Aqueous carbon nanotube applicator liquids and methods for producing applicator liquids thereof

• US 8,771,628 B2
• Filed: 11/04/2009
• Issued: 07/08/2014
• Est. Priority Date: 12/16/2004
• Status: Active Grant

• Current Assignee: ZEON Corporation
• Original Assignee: Nantero Incorporated
• Inventors: Sivarajan, Ramesh, Rueckes, Thomas, Sen, Rahul, Segal, Brent M., Ghenciu, Eliodor G., Ward, Jonathan W., Han, Tzong-Ru T.
• Primary Examiner(s): MCCRACKEN, DANIEL
• Application Number:
  US12/612,445
• Publication Number:
  US 20100051880A1
• Time in Patent Office: 1,707 Days
• Field of Search: 4234471-4473, 423/445.B, 977742-754, 977842-848, 428/367, 252/502
• US Class Current: 423/447.1
• CPC Class Codes: B82Y 10/00 Nanotechnology for information processing, storage or transmission, e.g. quantum computing or single electron logic
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: B82Y 40/00 Manufacture or treatment of nanostructures
• CPC Class Codes: C01B 2202/02 Single-walled nanotubes
• CPC Class Codes: C01B 2202/28 Solid content in solvents
• CPC Class Codes: C01B 32/168 After-treatment
• CPC Class Codes: C01B 32/17 Purification
• CPC Class Codes: D06M 10/02 ultrasonic or sonic; Corona discharge
• CPC Class Codes: D06M 11/50 with hydrogen peroxide or peroxides of metals; with persulfuric, permanganic, pernitric, percarbonic acids or their salts
• CPC Class Codes: D06M 11/55 with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
• CPC Class Codes: D06M 11/64 with nitrogen oxides; with oxyacids of nitrogen or their salts with pernitric acids or their salts D06M11/50
• CPC Class Codes: D06M 2101/40 Fibres of carbon
• CPC Class Codes: H10K 71/12 using liquid deposition, e.g. spin coating
• CPC Class Codes: H10K 85/221 Carbon nanotubes
• CPC Class Codes: Y10S 977/746 Modified with biological, organic, or hydrocarbon material
• CPC Class Codes: Y10S 977/845 Purification or separation of fullerenes or nanotubes

Abstract

Certain applicator liquids and method of making the applicator liquids are described. The applicator liquids can be used to form nanotube films or fabrics of controlled properties. An applicator liquid for preparation of a nanotube film or fabric includes a controlled concentration of nanotubes dispersed in a liquid medium containing water. The controlled concentration is sufficient to form a nanotube fabric or film of preselected density and uniformity.

Claims

1. A method for making an applicator liquid, the method comprising:

purifying a plurality of nanotubes to obtain purified nanotubes, wherein said step of purifying is accomplished by;

contacting said plurality of nanotubes with an acid to create a nanotube-acid solution and dissolve metal impurities,

separating the dissolved metal impurities from said nanotube-acid solution to obtain said purified nanotubes in said nanotube-acid solution, and

contacting said plurality of nanotubes in the nanotube-acid solution with a base to return the pH level of the nanotube-acid solution to approximately neutral to obtain purified nanotubes; and

contacting said purified nanotubes with water;

wherein

said applicator liquid contains said purified nanotubes distributed in said water without substantial precipitation for at least one hour after said contacting;

said applicator liquid is free of polymers and surfactants; and

said applicator liquid has a group I metal impurities content of less than 100 ppb.

2. The method of claim 1, wherein said acid is a nitric acid, a hydrochloric acid, or a mixture thereof.

3. The method of claim 1, wherein said base is an ammonia hydroxide, tetramethylammonium hydroxide, alkyl ammonium bases, or combinations thereof.

4. The method of claim 1, wherein said contacting said plurality of nanotubes with a base reduces amorphous carbon impurities.

5. The method of claim 1, wherein said applicator liquid is substantially free of amorphous carbon impurities.

6. The method of claim 1, wherein said step of separating said dissolved metal impurities comprises removing said dissolved metal impurities using centrifugation.

7. The method of claim 6, wherein said centrifugation comprises ultracentrifugation, continuous flow centrifugation, or combinations thereof.

8. The method of claim 1, wherein said purifying comprises oxidizing non-fullerenic carbonaceous materials.

9. The method of claim 8, wherein said oxidizing comprises contacting said plurality of nanotubes with hydrogen peroxide.

10. The method of claim 8, wherein said plurality of nanotubes are heated in an oxygen-containing environment.

11. The method of claim 1, further comprising repeating said purifying a plurality of nanotubes.

12. The method of claim 1, wherein said contacting said purified nanotubes with water comprises grinding said purified nanotubes in water.

13. The method of claim 1, wherein said contacting said purified nanotubes with water comprising agitating said purified nanotubes in water.

14. The method of claim 1, wherein said applicator liquid contains said purified nanotubes distributed in said water at a concentration greater than or equal to 1 mg/L.

15. The method of claim 1, wherein said applicator liquid is substantially free of particulates having a diameter greater than about 500 nm.

16. The method of claim 1, wherein said purifying comprises removing impurities using gravity filtration, cross flow filtration, vacuum filtration, or combinations thereof.

17. The method of claim 1, wherein said applicator liquid has a group I metal impurities content of less than 50 ppb.

18. The method of claim 1, wherein separating said dissolved metal impurities comprises performing a cross-flow filtration process to said acid.

19. The method of claim 1, wherein said step of separating said dissolved metal impurities comprises performing a cross-flow filtration process.