US 12,252,812 B2
Ultrapure mineralizer and improved methods for nitride crystal growth
Mark P. D'Evelyn, Vancouver, WA (US); Paul M. Von Dollen, Brush Prairie, WA (US); Lisa M. Gay, Vancouver, WA (US); Douglas W. Pocius, Aguanga, CA (US); and Jonathan D. Cook, Santa Barbara, CA (US)
Assigned to SLT Technologies, Inc., Los Angeles, CA (US)
Filed by SLT Technologies, Inc., Los Angeles, CA (US)
Filed on Feb. 6, 2024, as Appl. No. 18/434,568.
Application 18/434,568 is a continuation of application No. 17/514,656, filed on Oct. 29, 2021, granted, now 12,024,795.
Claims priority of provisional application 63/108,830, filed on Nov. 2, 2020.
Prior Publication US 2024/0240352 A1, Jul. 18, 2024
This patent is subject to a terminal disclaimer.
Int. Cl. C30B 7/10 (2006.01); C30B 29/40 (2006.01)
CPC C30B 7/105 (2013.01) [C30B 29/403 (2013.01)] 19 Claims
OG exemplary drawing
 
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.