Apparatus for processing materials at high temperatures and pressures
View Patent ↗An apparatus for processing materials at high temperatures comprises a high strength enclosure; a plurality of high strength radial segments disposed adjacent to and radially inward from the high strength enclosure; a liner disposed adjacent to and radially inward from the radical segments; a chamber defined interior to the liner; a heating device disposed within the chamber; and a capsule disposed within the chamber, the capsule configured to hold a supercritical fluid. The apparatus may be used for growing crystals, e.g., GaN, under high temperature and pressure conditions.
1. An apparatus comprising:
a high strength enclosure;
a plurality of high strength radial segments disposed adjacent to and radially inward from the high strength enclosure;
a liner disposed adjacent to and radially inward from the high strength radial segments, the liner comprising one of a high temperature steel or a high temperature metal alloy;
a chamber that is defined by an inner surface of the liner;
a heating device disposed within the chamber, the heating device having an outer surface and an inner surface, and defining a cavity radially inward from the inner surface; and
a capsule for growing crystals therein under high temperature and pressure conditions, the capsule being disposed within the cavity of the heating device, and holding reactants and materials, wherein
a first gap is disposed between the liner and the outer surface of the heating device and the inner surface of the liner,
the first gap is configured to be filled with a high-pressure gas, and
the capsule is configured such that there is a second gap between an exterior surface of the capsule and the inner surface of the heating device, and the second gap between the exterior surface of the capsule and the inner surface of the heating device being configured to be filled with a high-pressure gas.
2. The apparatus of claim 1 , wherein the liner comprises a nickel-chromium based super alloy.
3. The apparatus of claim 1 , where the liner has a thickness of about 0.1 mm to 10 mm.
4. The apparatus of claim 1 , wherein the high strength radial segments comprise a material chosen from a ceramic, a refractory metal, a cement, or a combination of two or more thereof.
5. The apparatus of claim 1 , wherein the high strength radial segments comprise a material chosen from alumina, silicon nitride, silicon carbide, zirconia, tungsten, molybdenum, cobalt-cemented tungsten carbide, or a combination of two or more thereof.
6. The apparatus of claim 1 , wherein the high strength radial segments have a wedge shaped structure.
7. The apparatus of claim 1 , comprising a pressure control device configured to adjust (a) a pressure within the capsule, or (b) a surrounding pressure of a pressurized gas within the high strength enclosure in response to sensed environmental conditions within the capsule or high strength enclosure.
8. The apparatus of claim 7 comprising a sensor configured to sense a pressure difference between an interior and an exterior of the capsule.
9. The apparatus of claim 8 , where the capsule has a first coefficient of thermal expansion, the sensor has a second coefficient of thermal expansion, and the second coefficient of thermal expansion is within 35% of the first coefficient of thermal expansion.
10. The apparatus of claim 8 , wherein the sensor physically engages the capsule.
11. The apparatus of claim 8 , wherein the capsule comprises a lid, and the lid is configured such that it has a first region having a first thickness, a second region having a second thickness that is less than the first thickness.
12. The apparatus of claim 11 , wherein the sensor is disposed on the lid of the capsule such that it overlies at least a portion of the second region having the second thickness.
13. The apparatus of claim 7 , comprising a displacement sensor configured to measure deformation of the capsule due to a pressure difference between an interior pressure of the capsule and a surrounding pressure.
14. The apparatus of claim 1 , wherein a sleeve is disposed about the outer surface of the heating device.
15. The apparatus of claim 14 , wherein the sleeve comprises a thermal insulating material.
16. The apparatus of claim 15 , wherein sleeve comprises pyrolytic boron nitride.
17. An apparatus comprising: a high strength enclosure;
a plurality of high strength radial segments disposed adjacent to and radially inward from the high strength enclosure, wherein
the high strength radial segments comprise a material chosen from a ceramic, a refractory metal, a cement, or a combination of two or more thereof;
a liner disposed adjacent to and radially inward from the high strength radial segments;
a chamber that is defined by an inner surface of the liner;
a heating device disposed within the chamber, the heating device having an outer surface an inner surface, and defining a cavity radially inward from the inner surface; and
a capsule for growing crystals therein under high temperature and pressure conditions, the capsule being disposed within the cavity of the heating device, and holding reactants and materials, wherein
a first gap is disposed between the liner and the outer surface of the heating device,
a second gap is disposed between an exterior surface of the capsule and the inner surface of the heating device, and
the first gap and the second gap are configured to be filled with a high-pressure gas.
18. The apparatus of claim 17 where the liner comprises a high temperature steel or a high temperature metal alloy.
19. The apparatus of claim 18 where in the liner comprises a nickel-chromium based super alloy.
20. The apparatus of claim 17 , where the liner has a thickness of about 0.1 mm to 10 mm.
21. The apparatus of claim 17 , wherein the high strength radial segments comprise a material chosen from alumina, silicon nitride, silicon carbide, zirconia, tungsten, molybdenum, cobalt-cemented tungsten carbide, or a combination of two or more thereof.
22. The apparatus of claim 17 , wherein the high strength radial segments have a wedge shaped structure.
23. The apparatus of claim 17 , comprising a pressure control device configured to adjust (a) a pressure within the capsule, or (b) a surrounding pressure of a pressurized gas within the high strength enclosure in response to sensed environmental conditions within the capsule or high strength enclosure.
24. The apparatus of claim 23 comprising a sensor configured to sense a pressure difference between an interior and an exterior of the capsule.
25. The apparatus of claim 24 , where the capsule has a first coefficient of thermal expansion, the sensor has a second coefficient of thermal expansion, and the second coefficient of thermal expansion is within 35% of the first coefficient of thermal expansion.
26. The apparatus of claim 24 , wherein the sensor physically engages the capsule.
27. The apparatus of claim 24 , wherein the capsule comprises a lid, and the lid is configured such that it has a first region having a first thickness, and a second region having a second thickness that is less than the first thickness.
28. The apparatus of claim 27 , wherein the sensor is disposed on the lid of the capsule such that it overlies at least a portion of the second region having the second thickness.
29. The apparatus of claim 17 , comprising a displacement sensor configured to measure deformation of the capsule due to a pressure difference between an interior pressure of the capsule and a surrounding pressure.
30. The apparatus of claim 18 , wherein a sleeve is disposed about the outer surface of the heating device.
31. The apparatus of claim 30 , wherein the sleeve comprises a thermal insulating material.
32. The apparatus of claim 31 , wherein sleeve comprises pyrolytic boron nitride.
33. The apparatus of claim 1 , wherein the apparatus is configured to increase the operating condition within the capsule to a pressure of about 5 kbar or greater and a temperature of about 550° C. or greater.
34. The apparatus of claim 1 comprising a gallium nitride crystal, wherein the gallium nitride crystal is grown in super critical ammonia.
35. A method of growing a crystal, comprising reacting a seed crystal and a nutrient material under temperature and pressure conditions sufficient to facilitate crystal growth, where the method is conducted in an apparatus of claim 1 .
36. The method of claim 35 , comprising reacting the seed crystal and nutrient at a temperature of about 550° C. or greater and a pressure of about 5 kbar or greater.
37. The apparatus of claim 1 , wherein the liner has a cylindrical shape and two opposing ends, and the apparatus further comprises:
end caps that are disposed at the two opposing ends of the liner to form a sealed environment surrounding the heating device and the capsule.