IP Library Granted Patent US 9,840,414
Granted Patent B2
US 9,840,414 · App. 15/408,297 · Granted Dec 12, 2017

Crystalline boron nitride aerogels

Inventors: Alexander K. Zettl (Kensington, CA); Michael Rousseas (Burlingame, CA); Anna P. Goldstein (Berkeley, CA); William Mickelson (Albany, CA); Marcus A. Worsley (Hayward, CA); Leta Woo (Oakland, CA)
Assignees: Lawrence Livermore National Security, LLC; The Regents of the University of California
C01B21/0645C01B21/064
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Quick Facts
Patent No.
US 9,840,414
App. No.
15/408,297
Granted
Dec 12, 2017
Kind
B2
Abstract

This disclosure provides methods and materials related to boron nitride aerogels. For example, one aspect relates to a method for making an aerogel comprising boron nitride, comprising: (a) providing boron oxide and an aerogel comprising carbon; (b) heating the boron oxide to melt the boron oxide and heating the aerogel; (c) mixing a nitrogen-containing gas with boron oxide vapor from molten boron oxide; and (d) converting at least a portion of the carbon to boron nitride to obtain the aerogel comprising boron nitride. Another aspect relates to a method for making an aerogel comprising boron nitride, comprising heating boron oxide and an aerogel comprising carbon under flow of a nitrogen-containing gas, wherein boron oxide vapor and the nitrogen-containing gas convert at least a portion of the carbon to boron nitride to obtain the aerogel comprising boron nitride.

Claims (24)

1. A method for making an aerogel comprising boron nitride, comprising:

(a) providing boron oxide and an aerogel comprising carbon;

(b) heating the boron oxide to melt the boron oxide and heating the aerogel;

(c) mixing a nitrogen-containing gas with boron oxide vapor from molten boron oxide; and

(d) converting at least a portion of the carbon to boron nitride to obtain the aerogel comprising boron nitride.

2. The method of claim 1 , wherein the aerogel comprising carbon comprises sp 2 carbon.

3. The method of claim 1 , wherein the aerogel comprising carbon is a graphene aerogel.

4. The method of claim 1 , wherein the boron oxide is heated to a temperature of at least about 1500° C.

5. The method of claim 1 , wherein the boron oxide is heated to a temperature of about 1600° C. to about 1800° C.

6. The method of claim 1 , wherein flow rate of the nitrogen-containing gas is about 1000 sccm to about 2000 sccm.

7. The method of claim 1 , wherein the nitrogen-containing gas is N 2 .

8. The method of claim 1 , wherein the aerogel comprising carbon is substantially free of contact with liquid boron oxide.

9. The method of claim 1 , wherein at least about 95 atomic percent of the carbon is converted to boron nitride.

10. The method of claim 1 , wherein the aerogel comprising boron nitride obtained has an ordered crystalline structure comprising atomic layers of hexagonal boron nitride laying on top of one another, and wherein atoms contained in a first layer are superimposed on atoms contained in a second layer.

11. A method for making an aerogel comprising boron nitride, comprising heating boron oxide and an aerogel comprising carbon under flow of a nitrogen-containing gas, wherein boron oxide vapor and the nitrogen-containing gas convert at least a portion of the carbon to boron nitride to obtain the aerogel comprising boron nitride.

12. The method of claim 11 , wherein the aerogel comprising carbon comprises sp 2 carbon.

13. The method of claim 11 , wherein the aerogel comprising carbon is a graphene aerogel.

14. The method of claim 11 , wherein the boron oxide is heated to a temperature of at least about 1500° C.

15. The method of claim 11 , wherein the boron oxide is heated to a temperature of about 1600° C. to about 1800° C.

16. The method of claim 11 , wherein flow rate of the nitrogen-containing gas is about 1000 sccm to about 2000 sccm.

17. The method of claim 11 , wherein the nitrogen-containing gas is N 2 .

18. The method of claim 11 , wherein the aerogel comprising carbon is substantially free of contact with liquid boron oxide.

19. The method of claim 11 , wherein at least about 95 atomic percent of the carbon is converted to boron nitride.

20. The method of claim 11 , wherein the aerogel comprising boron nitride obtained has an ordered crystalline structure comprising atomic layers of hexagonal boron nitride laying on top of one another, and wherein atoms contained in a first layer are superimposed on atoms contained in a second layer.

Assignments (5)
CONFIRMATORY LICENSE Recorded May 14, 2018
From: UNIVERSITY OF CALIF-LAWRENC BERKELEY LAB
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 045795/0893 →
CONFIRMATORY LICENSE Recorded Mar 27, 2017
From: REGENTS OF THE UNIVERSITY OF CALIFORNIA, THE
To: ENERGY, UNITED STATES DEPARTMENT OF
Reel/Frame 042097/0612 →
CONFIRMATORY LICENSE Recorded Feb 7, 2017
From: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 041190/0423 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 31, 2017
From: ZETTL, ALEXANDER K.; ROUSSEAS, MICHAEL; GOLDSTEIN, ANNA P.; MICKELSON, WILLIAM
To: THE REGENTS OF THE UNIVERSITY OF CALIFORNIA
Reel/Frame 041132/0700 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 18, 2017
From: WORSLEY, MARCUS A.; WOO, LETA
To: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
Reel/Frame 041004/0463 →
Continuity (3)
Division 14320300 · Jun 30, 2014
Provisional Application 61841716 · Jul 1, 2013
Related Publication 20170297915A1 · Oct 19, 2017