Low pressure vapor phase deposition of organic thin films

• US 6,337,102 B1
• Filed: 11/17/1997
• Issued: 01/08/2002
• Est. Priority Date: 11/17/1997
• Status: Expired due to Term

• Current Assignee: The Trustees of Princeton University (Princeton University)
• Original Assignee: The Trustees of Princeton University (Princeton University)
• Inventors: Burrows, Paul E., Forrest, Stephen R., Ban, Vladimir S.
• Primary Examiner(s): MEEKS, TIMOTHY HOWARD
• Application Number:
  US08/972,156
• Time in Patent Office: 1,513 Days
• Field of Search: 427/64, 427/66, 427/255.1, 427/255.6, 427/255.5, 427/255.23, 117/925, 117/927
• US Class Current: 427/64
• CPC Class Codes: C23C 14/12 Organic material
• CPC Class Codes: C23C 14/50 Substrate holders
• CPC Class Codes: C23C 14/54 Controlling or regulating the coating process
• CPC Class Codes: C23C 14/568 Transferring the substrates through a series of coating stations C23C14/562 takes precedence
• CPC Class Codes: C23C 16/30 Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
• CPC Class Codes: C23C 16/45561 Gas plumbing upstream of the reaction chamber
• CPC Class Codes: H10K 71/00 Manufacture or treatment specially adapted for the organic devices covered by this subclass
• CPC Class Codes: H10K 71/10 Deposition of organic active material
• CPC Class Codes: H10K 71/164 using vacuum deposition
• CPC Class Codes: H10K 71/40 Thermal treatment, e.g. annealing in the presence of a solvent vapour
• CPC Class Codes: H10K 85/324 comprising aluminium, e.g. Alq3
• CPC Class Codes: H10K 85/631 Amine compounds having at least two aryl rest on at least one amine-nitrogen atom, e.g. triphenylamine

Abstract

Methods for preparing organic thin films on substrates, the method comprising the steps of providing a plurality of organic precursors in the vapor phase, and reacting the plurality or organic precursors at a sub-atmospheric pressure. Also included are thin films made by such a method and apparatuses used to conduct such a method. The method is well-suited to the formation of organic light emitting devices and other display-related technologies.

Claims

1. A method for fabricating organic films comprising:

providing a first carrier gas stream;

volatilizing a first organic small molecule material into the first carrier gas stream;

passing the first carrier gas stream through an apparatus;

maintaining the wall temperature of the apparatus at a sufficiently high temperature to avoid condensation of the volatilized first organic small molecule material;

passing the first carrier gas stream at a pressure of about 0.001 torr to about 100 torr over a substrate; and

depositing said first organic small molecule material on said substrate so as to form a first film comprising the first organic small molecule material on said substrate.

2. The method of claim 1, wherein said pressure is from about 0.1 torr to about 10 torr.

3. The method of claim 1, wherein said wherein said carrier gas is selected from the group consisting of nitrogen, argon, helium, neon, krypton and xenon.

4. The method of claim 1, wherein said first organic small molecule material is selected from the group consisting of tris(8-quinoline)aluminum;

N,N′

-diphenyl-N-N′

-bis(3-methylphenyl)-1,1′

-bisphenyl-4,4′

-diamine;

α

-4,4′

-bis[N-(1-naphthyl)-N-phenyl-amino]biphenyl;

4,4′

,4″

-tris[N-(3-methylphenyl)-N-phenylamino]triphenylamine; and

bis-(8-hydroxyquinoline)aluminum oxyphenyl.

5. The method of claim 1, wherein the first film comprises N,N′

-diphenyl-N-N′

-bis(3-methylphenyl)-1,1′

-bisphenyl-4,4′

-diamine.

6. The method of claim 1, wherein said method further comprises:

volatilizing a second organic small molecule material into a second carrier gas stream; and

combining the second carrier gas stream with the first carrier gas stream;

wherein said depositing includes depositing said second organic small molecule material along with said first organic small molecule material on said substrate such that said first film comprises the first organic small molecule material and the second organic small molecule material.

7. The method of claim 6, wherein said pressure is from about 0.1 torr to about 10 torr.

8. The method of claim 6, wherein the first film is incorporated into an organic light emitting device.

9. The method of claim 1 wherein said method further comprises:

volatilizing a third organic small molecule material into a third carrier gas stream;

passing the third carrier gas stream at a pressure of about 0.001 torr to about 100 torr over the first film; and

depositing said third organic small molecule material over said first film so as to form a second film comprising the third organic small molecule material over said first film.

10. The method of claim 9, wherein said pressure of the third carrier gas stream is from about 0.1 torr to about 10 torr.

11. The method of claim 9, wherein said first and second films are incorporated into an organic light emitting device.

12. The method of claim 9, wherein the second film comprises tris(8-quinoline)aluminun.

13. The method of claim 1, wherein said first film comprises Alq₃ having an RMS surface roughness of from 9 to 11 angstroms.

14. The method of claim 1, wherein said first film comprises TPD having an RMS surface roughness of from 6 to 8 angstroms.

15. A method for fabricating organic films comprising:

providing a first carrier gas stream comprising one or more volatilized first organic small molecule materials;

passing the first carrier gas stream through a first apparatus;

maintaining the wall temperature of the first apparatus at a sufficiently high temperature to avoid condensation of the one or more volatilized first organic small molecule materials;

exposing the first carrier gas stream at a pressure of about 0.001 torr to about 100 torr to a substrate;

depositing the one or more volatilized first organic small molecule materials on said substrate so as to form a first film on said substrate, said first film comprising the one or more first organic small molecule materials;

providing a second carrier gas stream comprising one or more volatilized second organic small molecule materials;

passing the second carrier gas stream through a second apparatus;

maintaining the wall temperature of the second apparatus at a sufficiently high temperature to avoid condensation of the one or more volatilized second organic small molecule materials;

exposing the second carrier gas stream at a pressure of about 0.001 torr to about 100 torr to said first film on said substrate; and

depositing the one or more volatilized second organic small molecule materials on said first film so as to form a second film on said first film on said substrate, said second film comprising said one or more second organic small molecule materials.

16. The method of claim 15, wherein said one or more first organic small molecule materials comprise a single first organic small molecule material.

17. The method of claim 15, wherein said one or more first organic small molecule materials comprise two or more first organic small molecule materials.

18. The method of claim 15, wherein said one or more second organic small molecule materials comprise a single second organic small molecule material.

19. The method of claim 15, wherein said one or more second organic small molecule materials comprise two or more second organic small molecule materials.

20. The method of claim 15, wherein said first and second films are incorporated into an organic light emitting device.

21. The method of claim 20, wherein one of said first and second films is a light emitting layer.

22. The method of claim 21, wherein said light emitting layer comprises tris(8-quinoline)aluminum.

23. The method of claim 20, wherein one of said first and second films is a hole transporting layer.

24. The method of claim 23, wherein said hole transporting layer comprises N,N′

-diphenyl-N-N′

-bis(3-methylphenyl)-1,1′

-bisphenyl-4,4′

-diamine.

25. The method of claim 20, wherein one of said first and second films is a light emitting layer and the other of said first and second films is a hole transporting layer.

26. The method of claim 25, wherein said light emitting layer comprises tris(8-quinoline)aluminum and said hole transporting layer comprises N,N′

-diphenyl-N-N′

-bis(3-methylphenyl)-1,1′

-bisphenyl-4,4′

-diamine.

27. The method of claim 15, wherein said substrate comprises a polymer film material, a glass material or a semiconductor material.

28. The method of claim 15, wherein said substrate comprises a layer of indium tin oxide.

29. The method of claim 28, wherein said substrate is polyester coated with indium tin oxide.

30. A method for fabricating organic films comprising:

providing a carrier gas stream comprising one or more volatilized first organic small molecule materials;

exposing the carrier gas stream at a pressure of about 0.001 torr to about 100 torr to a substrate; and

depositing the one or more volatilized first organic small molecule materials on said substrate so as to form a first film on said substrate, said first film comprising the one or more first organic small molecule materials;

wherein said carrier gas stream is passed through an apparatus in which inside walls of said apparatus are sufficiently elevated to prevent condensation of the one or more first organic small molecule materials before the depositing step.

31. The method of claim 30, wherein said film is a light emitting layer.

32. The method of claim 31, wherein said film comprises a single first organic small molecule material.

33. The method of claim 31, wherein said film comprises two or more first organic small molecule materials.

34. The method of claim 31, wherein said pressure is from about 0.1 torr to about 10 torr.

35. The method of claim 31, wherein said pressure is from about 0.001 torr to about 0.1 torr.

36. The method of claim 31, wherein said pressure is from about 0.001 torr to about 10 torr.

37. The method of claim 31, wherein said pressure is from about 0.1 torr to about 100 torr.

38. The method of claim 36, wherein said pressure is from about 10 torr to about 100 torr.

39. The method of claim 31, wherein said substrate is cooled.

40. The method of claim 31, wherein said substrate comprises a polymer film material, a glass material or a semiconductor material.

41. The method of claim 31, wherein said substrate comprises a layer of indium tin oxide.

42. The method of claim 31, wherein said substrate is polyester coated with indium tin oxide.

43. The method of claim 31, wherein said substrate is polyester coated with indium tin oxide, which is further coated with a hole transporting layer.