High optical transparency polymer aerogels using low refractive index monomers

Patent metadata

Field	Value
Publication number	US-11851543-B2
Application number	US-202117245418-A
Country	US
Kind code	B2
Filing date	Apr 30, 2021
Priority date	Dec 20, 2018
Publication date	Dec 26, 2023
Grant date	Dec 26, 2023

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.

First claim

What is claimed is:

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.

Assignees

• Palo Alto Res Ct Inc
• Xerox Corp

Inventors

• Bulger Eli
• Chintapalli Mahati
• Iftime Gabriel
• Van Overmeere Quentin
• Rivest Jessica Louis Baker
• Neelakantan Ravi
• Meckler Stephen

Classifications

• C08J9/0004 Primary

  Use of compounding ingredients, the chemical constitution of which is unknown, broadly defined, or irrelevant · CPC title

• C08J3/242

  Applying crosslinking or accelerating agent onto compounding ingredients such as fillers, reinforcements · CPC title

• C08J9/286

  the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers · CPC title

• C08J2205/026

  Aerogel, i.e. a supercritically dried gel · CPC title

• C08J2205/044

  Micropores, i.e. average diameter being between 0,1 micrometer and 0,1 millimeter · CPC title