IP Library Granted Patent US 10,379,439
Granted Patent B2
US 10,379,439 · App. 15/400,790 · Granted Aug 13, 2019

Architected three dimensional graphene via additive manufacturing

Inventors: Marcus A. Worsley (Hayward, CA); Patrick G. Campbell (Oakland, CA); Eric B. Duoss (Dublin, CA); James S. Oakdale (Castro Valley, CA); Christopher M. Spadaccini (Oakland, CA); Ryan Hensleigh (Colstrip, MT)
Assignee: Lawrence Livermore National Security, LLC
G03F7/0037B01J13/0091B01J13/0095B29C35/0805B29C64/129B33Y10/00C01B32/382G03F7/0047B29C2035/0827
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 10,379,439
App. No.
15/400,790
Granted
Aug 13, 2019
Kind
B2
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.

Claims (18)

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.

Assignments (2)
CONFIRMATORY LICENSE Recorded Feb 7, 2017
From: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 041190/0928 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 9, 2017
From: WORSLEY, MARCUS A.; CAMPBELL, PATRICK G.; DUOSS, ERIC B.; OAKDALE, JAMES S.; SPADACCINI, CHRISTOPHER M.; HENSLEIGH, RYAN
To: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
Reel/Frame 040901/0663 →
Continuity (1)
Related Publication 20180196345A1 · Jul 12, 2018