Induction-coupled plasma synthesis of boron nitrade nanotubes

• US 10,640,378 B2
• Filed: 06/06/2019
• Issued: 05/05/2020
• Est. Priority Date: 11/01/2013
• Status: Active Grant

• Current Assignee: BNNT, LLC
• Original Assignee: BNNT, LLC
• Inventors: Smith, Michael W., Stevens, Jonathan C., Jordan, Kevin C.
• Primary Examiner(s): Gregorio, Guinever S
• Application Number:
  US16/433,782
• Publication Number:
  US 20190322529A1
• Time in Patent Office: 334 Days
• Field of Search: None
• CPC Class Codes: B01J 10/005 carried out at high temperatures in the presence of a molten material
• CPC Class Codes: B01J 19/08 Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor application of shock waves B01J3/08
• CPC Class Codes: B01J 19/088 giving rise to electric discharges for heating purposes H05B7/00; for the production of ozone C01B13/11, H01T19/00
• CPC Class Codes: B01J 2219/0898 Hot plasma
• CPC Class Codes: B82Y 40/00 Manufacture or treatment of nanostructures
• CPC Class Codes: C01B 21/064 with boron
• CPC Class Codes: C01B 21/0641 Preparation by direct nitridation of elemental boron
• CPC Class Codes: C01P 2004/13 Nanotubes
• CPC Class Codes: C01P 2004/133 Multiwall nanotubes

Abstract

Described herein are processes and apparatus for the large-scale synthesis of boron nitride nanotubes (BNNTs) by induction-coupled plasma (ICP). A boron-containing feedstock may be heated by ICP in the presence of nitrogen gas at an elevated pressure, to form vaporized boron. The vaporized boron may be cooled to form boron droplets, such as nanodroplets. Cooling may take place using a condenser, for example. BNNTs may then form downstream and can be harvested.

Claims

1. A process for synthesizing boron nitride nanotubes (BNNTs), the process comprising:

feeding nitrogen gas into a chamber having a boron-containing feedstock;

heating the nitrogen gas and boron-containing feedstock with an induction-coupled plasma to form heated reactants in a growth zone, the growth zone downstream of the induction coupled plasma;

maintaining a growth zone temperature at a temperature above the melting point of boron and below the boiling point of boron; and

collecting, in a collection zone downstream of the growth zone, BNNTs forming from the heated reactants in the growth zone.

2. The process of claim 1, further comprising triggering formation of BNNTs in the grown zone from the heated reactants by at least one of introducing asperities into the chamber, natural nucleation, and cooling with a condenser.

3. The process of claim 1, further comprising introducing a noble gas to the induction coupled plasma.

4. The process of claim 1, wherein collecting is performed using at least one of a solid surface condenser, a collection surface, and a filter.

5. The process of claim 1, further comprising feeding a boron-containing feedstock into the chamber.

6. The process of claim 1, wherein feeding nitrogen gas into a chamber is a continuous process.

7. The process of claim 1, wherein collecting BNNTs is a continuous process.

8. The process of claim 1, wherein collecting BNNTs is a batch process.

9. The process of claim 1, wherein the chamber is at an elevated pressure of at least 2 atmospheres to about 250 atmospheres.

10. The process of claim 9, wherein the chamber is at an elevated pressure of at least 2 atmospheres to about 12 atmospheres.

11. The process of claim 1, wherein the boron-containing feedstock comprises at least one of elemental boron, elemental boron powder, boron nitride, boron nitride powder, cubic boron nitride powder, and hexagonal boron nitride powder.

12. The process of claim 1, wherein the nitrogen gas is fed at a feed inlet, and the heated reactants are formed downstream of the feed inlet.

13. A process for synthesizing boron nitride nanotubes (BNNTs) from an induction-coupled plasma, the process comprising:

introducing nitrogen and a boron-containing feedstock into a chamber to form a reactant feed;

passing the reactant feed through an induction-coupled plasma;

heating, with the induction-coupled plasma, the reactant feed to a temperature sufficient to form a heated reactant having vaporized boron;

passing the heated reactant feed through a grown zone downstream of the induction-coupled plasma;

maintaining a temperature in the growth zone at a temperature above the melting point of boron and below the boiling point of boron; and

collecting BNNTs forming from the heated reactants in the growth zone.

14. The process of claim 13, further comprising triggering formation of BNNTs in the grown zone from the heated reactant feed by at least one of introducing asperities into the chamber, natural nucleation, and cooling with a condenser.

15. The process of claim 13, further comprising introducing a noble gas to the induction coupled plasma.

16. The process of claim 13, wherein the chamber is at an elevated pressure of at least 2 atmospheres to about 250 atmospheres.

17. The process of claim 16, wherein the chamber is at an elevated pressure of at least 2 atmospheres to about 12 atmospheres.

18. The process of claim 13, further comprising triggering formation of BNNTs in the grown zone from the heated reactant feed by at least one of a copper rod, a tungsten wire, a network of copper rods, a network of tungsten wires, a grid of copper rods, and a grid of tungsten wires.

19. The process of claim 13, wherein collecting BNNTs is a batch process.

20. The process of claim 13, wherein collecting BNNTs is performed using at least one of a solid surface condenser, collection surfaces, and filters downstream of the growth zone.