IP Library Granted Patent US 12,534,369
Granted Patent B2
US 12,534,369 · App. 18/369,933 · Granted Jan 27, 2026

Method of preparing carbon nanomaterials

Inventors: Michael Kwabena Opoku (San Marcos, TX); Gary W. Beall (New Braunfels, TX)
C01B32/15B82Y30/00B82Y40/00C01P2004/64C01P2006/12C01P2006/14
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Quick Facts
Patent No.
US 12,534,369
App. No.
18/369,933
Granted
Jan 27, 2026
Kind
B2
Abstract

This disclosure relates generally to the field of carbon, graphene, energy storage materials, carbon films, and nanocomposites. Specifically, this disclosure relates to novel eco-friendly, cost-effective methods of preparing doped and/or intercalated carbon nanomaterials.

Claims (32)

1 . A process for preparing a carbon nanomaterial, wherein the carbon nanomaterial is doped and/or intercalated, the process comprising:

providing a carbon-containing material to a reactor comprising a solvent;

providing one or more of: an oxidizing or reducing solution, and a doping and/or intercalating agent to the reactor comprising the carbon-containing material to obtain a reaction mixture,

heating the reaction mixture to a temperature and for a time period sufficient to obtain an intermediate material;

further comprising contacting the intermediate material with one or more of hydrazine, lithium aluminum hydride, diborane, and sodium borohydride prior to further heating; and

further heating the intermediate material to a temperature and for a time period sufficient to obtain the carbon nanomaterial.

2 . The process of claim 1 , wherein the carbon nanomaterial is Li-, Na-, O-, P-, K-, and/or Si-doped.

3 . The process of claim 1 , wherein the carbon nanomaterial is in a form of a particulate, porous foam, film, or pellet, or is dispersed in a solvent.

4 . The process of claim 1 , wherein the carbon-containing material comprises carbon nanosheet, graphene, fullerene, amorphous carbon, graphene oxide, carbon black, activated carbon, charcoal, carbon nanotubes, graphite, coal, or a combination of two or more thereof.

5 . The process of claim 1 , wherein said carbon-containing material is or is derived from the group consisting of cassava root, tapioca flour, yam root, potato root, sugarcane, sugar beet, sucrose, rice grain, corn, and wheat grain.

6 . The process of claim 1 , wherein the solvent is distilled water, deionized water, ethanol, N-methyl-2-pyrrolidone, ethylene glycol, propylene glycol, or a combination thereof.

7 . The process of claim 1 , wherein the oxidizing or reducing solution is selected from one or more of: sodium hydroxide, potassium hydroxide, hydrochloric acid, phosphoric acid, phosphorous acid, and nitric acid.

8 . The process of claim 1 , wherein the doping and/or intercalating agent selected from lithium chloride, 3,4-dihydroxybenzonitrile dilithium, lithium hydroxide, lithium acetate, lithium citrate, lithium bis(trifluoromethylsulfonyl)imide, lithium hexafluorophosphate, aluminium triacetate, calcium hydroxide, magnesium acetate, silicon oxide, and a combination of two or more thereof.

9 . The process of claim 1 , wherein the doping and/or intercalating agent is lithium acetate or silicon oxide.

10 . The process of claim 1 , wherein the temperature sufficient to obtain the intermediate material is in a range of about 45 to 1050° C., and the temperature sufficient to obtain the carbon nanomaterial is in a range of about 500 to 1500° C.

11 . A process for preparing a carbon nanomaterial, wherein the carbon nanomaterial is doped and/or intercalated, the process comprising:

providing a carbon-containing material to a reactor comprising a solvent;

providing one or more of: an oxidizing or reducing solution, and a doping and/or intercalating agent to the reactor comprising the carbon-containing material to obtain a reaction mixture, heating the reaction mixture to a temperature and for a time period sufficient to obtain an intermediate material;

washing the carbon nanomaterial with hydrogen peroxide or hydrochloric acid to obtain a washed carbon nanomaterial;

rising the washed carbon nanomaterial with distilled or deionized water to obtain a rinsed carbon nanomaterial; and

heating the rinsed carbon nanomaterial in an third gas at a temperature in a range of about 700 to 1500° C. to obtain the carbon nanomaterial having a BET surface area of at least 1900 m 2 /g and pore volume of at least 2.4 cm 3 /g.

12 . The process of claim 11 , further comprising contacting the intermediate material with one or more of hydrazine, lithium aluminum hydride, diborane, and sodium borohydride prior to further heating.

13 . A process for preparing a carbon nanomaterial film, wherein the carbon nanomaterial is doped and/or intercalated, the process comprising:

performing the process of claim 1 to provide a carbon nanomaterial;

providing the carbon nanomaterial and one or more of additives selected from a conductive agent, binder, and thickening agent, to a second solvent to obtain the slurry of the carbon nanomaterial;

coating a surface of a substrate with the slurry to obtain a coated substrate; and

heating the coated substrate to a temperature and for a time period sufficient to obtain the carbon nanomaterial film.

14 . The process of claim 13 , wherein the temperature sufficient to obtain the film is in a range of about 25 to 150° C.

15 . A process for preparing a nanocomposite comprising a carbon nanomaterial, wherein the carbon nanomaterial is doped and/or intercalated, the process comprising:

performing the process of claim 1 to provide a carbon nanomaterial; and

providing the carbon nanomaterial to a polymer to obtain the nanocomposite.

16 . The process of claim 15 , wherein the carbon nanomaterial is provided in an amount sufficient to increase one or more of mechanical, absorption, adsorption, electrical, electronic, magnetic, and optical properties of the nanocomposite by at least a factor greater than 1 compared to the same properties of the polymer.

Continuity (3)
Continuation 17164770 · Feb 1, 2021
Provisional Application 62968958 · Jan 31, 2020
Related Publication 20240158236A1 · May 16, 2024
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