Process for production of graphene/silicon carbide ceramic composites

Patent metadata

Field	Value
Publication number	US-9988313-B2
Application number	US-201314429546-A
Country	US
Kind code	B2
Filing date	Sep 19, 2013
Priority date	Sep 20, 2012
Publication date	Jun 5, 2018
Grant date	Jun 5, 2018

Abstract

We provide a method for the in situ development of graphene containing silicon carbide (SiC) matrix ceramic composites, and more particularly to the in situ graphene growth within the bulk ceramic through a single-step approach during SiC ceramics densification using an electric current activated/assisted sintering (ECAS) technique. This approach allows processing dense, robust, highly electrical conducting and well dispersed nanocomposites having a percolated graphene network, eliminating the handling of potentially hazardous nanostructures. Graphene/SiC components could be used in technological applications under strong demanding conditions where good electrical, thermal, mechanical and/or tribological properties are required, such as micro and nanoelectromechanical systems (MEMS and NEMS), sensors, actuators, heat exchangers, breaks, components for engines, armors, cutting tools, microturbines or microrotors.

First claim

We claim:

1. A method for manufacturing in situ graphene containing silicon carbide matrix ceramic composites, the method comprising:
a) mixing a ceramic powder composition consisting of silicon carbide and at least one sintering additive;
b) densifying the ceramic powder composition by electric current activated/assisted sintering (ECAS), resulting in graphene growth from thermal decomposition of silicon carbide within a ceramic material from the ceramic powder composition.

2. The method according to claim 1 , wherein said silicon carbide is a silicon carbide powder comprising one or more types of silicon carbide selected from the group consisting of alpha-phase silicon carbide and beta-phase silicon carbide.

3. The method according to claim 2 , wherein said silicon carbide powder has an average particle size between 0.05 μm and 10.0 μm.

4. The method according to claim 1 , wherein said at least one sintering additive comprises at least one member of the group consisting of metallic oxides and mixtures of metallic oxides and non-metallic oxides.

5. The method according to claim 4 , wherein said sintering additive is selected from the group consisting of aluminum oxide, silicon dioxide, aluminum nitrate, yttrium nitrate, yttrium oxide, lutetium oxide, ytterbium oxide, gadolinium oxide and lanthanum oxide.

6. The method according to claim 1 , wherein said sintering additive comprises aluminium oxide powder and yttrium oxide powder, and wherein the sintering additive constitutes more than 0% and up to 21% of said ceramic powder composition by weight.

7. The method according to claim 6 , wherein said ceramic powder composition comprises 2 weight % of aluminium oxide and 5 weight % of yttrium oxide.

8. The method according to claim 1 , wherein said graphene comprises at least one of monolayer, 2 to 20 layer, and multilayer graphene, or combinations thereof.

9. The method according to claim 1 , wherein said electric current activated/assisted sintering (ECAS) technique is selected from the group consisting of resistance sintering (RS), electric discharge sintering (EDS), spark plasma sintering (SPS), field activated sintering technique (FAST), pulsed electric current sintering (PECS), pulse discharge sintering (PDS), plasma activated sintering (PAS), and pulse current sintering (PCS).

10. The method according to claim 1 , wherein said densification of the ceramic powder composition and graphene growth are effected through application of a vacuum atmosphere between 10 Pa and 0.1 Pa.

11. The method according to claim 1 , wherein said densification of the ceramic powder composition and graphene growth are effected under uniaxial pressure between 20 MPa and 100 MPa.

12. The method according to claim 1 , wherein said densification of the ceramic powder composition and graphene growth are conducted at maximum temperatures between 1600° C. and 2000° C.

13. The method according to claim 1 , wherein densification of the ceramic powder composition and graphene growth are conducted at a holding time of between 0 and 30 minutes at a maximum temperature.

14. The method according to claim 1 , wherein the densification of the ceramic powder composition and graphene growth includes application of heating rate ramps as a function of a maximum temperature, Tmax, selected from the group consisting of a) 133° C.·min −1 up to 1400° C.; b) from 1400° C. to Tmax−75° C. at 75° C.·min −1 ; c) from Tmax−75° C. to Tmax−25° C. at 50° C.·min −1 ; and d) from Tmax−25° C. to Tmax at 25° C.·min −1 .

Assignees

• Penn State Res Found
• Consejo Superior Investigacion

Inventors

• Miranzo Pilar
• Ocal Carmen
• Osendi Maria Isabel
• Belmonte Manuel
• Ramirez Cristina
• Roman-Manso Benito
• Gutierrez Humberto R
• Terrones Mauricio

Classifications

• C04B2235/3225

  Yttrium oxide or oxide-forming salts thereof · CPC title

• C04B2235/3834

  Beta silicon carbide · CPC title

• C04B35/64

  Burning or sintering processes (C04B33/32 takes precedence {; powder metallurgy B22F}) · CPC title

• C04B2235/5436

  micrometer sized, i.e. from 1 to 100 micron · CPC title

• C04B2235/78

  Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures · CPC title