Preparation of polymeric resins and carbon materials

Patent metadata

Field	Value
Publication number	US-11725074-B2
Application number	US-202217944946-A
Country	US
Kind code	B2
Filing date	Sep 14, 2022
Priority date	Feb 9, 2012
Publication date	Aug 15, 2023
Grant date	Aug 15, 2023

Abstract

The present application is directed to methods for preparation of carbon materials. The carbon materials comprise enhanced electrochemical properties and find utility in any number of electrical devices, for example, as electrode material in ultracapacitors or batteries.

First claim

The invention claimed is:

1. A method of fabricating a battery anode electrode composition comprising a plurality of composite particles, each particle in the plurality of composite particles comprising a porous carbon particle and an electrochemical modifier incorporated into the pores of the porous carbon particle by the method comprising:
a. forming the porous carbon particle by:
i. pyrolyzing a polymer to form a carbon particle;
ii. activating the carbon particle to form an activated carbon particle; and
iii. performing a particle size reduction of the activated carbon particle to form the porous carbon particle; and

b. introducing the electrochemical modifier into the pores of the porous carbon particle through the vapor phase to form the composite particle,
wherein:
the polymer is formed from a polymer precursor; and
the polymer precursor comprises a saccharide, a protein, a biopolymer, or a combination thereof.

2. The method of claim 1 , wherein the porous carbon particle is spherical.

3. The method of claim 1 , wherein the polymer precursor comprises a protein.

4. The method of claim 1 , wherein the polymer precursor comprises a biopolymer.

5. The method of claim 1 , wherein pyrolyzing the polymer comprises heating polymer gel particles in an inert atmosphere at temperatures ranging from 500° C. to 2400° C.

6. The method of claim 1 , wherein activating the carbon particle comprises introducing the carbon particle to an atmosphere comprising carbon dioxide, carbon monoxide, steam, oxygen, or combinations thereof at a temperature ranging from 800° C. to 1300° C.

7. The method of claim 1 , wherein performing a particle size reduction is accomplished by milling, grinding, jet milling, Fritsch milling, or a combination thereof, the activated carbon.

8. The method of claim 1 , wherein each particle in the plurality of composite particles further comprises micropores and mesopores, and wherein the plurality of composite particles have a Dv,50 of less than 1 mm and a span of 3 or less, wherein the span is defined as (Dv,90−Dv,10)/Dv,50 where Dv,10, Dv,50, and Dv,90 refer to pore sizes at 10%, 50%, and 90% respectively within a pore size distribution by volume of the plurality of composite particles.

9. The method of claim 8 , wherein the electrochemical modifier is introduced into the pores of the porous carbon particle through the vapor phase by contacting the carbon particle with a gas comprising the electrochemical modifier.

10. The method of claim 8 , wherein the electrochemical modifier is silicon.

11. The method of claim 1 , wherein the electrochemical modifier is silicon.

12. The method of claim 1 , further comprising decomposing from a gas phase carbon, a carbon layer on the surface of the composite particle.

13. The method of claim 12 , wherein the gas phase carbon is a hydrocarbon.

14. The method of claim 12 , wherein the carbon layer is between 1 nm and 50 nm thick.

15. The method of claim 12 , wherein the carbon layer is less than 5 nm in thickness.

16. The method of claim 1 , wherein the electrochemical modifier comprises between 0.5% and 99.5% by weight of the composite particles.

17. The method of claim 1 , wherein the polymer precursor comprises a saccharide.

18. The method of claim 1 , wherein the polymer precursor comprises a lignin.

19. A method of fabricating a battery anode electrode composition comprising a silicon-carbon composite particle, the method comprising:
a. forming a porous carbon particle comprising micropores by:
i. polymerizing one or more polymer precursors to form a polymer particle having pores;
ii. pyrolyzing the polymer particle to form a carbon particle having pores; and
iii. activating the carbon particle to form the porous carbon particle; and

b. introducing the porous carbon particle to an electrochemical modifier comprising silicon,
wherein:
the one or more polymer precursors comprise a saccharide, a protein, a biopolymer, or a combination thereof; and
the electrochemical modifier comprising silicon is introduced in the vapor phase and wherein electrochemical modifier is elemental silicon incorporated within the pores of the porous carbon particle to form the silicon-carbon composite particle.

20. The method of claim 19 , wherein the battery anode electrode composition comprises a plurality of the silicon-carbon composite particles having a Dv50 of less than 1 mm and a span of 3 or less, wherein the span is defined as (Dv90−Dv10)/Dv50 where Dv10, Dv50, and Dv90 refer to particle sizes at 10%, 50%, and 90% respectively within a particle size distribution by volume of the plurality of the silicon-carbon composite.

21. The method of claim 19 , wherein the porous carbon further comprises a total pore volume of at least 0.5 cc/g.

22. The method of claim 19 , wherein the porous carbon further is electrically conductive.

23. The method of claim 19 , wherein the silicon-carbon composite particle comprises a silicon content of 0.5% and 99.5% weight percent.

24. The method of claim 19 , wherein the silicon-carbon composite particle comprises a silicon content of at least 25% to 95% weight percent.

25. The method of claim 19 , wherein the activated carbon further comprises at least 0.1 cc/g of pores with a pore size greater than 20 Angstroms.

26. The method of claim 19 , wherein the activated carbon further comprises a total of less than 500 ppm of all other elements, excluding the electrochemical modifier, having atomic numbers ranging from 11 to 92 as measured by proton induced x-ray emission.

27. The method of claim 19 , wherein the activated carbon comprises at least 0.2 cc/g of pores with a pore size less than 20 Angstroms.

28. The method of claim 19 , wherein the activated carbon comprises a peak pore volume range from 2 to 100 nm.

29. The method of claim 19 , wherein the porous carbon particle is spherical.

30. The method of claim 19 , wherein the one or more polymer precursors comprise a saccharide.

31. The method of claim 19 , wherein the one or more polymer precursors comprise a lignin.

32. The method of claim 19 , wherein the one or more polymer precursors comprise a protein.

33. The method of claim 19 , wherein the one or more polymer precursors comprise a biopolymer.

Assignees

• Group14 Technologies Inc
• Group 14 Tech Inc

Inventors

• Geramita Katharine
• Kron Benjamin E
• Costantino Henry R
• Feaver Aaron M
• Sakshaug Avery J
• Thompkins Leah A
• Chang Alan Tzu-Yang

Classifications

• C01B32/312

  Preparation · CPC title

• C01B32/30

  Active carbon · CPC title

• C08G8/22 Primary

  Resorcinol · CPC title

• C01B32/05

  Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30 · CPC title

• C01B32/336

  characterised by gaseous activating agents · CPC title