IP Library Granted Patent US 7,459,024
Granted Patent B2
US 7,459,024 · App. 10/977,568 · Granted Dec 2, 2008

Method of forming an N-type doped single crystal diamond

Assignee: Apollo Diamond, Inc.
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Quick Facts
Patent No.
US 7,459,024
App. No.
10/977,568
Granted
Dec 2, 2008
Kind
B2
Abstract

Synthetic monocrystalline diamond compositions having one or more monocrystalline diamond layers formed by chemical vapor deposition, the layers including one or more layers having an increased concentration of one or more impurities (such as boron and/or isotopes of carbon), as compared to other layers or comparable layers without such impurities. Such compositions provide an improved combination of properties, including color, strength, velocity of sound, electrical conductivity, and control of defects. A related method for preparing such a composition is also described, as well as a system for use in performing such a method, and articles incorporating such a composition.

Claims (66)

1. A method of forming an n-type doped single crystal diamond, the method comprising:

polishing a CVD grown single crystal seed having a (100) orientation;

placing the seed in a substrate holder in a hot filament chemical vapor deposition reactor;

evacuating the reactor to a pressure of less than 10 millitorr;

backfilling the reactor with hydrogen having a purity of at least approximately 99.999%;

providing power to the filament;

heating the substrate holder to approximately 950° C.;

adding 13 C enriched methane containing phosphene to obtain a mixture of approximately 1% methane, 99% hydrogen containing approximately 100 ppm phosphene with a gas flow of approximately 100 sccm;

converting part of the hydrogen to atomic hydrogen;

after formation of a desired thickness of single crystal phosphorous doped diamond, terminating the flow of methane;

after the end of flow of the methane, terminating the power; and

cooling the substrate holder to room temperature.

2. The method of claim 1 wherein the desired thickness of the single crystal phosphorous doped diamond is less than approximately 0.17 micrometers.

3. The method of claim 1 wherein the single crystal phosphorous doped diamond has a (100) crystal orientation.

4. The method of claim 1 wherein the growth rate of diamond is approximately 1 micrometer per hour.

5. The method of claim 1 and further comprising cleaning the single crystal phosphorous doped diamond in a mixture of chromic acid and sulfuric acid at a temperature of approximately 250° C.

6. The method of claim 1 wherein hydrogen is backfilled to approximately 40 Torr at a rate of approximately 100 sccm.

7. A method of forming an n-type doped single crystal diamond, the method comprising:

polishing a single crystal seed having a (100) orientation;

placing the seed in a substrate holder in a hot filament chemical vapor deposition reactor;

filling the reactor with hydrogen having a purity of at least approximately 99.999%;

providing power to the filament;

heating the substrate holder to approximately 950° C.;

adding 13 C enriched methane containing phosphene;

converting part of the hydrogen to atomic hydrogen;

after formation of a desired thickness of single crystal phosphorous doped diamond, terminating the flow of methane;

after the end of flow of the methane, terminating the power; and

cooling the substrate holder to room temperature.

8. The method of claim 7 wherein the desired thickness of the single crystal phosphorous doped diamond is at least approximately 0.17 micrometers.

9. The method of claim 7 wherein the single crystal phosphorous doped diamond has a (100) crystal orientation.

10. The method of claim 7 wherein the growth rate of diamond is approximately 1 micrometer per hour.

11. The method of claim 7 and further comprising cleaning the single crystal phosphorous doped diamond in a mixture of chromic acid and sulfuric acid at a temperature of approximately 250° C.

12. A method of forming an n-type doped single crystal diamond, the method comprising:

placing a polished seed in a substrate holder in a hot filament chemical vapor deposition reactor;

filling the reactor with hydrogen;

providing power to the filament;

heating the substrate holder to approximately 950° C.;

adding 13 C enriched methane containing phosphene;

after formation of a desired thickness of single crystal phosphorous doped diamond, terminating the flow of methane;

after the end of flow of the methane, terminating the power; and

cooling the substrate holder to room temperature.

13. The method of claim 12 wherein the desired thickness of the single crystal phosphorous diamond is less than approximately 0.17 micrometers.

14. The method of claim 12 wherein the single crystal phosphorous doped diamond has a (100) crystal orientation.

15. The method of claim 12 wherein the growth rate of diamond is approximately 1 micrometer per hour.

16. The method of claim 12 wherein the methane concentration is less than approximately 1%.

17. A method of forming an n-type doped single crystal diamond, the method comprising:

placing a polished seed in a substrate holder in a hot filament chemical vapor deposition reactor;

filling the reactor with hydrogen;

providing power to the filament;

heating the substrate holder;

adding 13 C enriched methane containing phosphene;

after formation of a desired thickness of single crystal phosphorous doped diamond, terminating the flow of methane;

after the end of flow of the methane, terminating the power; and

stopping heating of the substrate holder.

18. The method of claim 17 wherein the desired thickness of the single crystal phosphorous doped diamond is less than approximately 0.17 micrometers.

19. The method of claim 17 wherein the single crystal phosphorous doped diamond has a (100) crystal orientation.

20. The method of claim 17 wherein the growth rate of diamond is approximately 1 micrometer per hour.

21. The method of claim 17 wherein the methane concentration is less than approximately 1%.

22. A method of forming an n-type doped single crystal diamond, the method comprising:

placing a polished seed in a substrate holder in a hot filament chemical vapor deposition reactor;

filling the reactor with hydrogen;

providing power to the filament;

heating the substrate holder;

adding 13 C enriched methane containing phosphene;

after formation of a desired thickness of single crystal phosphorous doped diamond, terminating the flow of methane.

23. The method of claim 22 wherein the methane concentration is less than approximately 1%.

Assignments (2)
SECURITY INTEREST Recorded Jan 16, 2015
From: SCIO DIAMOND TECHNOLOGY CORPORATION
To: HERITAGE GEMSTONE INVESTORS, LLC
Reel/Frame 034736/0179 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 4, 2013
From: APOLLO DIAMOND, INC.
To: SCIO DIAMOND TECHNOLOGY CORPORATION
Reel/Frame 030615/0853 →
Continuity (4)
Continuation 1040998200 · Apr 8, 2003
Division 0931232600 · May 14, 1999
Provisional Application 6008554200 · May 15, 1998
Related Publication 20050061233A1 · Mar 24, 2005