Capsule for high pressure, high temperature processing of materials and methods of use

• US 10,029,955 B1
• Filed: 10/22/2012
• Issued: 07/24/2018
• Est. Priority Date: 10/24/2011
• Status: Active Grant

• Current Assignee: SL Technology Incorporated (Reliv' International, Inc.)
• Original Assignee: SL Technology Incorporated (Reliv' International, Inc.)
• Inventors: Rajeev, Pakalapati Tirumala, Pocius, Douglas Wayne, Kamber, Derrick S., Coulter, Michael
• Primary Examiner(s): Qian, Yun
• Application Number:
  US13/657,551
• Time in Patent Office: 2,101 Days
• CPC Class Codes: B01J 21/06 Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
• CPC Class Codes: C07B 33/00 Oxidation in general
• CPC Class Codes: C30B 29/38 Nitrides
• CPC Class Codes: C30B 29/40 AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
• 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 35/002 Crucibles or containers
• 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

Abstract

An improved capsule and method of use for processing materials or growing crystals in supercritical fluids is disclosed. The capsule is scalable up to very large volumes and provides for cost-effective processing. In conjunction with suitable high pressure apparatus, the capsule is capable of processing materials at pressures and temperatures of up to approximately 8 GPa and 1500° C., respectively.

Claims

1. A method for preparing a crystalline material in a supercritical fluid, the method comprising:

disposing a process capsule into an interior volume of a support capsule, the process capsule comprising a first material and the support capsule comprising a second material;

loading at least one fluid into said process capsule;

sealing the process capsule, wherein the process capsule is sealed and the support capsule is left unsealed, said at least one fluid generating internal pressure in said sealed process capsule, said support capsule providing structural support for said sealed process capsule, enabling said sealed process capsule to be pressurized to 150 psi;

disposing said support capsule containing said sealed process capsule in a high pressure apparatus; and

heating the process capsule to a temperature between room temperature and 1500°

C. to generate the supercritical fluid within the process capsule to form a crystalline material within the process capsule.

2. The method of claim 1, wherein the crystalline material comprises a [III-]nitride of a croup III element of the periodic table selected from GaN, AlN, InN, an alloy of any of the foregoing, and a combination of any of the foregoing.

3. The method of claim 1, further comprising removing thermal energy from the process capsule, wherein removing energy from the process capsule comprises reducing the temperature of the process capsule.

4. The method of claim 1, wherein sealing the process capsule is selected from welding, tungsten inert gas (TIG) welding, orbital welding, arc welding, e-beam welding, ultrasonic welding, magnetic pulse welding, torch welding, vibratory welding, pinch sealing, brazing, and cold welding.

5. The method of claim 1, wherein disposing said process capsule in said support capsule comprises attaching a cap device by at least one of welding, tungsten inert gas (TIG) welding, orbital welding, arc welding, e-beam welding, ultrasonic welding, magnetic pulse welding, torch welding, vibratory welding, pinch sealing, brazing, cold welding and the use of fasteners, bolts, threads, retaining rings, constant section rings, threaded screws, springs, or wave springs.

6. The method of claim 5, wherein the attaching comprises orbital welding of a butt joint.

7. The method of claim 1, further comprising providing a material disposed between the process capsule and the support capsule, the material selected from steel, stainless steel, carbon steel, nickel, nickel alloy, nickel-chromium and iron alloy, nickel-molybdenum-chromium alloy, polycrystalline nickel alloy, nickel-copper alloy, cobalt-chromium alloy, copper, copper alloy, zirconium, niobium, molybdenum, molybdenum disulfide, tantalum, tungsten, rhenium, platinum, platinum alloy, palladium, iridium, ruthenium, rhodium, rhenium, osmium, tantalum, titanium, vanadium, chromium, iron, iron alloy, gold, silver, aluminum, graphite, boron nitride, beryllium, magnesium, calcium, strontium, barium, lithium, rubidium, cesium, MC_xN_yO_z, wherein M is at least one of aluminum, boron silicon, titanium, vanadium, chromium, yttrium, zirconium, lanthanum, a rare earth metal, hafnium, tantalum, tungsten, and wherein each of x, y, and z is between 0 and 3 (i.e., 0<

x, y, z<

3), and a combination of any of the foregoing.

8. The method of claim 1, further comprising providing a material disposed between the support capsule and a pressure apparatus, the material selected from steel, stainless steel, carbon steel, nickel, nickel alloy, nickel-chromium and iron alloy, nickel-molybdenum-chromium alloy, polycrystalline nickel alloy, nickel-copper alloy, cobalt-chromium alloy, copper alloy, zirconium, niobium, molybdenum, molybdenum disulfide, tantalum, tungsten, rhenium, platinum, platinum alloy, palladium, iridium, ruthenium, rhodium, rhenium, osmium, tantalum, titanium, vanadium, chromium, iron, ion alloy, gold, silver, aluminum, graphite, boron nitride, beryllium, magnesium, calcium, strontium, barium, lithium, rubidium, cesium, and a combination of any of the foregoing.

9. The method of claim 1, wherein said second material is selected from steel, stainless steel, carbon steel, nickel, nickel alloy, nickel-chromium and iron alloy, nickel-molybdenum-chromium alloy, polycrystalline nickel alloy, nickel-copper alloy, cobalt-chromium alloy, copper, copper alloy, zirconium, niobium, molybdenum, tantalum, tungsten, rhenium, platinum, platinum alloy, palladium, iridium, ruthenium, rhodium, osmium, titanium, vanadium, chromium, chromium alloy, iron, iron alloy, gold, silver, aluminum, and a combination of any of the foregoing.

10. The method of claim 1, wherein said first material is selected from copper, copper alloy, gold, silver, palladium, platinum, platinum alloy, iridium, ruthenium, rhodium, osmium, titanium, vanadium, chromium, chromium alloy, iron, iron alloy, nickel, nickel alloy, zirconium, niobium, molybdenum, tantalum, tungsten, rhenium, and a combination of any of the foregoing.

11. The method of claim 1, further comprising providing a first fluid disposed between the process capsule and the support capsule, or providing a second fluid disposed between the support capsule and a pressure apparatus, the first fluid and the second fluid independently selected from air, oxygen, hydrogen, ammonia, argon, water, nitrogen, helium, nitrous oxide, carbon dioxide, methane, ethane, propane, ethylene, propylene, methanol, isopropanol, acetic acid, benzene, toluene, ethanol, acetone, and a combination of any of the foregoing.

12. The method of claim 1, further comprising disposing a baffle between a first region of the interior volume and a second region of the interior volume.

13. The method of claim 1, further comprising forming of a wafer from the crystalline material.

14. The method of claim 13, further comprising forming a device on the wafer.

15. The method of claim 1, wherein said second material is less expensive than said first material.

16. The method of claim 1, wherein the wall thickness of said support capsule is greater than the wall thickness of said process capsule.

17. The method of claim 1, wherein said process capsule comprises a fill tube extending from a first open end through which the fluid is passed to fill an interior volume of the process capsule.

18. The method of claim 17, wherein sealing comprising pinching said fill tube.

19. The method of claim 1, wherein loading said at least one fluid is performed at below room temperature.

20. The method of claim 1, wherein said at least one fluid expands said process capsule at room temperature.

21. The method of claim 1, wherein said second material is less inert than said first material to the supercritical fluid.

22. The method of claim 1, wherein the second material has a higher yield strength than the first material.

23. The method of claim 1, wherein the second material has a higher Young'"'"'s modulus than the first material.

24. The method of claim 1, wherein the process capsule is mechanically coupled to a wall of the support capsule.