High pressure apparatus and method for nitride crystal growth

• US 8,871,024 B2
• Filed: 01/25/2011
• Issued: 10/28/2014
• Est. Priority Date: 06/05/2008
• Status: Active Grant

• Current Assignee: SL Technology Incorporated (Reliv' International, Inc.)
• Original Assignee: Soraa, Inc.
• Inventors: D'Evelyn, Mark P.
• Primary Examiner(s): Kunemund, Bob M
• Application Number:
  US13/013,697
• Publication Number:
  US 20110183498A1
• Time in Patent Office: 1,372 Days
• Field of Search: 117/68, 117/69, 117/70, 117/201
• US Class Current: 117/68
• CPC Class Codes: B01J 2203/0665 Gallium nitrides
• CPC Class Codes: B01J 2203/067 Aluminium nitrides
• CPC Class Codes: B01J 2203/068 Crystal growth
• CPC Class Codes: B01J 3/008 Processes carried out under supercritical conditions
• CPC Class Codes: B01J 3/042 in the form of a tube
• CPC Class Codes: B01J 3/065 Presses for the formation of diamonds or boronitrides
• CPC Class Codes: C30B 29/403 AIII-nitrides
• CPC Class Codes: C30B 29/406 Gallium nitride
• CPC Class Codes: C30B 7/10 by application of pressure, e.g. hydrothermal processes
• CPC Class Codes: Y02P 20/54 using solvents, e.g. supercritical solvents or ionic liquids
• CPC Class Codes: Y10T 117/1004 with means for measuring, testing, or sensing
• CPC Class Codes: Y10T 117/1024 for crystallization from liquid or supercritical state

Abstract

An improved high pressure apparatus and methods for processing supercritical fluids is described. The apparatus includes a capsule, a heater, and at least one ceramic ring contained by a metal sleeve. The apparatus is capable of accessing pressures and temperatures of 0.2-2 GPa and 400-1200° C.

Claims

1. Apparatus for high pressure material processing, the apparatus comprising:

a cylindrical capsule region including a first region and a second region, having a length between the first region and the second region;

a heating member enclosing the cylindrical capsule region;

a sleeve member adapted to form a sealed region enclosing the heating member, the sealed region being characterized by an internal pressure level capable of tightening a contact between the sleeve member and a seal;

a gas pressure intensifier for pumping gaseous species into the sealed region at a predetermined range of pressure levels;

at least one annular ceramic member having a predetermined thickness disposed continuously around a perimeter of the sleeve member, the annular member being made of a material having a compressive strength of at least 0.5 GPa and having a thermal conductivity of less than about 4 watts per meter-Kelvin; and

a high strength enclosure material over the annular ceramic member to form a high strength enclosure.

2. The apparatus of claim 1 further comprising a control module to control an amount of a gaseous species to be pumped into the sealed region by the gas pressure intensifier based.

3. The apparatus of claim 1 further comprising a temperature sensor positioned within the heating member in proximity to the cylindrical capsule region.

4. The apparatus of claim 1 wherein the gaseous species comprises an inert gas.

5. The apparatus of claim 1 further comprising a displacement sensor positioned within the heating member in proximity to the cylindrical capsule region.

6. The apparatus of claim 1 wherein the seal comprises at least one grand nuts.

7. The apparatus of claim 1 wherein the seal and the sleeve member form a Bridgman seal, a modified Bridgman seal, a Grayloc™

seal, an o-ring seal, a confined gasket seal, a bolted closure, an AE™

closure, an EZE-Seal™

, a Keuntzel closure, a ZipperClave™

closure, a threadless pin closure, or a Gasche™

gasket seal.

8. The apparatus of claim 1 wherein the cylindrical capsule region comprises a capsule member.

9. The apparatus of claim 1 wherein the cylindrical capsule region comprises a liner member.

10. The apparatus of claim 1 wherein the annular ceramic member comprises a plurality of wedge-shaped radial ceramic members.

11. The apparatus of claim 1 wherein the annular ceramic member comprises a continuous annular ceramic member.

12. The apparatus of claim 1 wherein the cylindrical capsule region comprises a baffle member.

13. The apparatus of claim 1 wherein the seal comprises a plunger, a grand nut, a gasket, or a plug.

14. The apparatus of claim 9, wherein the interior of the liner member is accessible to at least a valve and a pressure transducer.

15. The apparatus of claim 14, further comprising a plunger having an upward-trending element forming an angle a from the horizontal between about 2 degrees and about 88 degrees.

16. A method for operating a high pressure crystal growth apparatus, the method comprising:

providing an apparatus for high pressure material processing, the apparatus comprising a cylindrical capsule having a first region and a second region, and a length defined between the first region and the second region, an annular heating member enclosing the capsule, a sleeve enclosing the annular heating member having predetermined thickness disposed continuously around the sleeve, and a high strength enclosure material disposed over the annular member;

placing a baffle, nutrient, mineralizer, and a plurality of seed crystals within the capsule or liner;

forming a gas-tight seal between each of regions of the cylindrical capsule or liner, the environment of the annular heating member, and the exterior of the apparatus;

filling a predetermined fraction of the interior of the capsule or liner with a solvent and sealing the capsule or liner;

filling one or more inert gases into the environment of the annular heating member;

processing the cylindrical capsule or liner with a thermal energy to cause an increase in temperature within the capsule or liner to greater than 200 Degrees Celsius to cause the solvent to be heat to a superheated state;

forming a crystalline material from a process of the superheated solvent;

removing thermal energy from the cylindrical capsule or liner to cause a temperature of the liner to change from a first temperature to a second temperature, the second temperature being lower than the first temperature;

removing the solvent from the capsule or liner;

opening a top portion of the apparatus;

exposing at least one region of the cylindrical capsule or liner; and

removing the crystalline material.

17. The method of claim 16 wherein the plurality of seed crystals comprises at least 10 seed crystals.

18. The method of claim 16 wherein the annular member comprises one continuous ceramic, annular metal, cermet member, or a set of radial wedge segments.

19. The method of claim 16 further comprising forming the crystalline material into one or more wafers and forming one or more devices on the one or more wafers.

20. The method of claim 19 wherein the one or more devices comprises an optoelectronic or electronic device selected from among a light emitting diode, a laser diode, a photodetector, an avalanche photodiode, a transistor, a rectifier, and a thyristor;

one of a transistor, a rectifier, a Schottky rectifier, a thyristor, a p-i-n diode, a metal-semiconductor-metal diode, high-electron mobility transistor, a metal semiconductor field effect transistor, a metal oxide field effect transistor, a power metal oxide semiconductor field effect transistor, a power metal insulator semiconductor field effect transistor, a bipolar junction transistor, a metal insulator field effect transistor, a heterojunction bipolar transistor, a power insulated gate bipolar transistor, a power vertical junction field effect transistor, a cascode switch, an inner sub-band emitter, a quantum well infrared photodetector, a quantum dot infrared photodetector, a solar cell, and a diode for photoelectrochemical water splitting and hydrogen generation.