Carbon supercapacitor electrode materials

• US 5,993,996 A
• Filed: 09/16/1997
• Issued: 11/30/1999
• Est. Priority Date: 09/16/1997
• Status: Expired due to Term

• Current Assignee: Inorganic Specialists, Inc.
• Original Assignee: Inorganic Specialists, Inc.
• Inventors: Firsich, David W.
• Primary Examiner(s): Griffin, Steven P.
• Assistant Examiner(s): Hendrickson, Stuart L.
• Application Number:
  US08/931,466
• Time in Patent Office: 805 Days
• Field of Search: 429/218, 429/231.8, 429/231.4, 423/449.2, 423/449.3
• US Class Current: 429/231.8
• CPC Class Codes: C04B 35/52 based on carbon, e.g. graphite
• CPC Class Codes: C04B 38/0022 obtained by a chemical conversion or reaction other than those relating to the setting or hardening of cement-like material or to the formation of a sol or a gel, e.g. by carbonising or pyrolysing preformed cellular materials based on polymers, organo-metallic or organo-silicon precursors
• CPC Class Codes: C04B 41/4556 coating or impregnating with a product reacting with the substrate, e.g. generating a metal coating by surface reduction of a ceramic substrate
• 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: Y02E 60/10 Energy storage using batteries
• CPC Class Codes: Y02E 60/13 Energy storage using capacitors
• CPC Class Codes: Y02T 10/70 Energy storage systems for electromobility, e.g. batteries

Abstract

A carbon material useful as an electrode in supercapacitors and a method for preparing the same. In one method, a phenolic resin powder, optionally combined with a carbon powder, is formed into a layer less than 0.01 inches thick; the temperature of the resin is increased at a rate of approximately 0.1 to 4° C. per minute, thereby melting the resin into a porous network; the network is carbonized, hydrogenated in a hydrogen atmosphere and sulfonated.

Claims

1. A carbon electrode formed from a carbon, which carbon is prepared by a process comprising the step of hydrogenating the carbon followed by the step of sulfonating the carbon.

2. The carbon electrode of claim 1 wherein the sulfonating step is carried out by heating said carbon in fuming sulfuric acid, concentrated sulfuric acid, SO₃, or chlorosulfonic acid.

3. A carbon electrode formed from a carbon which is prepared by a process comprising the steps of:

forming a layer of phenolic resin powder;

melting said phenolic resin powder under such conditions that the particles of said powder stick to themselves to form a porous network;

carbonizing said porous network to form a carbonized network; and

sulfonating said carbonized network.

4. The carbon electrode of claim 3 wherein the sulfonating step is carried out by heating said carbonized network in fuming sulfuric acid, concentrated sulfuric acid, SO₃, or chlorosulfonic acid.

5. The carbon electrode of claim 3 further comprising a hydrogenating step prior to the sulfonating step wherein said carbonized network is hydrogenated.

6. The carbon electrode of claim 3 wherein the carbonizing step is carried out in the presence of hydrogen.

7. The carbon electrode of claim 4 wherein the sulfonating step is carried out by heating said carbonized network in fuming sulfuric acid.

8. The carbon electrode of claim 5 wherein said hydrogenating step is carried out by heating said carbonized network in a hydrogen-containing atmosphere at a temperature greater than 650°

C.

9. The carbon electrode of claim 8 further comprising an oxidizing step immediately prior to said hydrogenating step wherein said carbonized network is treated with nitric acid.

10. The carbon electrode of claim 9 wherein the melting step further includes increasing the temperature at a rate of approximately 0.1 to 4°

C. per minute to a temperature approximately between 80 and 160°

C.

11. The carbon electrode of claim 10 wherein the step of forming the layer further includes step of forming a layer less than 0.01 inches thick.

12. A carbon electrode formed from a carbon which is prepared by a process comprising the steps of:

forming a layer of phenolic resin powder and carbon powder;

melting said phenolic resin powder under such conditions that the particles of said powder stick to themselves and to the carbon particles of said carbon powder to form a porous network;

carbonizing said porous network to form a carbonized network; and

sulfonating said carbonized network.

13. The carbon electrode of claim 12 wherein the sulfonating step is carried out by heating said carbonized network in fuming sulfuric acid, concentrated sulfuric acid, SO₃, or chlorosulfonic acid.

14. The carbon electrode of claim 12 further comprising a hydrogenating step prior to the sulfonating step wherein said carbonized network is hydrogenated.

15. The carbon electrode of claim 14 wherein said hydrogenating step is carried out by heating said carbonized network in a hydrogen-containing atmosphere at a temperature greater than 650°

C.

16. The carbon electrode of claim 15 further comprising an oxidizing step immediately prior to said hydrogenating step wherein said carbonized network is treated with nitric acid.

17. The carbon electrode of claim 16 wherein the melting step further includes increasing the temperature at a rate of approximately 0.1 to 4°

C. per minute to a temperature approximately between 80 and 160°

C.

18. The carbon electrode of claim 17 wherein the step of forming the layer includes step of forming a layer less than 0.01 inches thick.

19. The carbon electrode of claim 13 wherein the sulfonating step is carried out by heating said carbonized network in fuming sulfuric acid.

20. The carbon electrode of claim 12 wherein the carbonizing step is carried out in the presence of hydrogen.