Prototyping of patterned functional nanostructures

• US 6,471,761 B2
• Filed: 04/20/2001
• Issued: 10/29/2002
• Est. Priority Date: 04/21/2000
• Status: Expired due to Term

• Current Assignee: National Technology & Engineering Solutions Of Sandia LLC (Honeywell International Inc.), New Mexico State University, UNM Rainforest Innovations (f/k/a STC.UNM) (The University of New Mexico)
• Original Assignee: Sandia National Laboratories (Government of the United States of America), The University of New Mexico
• Inventors: Lu, Yunfeng, Lopez, Gabriel P., Brinker, Charles Jeffrey, Fan, Hongyou
• Primary Examiner(s): BRUNSMAN, DAVID M
• Application Number:
  US09/838,153
• Publication Number:
  US 20020046682A1
• Time in Patent Office: 557 Days
• Field of Search: 106/287.11, 106/287.13, 106/287.14, 106/287.16, 427/256, 427/387, 101/450.1, 347/96
• US Class Current: 106/287.16
• CPC Class Codes: C08G 77/04 Polysiloxanes
• CPC Class Codes: C08G 77/26 nitrogen-containing groups
• CPC Class Codes: C08G 77/28 sulfur-containing groups
• CPC Class Codes: C09D 183/02 Polysilicates
• CPC Class Codes: C09D 183/08 containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
• CPC Class Codes: C09D 4/00 Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
• CPC Class Codes: C30B 29/605 Products containing multiple oriented crystallites, e.g. columnar crystallites
• CPC Class Codes: C30B 7/00 Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions from molten solvents C30B9/00; by normal or gradient freezing C30B11/00; under a protective fluid C30B27/00
• CPC Class Codes: C30B 7/005 Epitaxial layer growth
• CPC Class Codes: Y10T 428/31663 As siloxane, silicone or silane

Abstract

The present invention provides a coating composition comprising: A coating composition comprising: TEOS; a surfactant; at least one organosilane; HCl; water; and ethanol. The present invention also provides films made from such a coating composition and a method for making such films.

Claims

1. A coating composition comprising:

TEOS;

a surfactant;

at least one organosilane;

HCl;

water; and

ethanol.

2. The coating composition of claim 1, wherein said organosilane comprises tridecafluoro-1,1,2,2,-tetrahydrooctyltriethyoxysilane.

3. The coating composition of claim 1, wherein said organosilane comprises mercaptopropyltrimethyoxysilane.

4. The coating composition of claim 1, wherein said organosilane comprises an aminoorganosilane.

5. The coating composition of claim 1, wherein said organosilane comprises aminopropyltrimethyoxysilane.

6. The coating composition of claim 5, further comprising a dye coupled to aminopropyltrimethyoxysilane.

7. The coating composition of claim 1, wherein said organosilane comprises 3-(2,4,-dinitrophenylamino)propyltriethoxysilane.

8. The coating composition of claim 1, wherein said organosilane comprises (H₅C₂O )₃SiCH₂CH₂Si(OC₂H₅)₃.

9. The coating composition of claim 1, wherein said coating composition further comprises a dye.

10. The coating composition of claim 9, wherein said dye comprises rhodamine B.

11. The coating composition of claim 1, wherein said surfactant comprises a cationic surfactant.

12. The coating composition of claim 11, wherein said cationic surfactant comprises cetyl trimethyl ammonium bromide.

13. The coating composition of claim 1, wherein said surfactant comprises a nonionic surfactant.

14. The coating composition of claim 13, wherein said nonionic surfactant comprises polyoxyethylene cetyl ether.

15. The coating composition of claim 1, wherein said surfactant comprises an anionic surfactant.

16. The coating composition of claim 15, wherein said anionic surfactant comprises sodium dodecyl sulfate.

17. The coating composition of claim 1, wherein said coating composition comprises Si:

ethanol;

water;

HCl;

surfactant;

organosilane in a ratio of 1;

22;

5;

0.004;

0.093-0.31;

0.039-0.8.

18. The coating composition of claim 1, wherein said coating composition further comprises an organic additive.

19. The coating composition of claim 1, wherein said coating composition comprises Si:

ethanol;

water;

HCl;

surfactant;

organosilane;

organic additive in a ratio of 1;

22;

5;

0.004;

0.093-0.31;

0.039-0.8;

2.6×

10<sup>−

5</sup>.

20. The coating composition of claim 1, wherein said at least one organosilane comprises (H₅C₂O)₃SiCH₂CH₂Si(OC₂H₅)₃ said coating composition comprises Si:

EtOH;

H₂O;

HCl;

surfactant in the ratio 1;

22;

5;

0.004;

(0.054-0.18).

21. A method for forming a film comprising:

providing at least one coating composition comprising;

TEOS;

a surfactant;

at least one organosilane;

HCl;

water; and

ethanol;

applying said coating composition on a substrate to form a coating on said substrate; and

drying said coating to form a patterned silsequioxane film.

22. The method of claim 21, wherein said organosilane comprises tridecafluoro-1,1,2,2,-tetrahydrooctyltriethyoxysilane.

23. The method of claim 21, wherein said organosilane comprises mercaptopropyltrimethyoxysilane.

24. The method of claim 21, wherein said organosilane comprises an aminoorganosilane.

25. The method of claim 21, wherein said organosilane comprises aminopropyltrimethyoxysilane.

26. The method of claim 25, wherein said coating composition further comprises a dye coupled to aminopropyltrimethyoxysilane.

27. The method of claim 21, wherein said organosilane comprises 3-(2,4,-dinitrophenylamino)propyltriethoxysilane .

28. The method of claim 21, wherein said organosilane comprises (H₅C₂O)₃SiCH₂CH₂Si(OC₂H₅)₃.

29. The method of claim 21, wherein said coating composition further comprises a dye.

30. The method of claim 29, wherein said dye comprises rhodamine B.

31. The method of claim 21, wherein said surfactant comprises a cationic surfactant.

32. The method of claim 31, wherein said cationic surfactant comprises cetyl trimethyl ammonium bromide.

33. The method of claim 21, wherein said surfactant comprises a nonionic surfactant.

34. The method of claim 33, wherein said nonionic surfactant comprises polyoxyethylene cetyl ether.

35. The method of claim 21, wherein said surfactant comprises an anionic surfactant.

36. The method of claim 35, wherein said anionic surfactant comprises sodium dodecyl sulfate.

37. The method of claim 21, wherein said coating composition is coated on said substrate by dip coating.

38. The method of claim 21, wherein said coating composition is coated on said substrate by micro-pen lithography.

39. The method of claim 21, wherein said coating composition is coated on said substrate by ink jet printing.

40. The method of claim 39, wherein said at least one coating composition comprises a plurality of coating compositions and wherein each of said plurality of coating compositions is stored separately from each other prior to coating each of said plurality of coating compositions on a substrate.

41. The method of claim 21, wherein providing said coating composition comprises heating an initial composition comprising TEOS, ethanol, water and HCl at temperature of at least 60°

C. for at least 90 minutes.

42. The method of claim 41, wherein said initial composition contains TEOS, ethanol, water and HCl in the mole ratio of 1:

3.7;

1;

5×

10<sup>−

5</sup>.

43. The method of claim 41, wherein providing said coating composition further comprises diluting said initial composition with ethanol to provide an ethanol-diluted composition.

44. The method of claim 43, wherein said initial composition is diluted with 2 volumes of ethanol for every 1 volume of initial composition.

51. The method of claim 21, wherein said coating composition comprises Si:

ethanol;

water;

HCl;

surfactant;

organosilane in a ratio of 1;

22;

5;

0.004;

0.093-0.31;

0.039-0.8.

53. The method of claim 21 wherein said coating is dried at a temperature of 25°

C. to 100°

C.

54. The method of claim 21, further comprising removing substantially all of said surfactant from said film.

55. The method of claim 54, wherein said surfactant is removed by heating said thin film at a temperature of at least 300°

C.

56. The method of claim 21, further comprising vapor-treating said film with hexamethyldisilazane.

57. The method of claim 21, wherein said film has a thickness of 50 nm-1 μ

m.

58. The method of claim 21, wherein said film is mesoporous.

45. The method of 43, wherein providing said coating composition further comprises diluting said ethanol-diluted composition with water and HCl to provide an acidic sol.

46. The method of claim 45, wherein providing said coating composition further comprises adding said at least one organosilane to said acidic sol to form proto-composition.

47. The method of claim 46, wherein providing said coating composition further comprises adding said surfactant to said proto-composition to form said coating composition.

48. The method of claim 47, wherein said surfactant is present in said coating composition at a concentration of 0.04 to 0.23 M.

49. The method of claim 48, wherein providing said coating composition further comprises adding at least one organic additive to said acid sol.

50. The method of claim 49, wherein said coating composition comprises Si:

ethanol;

water;

HCl;

surfactant;

organosilane;

organic additive in a ratio of 1;

22;

5;

0.004;

0.093-0.31;

0.039-0.8;

2.6×

10<sup>−

5</sup>.

52. The method of 21, wherein said at least one organosilane comprises (H₅C₂O)₃SiCH₂CH₂Si(OC₂H₅)₃ and said coating composition comprises Si:

EtOH;

H₂O;

HCl;

surfactant in the ratio 1;

22;

5;

0.004;

(0.054-0.18).