# US 10,370,306 B2 · Polymer composite having dispersed transition metal oxide particles > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,370,306 B2 - Document ID: US10370306B2 - Status: Granted - Kind: B2 - Application number: 13/797,448 - Filed: 2013-03-12 - Published: 2015-12-10 - Granted: 2019-08-06 - Earliest claimed: 2012-03-12 - Assignees: University of Central Florida Research Foundation, Inc.; The Texas A&M University System - Applicants: University of Central Florida Research Foundation, Inc. - Inventors: David L. Reid; Sudipta Seal; Eric Petersen; Robert Draper - Web page: https://patentgrep.com/patent/US10370306B2 ## CPC - C06B 45/105: {The resin being a polymer bearing energetic groups or containing a soluble organic explosive} - C06B 23/007: {Ballistic modifiers, burning rate catalysts, burning rate depressing agents, e.g. for gas generating} - C06B 45/10: the organic component containing a resin - C08F 136/06: Butadiene - C08J 3/205: in the presence of a {continuous} liquid phase - C06B: EXPLOSIVES OR THERMIC COMPOSITIONS (blasting F42D); MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES (compounds in general C01, C07 or C08; {demolition agents based on cementitious or like materials C04B41/0009}) - C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS - C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29) ## 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 ### Claim 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. ### Claim 2 (depends on 1) The composition of matter of claim 1, wherein said polymer provides OH functionality. ### Claim 3 (depends on 1) The composition of matter of claim 1, wherein said crystalline transition metal oxide nanoparticles comprise titania. ### Claim 4 (depends on 1) The composition of matter of claim 1, wherein said polymer comprises hydroxyl-terminated polybutadiene (HTPB) or polybutadiene acrylonitrile (PBAN). ### Claim 5 (depends on 1) The composition of matter of claim 1, further comprising an oxidizer in said continuous phase. ### Claim 6 (depends on 1) 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. ### Claim 7 (depends on 1) 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. ### Claim 8 (depends on 7) The method of claim 7, wherein said polymer provides OH functionality or COOH functionality. ### Claim 9 (depends on 7) The method of claim 7, wherein said transition metal comprises titanium. ### Claim 10 (depends on 7) 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. ### Claim 11 (depends on 7) The method of claim 7, wherein said hydrolyzing is performed at a temperature below 100° C. ### Claim 12 (depends on 7) 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. ### Claim 13 (depends on 7) 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. ### Claim 14 (depends on 13) 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. ### Claim 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. ### Claim 16 (depends on 15) The composition of matter of claim 15, wherein said polymer provides OH functionality. ### Claim 17 (depends on 15) The composition of matter of claim 15, wherein said crystalline transition metal oxide nanoparticles comprise titania. ### Claim 18 (depends on 15) The composition of matter of claim 15, further comprising fuel particles in said continuous phase. ### Claim 19 (depends on 15) The composition of matter of claim 15, further comprising an oxidizer in said continuous phase. ### Claim 20 (depends on 15) 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.