IP Library › Granted Patent US 8,197,596
Granted Patent B2
US 8,197,596 · App. 11/829,385 · Granted Jun 12, 2012

Crystal growth method and reactor design

Assignee: Pronomic Industry AB
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Quick Facts
Patent No.
US 8,197,596
App. No.
11/829,385
Granted
Jun 12, 2012
Kind
B2
Abstract

A crystal growth process comprising providing a reactor having a crucible with an injector apparatus and a seed holder. The injector apparatus has an inner gas conduit and an outer gas conduit wherein an inert gas is introduced into the outer conduit. The injector apparatus has an upper injector and a lower injector and a gap therebetween. The upper injector temperature is maintained at a higher temperature than the lower injector.

Claims (68)

1. A crystal growth process comprising:

providing a reactor having a crucible with an injector apparatus for injecting material into the reactor, and a seed holder on which crystal growth takes place;

wherein the injector apparatus has an inner gas conduit and an outer gas conduit, both terminating in a lower injector, and further which has an upper gas injector extending into a crucible of the reactor;

providing a gap between the upper injector and the lower injector;

maintaining the upper injector at a higher temperature than the lower injector;

providing a seed crystal on the seed holder;

introducing into the reactor through the injector apparatus, a flow of one or more precursors to cause crystal growth;

introducing into the reactor through the outer gas conduit, a flow of inert gas.

2. The crystal growth process of claim 1 wherein the inert gas is a gas with an atomic weight greater than 28 amu.

3. The crystal growth process of claim 1 wherein the inert gas is argon.

4. The crystal growth process of claim 1 wherein the inert gas is krypton.

5. The crystal growth process of claim 1 wherein the inert gas is xenon.

6. The crystal growth process of claim 1 wherein the inert gas is a mixture of argon and helium.

7. The crystal growth process of claim 1 wherein the crystal growth process is a gas phase bulk growth process.

8. The crystal growth process of claim 1 wherein the temperature is in the range of about 2000° C. to about 2400° C. as measured on a top surface of the washer holding the seed crystal.

9. The crystal growth process of claim 8 wherein the temperature is in the range of about 2200° C. to about 2270° C. as measured on a top surface of the washer holding the seed crystal.

10. The crystal growth process of claim 1 wherein the bottom temperature is in the range of about 2300° C. to about 2600° C., as measured in a 30-40 mm deep slot located at the bottom of the crucible and penetrating into the a side wall of the crucible.

11. The crystal growth process of claim 1 wherein the bottom temperature is in the range of about 2400° C. to about 2530° C., as measured in a 30-40 mm deep slot located at the bottom of the crucible and penetrating into the a side wall of the crucible.

12. The crystal growth process of claim 1 wherein the thermal gradient between the top surface of the washer and the bottom of the crucible is in the range of about 200° C. to about 300° C.

13. The crystal growth process of claim 1 wherein a silicon precursor has a flow rate of about 400 sccm to about 800 sccm.

14. The crystal growth process of claim 13 wherein the silicon precursor is silane.

15. The crystal growth process of claim 1 wherein the carbon precursor flow rate is in the range of about 200 sccm to about 300 sccm.

16. The crystal growth process of claim 12 wherein the carbon precursor is ethylene.

17. The crystal growth process of claim 1 wherein the carbon precursor to silicon precursor ration is in the range of about 0.3 and about 0.7.

18. The crystal growth process of claim 1 wherein a carrier gas is introduced in the inner conduit with the precursors at a flow rate of less than about 1 SLM.

19. The crystal growth process of claim 1 wherein helium is introduced into the inner gas conduit with the precursor flow.

20. The crystal growth process of claim 1 wherein a mixture of helium and hydrogen are introduced into the inner gas conduit with the precursor flow.

21. The crystal growth process of claim 6 wherein the argon flow in the outer conduit is in the range about 0.4 SLM to about 1.0 SLM.

22. The crystal growth process of claim 6 wherein the helium flow in the outer conduit is in the range about 1 SLM to about 5 SLM.

23. The crystal growth process of claim 6 wherein the helium flow is about 1.2 SLM and the argon flow is about 0.4 SLM.

24. The crystal growth process of claim 6 wherein the helium flow is about 1.5 SLM and the argon flow is about 0.5 SLM.

25. The crystal growth process of claim 1 further comprising a flow of etchant through a shaft to the seed holder in the range of about 0.3 SLM to about 3 SLM.

26. The crystal growth process of claim 25 wherein the etchant is HCl.

27. The crystal growth process of claim 25 comprising a flow rate of helium, argon, or a combination thereof in the range of about 1 SLM to about 3 SLM.

28. The crystal growth process of claim 27 comprising the flow rate of hydrogen in the range of about 1 SLM to about 5 SLM.

29. The crystal growth process of claim 26 wherein the flow rate of HCl is about 0.7, and comprising a flow of helium at a rate of about 2 SLM and a flow rate of hydrogen at a rate of about 3 SLM.

30. The crystal growth process of claim 1 wherein the pressure is in the range about 200 torr to about 800 torr.

31. The crystal growth process of claim 1 wherein the temperature difference between the upper injector and the lower injector is on the range of about 50° C. to about 100° C.

32. The crystal growth process of claim 1 wherein the seed holder comprises:

a drool and a washer disposed around the drool to form the seed holder;

a main body disposed over the washer and drool, forming an enclosure above the washer and drool, the enclosure forming a cavity above the washer and drool;

one or more main body apertures in the main body for the introduction of gases into the cavity;

wherein gases introduced into the cavity can seep through an interface between the drool inner edge and the washer outer edge.

33. The crystal growth process of claim 32 wherein the circumference of the seed holder main body decreases over at least a portion of the main body extending from a point nearer to the crucible to a point farther from the crucible.

34. The crystal growth process of claim 32 wherein the washer comprises one or more carve outs to regulate the temperature gradient.

35. The crystal growth process of claim 32 wherein the top of the washer has a larger diameter than the bottom of the washer.

36. The crystal growth process of claim 1 further comprising:

providing insulation around at least the crucible with a gap therebetween; and

flowing a gas in the gap to reduce insulation degradation.

37. The crystal growth process of claim 36 wherein the gas is argon.

38. The crystal growth method of claim 32 further comprising:

providing a graphite-etching inhibitor coating on a top surface of the washer.

39. The crystal growth method of claim 32 wherein the washer is about 2 mm to about 7 mm larger in diameter than the seed.

40. The crystal growth method of claim 1 wherein the upper injector is comprised of a metal carbide.

41. The crystal growth method of claim 40 wherein the upper injector is comprised on niobium carbide.

42. The crystal growth method of claim 40 wherein the upper injector is comprised on tantalum carbide.

43. The crystal growth method of claim 40 wherein the upper injector is comprised on tungsten carbide.

44. A crystal grown according to the growth method of claim 1 .

45. A semiconductor device comprising the crystal of claim 44 .

46. A method of insulating a crystal growth reactor comprising:

providing insulation disposed around at least a crucible and outlet section of the reactor apparatus;

providing a gap between the insulation and the crucible and outlet section;

flowing an inert gas into the gap.

47. The method of claim 46 wherein the gas is argon.

48. The method of claim 46 wherein the flow rate of the gas is in the range of about 10 SLM to about 35 SLM.

49. The method of claim 48 wherein the flow rate of the gas is in the range of about 18 SLM to about 20 SLM.

50. The method of claim 46 wherein the gap width is in the range of about 3 mm to about 6 mm.

51. The method of claim 50 wherein the gap width is about 5 mm.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 7, 2010
From: CARACAL, INC.
To: PRONOMIC INDUSTRY AB
Reel/Frame 024483/0988 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 15, 2008
From: CARACAL, INC.
To: CARACAL, INC.
Reel/Frame 021395/0872 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 2, 2007
From: KORDINA, OLOF CLAES ERIK; RAO, SHAILAJA
To: CARACAL, INC.
Reel/Frame 019906/0437 →
Continuity (2)
Provisional Application 60833951 · Jul 28, 2006
Related Publication 20080026546A1 · Jan 31, 2008