IP Library Granted Patent US 12,330,948
Granted Patent B2
US 12,330,948 · App. 15/939,423 · Granted Jun 17, 2025

SiC volumetric shapes and methods of forming boules

Inventors: Douglas M Dukes (Troy, NY); Glenn Sandgren (Ambler, PA); Andrew R Hopkins (Houston, TX); Isabel Burlingham (Troy, NY); Mark S Land (Houston, TX)
Assignee: Pallidus, Inc.
C01B32/963C30B23/005C30B23/02C30B25/165C30B29/36C30B29/66C01P2004/30C01P2004/61C01P2004/62C01P2006/10C01P2006/40C01P2006/80
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Quick Facts
Patent No.
US 12,330,948
App. No.
15/939,423
Granted
Jun 17, 2025
Kind
B2
Abstract

Volumetric shapes of SiC starting materials for boule growth. Methods of controlling vapor deposition growth of SiC boules, and providing directional flux. Methods of increase the number of wafers, the number of electronic components and the number of operable devices from a single boule growth cycle.

Claims (101)

1. A source material for use as a starting material in a vapor deposition process to grow an SiC boule, the source material defining a volumetric shape of SiC, the volumetric shape comprising:

a. about 100 g to about 12,000 g of SiC granules, having a particle size of from about 0.1 μm to about 100 μm,

b. the SiC granules defining a volumetric shape having a structural integrity;

c. a binder, wherein the binder binds the SiC granules, whereby the volumetric shape is capable of maintaining the structural integrity when placed in a vapor deposition apparatus during a growth cycle of a boule;

d. the volumetric shape defining a void; and,

e. the volumetric shape having pores defining a porosity, wherein the volumetric shape has an apparent density of less than 3.0 g/cc.

2. The source material of claim 1 , wherein the weight of SiC granules is form about 1000 g to about 9000 g.

3. The source material of claim 1 , wherein the granules have a primary particle D 50 size of from about 0.1 μm to about 20.0 μm.

4. The source material of claim 1 , wherein the void defines a channel in a top of the volumetric shape.

5. The source material of claim 4 , where in the channel is an angled annular channel.

6. The source material of claim 1 , the void is located in a top of the volumetric shape.

7. The source material of claim 1 , the void comprises a void located in a top and a bottom of the volumetric shape.

8. The source material of claim 1 , wherein the void defines a cylindrical channel extending through the volumetric shape.

9. The source material of claim 1 , wherein shape is a puck.

10. The source material of claim 1 , wherein the apparent density is from about 1.5 g/cc to 2.8 g/cc.

11. The source material of claim 1 , wherein the SiC granules are polymer derived SiC and have a purity of at least 99.999%.

12. The source material of claim 1 , having a molar ratio of Si:C of 0.5:2.

13. The source material of claim 1 , having a molar ratio of Si:C of 2:0.5.

14. A source material for use as a starting material in a vapor deposition process to grow an SiC boule, the source material defining a volumetric shape of SiC, the volumetric shape comprising:

a. About 100 g to about 12,000 g of SiC granules, having a particle size of from about 0.1 μm to about 100 μm,

b. the SiC granules defining a volumetric shape having a structural integrity, wherein the volumetric shape is capable of maintaining the structural integrity when placed in a vapor deposition apparatus during a growth cycle of a boule;

c. the volumetric shape defining a void; and,

d. the volumetric shape having pores defining a porosity, wherein the volumetric shape has an apparent density of less than 3.0 g/cc.

15. The source material of claim 14 , wherein the granules have a primary particle D 50 size of from about 0.5 μm to about 3 μm.

16. The source material of claim 14 , wherein the void defines a channel in a top of the volumetric shape.

17. The source material of claim 14 , wherein the SiC granules are polymer derived SiC and have a purity of at least 99.9999%.

18. A volumetric shape of SiC, for use as a starting material in a vapor deposition process to grow an SiC boule, the volumetric shape comprising:

a. SiC granules, having a particle size of from about 0.1 μm to about 100 μm,

b. the SiC granules defining a volumetric shape having a structural integrity;

c. a binder, wherein the binder binds the SiC granules, whereby the volumetric shape is capable of maintaining the structural integrity when placed in a vapor deposition apparatus during a growth cycle of a boule;

d. the volumetric shape defining a void; and,

e. the volumetric shape having a porosity, wherein the volumetric shape has an apparent density of less than 3.1 g/cc;

f. wherein the volumetric shape is configured to provide a predetermined flux during a growth cycle of a boule.

19. The volumetric shape of claim 18 , wherein the predetermined flux is a uniform and consistent flux.

20. The volumetric shape of claim 18 , wherein the predetermined flux has increased flux density near an outer area of a growth face of a boule during the last 20% of the growth cycle.

21. The volumetric shape of claim 18 , wherein the predetermined flux has increased flux density near an outer area of a growth face of a boule during the last 30% of the growth cycle.

22. The volumetric shape of claim 18 , wherein the predetermined flux has increased flux density near an outer area of a growth face of a boule during the last 40% of the growth cycle.

23. A volumetric shape of SiC, for use as a starting material in an SiC vapor deposition process, the volumetric shape comprising:

a. SiC granules, having a particle size of from about 0.1 μm to about 100 μm,

b. the SiC granules defining a volumetric shape having a structural integrity, such that the shape is not friable;

c. the volumetric shape defining a void; and,

d. the volumetric shape having a porosity, wherein the volumetric shape has an apparent density of less than 3.1 g/cc;

e. wherein the volumetric shape is configured to provide a predetermined flux during a growth cycle of a boule.

24. The volumetric shape of claim 23 , wherein the predetermined flux has increased flux density near an outer area of a growth face of a boule during the last 20% of the growth cycle.

25. The volumetric shape of claim 23 , wherein the predetermined flux has increased flux density near an outer area of a growth face of a boule during the last 30% of the growth cycle.

26. A volumetric shape of SiC, for use as a starting material in a SiC vapor deposition process, the volumetric shape comprising:

a. About 100 g to about 12,000 g of SiC granules, having a particle size of from about 0.1 μm to about 100 μm,

b. the SiC granules defining a volumetric shape;

c. the volumetric shape having a porosity, wherein the volumetric shape has an apparent density of less than 2.9 g/cc;

d. wherein the volumetric shape when placed in a vapor deposition apparatus during a growth cycle of a boule is configured to provide a consistent rate of flux formation during a growth cycle.

27. A volumetric shape of SiC, for use as a starting material in a SiC vapor deposition process, the volumetric shape comprising:

a. about 100 g to about 12,000 g of SiC granules, having a particle size of from about 0.1 μm to about 100 μm,

b. the SiC granules defining a volumetric shape;

c. a binder, wherein the binder binds the SiC granules; and,

d. wherein the volumetric shape when placed in a vapor deposition apparatus during a growth cycle of a boule is configured to provide a predetermined rate of flux formation during a growth cycle.

28. A method of growing a SiC boule, the method comprising:

a. placing a starting material having a shape comprising SiC in a vapor deposition apparatus;

b. heating the starting material to a temperature whereby the SiC sublimates forming a flux comprising species of Si and C;

c. flowing the flux across an area directly adjacent to the growth face of a boule; wherein the area is the same as and coincident with the growth face of the boule;

d. whereby the shape predetermines the flux across the entirety of the area; and,

e. depositing the flux on the growth face of the boule to grow the boule in length.

29. The method of claim 28 , wherein the flux is uniform across the entirety of the area during boule growth.

30. The method of claim 28 , wherein the flux is greater near an outer area of the boule face during at a time during the growth of the boule when at least half of the length of the boule has been grown.

31. The method of claim 28 , wherein the growth face of the boule is a seed crystal.

32. The method of claim 28 , wherein the growth face of the boule is a face of the boule.

33. The method of claim 28 , wherein the boule as grown is single crystalline.

34. The method of claim 28 , wherein the boule as grown is a single polytype.

35. The method of claim 28 , whereby the boule as grown is characterized by a diameter of about 3 inches to about 6 inches, a length of about 2 inches to about 8 inches, and a radius of curvature for the growth face of the boule is at least 2× the length.

36. The method of claim 28 , whereby the boule as grown is characterized by a diameter of about 3 inches to about 6 inches, a length of about 2 inches to about 8 inches, and a radius of curvature for the growth face of the boule is at least 5× the length.

37. The method of claim 28 , whereby the boule as grown is characterized by a diameter of about 3 inches to about 6 inches, a length of about 2 inches to about 8 inches, and a radius of curvature for the growth face of the boule is at least 10× the length.

38. The method of claim 28 , whereby the boule as grown is characterized by a diameter of about 3 inches to about 6 inches, a length of about 2 inches to about 8 inches, and a radius of curvature for the growth face that is infinite.

39. A method of growing a SiC boule, the method comprising:

a. placing a volumetric shape of starting material comprising SiC in a vapor deposition apparatus; the volumetric shape configured to provide a directional flux;

b. heating the volumetric shape to provide the directional flux during a growth cycle of a boule; and,

c. depositing the directional flux on a growth face of the boule to grow the boule in length.

40. The method of claim 39 , wherein in the directional flux provide increased flux density to the outer areas of the growth face, whereby during a time in the growth cycle, the boule has a planar growth face.

41. The method of claim 39 , wherein the boule is free from defects.

42. A method of providing a large number of devices from a single growth cycle of a boule, the method comprising:

a. placing a volumetric shape of starting material comprising SiC in a vapor deposition apparatus; the volumetric shape configured to provide a direction flux;

b. heating the volumetric shape to provide the directional flux during a growth cycle of a boule; and,

c. depositing the directional flux on a growth face of the boule to grow the boule in length;

d. converting the boule to provide wafers.

43. The method of claim 42 , whereby about 80% of the length of the boule is capable of being cut to provide defect free wafers.

44. The method of claim 42 , whereby about 95% of the length of the boule is capable of being cut to provide defect free wafers.

45. The method of claim 42 , whereby the wafers have MPD (≤0.1 cm-2), TSD (≤300 cm-2) and BPD (≤500 cm-2).

46. The method of claim 43 , wherein the wafers have resistivities greater than about 10,000 ohm-cm at 20° C.

47. The method of claim 42 , wherein the wafers have resistivities not less than about 10,000 ohm-cm at 20° C.

48. A source material for use as a starting material in a vapor deposition process, the source material defining a volumetric shape comprising ultra pure silicon carbide particles and a binder, for use in vapor deposition growth of silicon carbide boules, the volumetric shape comprising:

a. silicon carbide particles, wherein the particles are at least 99.999% pure, wherein the particles have a D 50 particle size from about 0.1 μm to about 20.0 μm;

b. a binder joining the silicon carbide particles together and thereby defining a volumetric shape;

c. the binder comprising a cross linked polymeric material comprising carbon and silicon; and,

d. wherein the binder is incapable of interfering with boule growth and incapable of adversely affecting boule quality.

49. The volumetric shape of claim 48 , having an elastic modules of from about 10 GPa to about 300 GPa.

50. The volumetric shape of claim 48 , having a hardness of from about 300 Kg/mm 2 to about 2,000 Kg/mm 2 .

51. The method of claim 42 , whereby at least about 80% of the length of the boule is capable of being cut to provide wafers having one or more of a MPD (≤0.1 cm-2), a TSD (≤300 cm-2), and a BPD (≤500 cm-2).

52. The method of claim 42 , whereby at least about 80% of the length of the boule is capable of being cut to provide wafers having at least two of a MPD (≤0.1 cm-2), a TSD (≤300 cm-2), and a BPD (≤500 cm-2).

53. The method of claim 42 , whereby wherein about 80% of the length of the boule is capable of being cut to provide wafers having a MPD (≤0.1 cm-2), a TSD (≤300 cm-2), and a BPD (≤500 cm-2).

54. The method of claim 42 , whereby about 95% of the length of the boule is capable of being cut to provide wafers having one or more of a MPD (≤0.1 cm-2), a TSD (≤ 300 cm-2), and a BPD (≤500 cm-2).

55. The method of claim 42 , whereby about 95% of the length of the boule is capable of being cut to provide wafers having at least two of a MPD (≤0.1 cm-2), a TSD (≤300 cm-2), and a BPD (≤500 cm-2).

56. The method of claim 42 , whereby about 95% of the length of the boule is capable of being cut to provide wafers having a MPD (≤0.1 cm-2), a TSD (≤300 cm-2), and a BPD (≤ 500 cm-2).

57. The method of claim 42, 46, 47, 51, 52, 53, 54, 55 or 56 , whereby the boule is about 6-inches in diameter, at least about 80% of the length of the boule is capable of being cut to provide about 6-inch diameter wafers.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 24, 2025
From: DUKES, DOUGLAS M.; HOPKINS, ANDREW R.; BURLINGHAM, ISABEL
To: PALLIDUS, INC.
Reel/Frame 071214/0581 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 24, 2025
From: LAND, MARK S.
To: PALLIDUS, INC.
Reel/Frame 071214/0588 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 24, 2025
From: SANDGREN, GLENN
To: PALLIDUS, INC.
Reel/Frame 071214/0592 →
SECURITY INTEREST Recorded Jan 10, 2025
From: PALLIDUS, INC.
To: R&R PALLIDUS HOLDINGS II LLC, AS ADMINISTRATIVE AGENT
Reel/Frame 069818/0486 →
Continuity (4)
Continuation PCTUS2018024978 · Mar 28, 2018
Provisional Application 62545367 · Aug 14, 2017
Provisional Application 62478383 · Mar 29, 2017
Related Publication 20180290893A1 · Oct 11, 2018
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