Methods for producing GaN nutrient for ammonothermal growth
원문보기
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
C30B-025/02
C30B-025/00
C30B-029/40
C01B-021/06
C30B-007/10
출원번호
US-0624006
(2009-11-23)
등록번호
US-8852341
(2014-10-07)
발명자
/ 주소
Letts, Edward
Hashimoto, Tadao
Ikari, Masanori
출원인 / 주소
Sixpoint Materials, Inc.
대리인 / 주소
K&L Gates, LLP
인용정보
피인용 횟수 :
4인용 특허 :
30
초록▼
The present invention discloses methods to produce large quantities of polycrystalline GaN for use in the ammonothermal growth of group III-nitride material. High production rates of GaN can be produced in a hydride vapor phase growth system. One drawback to enhanced polycrystalline growth is the in
The present invention discloses methods to produce large quantities of polycrystalline GaN for use in the ammonothermal growth of group III-nitride material. High production rates of GaN can be produced in a hydride vapor phase growth system. One drawback to enhanced polycrystalline growth is the increased incorporation of impurities, such as oxygen. A new reactor design using non-oxide material that reduces impurity concentrations is disclosed. Purification of remaining source material after an ammonothermal growth is also disclosed. The methods described produce sufficient quantities of polycrystalline GaN source material for the ammonothermal growth of group III-nitride material.
대표청구항▼
1. A method for producing polycrystalline group III nitride comprising: (a) contacting a gaseous hydrogen halide with a group III element source material in a first heated region to produce a group III halide gas; (b) contacting the group III halide gas with ammonia gas in a growth region, the gaseo
1. A method for producing polycrystalline group III nitride comprising: (a) contacting a gaseous hydrogen halide with a group III element source material in a first heated region to produce a group III halide gas; (b) contacting the group III halide gas with ammonia gas in a growth region, the gaseous group III halide gas migrating from the first heated region to the growth region; and (c) producing a crystalline group III nitride in the growth region positioned downstream of the first heated region, wherein greater than 80% of the total produced group III nitride is polycrystalline group III nitride. 2. The method of claim 1, wherein the group III element is Ga; the group III halide gas is GaXz, where X is a halide and z is an integer from 1 to 3; and the group III nitride is GaN. 3. The method of claim 1, wherein the hydrogen halide is hydrogen chloride. 4. The method of claim 2, wherein the Ga source material is selected from the group consisting of metallic Ga, liquid Ga, Ga powder, Ga pellets, Ga granules, Ga wire, Ga rods and mixtures of any thereof. 5. The method of claim 2, wherein at least 90% of the total produced GaN is polycrystalline GaN. 6. The method of claim 1, wherein all surfaces in direct contact with the gases in one or both of the first heated region and the growth region are of a non-oxide material. 7. The method of claim 6, wherein the non-oxide material is pyrolytic boron nitride. 8. The method of claim 1, wherein the oxygen content of the polycrystalline group III nitride is less than 1019 atoms/cm3. 9. The method of claim 1, wherein the oxygen content of the polycrystalline group III nitride is less than 1017 atoms/cm3. 10. The method of claim 1, wherein the temperature of the first heated region and the temperature of the growth region are greater than 700° C. 11. The method of claim 1, wherein the polycrystalline group III nitride is produced at a rate of greater than 5 g/hr. 12. The method of claim 1, wherein greater than 70% of the group III element source material is converted to polycrystalline group III nitride. 13. The method of claim 1, wherein producing the crystalline group III nitride comprises crystallizing the crystalline group III nitride on a back etched surface of a polycrystalline group III nitride base material. 14. The method of claim 13, wherein the polycrystalline group III nitride base material comprises recycled polycrystalline group III nitride from an ammonothermal process. 15. The method of claim 13, wherein the polycrystalline group III nitride base material is pyrolytic boron nitride. 16. The method of claim 13, wherein the polycrystalline group III nitride base material comprises pyrolytic boron nitride and recycled polycrystalline group III nitride from an ammonothermal process. 17. The method of claim 1, further comprising: submitting the polycrystalline group III nitride to an ammonothermal process to produce single-crystal group III nitride. 18. A reactor for growing polycrystalline GaN comprising: a first heated region comprising a first gas inlet configured to introduce a nitrogen-containing gas; a second heated region comprising a second gas inlet configured to introduce a Ga halide-containing gas, the first heated region and the second heated region being configured to maintain separation of the gases in each region; and a growth region downstream of the first heated region and the second heated region, the growth region being in gaseous contact with the first heated region and the second heated region and configured to allow growth of polycrystalline GaN. 19. The reactor of claim 18, wherein the growth region has a surface configured to contact the gases and formed of a material other than an oxide. 20. The reactor of claim 19, wherein the material comprises pyrolytic boron nitride. 21. The reactor of claim 18, wherein the halide-containing gas comprises HCl. 22. The reactor of claim 21, wherein the second heated region is further configured to contain a gallium source material in contact with the halide containing gas. 23. The reactor of claim 18, wherein the halide-containing gas comprises GaClz where z is an integer from 1-3. 24. Polycrystalline GaN formed by the method of claim 1. 25. The method of claim 13, wherein the group III element is Ga; the group III halide gas is GaXz, where X is a halide and z is an integer from 1 to 3; and the group III nitride is GaN. 26. The method of claim 13, wherein the hydrogen halide is hydrogen chloride. 27. The method of claim 25, wherein the Ga source material is selected from the group consisting of metallic Ga, liquid Ga, Ga powder, Ga pellets, Ga granules, Ga wire, Ga rods and mixtures of any thereof. 28. The method of claim 25, wherein at least 90% of the total produced GaN is polycrystalline GaN. 29. The method of claim 13, wherein all surfaces in direct contact with the gases in one or both of the first heated region and the growth region are of a non-oxide material. 30. The method of claim 29, wherein the non-oxide material is pyrolytic boron nitride. 31. The method of claim 13, wherein the oxygen content of the polycrystalline group III nitride is less than 1019 atoms/cm3. 32. The method of claim 13, wherein the oxygen content of the polycrystalline group III nitride is less than 1017 atoms/cm3. 33. The method of claim 13, wherein the temperature of the first heated region and the temperature of the growth region are greater than 700° C. 34. The method of claim 13, wherein the polycrystalline group III nitride is produced at a rate of greater than 5 g/hr. 35. The method of claim 13, wherein greater than 70% of the group III element source material is converted to polycrystalline group III nitride. 36. The reactor of claim 18, wherein the first and second heated regions are positioned in a first portion of a chamber of the reactor, the growth region is positioned in a remaining portion of the chamber of the reactor, and the first portion of the chamber is separated from the remaining portion to prevent having a mixture of the nitrogen-containing gas and the halide-containing gas in the first portion of the chamber. 37. The method of claim 1, wherein the first heated region comprises a first portion of a chamber of a reactor, the growth region is positioned in a remaining portion of the chamber of the reactor, wherein the ammonia gas and a halide gas comprised of at least one of the hydrogen halide gas and the group III halide gas are heated in said first portion of the chamber, and the remaining portion of the chamber is separated from said first portion of the chamber to prevent having a gas mixture in said first portion of the chamber, said gas mixture being comprised of the ammonia gas and the halide gas.
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