Method for making crystalline composition
View Patent ↗A method of making a metal nitride is provided. The method may include introducing a metal in a chamber. A nitrogen-containing material may be flowed into the chamber. Further, a hydrogen halide may be introduced. The nitrogen-containing material may react with the metal in the chamber to form the metal nitride.
1. A method, comprising:
flowing a nitrogen-containing material into a chamber defined by a housing;
providing a metal to the chamber in a crucible;
heating the chamber to a determined temperature, and pressurizing the chamber to a determined pressure;
flowing hydrogen halide to the chamber;
mixing the nitrogen-containing material and the hydrogen halide to form a mixture; and
reacting the mixture with the metal in the chamber, forming a metal nitride in the crucible that originally contained the metal.
2. The method as defined in claim 1 , wherein the metal comprises one or more of aluminum, gallium, or indium.
3. The method as defined in claim 1 , wherein the step of flowing a nitrogen-containing material comprises flowing ammonia.
4. The method as defined in claim 1 , wherein the step of reacting the nitrogen-containing material with the metal comprises forming gallium nitride.
5. The method as defined in claim 1 , wherein the step of heating the chamber comprises achieving or maintaining a temperature in the chamber that is in a range of from about 800 degree Celsius to about 1300 degree Celsius for a period of greater than about 30 minutes.
6. The method as defined in claim 1 , wherein the step of pressurizing comprises achieving or maintaining a pressure in the chamber that has at least one dimension that is greater than about 1 meter.
7. The method as defined in claim 1 , wherein the step of providing the metal comprises one or both of preloading the metal in the chamber, or flowing the metal into the chamber.
8. The method as defined in claim 1 , wherein the step of flowing a nitrogen-containing material comprises achieving a flow rate of nitrogen-containing material in a range of from about 100 cubic centimeters per minute to about 1200 cubic centimeters per minute.
9. The method as defined in claim 1 , further comprising setting a ratio of flow rate of the nitrogen-containing material to a flow rate of the hydrogen halide to be in a range of from about 1:1 to about 30:1.
10. The method as defined in claim 1 , further comprising setting a ratio of flow rate of the nitrogen-containing material to a flow rate of the hydrogen halide to be in a range of from about 1:1 to about 15:1.
11. The method as defined in claim 1 , further comprising flowing a carrier gas into the chamber.
12. The method as defined in claim 1 , further comprising flowing one or more dopant precursors into the chamber.
13. The method as defined in claim 12 , further comprising achieving or maintaining a flow rate of the dopant precursor into the chamber to be in a range of from about 100 cubic centimeters per minute to about 1200 cubic centimeters per minute.
14. The method as defined in claim 1 , further comprising evacuating the chamber.
15. The method as defined in claim 14 , further comprising achieving or maintaining a pressure within the chamber to be in a range of less than about 10 −7 millibar.
16. The method as defined in claim 1 , further comprising flowing a fluid in a pathway that is between walls of the housing, and controlling the fluid temperature to control the temperature of contents of the chamber.
17. The method as defined in claim 1 , further comprising maintaining an outlet vent temperature to be greater than about 200 degree Celsius.
18. The method as defined in claim 1 , further comprising processing the metal nitride by one or more of:
scraping, scouring or scarifying a surface of the metal nitride;
oxidizing the surface of the metal nitride in air or in a dry oxygen atmosphere; or
boiling the metal nitride in perchloric acid.
19. The method as defined in claim 18 , further comprising pulverizing the metal nitride into a plurality of seed crystals, each of the seed crystal having an average size to be in a range that is less than about 10 millimeters.
20. The method as defined in claim 19 , wherein pulverizing comprises one or more of wire sawing, ball milling, jet milling, laser cutting, or cryofracturing.
21. The method as defined in claim 1 , further comprising preparing a sputter target from the metal halide by one or both of:
trimming the metal nitride to a shape having one or more pre-determined dimensions; or
removing residual contaminants.
22. The method as defined in claim 21 , wherein the step of removing residual contaminants comprises one or more of:
washing the metal nitride in one or more of organic solvent, acid, base, or oxidizer;
sonicating the metal nitride in one or more of organic solvent, acid, base, or oxidizer; or
annealing the metal nitride in a reduced pressure environment.
23. The method as defined in claim 1 , wherein the nitrogen-containing material and hydrogen halide flows are both upstream of the metal.
24. The method as defined in claim 23 , wherein the nitrogen-containing material and the hydrogen halide pre-mix before contacting the metal.
25. A method, comprising:
flowing a nitrogen-containing gas and a halide-containing gas into a chamber defined by a housing;
mixing the nitrogen-containing gas and the halide-containing gas in the chamber to form a gas mixture;
contacting the gas mixture with a metal in the chamber; and
reacting the nitrogen-containing gas with the metal in the chamber to form a metal nitride and further comprising one or more of:
adding a dopant to a carrier gas and flowing the dopant and carrier gas into the chamber,
purifying one or more of the carrier gas, nitrogen-containing gas, or halide-containing gas immediately prior to flowing the one or more of the carrier gas, nitrogen-containing gas, or halide-containing gas into the chamber,
outgassing the chamber prior to flowing the one or more of the carrier gas, nitrogen-containing gas, or halide-containing gas into the chamber, or
spinning the one or more of the carrier gas, nitrogen-containing gas, or halide-containing gas while flowing the one or more of the carrier gas, nitrogen-containing gas, or halide-containing gas into the chamber.
26. The method as defined in claim 25 , wherein the metal is a liquid during the contacting with the gas mixture, and further comprising flowing the metal into the chamber.
27. The method as defined in claim 25 , further comprising flowing the metal into the chamber, and wherein the metal is a flowable liquid.
28. The method as defined in claim 25 , wherein mixing the nitrogen-containing gas and the halide-containing gas in the chamber to form a gas mixture comprises impinging the nitrogen-containing gas with the halide-containing gas.
29. The method as defined in claim 25 , further comprising maintaining an outlet vent temperature to be greater than about 200 degree Celsius.