SIC SINGLE CRYSTAL INGOT AND PRODUCTION METHOD THEREFOR

• US 20150167196A1
• Filed: 05/08/2013
• Published: 06/18/2015
• Est. Priority Date: 07/19/2012
• Status: Active Grant

• Current Assignee: Toyota Jidosha Kabushiki Kaisha (Toyota Motor Corporation)
• Original Assignee: Nippon Steel & Sumitomo Metal Corporation (Nippon Steel Corporation), Toyota Jidosha Kabushiki Kaisha (Toyota Motor Corporation)
• Inventors: Kado, Motohisa, Daikoku, Hironori, Sakamoto, Hidemitsu, Okada, Nobuhiro, Kusunoki, Kazuhiko
• Granted Patent: US 9,523,156 B2
• Time in Patent Office: Days
• US Class Current: 1/1
• CPC Class Codes: C30B 17/00 Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method C30B15/00 takes precedence
• CPC Class Codes: C30B 19/04 the solvent being a component of the crystal composition
• CPC Class Codes: C30B 19/062 Vertical dipping system
• CPC Class Codes: C30B 19/068 Substrate holders
• CPC Class Codes: C30B 19/10 Controlling or regulating controlling or regulating in general G05
• CPC Class Codes: C30B 29/36 Carbides
• CPC Class Codes: C30B 9/06 using as solvent a component of the crystal composition
• CPC Class Codes: Y10T 117/1008 with responsive control means
• CPC Class Codes: Y10T 428/21 Circular sheet or circular blank
• CPC Class Codes: Y10T 428/24488 Differential nonuniformity at margin

Abstract

Provided are: a high-quality SiC single crystal ingot that suppresses the generation of inclusions; and a production method for said SiC single crystal ingot. The present invention pertains to a SiC single crystal ingot including a seed crystal substrate and a SiC growth crystal grown using the solution method and using the seed crystal substrate as the origin thereof, the growth crystal having a recessed crystal growth surface and not including inclusions.

Claims

1. A method for producing a SiC single crystal by a solution process in which a seed crystal substrate held on a seed crystal holding shaft is contacted with a Si—

C solution having a temperature gradient such that the temperature decreases from the interior toward the surface, to cause crystal growth of the SiC single crystal, the method comprising

lowering the temperature of the Si—

C solution at the outer peripheral section directly below the interface with the crystal growth plane to be lower than the temperature of the Si—

C solution at the center section directly below the interface with the crystal growth plane, and causing the Si—

C solution to flow from the center section directly below the interface with the crystal growth plane to the outer peripheral section directly below the interface with the crystal growth plane.

2. The method for producing a SiC single crystal according to claim 1, wherein causing flow of the Si—

C solution comprises rotating the seed crystal substrate in a direction along the outer periphery of the seed crystal substrate while switching the rotational direction, and wherein rotating the seed crystal substrate comprises rotating the outer peripheral section of the seed crystal substrate at a speed faster than 25 mm/sec, and for a longer time than 30 seconds continuously in the same direction.

3. The method for producing a SiC single crystal according to claim 2, wherein the method comprises rotating the outer peripheral section of the seed crystal substrate at a speed of 63 mm/sec or more.

4. The method for producing a SiC single crystal according to claim 2, wherein the method comprises rotating the seed crystal substrate continuously in the same direction for a time of 360 seconds or more.

5. The method for producing a SiC single crystal according to claim 1, wherein lowering the temperature of the Si—

C solution comprises forming a meniscus between the seed crystal substrate and the Si—

C solution.

6. The method for producing a SiC single crystal according to claim 1, wherein the seed crystal holding shaft has a constitution in which the side section of the seed crystal holding shaft exhibits higher thermal conductivity than the center section.

7. The method for producing a SiC single crystal according to claim 6, wherein the center section of the seed crystal holding shaft has a hollow part.

8. The method for producing a SiC single crystal according to claim 7, wherein a heat-insulating material is disposed in at least part of the hollow part of the seed crystal holding shaft.

9. An apparatus for production of a SiC single crystal by a solution process in which a seed crystal substrate held on a seed crystal holding shaft is contacted with a Si—

C solution heated so as to have a temperature gradient such that the temperature decreases from the interior toward the surface, to cause crystal growth of the SiC single crystal from the seed crystal substrate, the apparatus comprising;

a crucible that houses a Si—

C solution,

a heating device situated surrounding the crucible, and

a seed crystal holding shaft situated in a movable manner in the up-down direction, the apparatus further comprising;

a temperature control means that lowers the temperature of the Si—

C solution at the outer peripheral section directly below the interface with the crystal growth plane to be lower than the temperature of the Si—

C solution at the center section directly below the interface with the crystal growth plane, and

a flow means that causes the Si—

C solution to flow from the center section directly below the interface with the crystal growth plane to the outer peripheral section directly below the interface with the crystal growth plane,

wherein the temperature control means comprises the seed crystal holding shaft, and the seed crystal holding shaft has a hollow part in the center section and a heat-insulating material in at least part of the hollow part so that the seed crystal holding shaft has higher thermal conductivity at the side sections than at the center section; and

wherein the flow means comprises a rotating device for a rotating the seed crystal substrate for mechanical stirring of the Si—

C solution, and/or

the heating device comprises a high-frequency heating device for high-frequency heating the Si—

C solution and the flow means comprises the high-frequency heating device for electrical magnetic stirring of the Si—

C solution.

10. A SiC single crystal ingot containing a seed crystal substrate and a SiC grown crystal grown from the seed crystal substrate by using a solution process, wherein the grown crystal has a concave crystal growth plane and contains no inclusions.

11. The SiC single crystal ingot according to claim 10, wherein the maximum angle θ

of the slope of the concave crystal growth plane with respect to the just plane of growth of the grown crystal is in the range of 0<

θ

≦

8°

.

12. The SiC single crystal ingot according to claim 10, wherein the growth thickness of the grown crystal is 3 mm or greater.

13. The SiC single crystal ingot according to claim 10, wherein the diameter of the grown crystal is 6 mm or greater.