IP Library Granted Patent US 10,995,191
Granted Patent B2
US 10,995,191 · App. 16/228,472 · Granted May 4, 2021

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: PALO ALTO RESEARCH CENTER INCOPORATED
C08J9/0004C08J3/242C08J9/286C08J2205/026C08J2205/044C08K5/0025
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Quick Facts
Patent No.
US 10,995,191
App. No.
16/228,472
Granted
May 4, 2021
Kind
B2
Abstract

A polymer aerogel has polymerizable monomers and crosslinkers, wherein at least one of the monomers or at least one of the crosslinkers has a refractive index of less than 1.5, and the polymer aerogel has a visible transmittance of at least 20%/3 mm, a haze of 50%/3 mm or lower, and a porosity of at least 10%. A method of producing an 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 an aerogel polymer.

Claims (21)

1. A polymer aerogel comprising polymerized monomers and crosslinkers, wherein at least one of the monomers or at least one of the crosslinkers has a refractive index of less than 1.45, and the polymer aerogel has a visible transmittance of at least 20%/3 mm, a haze of 50%/3 mm or lower, and a porosity of at least 10%.

2. The polymer aerogel of claim 1 , wherein the at least one of the monomers or the at least one of the crosslinkers has a refractive index of less than 1.4.

3. The polymer aerogel of claim 1 , wherein the polymer aerogel has a porosity of at least 40%, haze of 30%/3 mm or lower, and a specific surface area of at least 500 m 2 /g.

4. The polymer aerogel of claim 1 , wherein the polymer aerogel has a haze below 6%/3 mm, a specific surface area above 300 m 2 /g, a porosity above 20%, average pore size below 10 nm, and pore size distribution with full width at half maximum below 10 nm.

5. The polymer aerogel of claim 1 , wherein the polymer aerogel has a degradation onset temperature above 250° C.

6. The polymer aerogel of claim 1 , wherein the polymer aerogel has thermal conductivity below 0.1 W/mK.

7. A polymer aerogel manufactured from the process of:

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 an aerogel polymer.

8. The polymer aerogel as claimed in claim 1 , wherein the at least one monomer or at least one crosslinker has a stiffness of at least 3.5 GPa for the Young's modulus when polymerized.

9. The polymer aerogel as claimed in 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.

10. The polymer aerogel as claimed in claim 1 , wherein the at least one of the monomers or the at least one of the crosslinkers having a refractive index of 1.45 or lower comprises at least one selected from the group consisting of: 1H, 1H, 6H, 6H-Per-fluoro-1,6-hexanediol diacrylate (F-HDDA), 2,3,4,5,6-pentafluorostyrene, 1H, 1H, 2H-Perfluoro-l-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.

11. The polymer aerogel as claimed in claim 8 , wherein the polymer aerogel comprises at least one monomer or at least one crosslinker with a refractive index of less than 1.45 comprising 30-99.9 vol % of the polymerizable monomers and crosslinkers.

12. The polymer aerogel of claim 1 , wherein the polymer aerogel has a porosity of at least 40%, haze of 15%/3 mm or lower, and a specific surface area of at least 600 m 2 /g.

13. The polymer aerogel of claim 1 , wherein the polymer aerogel comprises at least 20 wt % of fluorine.

14. The polymer aerogel of claim 1 , wherein the aerogel includes a control agent.

15. The polymer aerogel of claim 14 , 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.

16. The polymer aerogel of claim 14 , 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.

17. The polymer aerogel of claim 14 , wherein the control agent comprises at least one selected from the group consisting of: 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.

18. The polymer aerogel of claim 1 , wherein the polymer aerogel includes at least a portion of an initiator or at least a portion of a chain transfer agent.

Assignments (11)
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 →
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 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 →
CONFIRMATORY LICENSE Recorded Sep 27, 2021
From: PALO ALTO RESEARCH CENTER
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 057606/0570 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 20, 2018
From: BULGER, ELI; CHINTAPALLI, MAHATI; IFTIME, GABRIEL; VAN OVERMEERE, QUENTIN; RIVEST, JESSICA LOUIS BAKER; NEELAKANTAN, RAVI; MECKLER, STEPHEN
To: PALO ALTO RESEARCH CENTER INCORPORATED
Reel/Frame 047836/0710 →
Continuity (1)
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