Process and apparatus for purifying BNNT

Patent metadata

Field	Value
Publication number	US-12172889-B2
Application number	US-201917253749-A
Country	US
Kind code	B2
Filing date	Jul 11, 2019
Priority date	Jul 11, 2018
Publication date	Dec 24, 2024
Grant date	Dec 24, 2024

Abstract

Provided is a process and an apparatus for purifying boron nitride nanotube (BNNT) materials. The process involves the use of a halogen gas to remove halogen-reactive impurities from boron nitride nanotube (BNNT) materials in a single step with minimal interactions to produce structurally pristine BNNT. Gaseous byproducts are produced that 5 can be removed without the need for solution phase treatments. Yield efficiencies and purity of recovered BNNT are high compared to the other known methods of purification for BNNT material.

First claim

The invention claimed is:

1. A process for purifying boron nitride nanotubes, the process comprising:
contacting a solid boron nitride nanotube (BNNT) material containing boron nitride nanotubes and impurities with a halogen gas selected from the group consisting of chlorine, bromine and fluorine at a temperature in a range of 600° C. to 1250° C. when chlorine is the halogen, 700° C. to 1250° C. when bromine is the halogen gas, and 500° C. to 700° C. when fluorine is the halogen gas, the impurities reacting with the halogen gas to produce gaseous halogen-containing byproducts; and,
removing the gaseous halogen-containing byproducts and unreacted halogen gas from the solid boron nitride nanotube material to produce purified boron nitride nanotubes.

2. The process of claim 1 conducted under dry conditions.

3. The process of claim 1 , wherein the impurities comprise boron-containing impurities.

4. The process of claim 1 , wherein the purity and crystallinity of BNNT material recovered from the process improves as the temperature is increased up to a maximum temperature of 1250° C.

5. The process of claim 3 , wherein the impurities removed comprise hexagonal boron nitride.

6. The process of claim 3 , wherein the impurities removed comprise defective BNNT material.

7. The process of claim 1 , wherein the gaseous halogen-containing byproducts comprise a boron trihalide.

8. The process of claim 1 , wherein the solid boron nitride nanotube material is a material produced in a catalyst-free process.

9. The process of claim 1 , wherein the gaseous halogen-containing byproducts and unreacted halogen gas are removed from the solid boron nitride nanotube material under a positive pressure of flowing gas.

10. The process of claim 1 , wherein the purity of the purified boron nitride nanotubes is at least 75%.

11. The process of claim 1 , wherein the solid boron nitride nanotube material is exposed to the halogen gas at the indicated temperature for a period of about 1-20 minutes per gram of solid boron nitride nanotube material.

Assignees

• Nat Res Council Canada

Inventors

• Simard Benoit
• Ingold Keith
• Walker Steven Kendrick
• Iannitto Robyn
• Cho Hyunjin
• Martinez-Rubi Yadienka
• Kim Keun Su
• Kingston Christopher
• Guan Jingwen
• Denommee Stephane
• Ruth Dean
• Plunkett Mark

Classifications

• C01P2004/13

  Nanotubes · CPC title

• C01P2004/03

  obtained by SEM · CPC title

• C01P2002/88

  by thermal analysis data, e.g. TGA, DTA, DSC · CPC title

• C01P2002/84

  by UV- or VIS- data · CPC title

• C01B35/146

  Compounds containing boron and nitrogen, e.g. borazoles (ammonium tetrafluoborates C01B35/063; ammonium borates C01B35/12) · CPC title