IP Library Granted Patent US 11,851,543
Granted Patent B2
US 11,851,543 · App. 17/245,418 · Granted Dec 26, 2023

High optical transparency polymer aerogels using low refractive index monomers

Inventors: Eli Bulger (Nottawa, CA); Mahati Chintapalli (Mountain View, CA); Gabriel Iftime (Dublin, CA); Quentin Van Overmeere (Mountain View, CA); Jessica Louis Baker Rivest (Palo Alto, CA); Ravi Neelakantan (Redwood City, CA); Stephen Meckler (Redwood City, CA)
Assignee: XEROX CORPORATION
C08J9/0004C08J3/242C08J9/286C08J2205/026C08J2205/044C08K5/0025
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Quick Facts
Patent No.
US 11,851,543
App. No.
17/245,418
Granted
Dec 26, 2023
Kind
B2
Abstract

A method of producing a polymer aerogel includes dissolving precursors into a solvent, wherein the precursors include monomers, crosslinkers, a controlling agent and an initiator to form a precursor solution, wherein at least one of the monomers or at least one of the crosslinkers has a refractive index of 1.5 or lower, polymerizing the precursor solution to form a gel polymer, and removing the solvent from the gel polymer to produce the polymer aerogel. A method of producing a polymer aerogel include dissolving precursors into a solvent, wherein the precursors include monomers, crosslinkers, a controlling agent and an initiator to form a precursor solution, polymerizing the precursor solution to form a gel polymer, removing the solvent from the gel polymer to produce the polymer aerogel, and reducing a refractive index of one of either the gel polymer or the polymer aerogel.

Claims (24)

1. A method of producing a polymer aerogel, comprising:

dissolving precursors into a solvent, wherein the precursors include monomers, crosslinkers, a controlling agent and an initiator to form a precursor solution, wherein at least one of the monomers or at least one of the crosslinkers has a refractive index of 1.4 or lower;

polymerizing the precursor solution to form a gel polymer; and

removing the solvent from the gel polymer to produce the polymer aerogel.

2. The method of claim 1 , wherein the precursors include at least one monomer or at least one crosslinker that has an elastic modulus of at least 3.5 GPa.

3. The method of claim 1 , wherein the at least one monomer or the at least one crosslinker comprises one selected from the group consisting of: divinylbenzene; hexanediol diacrylate; hexanediol dimethacrylate, trimethacrylate adamantane, and dipentaerythritol pentacrylate.

4. The method of claim 1 , wherein the at least one of the monomers or the at least one of the crosslinkers having a refractive index of 1.5 or lower comprises at least one selected from the group consisting of: 1H, 1H, 6H, 6H-Perfluoro-1,6-hexanediol diacrylate (FHDDA), 2, 3, 4, 5,6-pentafluorostyrene, 1H, 1H, 2H-Perfluoro-1-hexene, ethylene glycol diacrylate, 1,1,1,3,3,3-Hexafluoroisopropyl methacrylate, 2,2,2-Trifluoroethyl methacrylate, 1,1,1,3,3,3-Hexafluoroisopropyl acrylate, 2,2,2-Trifluoroethyl acrylate, methacrylate-functionalized perfluoropolyethers, and acrylate-functionalized perfluoropolyethers.

5. The method of claim 1 , wherein the initiator comprises at least one selected from the group consisting of: a thermal initiator, AIBN, lauroyl peroxide, benzoyl peroxide, tert-butyl peroxide, dicumyl peroxide, a photoinitiator, benzophenone, anthraquinone, camphorquinone, and benzoin.

6. The method of claim 1 , wherein the control agent comprises at least one selected from the group consisting of: a chain transfer agent, an organic thiol chain transfer agent, dodecanethiol, chloroform, octyl mercaptan, and 1,8-dimercapto-3,6-dioxaoctane.

7. The method of claim 1 , wherein the control agent comprises at least one selected from the group consisting of: reagents to enable stable free radical polymerization, a stable nitroxide, an alkoxyamine, 2,2,6,6-Tetramethyl-1-piperidinyloxy (TEMPO), and 4-hydroxy-TEMPO, a reagent capable of mediating a RAFT polymerization, a trithiocarbonate chain transfer agent, a xanthate chain transfer agent, a benzodithioate chain transfer agent, and a ligand-coordinated transition metal ion capable of mediating an ATRP polymerization.

8. The method of claim 1 , wherein the polymerizable precursors comprise 0.1-70 vol % of the precursor solution.

9. The method of claim 1 , wherein the initiator comprises 0.001-10 wt % of the precursor solution.

10. The method of claim 1 , wherein the control agent comprises 0.0001-10 wt % of the precursor solution.

11. The method of claim 1 , wherein the at least one low refractive index monomer or the at least one crosslinkers comprise 0.1-70 vol % of the polymerizable precursors.

12. The method of claim 1 , wherein monomers having an elastic modulus of at least 3.5 GPa and crosslinkers comprise 30-99.9 vol % of the polymerizable precursors.

13. The method of claim 1 , wherein polymerizing comprises one of either heating the precursor solution to a temperature between 50 and 150° C. for a period of time of at least 1 min, or exposure to electromagnetic radiation.

14. The method of claim 1 , further comprising drying the gel polymer by one of ambient drying, freeze drying, or supercritical CO2 drying.

15. A method of producing a polymer aerogel, comprising:

dissolving precursors into a solvent, wherein the precursors include monomers, crosslinkers, a controlling agent and an initiator to form a precursor solution, and the precursors include at least one monomer or at least one crosslinker that has an elastic modulus of at least 3.5 GPa;

polymerizing the precursor solution to form a gel polymer;

removing the solvent from the gel polymer to produce the polymer aerogel; and

reducing a refractive index of one of either the gel polymer or the polymer aerogel.

16. The method as claimed in claim 15 , wherein reducing a refractive index of the polymer aerogel occurs after one of either removing the solvent or drying the polymer aerogel.

17. The method as claimed in claim 15 , wherein reducing the refractive index comprises modifying the polymer gel or the polymer aerogel with one of fluorine, fluorine-containing chemical groups, or siloxane-containing chemical groups.

Assignments (8)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 14, 2025
From: XEROX CORPORATION
To: GENESEE VALLEY INNOVATIONS, LLC
Reel/Frame 073562/0677 →
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 →
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 →
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 Apr 30, 2021
From: BULGER, ELI; CHINTAPALLI, MAHATI; IFTIME, GABRIEL; OVERMEERE, QUENTIN VAN; BAKER RIVEST, JESSICA LOUIS; NEELAKANTAN, RAVI; MECKLER, STEPHEN
To: PALO ALTO RESEARCH CENTER INCORPORATED
Reel/Frame 056095/0471 →
Continuity (2)
Division 16228472 · Dec 20, 2018
Related Publication 20210309822A1 · Oct 7, 2021