Growth of large aluminum nitride single crystals with thermal-gradient control

• US 9,028,612 B2
• Filed: 06/30/2011
• Issued: 05/12/2015
• Est. Priority Date: 06/30/2010
• Status: Active Grant

• Current Assignee: Crystal IS, Inc. (Asahi Kasei Corporation)
• Original Assignee: Crystal IS, Inc. (Asahi Kasei Corporation)
• Inventors: Bondokov, Robert T., Rao, Shailaja P., Gibb, Shawn Robert, Schowalter, Leo J.
• Primary Examiner(s): Bratland, Jr., Kenneth A
• Application Number:
  US13/173,213
• Publication Number:
  US 20120000414A1
• Time in Patent Office: 1,412 Days
• Field of Search: 117/84, 117/88, 117/101, 117/937, 117/952
• US Class Current: 117/84
• CPC Class Codes: C30B 23/002 Controlling or regulating
• CPC Class Codes: C30B 23/025 characterised by the substrate
• CPC Class Codes: C30B 23/06 Heating of the deposition chamber, the substrate or the materials to be evaporated
• CPC Class Codes: C30B 29/403 AIII-nitrides

Abstract

In various embodiments, non-zero thermal gradients are formed within a growth chamber both substantially parallel and substantially perpendicular to the growth direction during formation of semiconductor crystals, where the ratio of the two thermal gradients (parallel to perpendicular) is less than 10, by, e.g., arrangement of thermal shields outside of the growth chamber.

Claims

1. A method of forming single-crystal aluminum nitride (AlN), the method comprising:

providing a plurality of thermal shields comprising (i) a first thermal shield defining a first opening therethrough and (ii) a second thermal shield defining a second opening therethrough larger than the first opening;

arranging the plurality of thermal shields over the lid of a growth chamber such that the first thermal shield is disposed between the lid of the growth chamber and the second thermal shield;

initiating the formation of an AlN single crystal substantially at a single growth center within the growth chamber proximate the lid of the growth chamber, a location of the single growth center being determined at least in part by a location of the first opening in the arranged first thermal shield;

condensing vapor comprising aluminum and nitrogen within the growth chamber, thereby increasing a size of the AlN single crystal along a growth direction; and

during formation of the AlN single crystal, forming and maintaining, within the growth chamber and at least in part via arrangement of the plurality of thermal shields outside of the growth chamber, (i) a first non-zero thermal gradient in a direction substantially parallel to the growth direction and (ii) a second non-zero thermal gradient in a direction substantially perpendicular to the growth direction,

wherein a ratio of the first thermal gradient to the second thermal gradient is less than 10.

2. The method of claim 1, further comprising subliming solid source material within the growth chamber to form the vapor.

3. The method of claim 2, wherein the solid source material comprises polycrystalline AlN.

4. The method of claim 1, wherein the second thermal gradient is larger than 4°

C./cm.

5. The method of claim 1, wherein the second thermal gradient is smaller than 85°

C./cm.

6. The method of claim 1, wherein the ratio of the first thermal gradient to the second thermal gradient is greater than 1.2.

7. The method of claim 1, wherein the first thermal gradient is larger than 5°

C./cm.

8. The method of claim 1, wherein the first thermal gradient is smaller than 100°

C./cm.

9. The method of claim 1, wherein the ratio of the first thermal gradient to the second thermal gradient is less than 5.5.

10. The method of claim 1, wherein the ratio of the first thermal gradient to the second thermal gradient is less than 3.

11. The method of claim 1, wherein each of the thermal shields comprises a refractory material.

12. The method of claim 1, wherein each of the thermal shields comprises tungsten.

13. The method of claim 1, wherein the first opening and the second opening each ranges from approximately 10 mm to approximately 2 mm less than a dimension of the growth chamber substantially perpendicular to the growth direction.

14. The method of claim 1, wherein at least two of the thermal shields have different thicknesses.

15. The method of claim 1, wherein a thickness of each of the thermal shields ranges from approximately 0.125 mm to approximately 0.5 mm.

16. The method of claim 1, wherein a thickness of the lid is less than approximately 0.5 mm.

17. The method of claim 1, wherein the lid comprises tungsten.

18. The method of claim 1, further comprising disposing a seed within the growth chamber before forming the AlN single crystal, the AlN single crystal forming on the seed and extending therefrom in the growth direction.

19. The method of claim 18, wherein a diameter of the seed is greater than approximately 25 mm.

20. The method of claim 1, wherein a growth rate of the AlN single crystal is greater than approximately 0.5 mm/hr.

21. The method of claim 1, wherein the AN single crystal forms on a seed disposed within the growth chamber.

22. The method of claim 1, wherein the lid of the growth chamber (i) is approximately planar, (ii) extends approximately perpendicular to the growth direction, and (iii) has an area larger than an area of the single growth center.

23. The method of claim 18, wherein an area of the first opening is smaller than a surface area of the seed.

24. The method of claim 21, wherein an area of the first opening is smaller than a surface area of the seed.