Coated fullerenes, composites and dielectrics made therefrom

• US 8,062,702 B2
• Filed: 11/20/2002
• Issued: 11/22/2011
• Est. Priority Date: 11/20/2001
• Status: Expired due to Fees

• Current Assignee: NewCyte, Inc. (Natcore Technology, Inc.), Rice University
• Original Assignee: Natcore Technology, Inc., Rice University
• Inventors: Whitsitt, Elizabeth, Barron, Andrew R., Flood, Dennis J.
• Primary Examiner(s): Cleveland; Michael
• Assistant Examiner(s): VETERE, ROBERT A
• Application Number:
  US10/496,066
• Publication Number:
  US 20050089684A1
• Time in Patent Office: 3,289 Days
• Field of Search: 427/213
• US Class Current: 427/213
• 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 2202/06 Multi-walled nanotubes
• CPC Class Codes: C01B 2202/28 Solid content in solvents
• CPC Class Codes: C01B 32/156 After-treatment
• CPC Class Codes: C01B 32/168 After-treatment
• CPC Class Codes: C01B 32/174 Derivatisation; Solubilisation; Dispersion in solvents
• CPC Class Codes: C01P 2002/54 one element only
• CPC Class Codes: C01P 2004/03 obtained by SEM
• CPC Class Codes: C01P 2004/04 obtained by TEM, STEM, STM or AFM
• CPC Class Codes: C01P 2004/12 with a cylindrical shape
• CPC Class Codes: C01P 2004/13 Nanotubes
• CPC Class Codes: C01P 2004/32 Spheres
• CPC Class Codes: C01P 2004/84 one phase coated with the other
• CPC Class Codes: C01P 2006/40 Electric properties
• CPC Class Codes: C04B 2235/5288 Carbon nanotubes
• CPC Class Codes: C04B 35/62807 Silica or silicates
• CPC Class Codes: C08K 9/02 Ingredients treated with inorganic substances
• CPC Class Codes: C09C 1/3045 : Treatment with inorganic compounds
• CPC Class Codes: C09C 1/44 : Carbon
• CPC Class Codes: H01L 21/76838 : characterised by the formation and the after-treatment of the conductors etching for patterning the conductors H01L21/3213
• CPC Class Codes: H01L 23/53276 : containing carbon, e.g. fullerenes superconducting fullerenes H10N60/853
• CPC Class Codes: H01L 2924/00 : Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
• CPC Class Codes: H01L 2924/0002 : Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
• CPC Class Codes: H10K 85/211 : Fullerenes, e.g. C60
• CPC Class Codes: H10K 85/221 : Carbon nanotubes
• CPC Class Codes: H10K 85/615 : Polycyclic condensed aromatic hydrocarbons, e.g. anthracene
• CPC Class Codes: Y10T 428/30 : Self-sustaining carbon mass or layer with impregnant or other layer

Abstract

The present invention relates to coated fullerenes comprising a layer of at least one inorganic material covering at least a portion of at least one surface of a fullerene and methods for making. The present invention further relates to composites comprising the coated fullerenes of the present invention and further comprising polymers, ceramics and/or inorganic oxides. A coated fullerene interconnect device wherein at least two fullerenes are contacting each other to form a spontaneous interconnect is also disclosed as well as methods of making. In addition, dielectric films comprising the coated fullerenes of the present invention and methods of making are further disclosed.

Claims

1. A method for making a coated fullerene, said method comprising:

(a) dispersing a fullerene in a solvent to provide a solution comprising a dispersed fullerene that is soluble in the solvent; and

(b) depositing a layer of at least one inorganic oxide from the solution onto at least a portion of at least one surface of the dispersed fullerene at a rate equal to or greater than 10 nm/hour,

wherein depositing comprises utilizing a liquid phase deposition technique that is not a sol-gel process.

2. The method according to claim 1, wherein the fullerene is selected from the group consisting of C₆₀, C₇₂, C₈₄, C₉₆, C₁₀₈, C₁₂₀, single-walled carbon nanotubes (SWNT) and multi-walled nanotubes (MWNT).

3. The method according to claim 2, wherein the fullerene is C₆₀.

4. The method according to claim 2, wherein the fullerene is single walled carbon nanotubes (SWNT).

5. The method according to claim 4, wherein the single walled carbon nanotubes (SWNT) are present in the form of an aggregate or individual tubes.

6. The method according to claim 5, wherein the aggregate is a rope or bundle.

7. The method according to claim 5, wherein the fullerene is an individual SWNT.

8. The method according to claim 1, wherein the inorganic oxide is an oxide of silicon.

9. The method according to claim 1, wherein the solvent is water.

10. The method according to claim 1, wherein the fullerene is dispersed by a technique of chemical functionalization or surfactant addition.

11. The method according to claim 10, wherein the fullerene is dispersed by a technique of chemical functionalization.

12. The method according to claim 11, wherein the technique of chemical functionalization comprises hydroxylation of the surface of the fullerene.

13. The method according to claim 10, wherein the fullerene is dispersed by a technique of surfactant addition.

14. The method according to claim 13, wherein the fullerene is single-walled carbon nanotubes (SWNT).

15. The method according to claim 14, wherein the technique of surfactant addition comprises the addition of sodium dodecylsulfate (SDS) to the solvent.

16. The method according to claim 14, wherein the technique of surfactant addition comprises the addition of dodecyltrimethyl ammonium bromide to the solvent.

17. The method according to claim 1, wherein the solution further comprises silica.

18. The method according to claim 17, wherein the silica is at least partially dissolved in the solution.

19. The method according to claim 17, wherein the solution further comprises H₂SiF₆.

20. The method according to claim 1, further comprising:

isolating the coated fullerene.

21. The method according to claim 20, wherein isolating the coated fullerene comprises using any technique of centrifugation.

22. The method according to claim 20, further comprising:

redispersing the coated fullerene in a solvent to produce a redispersed coated fullerene.

23. The method according to claim 22, further comprising:

isolating the redispersed coated fullerene.

24. The method according to claim 1, wherein the inorganic oxide is an insulating material.

25. The method according to claim 1, further comprising:

isolating the coated fullerene at equal to or less than 12 hours after depositing the at least one inorganic oxide.

26. The method according to claim 1, wherein depositing the layer of at least one inorganic oxide comprises growing the at least one inorganic oxide on the at least one surface of the dispersed fullerene;

wherein growth of the at least one inorganic oxide initiates at a plurality of nucleation sites on the surface of the dispersed fullerene.

27. The method according to claim 1, wherein depositing the layer of at least one inorganic oxide comprises contacting the dispersed fullerenes with a solution comprising the inorganic oxide to initiate growth thereof.

28. A method for making a coated fullerene, said method comprising:

activating at least a surface portion of a fullerene to form an activated region on the fullerene; and

growing an inorganic oxide on the activated region so as to at least partially coat the fullerene with the inorganic oxide;

wherein growing the inorganic oxide takes place at a rate equal to or greater than 10 nm/hour by a process comprising a liquid phase deposition technique that is not a sol-gel process.

29. The method according to claim 28, wherein the activated region comprises one or more nucleation sites for growth of the inorganic oxide.

30. The method according to claim 29, wherein the one or more nucleation sites are formed by hydroxylating at least a surface portion of the fullerene.

31. The method according to claim 29, wherein growing the inorganic oxide on the activated region comprises growing one or more layers of the inorganic oxide on the surface of the dispersed fullerene;

wherein growth of the one or more layers of the inorganic oxide initiates at the one or more nucleation sites on the surface of the dispersed fullerene.

32. The method according to claim 31, wherein growing one or more layers of inorganic oxide takes place by a condensation reaction.

33. The method according to claim 28, wherein the fullerene is an individual carbon nanotube.

34. The method according to claim 28, wherein the inorganic oxide comprises silica.

35. A method for coating a fullerene with an inorganic oxide, said method comprising:

dispersing a fullerene in a solvent;

chemically functionalizing at least a surface portion of the fullerene to form a functionalized surface portion on the fullerene; and

growing an inorganic oxide on the functionalized surface portion at a rate of equal to or greater than 10 nm/hour by a process comprising a liquid phase deposition technique that is not a sol-gel process.

36. The method according to claim 35, wherein chemically functionalizing at least a surface portion of the fullerene comprises reacting the surface portion of the fullerene with one or more reagents to generate at least one nucleation site for growth of the inorganic oxide.

37. The method according to claim 36, wherein reacting the surface portion of the fullerene to generate at least one nucleation site comprises hydroxylating at least a surface portion of the fullerene.

38. The method according to claim 35, further comprising:

adding a surfactant to the solvent to disperse the fullerene therein.

39. The method according to claim 38, wherein the surfactant is selected from the group consisting of sodium dodecylsulfate (SDS) and dodecyltrimethyl ammonium bromide.

40. The method according to claim 35, wherein growing the inorganic oxide comprises contacting the fullerene with a solution comprising silica.

41. The method according to claim 35, wherein growing is quenched when a desired thickness of the inorganic oxide is achieved.

42. The method according to claim 35, wherein the fullerene is an individual carbon nanotube.

43. The method according to claim 35, wherein the fullerene exhibits characteristic bands in the Raman spectra indicative of individual tubes.