Apparatus for large volume ammonothermal manufacture of gallium nitride crystals and methods of use

• US 9,724,666 B1
• Filed: 10/19/2012
• Issued: 08/08/2017
• Est. Priority Date: 10/21/2011
• Status: Active Grant

• Current Assignee: SL Technology Incorporated (Reliv' International, Inc.)
• Original Assignee: Soraa, Inc.
• Inventors: Rajeev, Pakalapati Tirumala, Pocius, Douglas W., D'Evelyn, Mark P.
• Primary Examiner(s): Deo, Duy
• Assistant Examiner(s): Bergner, Erin
• Application Number:
  US13/656,615
• Time in Patent Office: 1,754 Days
• CPC Class Codes: A61B 6/12 Arrangements for detecting or locating foreign bodies
• CPC Class Codes: A61M 2025/09133 having specific material compositions or coatings; Materials with specific mechanical behaviours, e.g. stiffness, strength to transmit torque
• CPC Class Codes: A61M 25/00 Catheters; Hollow probes dilators A61M29/00; peritoneal catheters A61M1/285; tracheal tubes A61M16/04; for drainage A61M27/00; for uterus, vagina or rectum A61M31/00 ; for measuring or testing A61B; materials for catheters A61L29/00
• CPC Class Codes: A61M 25/0105 Steering means as part of the catheter or advancing means; Markers for positioning systems for detection of markers A61B
• CPC Class Codes: A61M 25/0113 Mechanical advancing means, e.g. catheter dispensers
• CPC Class Codes: A61M 25/09 Guide wires
• CPC Class Codes: A61M 25/09041 Mechanisms for insertion of guide wires
• CPC Class Codes: A61M 25/0905 extendable, e.g. mechanisms for extension
• CPC Class Codes: B01J 19/06 Solidifying liquids making microcapsules B01J13/02
• CPC Class Codes: C30B 35/00 Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
• CPC Class Codes: C30B 7/10 by application of pressure, e.g. hydrothermal processes

Abstract

An apparatus to contain the reaction vessel in which gallium nitride crystals (henceforth referred to as bulk crystals) can be grown using the ammonothermal method at high pressure and temperature is disclosed. The apparatus provides adequate containment in all directions, which, for a typical cylindrical vessel, can be classified as radial and axial. Furthermore, depending on the specifics of the design parameters, the apparatus is capable of operating at a temperature up to 1,200 degrees Celsius, a pressure up to 2,000 MPa, and for whatever length of time is necessary to grow satisfactory bulk crystals. The radial constraint in the current disclosure is provided by using several stacked composite rings. The design of the apparatus is scalable to contain reaction volumes larger than 100 cubic centimeters.

Claims

1. An apparatus for processing material at elevated pressure, the apparatus comprising:

an upper crown member;

a lower crown member;

an upper die restraint member;

a lower die restraint member, said upper and lower die restraint members being disposed between said upper and lower crown members;

one or more radial restraint structures disposed between the upper die restraint member and the lower die restraint member, said radial restraint structures defining an interior region configured to receive a processing chamber, said radial restraint structures being configured to resist an outward radial force as a result of pressure in said processing chamber, said upper and lower crown members being disposed axially on either end of said interior region and configured to resist an outward axial force as a result of pressure in said processing chamber;

one or more first connecting members coupling the upper crown member and the lower die restraint member; and

one or more second connecting members coupling the lower crown member and the upper die restraint member,

wherein the first and second connecting members are configured for an axial restraint of the stack of radial restraint structures by transferring at least a portion of an outward axial force applied to said upper and lower crown members as a result of pressure in said processing chamber to said first and second connecting members, thereby compressively loading said radial restraint structures between said upper and lower die restraint members.

2. The apparatus of claim 1, further comprising one or more third connecting members coupling the upper crown member and the upper crown member.

3. The apparatus of claim 1, further comprising said a processing chamber disposed within said interior region.

4. The apparatus of claim 3, wherein a heater is disposed between the processing chamber and the one or more radial restraint structures.

5. The apparatus of claim 1, wherein the at least one radial restraint structures comprises a stack of two or more ring assemblies, the two or more ring assemblies comprising a high strength enclosure ring and a ceramic ring or ceramic radial segment assembly.

19. The apparatus of claim 1, wherein said first and second connecting members are tie rods.

20. The apparatus of claim 1, wherein at least one of said first and second die restraint members does not provide radial restraint.

21. The apparatus of claim 1, further comprising first and second plugs between said processing chamber and said upper and lower crown members.

22. The apparatus of claim 2, wherein a portion of said outward axial force applied to said upper and lower crown members is transferred to said third connection members.

6. An apparatus for growing a gallium and nitrogen containing material, the apparatus comprising:

a first crown plate structure comprising an opening region, the opening region comprising a first pattern configured to insert a capsule device there through;

a second crown plate structure operably coupled to the first crown plate structure to maintain a processing region between the first crown plate structure and the second crown plate structure, the processing region configured to house a capsule device; and

a crown insert structure configured to plug the opening region, the crown insert structure comprising a second pattern complementary with the first pattern, the second pattern configured to be insertable into the first pattern for plugging the opening region when the crown insert structure is moved in a direction normal to the first crown structure; and

the second pattern configured to be off-set from the first pattern when rotated in a predetermined manner while the crown insert is engaged with the first pattern in the opening region such that the crown insert is substantially held in place with the first crown plate structure to plug the opening region and support an axial load.

7. The apparatus of claim 6, wherein the first pattern comprises a first pair of opposing extension regions and the second pattern comprises a second pair of opposing extension regions.

8. The apparatus of claim 6, wherein the first pattern comprises a plurality of first extension regions and the second pattern comprises a plurality of second extension regions.

9. The apparatus of claim 6, wherein each of the first crown plate structure the second crown plate structure, and the crown insert structure comprise a material independently selected from steel, low-carbon steel, SA723 steel, SA266 carbon steel, 4340 steel, A-286 steel, iron based superalloy, 304 stainless steel, 310 stainless steel, 316 stainless steel, 340 stainless steel, 410 stainless steel, 17-4 precipitation hardened stainless steel, nickel and its alloys or superalloys, and cobalt and its alloys or superalloys.

10. The apparatus of claim 6, wherein an angle between a normal to planes of contact between the first pattern and the second pattern and a normal to the first crown plate structure lies between about 5 degrees and about 60 degrees.

11. The apparatus of claim 6, wherein the axial load is greater than about 500 tons.

12. An apparatus for growth of a gallium and nitrogen containing material, the apparatus comprising:

a first crown plate structure comprising an opening region, the opening region comprising a first pattern configured to insert a capsule device there through, the first pattern comprising a first open region in communication with a second open region, the second open region being larger than the first open region;

a second crown plate structure operably coupled to the first crown structure to maintain a processing region between the first crown plate structure and the second crown plate structure, the processing region being capable of housing a capsule device; and

a crown insert device configured to plug the opening region, the crown insert device comprising a plug member, a plurality of locking members, and at least one key member, the plurality of locking members being configured with the key member to hold the plug member within a vicinity of the opening region to plug the opening region with the crown insert device and support an axial load.

13. The apparatus of claim 12, wherein the plug member is configured as a truncated pyramid shape.

14. The apparatus of claim 12, wherein each of the plurality of locking members is configured as a sleeve to be disposed between a portion of the plug member and the first pattern.

15. The apparatus of claim 12, wherein the at least one key member comprises a square shape or a rectangular shape.

16. The apparatus of claim 12, wherein each of the first crown plate structure, the crown insert structure, and the second crown structure comprise a material independently selected from steel, low-carbon steel, SA723 steel, SA266 carbon steel, 4340 steel, A-286 steel, iron based superalloy, 304 stainless steel, 310 stainless steel, 316 stainless steel, 340 stainless steel, 410 stainless steel, 17-4 precipitation hardened stainless steel, nickel and its alloys or superalloys, and cobalt and its alloys or superalloys.

17. The apparatus of claim 12, wherein the angle between the normal to the planes of contact between the plug member and the locking members and the normal to the first crown plate structure lies between about 5 degrees and about 60 degrees.

18. The apparatus of claim 12, wherein the axial load is greater than about 500 tons.