDATION, INC.
Reel/Frame 030572/0535 →
Continuity (2)
Provisional Application 61609461 · Mar 12, 2012
Related Publication 20150353438A1 · Dec 10, 2015