IP Library Granted Patent US 10,850,324
Granted Patent B1
US 10,850,324 · App. 16/786,286 · Granted Dec 1, 2020

Titanium-group nano-whiskers and method of production

Inventors: Roland D. Seals (Oak Ridge, TN); Paul A. Menchhofer (Clinton, TN); James O. Kiggans, Jr. (Oak Ridge, TN)
Assignees: Consolidated Nuclear Security, LLC; UT-Battelle, LLC
B22F1/0007B22F1/02C01B32/914C01B32/921C22C32/0052C22C47/00C22C49/04C22C49/14C23C16/0218C23C16/32C23C16/4417C30B25/005C30B29/36C30B29/62H01B1/02B22F1/0018B22F2301/205B22F2302/10
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Quick Facts
Patent No.
US 10,850,324
App. No.
16/786,286
Granted
Dec 1, 2020
Kind
B1
Abstract

Disclosed herein are structures comprising a titanium, zirconium, or hafnium powder particle with titanium carbide, zirconium carbide, or hafnium carbide (respectively) nano-whiskers grown directly from and anchored to the powder particle. Also disclosed are methods for fabrication of such structures, involving heating the powder particles and exposing the particles to an organic gas.

Claims (36)

1. A method of forming titanium group nano-whiskers comprising:

disposing titanium-group powder particles in a furnace chamber, the titanium-group powder particles comprising at least one of titanium, zirconium, and hafnium;

establishing a controlled environment for the titanium-group powder particles;

heating the titanium-group powder particles in the controlled environment to establish heated titanium-group powder particles; and

exposing the heated titanium-group powder particles to an organic gas such that the titanium-group nano-whiskers are grown directly from and anchored to the titanium-group powder particles, the titanium-group nano-whiskers comprising at least one of titanium carbide, zirconium carbide, and hafnium carbide.

2. The method of claim 1 wherein the step of establishing the controlled environment consists of establishing a protective reducing environment.

3. The method of claim 1 wherein the step of establishing the controlled environment consists of establishing an inert environment.

4. The method of claim 1 wherein the step of establishing the controlled environment includes purging the furnace chamber with a mixture of inert and reducing gases.

5. The method of claim 1 wherein the heating step includes heating the titanium-group powder particles to a temperature that is in a temperature range from approximately 600° C. to approximately 650° C.

6. The method of claim 1 wherein the exposing step includes flowing the organic gas into the furnace chamber at a rate of about 300 cc/min while maintaining the furnace chamber at a temperature of about 600° C.-650° C.

7. The method of claim 1 wherein the exposing step includes exposing the heated titanium-group powder particles to the organic gas for a duration of time that is in a time range from about one hour to about 24 hours while maintaining the furnace chamber at a temperature of about 600° C.-650° C.

8. The method of claim 1 wherein the titanium-group powder particles comprise titanium and the titanium-group nano-whiskers comprise titanium carbide.

9. The method of claim 1 wherein the titanium-group powder particles comprise zirconium and the titanium-group nano-whiskers comprise zirconium carbide.

10. The method of claim 1 wherein the titanium-group powder particles comprise hafnium and the titanium-group nano-whiskers comprise hafnium carbide.

11. The method of claim 1 wherein at least some of the titanium-group powder particles comprise any combination of titanium, zirconium, and hafnium.

12. The method of claim 11 wherein the combination titanium-group powder particle forms titanium-group nano-whiskers comprising any combination of titanium carbide, zirconium carbide, and hafnium carbide.

13. The method of claim 1 wherein the titanium-group powder particles each have a maximum dimension between about ten microns and about one hundred microns.

14. The method of claim 1 wherein the titanium-group nano-whiskers each have a tapered structure.

15. The method of claim 1 wherein the titanium-group nano-whiskers each have a maximum diameter ranging from about one nanometer to about one hundred nanometers and a length that is at least about one hundred nanometers.

16. A method of forming titanium group nano-whiskers comprising:

disposing titanium-group powder particles in a furnace chamber, the titanium-group powder particles formed at least in part of a transition metal;

establishing a controlled environment for the titanium-group powder particles;

heating the titanium-group powder particles in the controlled environment to establish heated titanium-group powder particles; and

exposing the heated titanium-group powder particles to an organic gas to grow titanium-group nano-whiskers directly from and anchored to the titanium-group powder particles,

wherein during the exposing step, a portion of the transition metal from each of the heated titanium-group powder particles chemically reacts with the organic gas such that each of the titanium-group nano-whiskers are a jointless extension of one of the titanium-group powder particles.

17. The method of claim 16 wherein the step of establishing the controlled environment includes purging the furnace chamber with a mixture of inert and reducing gases to establish a protective reducing environment, and wherein the protective reducing environment is maintained through the heating and exposing steps.

18. The method of claim 16 wherein the heating step includes heating the titanium-group powder particles to a temperature that is in a temperature range from approximately 600° C. to approximately 650° C.

19. The method of claim 16 wherein the exposing step includes exposing the heated titanium-group powder particles to the organic gas for a duration of time that is in a time range from about one hour to about 24 hours while maintaining the furnace chamber at a temperature of about 600° C.-650° C.

20. The method of claim 16 wherein the titanium-group powder particles comprise titanium and the titanium-group nano-whiskers comprise titanium carbide.

21. A method of forming titanium group nano-whiskers comprising:

disposing titanium-group powder particles in a furnace chamber;

purging the furnace chamber with a mixture of inert and reducing gases to establish a protective reducing environment for the titanium-group powder particles;

heating the titanium-group powder particles in the protective reducing environment to establish heated titanium-group powder particles; and

exposing the heated titanium-group powder particles to an organic gas to grow titanium-group nano-whiskers directly from and anchored to the titanium-group powder particles,

wherein the protective reducing environment is maintained through the heating and exposing steps.

22. The method of claim 21 wherein the titanium-group nano-whiskers include carbide nano-whiskers.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 4, 2020
From: MENCHHOFER, PAUL A.; KIGGANS, JAMES O., JR.
To: UT-BATTELLE, LLC
Reel/Frame 052834/0912 →
CONFIRMATORY LICENSE Recorded Feb 12, 2020
From: CONSOLIDATED NUCELAR SECURITY, LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 051792/0113 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 10, 2020
From: SEALS, ROLAND D.
To: CONSOLIDATED NUCLEAR SECURITY, LLC
Reel/Frame 051771/0432 →
Continuity (2)
Division 15883416 · Jan 30, 2018
Continuation In Part 13162866 · Jun 17, 2011