Low pressure vapor phase deposition of organic thin films

• US 20010002279A1
• Filed: 12/13/2000
• Published: 05/31/2001
• Est. Priority Date: 11/17/1997
• Status: Abandoned Application

• Current Assignee: Paul E. Burrows, Stephen R. Forrest, Vladimir S. Ban
• Original Assignee: Paul E. Burrows, Stephen R. Forrest, Vladimir S. Ban
• Inventors: Burrows, Paul E., Forrest, Stephen R., Ban, Vladimir S.
• Application Number:
  US09/736,090
• Publication Number:
  US 20010002279A1
• Time in Patent Office: Days
• US Class Current: 427/255.26
• 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 preparing an organic thin film on a substrate, said method comprising the steps of:

providing a plurality of organic precursors, said organic precursors being in the vapor phase; and

reacting said plurality of organic precursors at a sub-atmospheric pressure in the presence of said substrate to form said thin film on said substrate.

2. The method of

claim 1

, wherein said substrate is located in a reaction chamber.

3. The method of

claim 2

, further comprising the step of transporting one of said plurality of organic precursors into said reaction chamber prior to said step of reacting.

4. The method of

claim 3

, wherein said step of transporting includes the step of using an inert gas to carry said transported organic precursor into said reaction chamber.

5. The method of

claim 4

, wherein said inert gas is selected from the group consisting of nitrogen, argon, helium, neon, krypton and xenon.

6. The method of

claim 1

, wherein at least one of said plurality of organic precursors is selected from the group consisting of MT, DASI, MM, M_fM, DASTh, MeOSI, DAS(Et)I, DAS(Et)OH, acetyl toluenesulfonate, MA_f, TTF, TCNQ, DCM, Alq₃, TPP, TPD, α

-NPD, MTDATA, and (Alq₂)′

-OPh.

7. The method of

claim 3

, further comprising the step of volatilizing said transported organic precursor prior to said step of transporting.

8. The method of

claim 7

, wherein:

said step of volatilizing includes the step of loading said transported organic precursor into a bubbler; and

said step of transporting includes the step of passing an inert gas through said bubbler for carrying said transported organic precursor into said reaction chamber.

9. The method of

claim 7

, wherein:

said step of volatilizing includes the steps of placing said transported organic precursor into an open container and heating said open container; and

said step of transporting includes the step of passing an inert gas over said open container for carrying said transported organic precursor into said reaction chamber.

10. The method of

claim 7

, wherein said step of volatilizing includes the steps of:

loading said transported organic precursor into a Knudsen cell, said Knudsen cell extending into said reaction chamber; and

heating said Knudsen cell.

11. The method of

claim 1

, wherein the substrate is mounted to a rotating sample holder.

12. The method of

claim 1

, wherein said sub-atmospheric pressure is within the range of about 10⁻

11-10² torr.

13. An organic film produced by the method of

claim 1

.

14. The organic film of

claim 13

, wherein said film comprises a light emitting material.

15. The organic film of

claim 13

, wherein said film comprises an optically non-linear material.

16. An apparatus for preparing an organic thin film on a substrate, said apparatus comprising:

a reaction chamber;

a heater substantially surrounding said reaction chamber;

tubing extending into said reaction chamber; and

a vacuum pump attached to said reaction chamber.

17. The apparatus of

claim 16

, wherein said reaction chamber comprises a reactor tube.

18. The apparatus of

claim 16

, wherein said heater is a multi-zone heater/cooler.

19. The apparatus of

claim 16

, wherein said tubing comprises:

a tube having a first end and a second end, the second end of said tube extending into said reaction chamber; and

a gas source connected to the first end of said tube.

20. The apparatus of

claim 19

, further comprising an open container located inside of said tube, said open container for holding organic precursor material.

21. The apparatus of

claim 20

, wherein said tube includes a pressure regulator and a valve.

22. The apparatus of

claim 16

, wherein said tubing comprises:

a first tube having a first end and a second end, said second end of said first tube extending into said reaction chamber;

a bubbler connected to the first end of said first tube, said bubbler for containing organic precursor material;

a second tube having a first end and a second end, said second end of said second tube connected to said bubbler; and

a gas source connected to the first end of said second tube.

23. The apparatus of

claim 22

, wherein said second tube includes a pressure regulator and a valve.

24. The apparatus of

claim 16

, further comprising a temperature-control block in contact with the substrate, said temperature-control block having a channel therein.

25. The apparatus of

claim 16

, further comprising a trap attached to said reaction chamber.

26. The apparatus of

claim 16

, further comprising a first roll and a second roll in said reaction chamber for passing the substrate between said first and second rolls.

27. An apparatus for preparing an organic thin film on a substrate, said apparatus comprising:

a reaction chamber;

a Knudsen cell extending into said reaction chamber;

a sample holder connected to the substrate;

said sample holder being rotatable; and

a vacuum pump attached to said reaction chamber.

28. The apparatus of

claim 27

, further comprising tubing extending into said reaction chamber, said tubing comprising:

a first tube having a first end and a second end, said second end of said first tube extending into said reaction chamber;

a bubbler connected to the first end of said first tube, said bubbler for containing organic precursor material;

a second tube having a first end and a second end, said second end of said second tube connected to said bubbler; and

a gas source connected to the first end of said second tube.

29. The apparatus of

claim 27

, wherein said first tube is heated.

30. The apparatus of

claim 27

, further comprising a cooled shroud in said reaction chamber.

31. The apparatus of

claim 27

, further comprising a sensor for detecting the thickness of the thin firm.

32. The apparatus of

claim 31

, wherein said sensor is a quartz crystal.

33. The apparatus of

claim 27

, further comprising a load-lock connected to said reaction chamber.

34. The apparatus of

claim 27

, wherein said vacuum pump is a turbomolecular pump.

35. The apparatus of

claim 27

, further comprising a first roll and a second roll in said reaction chamber for passing the substrate between said first and second rolls.

36. An apparatus for preparing an organic thin film on a substrate, said apparatus comprising:

a plurality of vacuum chambers, said plurality of vacuum chambers including a loading chamber and an organic layer deposition chamber; and

a conveyor belt passing through said plurality of vacuum chambers, said conveyor belt having a substrate thereon.

37. The apparatus of

claim 36

, wherein said organic layer deposition chamber includes a reactant gas distributor.

38. The apparatus of

claim 36

, wherein said organic layer deposition chamber includes a heater.

39. The apparatus of

claim 36

, further comprising a contact deposition chamber.

40. An apparatus for preparing an organic thin film on a substrate, said apparatus comprising:

a reaction chamber;

means for heating said reaction chamber;

means for introducing vapors of organic precursor materials into said reaction chamber; and

means for reducing the pressure in said reaction chamber to below atmospheric pressure.

41. A method for preparing an OLED, said method comprising the steps of:

providing a plurality of organic precursors, said organic precursors being in the vapor phase; and

reacting said plurality of organic precursors at a sub-atmospheric pressure.

42. The method of

claim 41

, wherein said organic precursors are light emitting materials.

43. The method of

claim 41

, wherein said step of reacting results in the formation of a light emitting material.