Processes for the preparation of polycrystalline diamond films

• US 4,925,701 A
• Filed: 05/27/1988
• Issued: 05/15/1990
• Est. Priority Date: 05/27/1988
• Status: Expired due to Term

• Current Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Original Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Inventors: Jansen, Frank, Machonkin, Mary A.
• Primary Examiner(s): Silverman, Stanley
• Application Number:
  US07/199,646
• Time in Patent Office: 718 Days
• Field of Search: 427/38, 427/45.1, 427/99, 427/162, 427/166, 427/168, 427/249, 427/255.1, 427/255.2, 427/294, 427/402, 428/408
• US Class Current: 427/575
• CPC Class Codes: C23C 16/0272 Deposition of sub-layers, e.g. to promote the adhesion of the main coating
• CPC Class Codes: C23C 16/27 Diamond only
• CPC Class Codes: C30B 25/02 Epitaxial-layer growth
• CPC Class Codes: C30B 29/04 Diamond
• CPC Class Codes: H01L 21/4803 Insulating or insulated parts, e.g. mountings, containers, diamond heatsinks H01L21/4846 takes precedence; printed circuit boards H05K1/00

Abstract

A process for the preparation of continuous polycrystalline diamond films which comprises applying to a substrate diamond powder in an amount of from about one particle per ten square microns to about 10 particles per square micron with an average particle diameter of from about 0.1 to about 0.4 micron; heating the resulting powdered substrate subsequent to incorporation in a processing apparatus; introducing a mixture of gases into the chamber, which gases provide a supply of carbon and hydrogen; and decomposing the gas mixture.

Claims

1. A process for the preparation of continuous polycrystalline diamond films which comprises applying to a substrate diamond powder in an amount of from about one particle per ten square microns to about 10 particles per square micron with an average particle diameter of from about 0.1 to about 0.4 micron;

heating the resulting powdered substrate subsequent to incorporation in a processing apparatus;

introducing a mixture of gases into the apparatus, which gases provide a supply of carbon and hydrogen; and

decomposing the gas mixture.

2. A process in accordance with claim 1 wherein the substrate is a semiconductive wafer.

3. A process in accordance with claim 1 wherein the substrate is a semiconductive wafer with microelectronic circuitry thereon.

4. A process in accordance with claim 1 wherein the substrate is a tool bit.

5. A process in accordance with claim 1 wherein the substrate is a razor blade.

6. A process in accordance with claim 1 wherein the substrate comprises an optical device.

7. A process in accordance with claim 1 wherein the diamond powder is applied from a suspension thereof by spin coating, dip coating, or spray coating.

8. A process in accordance with claim 1 wherein the processing apparatus is a deposition chamber.

9. A process in accordance with claim 1 wherein the diamond powder is applied from a suspension thereof by spray coating.

10. A process in accordance with claim 1 wherein the diamond powder is applied from a suspension of diamond powder and an aliphatic compound.

11. A process in accordance with claim 10 wherein the aliphatic compound is an alcohol.

12. A process in accordance with claim 11 wherein alcohol is isopropanol.

13. A process in accordance with claim 1 wherein the average diameter of the particle is from about 0.1 to about 0.25 micron.

14. A process in accordance with claim 1 wherein the powdered substrate is incorporated in a vacuum system.

15. A process in accordance with claim 1 wherein the powdered substrate is heated at a temperature of from about 600°

to about 950°

C.

16. A process in accordance with claim 1 wherein the powdered substrate is exposed to gases comprised of a mixture of carbonaceous gas and hydrogen at a reduced total pressure of less than 500 Torr.

17. A process in accordance with claim 16 wherein the gas mixture contains from about 0.1 percent to about 5 percent carbonaceous gas.

18. A process in accordance with claim 17 wherein the carbonaceous gas is methane.

19. A process in accordance with claim 17 wherein the carbonaceous gas is acetone vapor.

20. A process in accordance with claim 17 wherein the carbonaceous gas is carbon oxide.

21. A process in accordance with claim 1 wherein the decomposition of the gases is accomplished by heating.

22. A process in accordance with claim 21 wherein the decomposition of the gases is accomplished by heating at a temperature exceeding 1,700°

C.

23. A process in accordance with claim 22 wherein the decomposition of the gases is accomplished by heating refractory metal filaments at a temperature exceeding 1,700°

C.

24. A process in accordance with claim 1 wherein the decomposition of the gases is accomplished by the formation of a plasma.

25. A process in accordance with claim 24 wherein the decomposition of the gases is accomplished by the formation of a microwave plasma.

26. A process in accordance with claim 24 wherein the decomposition of the gases is accomplished by the formation of a direct current plasma.

27. A process in accordance with claim 24 wherein the decomposition of the gases is accomplished by a radio frequent plasma.

28. A process in accordance with claim 1 wherein the powdered diamond layer has an area coverage of about one particle per ten square microns to about one particle per square micron.

29. A process in accordance with claim 1 wherein the powdered diamond layer has an area coverage of about one particle per square micron to about ten particles per square micron.

30. A process in accordance with claim 1 wherein the polycrystalline diamond layer is of a thickness of from about 0.1 micron to about 1,000 microns.

45. A process in accordance with claim 1 wherein there results, subsequent to removal from the chamber, substantially pure polycrystalline diamond on the substrate.

47. A process in accordance with claim 1 wherein the powdered diamond is applied from a suspension thereof in alcohol, which suspension is formulated by mixing and ultrasonic vibrations.

49. A process in accordance with claim 1 wherein the decomposition is accomplished with heated refractory metal filament wires.

51. A process in accordance with claim 2 wherein the powdered diamond layer has an area coverage of about one particle per ten square microns to about one particle per square micron.

52. A process in accordance with claim 2 wherein the powdered diamond layer has an area coverage of about one particle per square micron to about ten particles per square micron.

53. A process in accordance with claim 2 wherein the polycrystalline diamond layer is of a thickness of from about 0.1 micron to about 1,000 microns.

54. A process in accordance with claim 1 wherein the powdered diamond layer has an area coverage of from about 5 particles per square micron to about 10 particles per square micron.

56. A process in accordance with claim 1 wherein the gas mixture contains a carbon containing gas in an amount of from about 0.1 to about 2 percent by volume.

31. A process for the preparation of continuous polycrystalline diamond which comprises applying to a substrate diamond powder in an amount of from about one particle per ten square microns to about 10 particles per square micron with a particle size of from about 0.1 to about 0.4 micron;

incorporating the substrate into a deposition system;

applying a vacuum of from about 1 mTorr to about 1 Torr;

heating the resulting powdered substrate to a temperature of from about 800°

to about 900°

C.;

introducing into the chamber a mixture of gases or vapors comprised of a carbon containing gas and hydrogen;

adjusting the total pressure to from about 10 Torr to about 100 Torr; and

decomposing the gas mixture whereby polycrystalline diamond is formed on the substrate on nucleation sites provided by the powder.

32. A process in accordance with claim 31 wherein the substrate is a semiconductive wafer.

33. A process in accordance with claim 31 wherein the diamond powder is applied from a suspension thereof in an aliphatic alcohol.

34. A process in accordance with claim 32 wherein alcohol is methanol.

35. A process in accordance with claim 31 wherein the particle size is from about 0.1 to about 0.25 micron.

36. A process in accordance with claim 31 wherein the powdered substrate is heated at a temperature of from about 800°

to about 850°

C.

37. A process in accordance with claim 31 wherein the gases are comprised of a mixture of methane and hydrogen.

38. A process in accordance with claim 37 wherein the gas mixture contains from about 0.05 percent to about 5 percent carbon containing gas.

39. A process in accordance with claim 31 wherein the decomposition of the gases is accomplished by heating.

40. A process in accordance with claim 39 wherein the decomposition of the gases is accomplished by heating at a temperature of up to 2,000°

C.

41. A process in accordance with claim 31 wherein the decomposition of the gases is accomplished by the formation of a plasma.

42. A process in accordance with claim 32 wherein the substrate is of a thickness of from about 100 microns to about 1,000 microns.

43. A process in accordance with claim 31 wherein the polycrystalline diamond layer is of a thickness of from about 1 micron to about 1,000 microns.

44. A process in accordance with claim 31 wherein the polycrystalline diamond film is deposited at a rate of from about 0.1 to about 1 micron per hour.

46. A process in accordance with claim 31 wherein there results, subsequent to removal from the chamber, substantially pure polycrystalline diamond on the substrate.

48. A process in accordance with claim 31 wherein the powdered diamond is applied from a suspension thereof in alcohol, which suspension is formulated by mixing and ultrasonic vibrations.

50. A process in accordance with claim 31 wherein the decomposition is accomplished with heated refractory metal filament wires.

55. A process in accordance with claim 31 wherein the powdered diamond layer has an area coverage of from about 5 particles per square micron to about 10 particles per square micron.

57. A process in accordance with claim 31 wherein the gas mixture contains a carbon containing gas in an amount of from about 0.1 to about 2 percent by volume.