IP Library › Granted Patent US 10,954,167
Granted Patent B1
US 10,954,167 · App. 16/261,246 · Granted Mar 23, 2021

Methods for producing metal carbide materials

Inventors: John E. Garnier (Idaho Falls, ID); George W. Griffith (Idaho Falls, ID)
Assignee: Advanced Ceramic Fibers, LLC
C04B35/62281B82Y30/00C01B32/956C04B35/565C04B35/571C04B35/573C04B35/806C04B2235/428C04B2235/46C04B2235/48C04B2235/526C04B2235/5244C04B2235/5248C04B2235/5264C04B2235/5284C04B2235/5445C04B2235/616C04B2235/72C04B2235/767Y10T428/24993Y10T428/249924Y10T428/249928Y10T428/249974Y10T428/292Y10T428/2918Y10T428/2933Y10T428/2958Y10T428/2964Y10T428/2967Y10T428/2975
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Quick Facts
Patent No.
US 10,954,167
App. No.
16/261,246
Granted
Mar 23, 2021
Kind
B1
Abstract

Methods of producing silicon carbide, and other metal carbide materials. The method comprises reacting a carbon material (e.g., fibers, or nanoparticles, such as powder, platelet, foam, nanofiber, nanorod, nanotube, whisker, graphene (e.g., graphite), fullerene, or hydrocarbon) and a metal or metal oxide source material (e.g., in gaseous form) in a reaction chamber at an elevated temperature ranging up to approximately 2400° C. or more, depending on the particular metal or metal oxide, and the desired metal carbide being produced. A partial pressure of oxygen in the reaction chamber is maintained at less than approximately 1.01×10 2 Pascal, and overall pressure is maintained at approximately 1 atm.

Claims (26)

1. A method of producing silicon carbide material, comprising:

reacting a carbon material and a silicon-containing gas in a reaction chamber at an elevated temperature of up to approximately 2400° C. and a pressure of about 1 atmosphere; and

maintaining a partial pressure of oxygen in the reaction chamber of less than approximately 1.01×10 2 Pascal to produce the silicon carbide material.

2. The method of claim 1 , wherein reacting a carbon material and a silicon-containing gas in a reaction chamber comprises reacting the carbon material with silicon monoxide in the reaction chamber.

3. The method of claim 2 , wherein reacting the carbon material and silicon monoxide in a reaction chamber comprises forming the silicon monoxide in situ in the reaction chamber.

4. The method of claim 3 , wherein forming the silicon monoxide in situ in the reaction chamber comprises reacting silicon dioxide and silicon in the reaction chamber.

5. The method of claim 1 , wherein reacting a carbon material and the silicon-containing gas in the reaction chamber comprises reacting a carbon nanoparticle and silicon monoxide in the reaction chamber.

6. The method of claim 5 , wherein maintaining the partial pressure of oxygen in the reaction chamber of less than approximately 1.01×10 2 Pascal to produce silicon carbide nanoparticles comprises producing the silicon carbide nanoparticles:

(i) that comprise a converted layer of silicon carbide on an unconverted carbon material, where the converted layer has been converted from carbon to silicon carbide; or

(ii) that are fully converted from carbon to silicon carbide.

7. The method of claim 1 , wherein reacting a carbon material and a silicon-containing gas in a reaction chamber at a temperature of up to approximately 2400° C. comprises reacting the carbon material and the silicon-containing gas at a temperature ranging from approximately 1500° C. to approximately 1800° C. to produce alpha silicon carbide.

8. The method of claim 1 , wherein reacting a carbon material and a silicon-containing gas in a reaction chamber at a temperature of up to approximately 2400° C. comprises reacting the carbon material and the silicon-containing gas at a temperature ranging from approximately 1100° C. to approximately 1450° C. to produce beta silicon carbide.

9. The method of claim 1 , wherein a pressure within the reaction zone is maintained at a positive pressure of from approximately 1 psig to approximately 10 psig above atmospheric pressure to prevent an external atmosphere from entering into the reaction chamber.

10. The method of claim 1 , wherein a vapor pressure of silicon monoxide species in the reaction chamber is maintained at approximately 1 atm.

11. The method of claim 1 , wherein the produced silicon carbide material comprises alpha silicon carbide nanoparticles.

12. The method of claim 1 , wherein the carbon material comprises carbon nanoparticles in the form of powder, platelet, foam, nanofiber, nanofilament, nanorod, nanotube, graphene, or fullerene.

13. The method of claim 1 , wherein the produced silicon carbide material is formed from nanocarbon particles having a size of approximately 1 nm or larger.

14. The method of claim 1 , wherein the produced silicon carbide material comprises a silicon carbide material in the form of powder, platelet, foam, nanofiber, nanorod, or nanotube.

15. The method of claim 1 , wherein the produced silicon carbide material comprises:

(i) a fully converted silicon carbide material, where the starting carbon material is a starting carbon nanoparticle material and has been substantially fully converted to the silicon carbide material, wherein the silicon carbide material comprises carbon from the starting carbon nanoparticle material that has been converted to the silicon carbide; or

(ii) a partially converted silicon carbide material, where the starting carbon material is a starting carbon nanoparticle material, the silicon carbide material comprising a silicon carbide material disposed over a carbon nanoparticle core, wherein the silicon carbide material comprises carbon from the starting carbon nanoparticle material that has been converted to the silicon carbide material, and wherein the carbon nanoparticle core comprises unconverted starting carbon nanoparticle material.

16. The method of claim 15 , wherein the produced silicon carbide material comprises a fully converted silicon carbide material, where the starting carbon material is a starting carbon nanoparticle material and has been substantially fully converted to the silicon carbide material, wherein the silicon carbide material comprises carbon from the starting carbon nanoparticle material that has been converted to the silicon carbide.

17. The method of claim 15 , wherein the produced silicon carbide material comprises a partially converted silicon carbide material, where the starting carbon material is a starting carbon nanoparticle material, the silicon carbide material comprising a silicon carbide material disposed over a carbon nanoparticle core, wherein the silicon carbide material comprises carbon from the starting carbon nanoparticle material that has been converted to the silicon carbide material, and wherein the carbon nanoparticle core comprises unconverted starting carbon nanoparticle material.

18. The method of claim 15 , wherein a size of the produced silicon carbide material is 1 nm or greater.

19. The method of claim 1 , wherein the method is a continuous process.

20. The method of claim 1 , wherein less than 1000 ppm of any iron or other impurities are present during the method to prevent formation of catalytically grown whiskers during conversion.

Assignments (2)
CONFIRMATORY LICENSE Recorded Sep 3, 2019
From: ADVANCED CERAMICS FIBERS
To: NAVY, SECRETARY OF THE UNITED STATES OF AMERICA
Reel/Frame 050274/0718 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 29, 2019
From: GARNIER, JOHN E.; GRIFFITH, GEORGE W.
To: ADVANCED CERAMIC FIBERS, LLC
Reel/Frame 048170/0858 →
Continuity (7)
Continuation In Part 14954518 · Nov 30, 2015
Continuation In Part 13215967 · Aug 23, 2011
Continuation In Part 12901326 · Oct 8, 2010
Continuation In Part 14570927 · Dec 15, 2014
Division 12901309 · Oct 8, 2010
Continuation In Part 14615685 · Feb 6, 2015
Provisional Application 61941001 · Feb 18, 2014
Cited By (2)
US 12,191,228 US 12,577,172