High pressure apparatus and method for nitride crystal growth

• US 9,157,167 B1
• Filed: 07/23/2012
• Issued: 10/13/2015
• 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., Pakalapati, Rajeev T.
• Primary Examiner(s): Kunemund, Robert M
• Application Number:
  US13/556,105
• Time in Patent Office: 1,177 Days
• US Class Current: 1/1
• 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: B30B 11/002 Isostatic press chambers; Press stands therefor
• CPC Class Codes: B30B 11/005 Control arrangements
• 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 117/10 Apparatus
• CPC Class Codes: Y10T 117/1024 for crystallization from liquid or supercritical state
• CPC Class Codes: Y10T 117/1096 including pressurized crystallization means [e.g., hydrothermal]

Abstract

A high pressure apparatus and related methods for processing supercritical fluids are disclosed. In certain embodiments, the present apparatus includes a capsule, a heater, at least one ceramic ring or multiple rings, optionally, with one or more scribe marks and/or cracks present. In certain embodiments, the apparatus has a metal sleeve containing each ceramic ring. The apparatus also has a high strength enclosure, end flanges with associated insulation, and a power control system. In certain embodiments, a high pressure apparatus is constructed such that the diametric annular gap between the outer diameter of the heater and the ceramic ring is selected to provide radial load-bearing contact above a particular temperature and pressure. In certain embodiments, the apparatus is capable of accessing pressures of 0.2 GPa to 2 GPa and temperatures of 400° C. to 1200° C.

Claims

1. An apparatus for high pressure material processing comprising:

a cylindrical capsule opening for retaining a capsule having a length;

an annular heating member having a length and an outer diameter, and surrounding at least a portion of the length of the capsule opening;

a radial heater restraint surrounding at least a portion of the length of the annular heating member, the radial heater restraint having an inner diameter and comprising a high strength enclosure; and

an annular gap defined by the outer diameter of the annular heating member and the inner diameter of the radial heater restraint, wherein the annular gap is at least 0.005 inch at room temperature and is configured to provide a radial load-bearing contact between the annular heating member and the radial heater restraint at a temperature not less than about 100 degrees Celsius.

2. The apparatus of claim 1, wherein the radial heater restraint comprises at least one annular ceramic member disposed continuously around a perimeter of the annular heating member, the at least one annular ceramic member comprising a material having a compressive strength of at least about 0.5 GPa and a thermal conductivity of less than about 100 watts per meter-Kelvin, and the high strength enclosure surrounds the at least one annular ceramic member.

3. The apparatus of claim 1, wherein the radial heater restraint comprises at least two annular ceramic radial segments arranged sequentially and disposed continuously around a perimeter of the annular heating member, the at least two annular ceramic radial segments comprising a material having a compressive strength of at least about 0.5 GPa and a thermal conductivity of less than about 100 watts per meter-Kelvin, and wherein the high strength enclosure surrounds the at least two annular radial segments.

4. The apparatus of claim 1, further comprising a capsule disposed within the capsule, wherein the capsule comprises a material selected from gold, platinum, silver, palladium, rhodium, titanium, rhenium, copper, stainless steel, zirconium, tantalum, and an alloy of any of the foregoing.

5. The apparatus of claim 2, further comprising a cylindrical sleeve having an outer diameter disposed between the at least one annular ceramic member and the high strength enclosure, wherein the cylindrical sleeve comprises a material selected from stainless steel, iron, steel, iron alloy, nickel, nickel alloy, and a combination of any of the foregoing.

6. The apparatus of claim 5, wherein the outer diameter of the cylindrical sleeve is tapered from a first end to a second end opposite to the first end with a taper angle between about 0.1 and about 5 degrees.

7. The apparatus of claim 1, wherein the high strength enclosure has a length, an outer diameter, and an inner diameter, wherein

an aspect ratio of the length to the inner diameter of the high strength enclosure is from about 2 to about 25;

the inner diameter of the high strength enclosure is between about two inches and about fifty inches;

the length of the high strength enclosure is between 6 inches and 500 inches; and

the ratio between the outer diameter of the high strength enclosure and the inner diameter of the high strength enclosure is between 1.2 and 5.

8. The apparatus of claim 1, wherein the radial heater restraint contains at least one crack.

9. A method of crystal growth, the method comprising:

providing an apparatus for high pressure crystal or material processing, the apparatus comprising;

a cylindrical capsule opening for retaining a capsule having a length;

an annular heating member having a length and an outer diameter, and surrounding at least a portion of the length of the capsule opening;

a radial heater restraint surrounding at least a portion of the length of the annular heating member, the radial heater restraint comprising a high strength enclosure; and

an annular gap defined by the outer diameter of the annular heating member and the inner diameter of the radial heater restraint, wherein the annular gap is at least 0.010 inch at room temperature and is configured to provide a radial load-bearing contact between the annular heating member and the radial heater restraint at a temperature not less than about 100 degrees Celsius;

providing a capsule containing a solvent;

placing the capsule within an interior region of the cylindrical capsule; and

processing the capsule with thermal energy to cause an increase in temperature within the capsule to be greater than 200 Degrees Celsius and to cause the solvent to be superheated.

10. The method of claim 9, wherein the radial heater restraint comprises at least one annular ceramic member disposed continuously around a perimeter of the annular heating member, the at least one annular ceramic member comprising a material having a compressive strength of at least about 0.5 GPa and a thermal conductivity of less than about 100 watts per meter-Kelvin, and wherein the high strength enclosure surrounds the at least one annular ceramic member.

11. The method of claim 9, wherein the radial heater restraint comprises at least two annular ceramic radial segments arranged sequentially and disposed continuously around a perimeter of the annular heating member, the at least two annular ceramic radial segments comprising a material having a compressive strength of at least about 0.5 GPa and a thermal conductivity of less than about 100 watts per meter-Kelvin, and wherein the high strength enclosure surrounds the at least two annular ceramic radial segments.

12. The method of claim 9, further comprising forming or recrystallizing a crystalline material from a process of the superheated solvent.

13. The method of claim 12, wherein the crystalline material comprises gallium-containing nitride.

14. The method of claim 9, wherein the annular gap is configured to provide radial load-bearing contact at a temperature not less than about 200 degrees Celsius.

15. A method of crystal growth, the method comprising:

providing an apparatus for high pressure crystal or material processing, the apparatus comprising;

a cylindrical capsule opening for retaining a capsule having a length;

a metal capsule disposed within the capsule opening, wherein the metal capsule contains ammonia and a mineralizer;

an annular heating member having a length and surrounding at least a portion of the length of the capsule opening; and

a radial heater restraint surrounding at least a portion of the length of the annular heating member, the radial heater restraint comprising a high strength enclosure, the radial heater restraint comprising at least one crack;

providing a capsule containing a solvent;

placing the capsule within an interior region of the cylindrical capsule; and

processing the capsule with thermal energy to cause an increase in temperature within the capsule to greater than 200 Degrees Celsius and to cause the solvent to be superheated.

16. The method of claim 15, wherein the radial heater restraint comprises at least one annular ceramic member disposed continuously around a perimeter of the annular heating member, the at least one annular ceramic member comprising a material having a compressive strength of at least about 0.5 GPa and a thermal conductivity of less than about 100 watts per meter-Kelvin, and wherein the high strength enclosure surrounds the at least one annular ceramic member.

17. The method of claim 15, wherein the radial heater restraint comprises at least two annular ceramic radial segments arranged sequentially and disposed continuously around a perimeter of the annular heating member, the at least two annular ceramic radial segments comprising a material having a compressive strength of at least about 0.5 GPa and a thermal conductivity of less than about 100 watts per meter-Kelvin, and wherein the high strength enclosure surrounds the at least two annular ceramic radial segments.

18. The method of claim 15, wherein the crystal or material comprises gallium-containing nitride.

19. An apparatus for high pressure material processing comprising:

a cylindrical capsule opening for retaining a capsule having a length;

an annular heating member having a length and an outer diameter, and surrounding at least a portion of the length of the capsule opening;

a radial heater restraint surrounding at least a portion of the length of the annular heating member, the radial heater restraint comprising a high strength enclosure; and

an annular gap defined by the outer diameter of the annular heating member and the inner diameter of the radial heater restraint, wherein the width of the annular gap is selected to provide a first radial load-bearing contact between the annular heating member and the radial heater restraint at a temperature not less than about 100 degrees Celsius.

20. The apparatus of claim 19, wherein the radial heater restraint comprises at least one annular ceramic member disposed continuously around a perimeter of the annular heating member, the at least one annular ceramic member comprising a material having a compressive strength of at least about 0.5 GPa and a thermal conductivity of less than about 100 watts per meter-Kelvin, and wherein the high strength enclosure surrounds the at least one annular ceramic member.