Process for making carbon foam

• US 6,033,506 A
• Filed: 09/02/1997
• Issued: 03/07/2000
• Est. Priority Date: 09/02/1997
• Status: Expired due to Term

• Current Assignee: Lockheed Martin Energy Research Corporation (Martin Marietta Corporation)
• Original Assignee: Lockheed Martin Energy Research Corporation (Martin Marietta Corporation)
• Inventors: Klett, James W.
• Primary Examiner(s): Tentoni, Leo B.
• Application Number:
  US08/921,875
• Time in Patent Office: 917 Days
• Field of Search: 264/29.6, 264/29.7, 264/42, 264/46.5, 264/85, 264/101, 156/78, 156/245
• US Class Current: 156/78
• CPC Class Codes: C04B 35/52 based on carbon, e.g. graphite
• CPC Class Codes: C04B 38/00 Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof treating slag with gases or gas generating material C04B5/06 ; expanded graphite C04B35/536
• CPC Class Codes: F28D 20/023 the latent heat storage material being enclosed in granular particles or dispersed in a porous, fibrous or cellular structure
• CPC Class Codes: Y02E 60/14 Thermal energy storage
• CPC Class Codes: Y10T 428/2982 Particulate matter [e.g., sphere, flake, etc.]
• CPC Class Codes: Y10T 428/30 Self-sustaining carbon mass or layer with impregnant or other layer

Abstract

The process obviates the need for conventional oxidative stabilization. The process employs mesophase or isotropic pitch and a simplified process using a single mold. The foam has a relatively uniform distribution of pore sizes and a highly aligned graphic structure in the struts. The foam material can be made into a composite which is useful in high temperature sandwich panels for both thermal and structural applications.

Claims

1. A process of producing carbon foam comprising:

selecting an appropriate mold shape;

introducing pitch to an appropriate level in a mold;

purging air from the mold;

heating the pitch to a temperature sufficient to coalesce the pitch into a liquid;

applying an inert fluid at a static pressure up to about 1000 psi;

heating the pitch to a temperature sufficient to cause gases to evolve and foam the pitch;

heating the pitch to a temperature sufficient to coke the pitch; and

cooling the foam to room temperature with a simultaneous release of pressure to produce a carbon foam.

2. The process of claim 1 wherein the pitch is introduced as granulated pitch.

3. The process of claim 1 wherein the pitch is introduced as powdered pitch.

4. The process of claim 1 wherein the pitch is introduced as pelletized pitch.

5. The process of claim 1 wherein the pitch is a synthetic mesophase or isotropic pitch.

6. The process of claim 1 wherein the pitch is a petroleum derived mesophase or isotropic pitch.

7. The process of claim 1 wherein the pitch is a coal-derived mesophase or isotropic pitch.

8. The process of claim 1 wherein the pitch is a blend of pitches selected from the group consisting of synthetic mesophase or isotropic pitch, petroleum derived mesophase or isotropic pitch, and coal derived mesophase or isotropic pitch.

9. The process of claim 1 wherein the pitch is a solvated pitch.

10. The process of claim 1 wherein the purging is effected by a vacuum step.

11. The process of claim 1 wherein the purging is effected by an inert fluid.

12. The process of claim 10 wherein the vacuum is applied at less than 1 torr.

13. The process of claim 1 wherein nitrogen is introduced as the inert fluid.

14. The process of claim 1 wherein the pitch is heated to a temperature in the range of about 500°

C. to about 1000°

C. to coke the pitch.

15. The process of claim 1 wherein the pitch is heated to a temperature of about 800°

C. to coke the pitch.

16. The process of claim 1 wherein the temperature to coke the pitch is raised at a rate of no greater than 5°

C. per minute.

17. The process of claim 1 wherein the pitch is soaked at the coking temperature for at least 15 minutes to effect the coking.

18. The process of claim 1 wherein the pitch is heated to a temperature of about 630°

C. to coke the pitch.

19. The process of claim 1 wherein the pitch is heated to a temperature of about 50°

C. to about 100°

C. to coalesce the pitch.

20. The process of claim 1 where the foam is cooled at a rate of approximately 1.5°

C./min with the release of pressure at a rate of approximately 2 psi/min.

21. The process of claim 1 further including the step of densifying the foam.

22. A process of producing carbon foam comprising:

selecting an appropriate mold shape and a mold composed of

a material that the molten pitch does not wet;

introducing pitch to an appropriate level in the mold;

purging the air from the mold;

heating the pitch to a temperature sufficient to coalesce the pitch into a liquid;

applying an inert fluid at a static pressure up to about 1000 psi;

heating the pitch to a temperature sufficient to coke the pitch; and

cooling the foam to room temperature with a simultaneous release of pressure to produce a carbon foam.

23. The process of claim 22 wherein the pitch is introduced as granulated pitch.

24. The process of claim 22 wherein the pitch is introduced as powdered pitch.

25. The process of claim 22 wherein the pitch is introduced as pelletized pitch.

26. The process of claim 22 where in the pitch is a synthetic mesophase or isotropic pitch.

27. The process of claim 22 where in the pitch is a petroleum-derived mesophase pitch.

28. The process of claim 22 where in the pitch is a coal-derived mesophase pitch.

29. The process of claim 22 wherein the mold is purged by a vacuum applied at less than 1 torr.

30. The process of claim 22 wherein the mold is purged by an inert fluid before heating.

31. A process of producing carbon foam core composite comprising:

selecting an appropriate mold shape;

introducing pitch to an appropriate level in a mold;

purging air from the mold;

heating the pitch to a temperature sufficient to coalesce the pitch into a liquid;

applying an inert fluid at a static pressure up to above 1000 psi;

heating the pitch to a temperature sufficient to cause gases to evolve and foam the pitch;

heating the pitch to a temperature sufficient to coke the pitch;

cooling the foam to room temperature with a simultaneous release of pressure;

placing facesheets on the opposite sides of the carbon foam; and

adhering the facesheets to the carbon foam to produce a carbon foam core.

32. The process of claim 31 wherein the adhering of the facesheets to the carbon foam is effected by a molding step.

33. The process of claim 31 wherein the adhering of the facesheets to the carbon foam is effected by a coating material.

34. A process for producing a carbon foam comprising:

providing pitch in a container;

heating said pitch in a non-oxidizing atmosphere at a pressure and temperature sufficient to coalesce said pitch to form a liquid of said pitch;

increasing said pressure of said non-oxidizing atmosphere in said container containing said liquid of said pitch from said pressure to an increased pressure having a range greater than said pressure to about 1000 psi; and

heating said container containing said liquid of said pitch at said increased pressure to a temperature sufficient to form a carbon foam.

35. A process for producing a carbon foam in accordance with claim 34 wherein said container containing said liquid of said pitch at said increased pressure of about 1000 psi is heated to a temperature from about 420°

C. to about 480°

C.

36. A process for producing a thermally conductive essentially graphitic carbon foam comprising:

providing pitch in a container;

heating said pitch in a non-oxidizing atmosphere at a pressure to a temperature sufficient to coalesce said pitch to form a liquid of said pitch;

increasing said pressure of said non-oxidizing atmosphere in said container containing said liquid of said pitch from said pressure to an increased pressure having a range greater than said pressure to about 1000 psi;

heating said container containing said liquid of said pitch at said increased pressure to a temperature sufficient to form a carbon form;

cooling said carbon foam and reducing said increased pressure to atmospheric pressure;

heating said carbon foam in a non-oxidizing atmosphere to a temperature sufficient to carbonize said carbon foam to form a carbonized carbon foam; and

heating said carbonized carbon foam in a non-oxidizing atmosphere to a temperature sufficient to form a thermally conductive essentially graphitic carbon foam.

37. A process for producing a carbon foam in accordance with claim 36 wherein said container containing said liquid of said pitch is heated to a temperature from about 420°

C. to about 480°

C., said carbon foam at atmospheric pressure is heated to a temperature from about 500°

C. to about 1050°

C. and said carbonized carbon foam is heated to a temperature equal to or greater than 2500°

C.

38. A process for producing a thermal conducting essentially graphitic carbon foam in accordance with claim 36 wherein said graphitic carbon foam has a specific thermal conductivity greater than 109 W.cm3/m.K.g.