IP Library Granted Patent US 6,840,999
Granted Patent B2
US 6,840,999 · App. 09/907,546 · Granted Jan 11, 2005

In situ regrowth and purification of crystalline thin films

Assignee: Board of Regents The University of Texas System
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Quick Facts
Patent No.
US 6,840,999
App. No.
09/907,546
Granted
Jan 11, 2005
Kind
B2
Abstract

Amorphous or polycrystalline films have been recrystallized into single-crystal thin films (of micrometer thickness) by a zone melting technique, in which an electrically heated wire generated a narrow heated or molten zone (0.5-2 mm wide) on the substrate sandwiched between two pieces of glass or indium-tin-oxide-coated glass. The substrate can be either an organic or inorganic compound. When the molten zone was moved slowly (3-120 μm/min) across the layer from one end of the cell to the other, a single-crystal film was produced after a single pass. This technique allows for thin film purification and an improvement in electronic, optical, and optoelectronic properties of the thin film. After this treatment, the steady-state short-circuit photocurrent can be improved by several orders of magnitude. These films are useful in the fields of optics and electronics for improving the performance in devices such as thin-film transistors and organic light-emitting diodes.

Claims (58)

1. A method for treating a single material or amorphous thin film comprising:

(a) providing a substrate coated with a single material or amorphous thin film;

(b) positioning said substrate proximal to a heat source at a distance and for a time sufficient to form a heating zone in said film, wherein said heat zone is below the decomposition temperature of said film; and

(c) moving said substrate relative to said heater source at a speed sufficient to permit formation of a heating zone in said thin film proximal to said heat source.

2. The method of claim 1 , wherein said thin film comprises an organic compound.

3. The method of claim 1 , wherein said thin film comprises an inorganic compound.

4. The method of claim 1 , wherein said substrate is passed proximal to said heat source twice.

5. The method of claim 1 , wherein said substrate is passed proximal to said heat source three times.

6. The method of claim 1 , wherein said substrate is passed proximal to said heat source four times.

7. The method of claim 1 , wherein said substrate is passed proximal to said heat source multiple times.

8. The method of claim 7 , wherein at least two different speeds are used for different passes.

9. The method of claim 1 , wherein the film is melted by said heat source.

10. A crystalline thin film produced by a method comprising:

(a) providing a substrate coated with a single material or amorphous thin film;

(b) positioning said substrate proximal to a heat source at a distance and for a time sufficient to form a heating zone in said film, wherein said heat zone is below the decomposition temperature of said film; and

(c) moving said substrate relative to said heater source at a speed sufficient to permit formation of a heating zone in said thin film proximal to said heat source.

11. A method for producing an organic crystalline thin film comprising:

(a) providing an organic compound in a sample holder, said organic compound being provided in the form of a single material or amorphous thin film;

(b) positioning said sample holder proximal to a heat source at a distance and for a time sufficient to form a molten zone in said organic compound proximal to said heater source; and

(c) moving said sample holder relative to said heater source at a speed sufficient to permit formation of a molten zone in said organic compound proximal to said heat source,

wherein said organic compound forms an organic single-crystal thin film after exposure to said heat source.

12. The method of claim 11 wherein said sample holder comprises two parallel flat surfaces.

13. The method of claim 12 , wherein said flat surfaces are glass.

14. The method of claim 13 , wherein said glass is coated with indium-tin-oxide.

15. The method of claim 12 , wherein said parallel flat surfaces are separated by about 0.1 μm to about 50 μm.

16. The method of claim 15 , wherein said parallel flat surfaces are separated by about 1.5 μm to about 2.5 μm.

17. The method of claim 10 , wherein said crystalline thin film has an enhanced steady-state short-circuit photocurrent as compared to the corresponding amorphous thin film.

18. The method of claim 17 , wherein the enhancement is an order of magnitude.

19. The method of claim 18 , where in the enhancement is two orders of magnitude.

20. The method of claim 19 , where in the enhancement is three orders of magnitude.

21. The method of claim 11 , wherein said organic single-crystal thin film contains fewer impurities than said organic compound of step (a).

22. The method of claim 11 wherein said speed is about 3 μm/min to about 120 μm/min relative to said heating source.

23. The method of claim 11 , wherein said heating source is a wire.

24. The method of claim 23 , wherein said wire is in a linear configuration.

25. The method of claim 23 , wherein said wire is about 10 μm to about 3.0 mm in diameter.

26. The method of claim 25 , wherein said wire is about 50 μm to about 2.0 mm in diameter.

27. The method of claim 23 , wherein said wire is platinum.

28. The method of claim 23 , wherein said wire is nichrome.

29. The method of claim 23 , wherein said wire is heated electrically.

30. The method of claim 23 , wherein said wire is tightened after initiation of heating.

31. The method of claim 11 , wherein said molten zone is about 0.5 mm to about 2.0 mm wide.

32. The method of claim 11 , wherein said organic compound is a porphoryin.

33. The method of claim 32 , wherein said organic compound is 1,4-bis(butylamino)-9,10-anthraquinone.

34. The method of claim 32 , wherein said organic compound is zinc(II)meso-5,10,15,20-tetrakis-n-(undecyl)porphyrin.

35. The method of claim 32 , wherein said organic compound is zinc(II)2,3,7,8,12,13,17,18-octa-n-decylporphorin.

36. The method of claim 11 , wherein said sample holder is passed proximal to said heat source twice.

37. The method of claim 11 , wherein said sample holder is passed proximal to said heat source three times.

38. The method of claim 11 , wherein said sample holder is passed proximal to said heat source four times.

39. The method of claim 11 , wherein said sample holder is passed proximal to said heat source multiple times.

40. The method of claim 39 , wherein at least two different speeds are used for different passes.

41. The method of claim 11 , wherein said thin film is prepared by evaporation onto a surface.

42. The method of claim 11 , wherein said thin film is prepared by capillary filling.

43. The method of claim 11 , wherein said thin film is prepared by deposition onto a surface.

44. The method of claim 11 , wherein said thin film is prepared by spin coating.

45. An organic crystalline thin film produced by a method comprising, said organic compound being provided in the form of a single material or amorphous thin film:

(a) providing an organic compound in a sample holder;

(b) positioning said sample holder proximal to a heat source at a distance and for a time sufficient to form a molten zone in said organic compound proximal to said heater source; and

(c) moving said sample holder relative to said heater source at a speed sufficient to permit formation of a molten zone in said organic compound proximal to said heat source.

Assignments (3)
CORRECTIVE ASSIGNMENT TO CORRECT THE FILED UNDER WRONG CONVEYANCE TYPE, SHOULD BE LICENSE PREVIOUSLY RECORDED ON REEL 020919 FRAME 0467. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT. Recorded May 30, 2008
From: THE BOARD OF REGENTS, THE UNIVERSITY OF TEXAS SYSTEM
To: INTELLECTUAL VENTURES HOLDING 40 LLC
Reel/Frame 021018/0551 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 9, 2008
From: THE BOARD OF REGENTS, THE UNIVERSITY OF TEXAS SYSTEM
To: INTELLECTUAL VENTURES HOLDING 40 LLC
Reel/Frame 020919/0467 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 8, 2002
From: LIU, CHONGYANG; BARD, ALLEN J.
To: BOARD OF REGENTS, THE UNIVERSITY OF TEXAS SYSTEM
Reel/Frame 012477/0051 →
Continuity (2)
Provisional Application 6022070100 · Jul 25, 2000
Related Publication 20020033129A1 · Mar 21, 2002