IP Library Granted Patent US 10,207,956
Granted Patent B2
US 10,207,956 · App. 15/195,313 · Granted Feb 19, 2019

Methods of forming silicon carbide by spark plasma sintering

Inventors: Henry S Chu (Idaho Falls, ID); Robert C O'Brien (Idaho Falls, ID); Steven K Cook (Idaho Falls, ID); Michael P Bakas (Raleigh, NC)
Assignee: Battelle Energy Alliance, LLC
C04B35/575C04B2235/6562C04B2235/6565C04B2235/6567C04B2235/666C04B2235/767C04B2235/77
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Quick Facts
Patent No.
US 10,207,956
App. No.
15/195,313
Granted
Feb 19, 2019
Kind
B2
Abstract

A method of forming silicon carbide by spark plasma sintering comprises loading a powder comprising silicon carbide into a die and exposing the powder to a pulsed current to heat the powder at a rate of between about 50° C./min and about 200° C./min to a peak temperature while applying a pressure to the powder. The powder is exposed to the peak temperature for between about 30 seconds and about 5 minutes to form a sintered silicon carbide material and the sintered silicon carbide material is cooled. Related structures and methods are disclosed.

Claims (22)

1. A method of forming silicon carbide by spark plasma sintering, the method comprising:

loading a powder comprising silicon carbide into a die;

exposing the powder to a current to heat the powder at a rate of between about 50° C./min and about 200° C./min to a peak temperature while applying a pressure to the powder;

while the powder is exposed to the peak temperature, exposing the powder to a current density less than about 0.1 A/mm 2 for between about 30 seconds and about 5 minutes to form a sintered silicon carbide structure; and

cooling the sintered silicon carbide structure.

2. The method of claim 1 , further comprising, after cooling the sintered carbide structure, exposing the sintered silicon carbide structure to the peak temperature again to increase a density of the sintered silicon carbide structure.

3. The method of claim 1 , further comprising selecting the powder to comprise silicon carbide and a sintering aid.

4. The method of claim 3 , further comprising selecting the sintering aid to comprise boron carbide.

5. The method of claim 1 , further comprising selecting the powder such that silicon carbide constitutes at least about 98 weight percent of the powder.

6. The method of claim 1 , wherein cooling the sintered silicon carbide structure comprises cooling the sintered silicon carbide structure at a rate between about 100° C./min and about 500° C./min.

7. The method of claim 1 , further comprising selecting the peak temperature to be between about 2,000° C. and about 2,100° C.

8. The method of claim 1 , further comprising exposing the powder to the peak temperature for about 2 minutes.

9. The method of claim 1 , wherein forming a sintered silicon carbide structure comprises forming the sintered silicon carbide structure to have a density of at least about 3.178 g/cm 3 .

10. The method of claim 1 , wherein exposing the powder to a current to heat the powder at a rate of between about 50° C./min and about 200° C./min to a peak temperature comprises exposing the powder to a current density of about 0.1 A/mm 2 .

11. The method of claim 1 , further comprising selecting the die to comprise at least one tapered sidewall.

12. The method of claim 11 , further comprising selecting the taper to comprise about a 1° taper.

13. The method of claim 1 , further comprising selecting the die to comprise graphite exhibiting a coefficient of thermal expansion equal to about a coefficient of thermal expansion of the sintered silicon carbide structure between a temperature of about 1,950° C. and about 2,100° C.

14. The method of claim 1 , wherein forming a sintered silicon carbide structure comprises forming a silicon carbide structure having a density of about 3.21 g/cm 3 .

15. The method of claim 1 , wherein providing a silicon carbide powder into the die comprises providing the silicon carbide powder into the die substantially free of a lubricant.

16. The method of claim 1 , further comprising selecting the die to comprise isotropic graphite.

17. The method of claim 1 , wherein exposing the powder to a current comprises pulsing a direct current through the powder in cycles, each cycle comprising pulsing the direct current for about 12 milliseconds followed by applying substantially no current for about 6 milliseconds.

18. The method of claim 1 , further comprising, after cooling the sintered carbide structure, exposing the sintered silicon carbide structure to the peak temperature again to increase a density of the sintered silicon carbide structure by at least about 0.1 g/cm 3 .

Assignments (4)
CONFIRMATORY LICENSE Recorded Feb 6, 2019
From: BATTELLE ENERGY ALLIANCE/IDAHO NAT'L LAB
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 048274/0195 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 26, 2017
From: CHU, HENRY S.; BAKAS, MICHAEL P.
To: BATTELLE ENERGY ALLIANCE, LLC
Reel/Frame 041094/0575 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 26, 2017
From: O'BRIEN, ROBERT C.
To: BATTELLE ENERGY ALLIANCE, LLC
Reel/Frame 041094/0726 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 26, 2017
From: COOK, STEVEN K.
To: BATTELLE ENERGY ALLIANCE, LLC
Reel/Frame 041094/0839 →
Continuity (1)
Related Publication 20170369381A1 · Dec 28, 2017
Cited By (1)
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