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

• US 7,666,382 B2
• Filed: 12/15/2005
• Issued: 02/23/2010
• Est. Priority Date: 12/16/2004
• Status: Active Grant

• Current Assignee: ZEON Corporation
• Original Assignee: Nantero Incorporated
• Inventors: Han, Tzong-Ru Terry, Ghenciu, Eliodor G., Ward, Jonathan W., Sivarajan, Ramesh, Segal, Brent M., Rueckes, Thomas, Sen, Rahul
• Primary Examiner(s): Silverman; Stanley S.
• Assistant Examiner(s): MCCRACKEN, DANIEL
• Application Number:
  US11/304,315
• Publication Number:
  US 20060204427A1
• Time in Patent Office: 1,531 Days
• Field of Search: 423/447.1, 423/447.2, 423/447.3, 423/460, 423/461, 252/500, 252/502, 977/845, 977/847
• 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. An applicator liquid comprising:

one or more carbon nanotubes and

an electronics-grade liquid medium comprising water,

wherein the carbon nanotubes are distributed in the liquid medium without substantial precipitation, flocculation or other macroscopic interaction and can remain separated for about at least one week,

wherein the nanotubes are at a concentration of greater than or equal to 10 mg/L,

wherein the nanotubes are pretreated to reduce a level of metal impurities to less than about 1×

10¹⁸ atoms/cm³,

wherein the applicator liquid is substantially free of polymers and surfactants, and

wherein the applicator liquid is substantially free of particulates having a diameter greater than about 500 nm.

2. The applicator liquid of claim 1, wherein the applicator liquid meets or exceeds specifications for use in class 1 semiconductor fabrication facility.

3. The applicator liquid of claim 1, wherein the applicator liquid is substantially free of metallic impurities.

4. The applicator liquid of claim 1, wherein the applicator liquid is substantially free of amorphous carbon impurities.

5. The applicator liquid of claim 1, wherein the applicator liquid comprises less than 500 parts per billion of metallic impurities.

6. The applicator liquid of claim 1, wherein the applicator liquid comprises less than 200 parts per billion of metallic impurities.

7. The applicator liquid of claim 1, wherein the applicator liquid comprises less than 50 parts per billion of metal impurities.

8. The applicator liquid of claim 1, wherein the applicator liquid comprises less than 500 parts per billion of heavy metal impurities.

9. The applicator liquid of claim 1, wherein the applicator liquid comprises from 0.1 to 10 parts per billion of heavy metal impurities.

10. The applicator liquid of claim 1, wherein the applicator liquid comprises less than 500 parts per billion of alkali (group I element) and alkaline earth (group II element) impurities.

11. The applicator liquid of claim 1, wherein the applicator liquid comprises from 1 to 25 parts per billion of alkali (group I element) and alkaline earth (group II element) impurities.

12. The applicator liquid of claim 1, wherein the applicator liquid comprises less than 500 parts per billion of transition metal impurities.

13. The applicator liquid of claim 1, wherein the applicator liquid comprises from 0.1 to 10 parts per billion of transition metal impurities.

14. The applicator liquid of claim 1, wherein the applicator liquid is substantially free of particle impurities having a diameter of greater than about 300 nm.

15. The applicator liquid of claim 1, wherein the applicator liquid is substantially free of particle impurities having a diameter of greater than about 45 nm.

16. The applicator liquid of claim 1, wherein the carbon nanotubes comprise conductive nanotubes.

17. The applicator liquid of claim 1, wherein the carbon nanotubes comprise semiconductive nanotubes.

18. The applicator liquid of claim 1, wherein the carbon nanotubes comprise single-walled carbon nanotubes.

19. The applicator liquid of claim 1, wherein the carbon nanotubes comprise multi-walled carbon nanotubes.

20. The applicator liquid of claim 1, wherein the applicator liquid comprise nanotubes at a concentration of greater than 100 mg/L.

21. The applicator liquid of claim 1, wherein the applicator liquid comprise nanotubes at a concentration of greater than 1000 mg/L.

22. A method for making the applicator liquid of claim 1, the method comprising:

a) contacting one or more carbon nanotubes with a liquid medium comprising water to obtain a mixture; and

b) removing impurities from the carbon nanotubes to obtain the applicator liquid,

wherein the applicator liquid meets or exceeds specifications for use in class 1 semiconductor fabrication facility.

23. The method of claim 22, wherein the applicator liquid is purified to comprise less than 500 parts per billion of metallic impurities.

24. The method of claim 22, wherein the applicator liquid is purified to comprise less than 200 parts per billion of metallic impurities.

25. The method of claim 22, wherein the applicator liquid is purified to comprise less than 50 parts per billion of metal impurities.

26. The method of claim 22, wherein the applicator liquid is purified to comprise less than 500 parts per billion of heavy metal impurities.

27. The method of claim 22, wherein the applicator liquid is purified to comprise from 0.1 to 10 parts per billion of heavy metal impurities.

28. The method of claim 22, wherein the applicator liquid is purified to comprise less than 500 parts per billion of alkali (group I element) and alkaline earth (group II element) impurities.

29. The method of claim 22, wherein the applicator liquid is purified to comprise from 1 to 25 parts per billion of alkali (group I element) and alkaline earth (group II element) impurities.

30. The method of claim 22, wherein the applicator liquid is purified to comprise less than 500 parts per billion of transition metal impurities.

31. The method of claim 22, wherein the applicator liquid is purified to comprise from 0.1 to 10 parts per billion of transition metal impurities.

32. The method of claim 22, wherein the applicator liquid is substantially free of particle impurities having a diameter of greater than about 300 nm.

33. The method of claim 22, wherein the applicator liquid is substantially free of particle impurities having a diameter of greater than about 45 nm.

34. The method of claim 22, wherein the carbon nanotubes comprise conductive nanotubes.

35. The method of claim 22, wherein the carbon nanotubes comprise semiconductive nanotubes.

36. The method of claim 22, wherein the carbon nanotubes comprise single-walled carbon nanotubes.

37. The method of claim 22, wherein the carbon nanotubes comprise multi-walled carbon nanotubes.

38. The method of claim 22, wherein the applicator liquid comprise nanotubes at a concentration of greater than 100 mg/L.

39. The method of claim 22, wherein the applicator liquid comprise nanotubes at a concentration of greater than 1000 mg/L.

40. The method of claim 22, wherein step b) comprises performing a filtration process.

41. The method of claim 40, wherein the filtration process is a cross-flow filtration process.

42. The method of claim 22, wherein step b) comprises performing a centrifugation process.

43. The method of claim 42, wherein the centrifugation process comprises a continuous flow centrifugation.

44. The method of claim 22, wherein step b) is carried after or simultaneously with step a).

45. The method of claim 44, wherein step b) comprises performing a sonication process.

46. The method of claim 44, wherein step b) comprises contacting the carbon nanotubes with an acid.

47. The method of claim 46, wherein step b) comprises contacting the mixture with a base.

48. The method of claim 47, wherein base is added to substantially neutralize the mixture.

49. A method for making the applicator liquid of claim 1:

a) contacting one or more carbon nanotubes with a liquid medium comprising water and an acid to obtain a mixture;

b) contacting the mixture with a base; and

c) removing soluble and particulate impurities,

wherein the applicator liquid meets or exceeds specifications for use in class 1 semiconductor fabrication facility.

50. The method of claim 49, wherein the base is added to neutralize the mixture.

51. The method of claim 49, wherein step a) comprises performing a sonciation process.

52. The method of claim 49, wherein step c) comprises performing a centrifugation process.

53. The method of claim 49, wherein step c) comprises performing a filtration process.