Granted Patent B2

US 12,252,812 · App. 18/434,568 · Granted Mar 18, 2025

Inventors: Mark P. D'Evelyn (Vancouver, WA); Paul M. Von Dollen (Brush Prairie, WA); Lisa M. Gay (Vancouver, WA); Douglas W. Pocius (Aguanga, CA); Jonathan D. Cook (Santa Barbara, CA)

Assignee: SLT Technologies, Inc.

C30B7/105C30B29/403

Abstract

Claims (52)

1. A method for growth of group III metal nitride crystals, comprising:

providing a manifold comprising at least two transfer vessels, a first source vessel containing a condensable mineralizer composition comprising HF, a second source vessel containing ammonia, and a receiving vessel;

evacuating the receiving vessel;

transferring a first quantity of the condensable mineralizer composition to a first transfer vessel via a vapor phase and causing condensation of the condensable mineralizer composition within the first transfer vessel;

measuring the first quantity of the condensable mineralizer composition within the first transfer vessel;

transferring a second quantity of the measured first quantity of condensable mineralizer composition from the first transfer vessel to the receiving vessel;

transferring a first quantity of ammonia to a second transfer vessel;

transferring a second quantity of ammonia from the second transfer vessel to the receiving vessel via a liquid phase through a fill tube, wherein the fill tube has an inner diameter greater than 1 millimeter; and

forming at least a portion of a group III metal nitride boule by an ammonothermal crystal growth process that comprises:

exposing a seed crystal to a temperature of at least about 400 degrees Celsius, and

exposing the seed crystal to a mineralizer that is formed from the second quantity of condensable mineralizer composition and the second quantity of ammonia that were transferred to the receiving vessel,

wherein the first transfer vessel is heated to a temperature between 2 degrees Celsius and 50 degrees Celsius higher than a temperature of the receiving vessel during the transfer of the condensable mineralizer composition.

2. The method of claim 1 , wherein the fill tube has an inner diameter greater than 2 millimeters.

3. The method of claim 1 , wherein the first transfer vessel and the fill tube comprise at least one of silver, a silver alloy, Monel® 400, gold, platinum, palladium, rhodium, iridium, or ruthenium.

4. The method of claim 1 , wherein the second quantity of the condensable mineralizer composition is in a liquid phase when transferred from the first transfer vessel to the receiving vessel.

5. The method of claim 1 , wherein the second quantity of ammonia is transferred from the second transfer vessel to the receiving vessel in a liquid phase through a large-throat-diameter valve that comprises a ball valve.

6. The method of claim 1 , wherein liquid ammonia has a pressure higher than 7 atmospheres during the transfer of the second quantity of ammonia from the second transfer vessel to the receiving vessel.

7. A method for growth of group III metal nitride crystals, comprising:

providing a manifold comprising at least two transfer vessels, a first source vessel containing a condensable mineralizer composition comprising HF, a second source vessel containing ammonia, and a receiving vessel;

evacuating the receiving vessel;

transferring a first quantity of the condensable mineralizer composition to a first transfer vessel via a vapor phase and causing condensation of the condensable mineralizer composition within the first transfer vessel;

measuring the first quantity of the condensable mineralizer composition within the first transfer vessel;

transferring a second quantity of the measured first quantity of condensable mineralizer composition from the first transfer vessel to the receiving vessel;

transferring a first quantity of ammonia to a second transfer vessel;

transferring a second quantity of ammonia from the second transfer vessel to the receiving vessel via a liquid phase through a fill tube, wherein the fill tube has an inner diameter greater than 1 millimeter; and

forming at least a portion of a group III metal nitride boule by an ammonothermal crystal growth process that comprises:

exposing a seed crystal to a temperature of at least about 400 degrees Celsius, and

exposing the seed crystal to a mineralizer that is formed from the second quantity of condensable mineralizer composition and the second quantity of ammonia that were transferred to the receiving vessel,

wherein a valve and a connection between the second transfer vessel and the receiving vessel are heated to a temperature between about 25 degrees Celsius and about 250 degrees Celsius during the transfer of the second quantity of ammonia from the second transfer vessel to the receiving vessel.

8. The method of claim 7 , wherein the valve and the connection between the second transfer vessel and the receiving vessel are heated to a temperature between about 30 degrees Celsius and about 100 degrees Celsius during the transfer of the second quantity of ammonia from the second transfer vessel to the receiving vessel.

9. The method of claim 1 , wherein condensation of the condensable mineralizer composition within the first transfer vessel is achieved by chilling a metallic member within the first transfer vessel, wherein the metallic member comprises at least one of silver, a silver alloy, Monel® 400, gold, platinum, palladium, rhodium, iridium, or ruthenium and has a metallic surface that is configured to condense and chill the condensable mineralizer composition in a liquid phase.

10. The method of claim 1 , wherein a transferred quantity of the condensable mineralizer composition within the first transfer vessel is determined volumetrically, and further comprising measuring a temperature of the condensable mineralizer composition.

11. The method of claim 1 , wherein a fluid height of the condensable mineralizer composition is measured by a fluid level sensor, wherein the fluid level sensor comprises at least one of an ultrasonic level transmitter, a laser level transmitter, a guide pulse sensor, or a sensing guide pulse transducer.

12. The method of claim 1 , further comprising transferring a second mineralizer composition comprising at least one of chlorine, bromine, or iodine to the receiving vessel.

13. The method of claim 1 , further comprising passing the condensable mineralizer composition through a fractionating column and performing a fractional distillation purification process on the condensable mineralizer composition.

14. The method of claim 9 , wherein a purification of at least five theoretical plates is achieved, relative to a mineralizer composition received directly from the first source vessel.

15. The method of claim 1 , wherein the second transfer vessel is heated to a temperature between temperature between 2 degrees Celsius and 50 degrees Celsius higher than a temperature of the receiving vessel during the liquid phase transfer of ammonia.

16. The method of claim 1 , further comprising forming at least one group III metal nitride wafer from the group III metal nitride boule grown ammonothermally.

17. A method for growth of group III metal nitride crystals, comprising:

providing a manifold comprising a first transfer vessel, a source vessel containing a condensable mineralizer composition comprising HF, and a receiving vessel;

chilling a metallic member within the first transfer vessel, wherein the metallic member comprises at least one of silver, a silver alloy, Monel® 400, gold, platinum, palladium, rhodium, iridium, or ruthenium and has a metallic surface that is configured to condense and chill the condensable mineralizer composition in a liquid phase;

transferring a quantity of the condensable mineralizer composition to the first transfer vessel via a vapor phase and causing condensation of the condensable mineralizer composition within the first transfer vessel;

measuring the quantity of the condensable mineralizer composition within the first transfer vessel;

transferring at least a portion of the condensable mineralizer composition from the first transfer vessel to the receiving vessel;

transferring a measured quantity of ammonia to a second transfer vessel;

transferring the measured quantity of ammonia from the second transfer vessel to the receiving vessel; and

forming at least a portion of a group III metal nitride boule by an ammonothermal crystal growth process that comprises:

exposing a seed crystal to a temperature of at least about 400 degrees Celsius, and

exposing the seed crystal to a mineralizer that is formed from the condensable mineralizer composition transferred from the receiving vessel,

wherein the first transfer vessel is heated to a temperature between 2 degrees Celsius and 50 degrees Celsius higher than a temperature of the receiving vessel during the transfer of the condensable mineralizer composition.

18. The method of claim 17 , wherein at least a portion of the condensable mineralizer composition is transferred from the first transfer vessel to the receiving vessel in a liquid phase.

19. The method of claim 17 , wherein the measured quantity of ammonia is transferred from the second transfer vessel to the receiving vessel in a liquid phase.

Assignments (1)

Continuity (3)

References Cited (144)