Process of manufacturing a porous carbon material and a capacitor having the same

• US 5,876,787 A
• Filed: 11/08/1996
• Issued: 03/02/1999
• Est. Priority Date: 11/30/1995
• Status: Expired due to Fees

• Current Assignee: Frankenburg Oil Company Est.
• Original Assignee: Alfar International, Ltd.
• Inventors: Mazaeva, Tatjana Vasilevna, Kravtjik, Aleksandr Efimovitj, Kukusjkina, Julia Aleksandrovna, Sokolov, Vasilij Vasilevitj, Avarbz, Robert Gustavovitj, Zelenov, Boris Aleksandrovitj, Kuznetsov, Viktor Petrovitj, Vartanova, Alla Vladilenovna, Pankina, Olga Sergeevna, Gordeev, Sergej Konstantinovitj, Zjukov, Sergej Germanovitj
• Primary Examiner(s): Beck, Shrive
• Assistant Examiner(s): CHEN, BRET P
• Application Number:
  US08/745,589
• Time in Patent Office: 844 Days
• Field of Search: 427/58, 427/79, 427/115, 427/122, 427/126.1, 427/215, 427/219, 427/376.2, 427/397.7
• US Class Current: 427/79
• CPC Class Codes: H01G 11/26 characterised by their structure, e.g. multi-layered, porosity or surface features
• CPC Class Codes: H01G 11/34 characterised by carbonisation or activation of carbon
• CPC Class Codes: H01G 11/44 Raw materials therefor, e.g. resins or coal
• CPC Class Codes: H01M 4/583 Carbonaceous material, e.g. graphite-intercalation compounds or CFx
• CPC Class Codes: H01M 4/625 Carbon or graphite
• CPC Class Codes: Y02E 60/10 Energy storage using batteries
• CPC Class Codes: Y02E 60/13 Energy storage using capacitors
• CPC Class Codes: Y10S 977/892 Liquid phase deposition

Abstract

A process of manufacturing a porous carbon material and a capacitor having the same is provided. The process is comprised of: forming an intermediate blank (in the shape of a desired electrode) made of a metal carbide material having a porosity in the range of substantially 30% to 50% by volume. The blank is then impregnated by exposure to a gaseous hydrocarbon mixture at a temperature exceeding the decomposition of the hydrocarbon until the mass of the blank increases by about 10% to 25%. Next the inner surface of the blank is activated by heating. The blank is then exposed to gaseous chlorine and heated to remove the metal and form the blank having transport channels. Further chlorination occurs which forms nano sized pores in the structure. Thus, a porous carbon material is made which contains transport channels and nano sized pores.

Claims

1. A method of manufacturing an electrode material having a solid carbon skeleton network with a plurality of pores, and a plurality of transport channels, comprising the steps of:

forming in the shape of said electrode an intermediate blank made of silicon carbide material having a porosity in the range of substantially 30% to 50% by volume;

impregnating said intermediate blank with a pyrocarbon by exposure to a gaseous hydrocarbon mixture at a temperature exceeding decomposition of said gaseous hydrocarbon mixture until the mass of said intermediate blank increases by substantially 10% to 25%;

activating the inner surface of said intermediate blank by heating said blank to a temperature substantially in the range of 1450°

C. to 1700°

C.;

saturating said intermediate blank with liquid silicon wherein said pyrocarbon interacts with said liquid silicon to form a secondary silicon carbide structure throughout said blank, with free silicon filling cavities in said blank; and

exposing said blank to gaseous chlorine at a temperature in the range of substantially 900°

C. to 1100°

C.;

wherein the free silicon is removed forming a plurality of transport channels, and the silicon carbide undergoes chlorination which forms a plurality of pores.

2. The method of claim 1 wherein the step of activating further comprises heating said blank in an inert atmosphere.

3. The method of claim 1 wherein the step of activating further comprises heating said blank in a vacuum.

4. The method of claim 1 wherein the step of saturating occurs at a temperature in the range of substantially 1500°

C. to 1700°

C.

5. The method of claim 1 wherein said intermediate blank is formed by pressing.

6. The method of claim 1 wherein said intermediate blank is formed by slurry casting.

7. The method of claim 1 wherein said intermediate blank is formed by slip casting.

8. The method of claim 1 wherein said silicon carbide material comprises silicon carbide particles having a size in the range of substantially of 5 to 40 micrometer.

9. The method of claim 1 wherein said silicon carbide material comprises silicon carbide fibers.

10. The method of claim 1 wherein said silicon carbide material comprises a mixture of silicon carbide fibers and particles.

11. The method of claim 1 wherein said silicon carbide material comprises a mixture of carbon fibers and silicon carbide particles.

12. A method of manufacturing an electrode material having a solid carbon skeleton network with a plurality of pores, and a plurality of transport channels, comprising the steps of:

forming in the shape of said electrode, an intermediate blank made of carbide material and a binding agent;

impregnating said intermediate blank with a pyrocarbon by exposure to a gaseous hydrocarbon mixture at a temperature exceeding decomposition of said gaseous hydrocarbon mixture until the mass of said intermediate blank increases by substantially 10% to 25%;

activating the inner surface of said intermediate blank by heating said blank to a temperature substantially in the range of 1450°

C. to 1700°

C.; and

exposing said blank to a halogen gas at a temperature in the range of substantially 600°

C. to 1100°

C. to remove the metal from said intermediate blank to form a solid carbon skeleton network with a plurality of pores, and a plurality of transport channels.

13. The method of claim 12 further comprising the step of saturating said intermediate blank with liquid silicon wherein said pyrocarbon interacts with said liquid silicon to form a secondary structure throughout said blank, with free silicon filling cavities in said blank.

14. The method of claim 12 wherein said carbide material is selected from the group of metals consisting of Group IV, V, and VI of the periodic table.

15. The method of claim 12 wherein said carbide material is silicon carbide.

16. The method of claim 12 wherein said carbide material comprises silicon carbide fibers.

17. The method of claim 12 wherein said carbide material comprises silicon carbide particles.

18. The method of claim 12 wherein said carbide material comprises a mixture of silicon carbide particles and fibers.

19. The method of claim 12 wherein said carbide material comprises a mixture of carbon fibers and silicon carbide particles.

20. A method of manufacturing an electrode material comprising the steps of:

forming in the shape of said electrode, an intermediate blank made of a mixture of carbide particles and a binding agent, said blank having a porosity in the range of substantially 30% to 50% by volume;

impregnating said intermediate blank by exposure to natural gas at a temperature of approximately 900°

C. until the mass of said intermediate blank increases by substantially 8% to 25%; and

exposing said blank to chlorine gas at a temperature of approximately 600°

C., wherein metal is removed from the blank leaving a solid carbon skeleton structure with a plurality of pores and a plurality of transport channels.

21. The method of claim 20 wherein said carbide particles comprise a mixture of particles such that 70% by weight of said particles have a size of approximately 40 microns, and 30% by weight of said particles have a size of approximately 3 microns.

22. The method of claim 20 wherein said binder comprises a 10% by weight solution of 10% phenolic resin and 90% C₂ H₅ OH.

23. The method of claim 20 wherein said electrode material has a total porosity of approximately 0.6 comprised from said pores having a porosity of approximately 0.33 and said transport channels having a porosity of approximately 0.27.

24. The method of claim 20 wherein said electrode material has a surface area of 700 m² /cm³.