Architected three dimensional graphene via additive manufacturing

Patent metadata

Field	Value
Publication number	US-10379439-B2
Application number	US-201715400790-A
Country	US
Kind code	B2
Filing date	Jan 6, 2017
Priority date	Jan 6, 2017
Publication date	Aug 13, 2019
Grant date	Aug 13, 2019

Abstract

Disclosed here is a method for making an architected three-dimensional aerogel, comprising providing a photoresin comprising a solvent, a photoinitiator, a crosslinkable polymer precursor, and a precursor for graphene, metal oxide or metal chalcogenide; curing the photoresin using projection microstereolithography layer-by-layer to produce a wet gel having a pre-designed three dimensional structure; drying the wet gel to produce a dry gel; and pyrolyzing the dry gel to produce an architected three-dimensional aerogel. Also disclosure is a photoresin for projection microstereolithography, comprising a solvent, a photoinitiator, a crosslinkable polymer precursor, and graphene oxide.

First claim

What is claimed is:

1. A method for making an architected three-dimensional aerogel, comprising:
providing a photoresin comprising a solvent, a photoinitiator, a crosslinkable polymer precursor, and a precursor for graphene, metal oxide or metal chalcogenide; wherein the crosslinkable polymer precursor comprises (a) polyethylene glycol diacrylate (PEGDA) and Bisphenol F ethoxylate (2 EO/phenol) diacrylate (BisF), or (b) PEGDA, resorcinol and formaldehyde;
curing the photoresin using projection microstereolithography layer-by-layer to produce a wet gel having a pre-designed three dimensional structure;
drying the wet gel to produce a dry gel; and
pyrolyzing the dry gel to produce an architected three-dimensional aerogel.

2. The method of claim 1 , wherein the solvent comprises an organic solvent.

3. The method of claim 1 , wherein the solvent comprises water.

4. The method of claim 1 , wherein the photoinitiator is soluble in an organic solvent.

5. The method of claim 1 , wherein the photoinitiator is soluble in water.

6. The method of claim 1 , wherein the photoinitiator comprises lithium phenyl(2,4,6-trimethylbenzoyl)phosphinate.

7. The method of claim 1 , wherein the crosslinkable polymer precursor comprise a non-aromatic prepolymer that is substantially removable by pyrolysis, and/or an aromatic prepolymer.

8. The method of claim 1 , wherein the crosslinkable polymer precursor comprises polyethylene glycol diacrylate (PEGDA) and Bisphenol F ethoxylate (2 EO/phenol) diacrylate (BisF).

9. The method of claim 1 , wherein the crosslinkable polymer precursor comprises PEGDA, resorcinol and formaldehyde.

10. The method of claim 1 , wherein the precursor for graphene, metal oxide or metal chalcogenide comprises graphene oxide.

11. The method of claim 1 , wherein the precursor for graphene, metal oxide or metal chalcogenide comprises a metal salt or metal alkoxide.

12. The method of claim 1 , wherein the curing step comprises curing the photoresin at a wavelength of 500 nm or less.

13. The method of claim 1 , wherein the drying step comprises drying by solvent exchange and/or supercritical drying.

14. The method of claim 1 , wherein the pyrolyzing step comprises pyrolyzing in an inert environment at a temperature of 800° C. or more.

Assignees

• L Livermore Nat Security Llc

Inventors

• Worsley Marcus A
• Campbell Patrick G
• Duoss Eric B
• Oakdale James S
• Spadaccini Christopher M
• HENSLEIGH Ryan

Classifications

• G03F7/0047

  characterised by additives for obtaining a metallic or ceramic pattern, e.g. by firing · CPC title

• G03F7/0037 Primary

  Production of three-dimensional images · CPC title

• B29C2035/0827

  using UV radiation · CPC title

• B01J13/0091

  Preparation of aerogels, e.g. xerogels · CPC title

• C01B32/382

  Making shaped products, e.g. fibres, spheres, membranes or foam · CPC title