Induction-coupled plasma synthesis of boron nitrade nanotubes

• US 10,343,908 B2
• Filed: 10/31/2014
• Issued: 07/09/2019
• 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:
  US15/033,498
• Publication Number:
  US 20160272496A1
• Time in Patent Office: 1,712 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. An apparatus for ICP-based BNNT synthesis, the apparatus comprising:

a. a chamber having an elevated pressure nitrogen gas inlet upstream of a boron-containing feedstock inlet;

b. an elevated pressure nitrogen gas supply connected to the elevated pressure nitrogen gas inlet;

c. a boron-containing feedstock supply connected to the feedstock inlet;

d. an induction-coupled plasma (ICP) head downstream of the gas inlet;

e. a nucleation zone within the chamber and downstream of the ICP head;

f. a growth zone within the chamber and downstream of the nucleation zone; and

g. a collection zone within the chamber and downstream of the growth zone.

2. The apparatus of claim 1, wherein the growth zone comprises at least one of an asperity and a condenser to trigger formation of BNNTs.

3. The apparatus of claim 2, wherein the condenser comprises 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.

4. The apparatus of claim 1, wherein the collection zone comprises at least one of a solid surface condenser, a collection surface, and a filter downstream of the growth zone.

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

6. The apparatus of claim 5, wherein the chamber is at an elevated pressure of at least 2 atmospheres to about 12 atmospheres.

7. The apparatus of claim 1, wherein boron-containing feedstock supply contains a boron-containing feedstock that comprises at least one of elemental boron, elemental boron powder, boron nitride, boron nitride powder, cubic boron nitride powder, and hexagonal boron nitride powder.

8. The apparatus of claim 1, wherein the nucleation zone cools the vaporized boron to form boron droplets.

9. The apparatus of claim 8, wherein cooling the vaporized boron is performed with at least one of a condenser and a plurality of asperities.

10. The apparatus of claim 8, wherein the cooling of the vaporized boron is performed with a condenser comprising 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.

11. The apparatus of claim 8, wherein the chamber holds the temperature of the boron droplets above the melting point of boron and below the boiling point of boron in the growth zone.

12. An apparatus for ICP-based BNNT synthesis, the apparatus comprising a chamber having:

a. an elevated pressure nitrogen gas inlet upstream of a boron-containing feedstock inlet;

b. a boron-containing feedstock supply connected to the feedstock inlet;

c. an induction-coupled plasma (ICP) head downstream of the gas inlet;

d. a nucleation zone downstream of the ICP head;

e. a growth zone downstream of the nucleation zone; and

f. a collection zone downstream of the growth zone and having at least one of a solid surface condenser, a collection surface, and a filter.

13. The apparatus of claim 12, further comprising an elevated pressure nitrogen gas supply connected to the elevated pressure nitrogen gas inlet.

14. The apparatus of claim 12, wherein the chamber is at an elevated pressure of at least 2 atmospheres to about 250 atmospheres.

15. The apparatus of claim 12, wherein the chamber is at an elevated pressure of at least 2 atmospheres to about 12 atmospheres.