High pressure apparatus and method for nitride crystal growth

• US 8,986,447 B2
• Filed: 01/04/2012
• Issued: 03/24/2015
• 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.
• Primary Examiner(s): Kunemund, Bob M
• Application Number:
  US13/343,563
• Publication Number:
  US 20120118223A1
• Time in Patent Office: 1,175 Days
• Field of Search: 117/68, 117/70, 117/200, 117/206
• 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: 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. In a specific embodiment, the present apparatus includes a capsule, a heater, at least one ceramic ring but can be multiple rings, optionally, with one or more scribe marks and/or cracks present. In a specific embodiment, the apparatus optionally 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 a specific embodiment, the apparatus is capable of accessing pressures and temperatures of 0.2-2 GPa and 400-1200° C., respectively.

Claims

1. An apparatus for crystal growth comprising:

a cylindrical capsule region for containing a cylindrical capsule within which a crystal is to be grown under elevated pressure and temperature, the cylindrical capsule region having a length and ends;

an annular heating member enclosing the length of the cylindrical capsule region for heating the contents of the cylindrical capsule to an elevated temperature to create an elevated pressure within the capsule;

at least one annular ceramic member disposed around the annular heating member, wherein the at least one annular ceramic member comprises one or more of a rare earth metal oxide, zirconium oxide, hafnium oxide, magnesium oxide, calcium oxide, aluminum oxide, yttrium oxide, sialon (Si—

Al—

O—

N), silicon nitride, silicon oxynitride, garnets, cristobalite, and mullite; and

an enclosure disposed around all of the at least one annular ceramic members.

2. Apparatus as in claim 1 wherein the annular heating member is substantially rigid.

3. Apparatus as in claim 1 wherein the annular heating member is disposed in contact with the cylindrical capsule.

4. Apparatus as in claim 1 wherein the annular heating member is disposed in contact with the at least one annular ceramic member.

5. Apparatus as in claim 1 further comprising a cylindrical sleeve surrounding at least one annular ceramic member.

6. Apparatus as in claim 5 wherein the cylindrical sleeve applies compressive force to the at least one annular ceramic member.

7. Apparatus as in claim 5 wherein the cylindrical sleeve comprises a material selected from steel, iron, nickel, and alloys thereof.

8. Apparatus as in claim 1 wherein the enclosure comprises a material selected from a group consisting of steel, zirconium, titanium, Monel, Inconel, Hastelloy, Udimet 50, Stellite, Rene 41, and Rene 88.

9. Apparatus as in claim 1 wherein the inner diameter is between about two inches and about fifty inches.

10. An apparatus for crystal growth comprising:

a cylindrical capsule region for containing a cylindrical capsule within which a crystal is to be grown under elevated pressure and temperature, the cylindrical capsule region having a length and ends;

an annular heating member enclosing the length of the cylindrical capsule region for heating the contents of the cylindrical capsule to an elevated temperature to create an elevated pressure within the capsule;

at least two stacked annular ceramic or cermet or metal members disposed around the annular heating member, wherein each of the at least two annular ceramic or cermet or metal members are made of a material having a compressive strength of about 0.5 GPa and greater; and

an enclosure disposed around all of the at least two annular ceramic members.

11. Apparatus as in claim 10 wherein the annular heating member is substantially rigid.

12. Apparatus as in claim 10 wherein the annular heating member is disposed in contact with the cylindrical capsule.

13. Apparatus as in claim 10 wherein the annular heating member is disposed in contact with the at least two annular ceramic or cermet or metal members.

14. Apparatus as in claim 10 further comprising a cylindrical sleeve surrounding each of the at least two annular ceramic or cermet or metal members.

15. Apparatus as in claim 14 wherein the cylindrical sleeve applies compressive force to the at least two annular ceramic or cermet or metal members.

16. Apparatus as in claim 14 wherein the cylindrical sleeve comprises a material selected from steel, iron, nickel, and alloys thereof.

17. Apparatus as in claim 10 wherein the enclosure comprises a material selected from a group consisting of steel, zirconium, titanium, Monel, Inconel, Hastelloy, Udimet 500, Stellite, Rene 41, and Rene 88.

18. Apparatus as in claim 10 wherein the inner diameter is between about two inches and about fifty inches.

19. A method of crystal growth comprising:

providing an apparatus for crystal growth which includes;

a cylindrical capsule within which a crystal is to be grown under elevated pressure and temperature, the cylindrical capsule region having a length and ends;

an annular heating member enclosing the length of the cylindrical capsule for heating the contents of the cylindrical capsule to an elevated temperature to create an elevated pressure within the capsule;

at least one annular ceramic member disposed around the annular heating member, each of the at least one annular ceramic members comprising one or more of a rare earth metal oxide, zirconium oxide, hafnium oxide, magnesium oxide, calcium oxide, aluminum oxide, yttrium oxide, sialon (Si—

Al—

O—

N), silicon nitride, silicon oxynitride, garnets, cristobalite, and mullite; and

an enclosure disposed around all of the at least one annular ceramic members

placing solvent in the capsule;

heating the capsule using the heating member to cause an increase in temperature within the capsule to greater than 200 degrees Celsius to cause the solvent to be superheated; and

slidably removing the capsule from the heating member after completing the crystal growth.

20. The method of claim 19 further comprising forming a crystalline material from the superheated solvent.