IP Library Granted Patent US 9,299,555
Granted Patent B1
US 9,299,555 · App. 14/033,107 · Granted Mar 29, 2016

Ultrapure mineralizers and methods for nitride crystal growth

Inventors: Alex Alexander (Santa Barbara, CA); John W. Nink, Jr. (Santa Barbara, CA); Mark P. D'Evelyn (Santa Barbara, CA)
Assignee: Soraa, Inc.
H01L21/02005C30B7/105C30B9/04C30B9/08C30B9/12C30B29/38
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Quick Facts
Patent No.
US 9,299,555
App. No.
14/033,107
Granted
Mar 29, 2016
Kind
B1
Abstract

An ultrapure mineralizer is formed by vaporization, condensation, and delivery of a condensable mineralizer composition. The mineralizer has an oxygen content below 100 parts per million. The ultrapure mineralizer is useful as a raw material for ammonothermal growth of bulk group III metal nitride crystals.

Claims (26)

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

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

chilling the at least one first transfer vessel;

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

measuring the quantity of the condensable mineralizer composition within the at least one transfer vessel;

transferring the condensable mineralizer composition to the receiving vessel; and

utilizing the transferred condensable mineralizer composition or a composition formed from the condensable mineralizer composition as a mineralizer for ammonothermal crystal growth of a group III metal nitride boule, the ammonothermal crystal growth being performed at a temperature of at least about 400 degrees Celsius.

2. The method of claim 1 , wherein a transferred quantity of the condensable mineralizer composition within the at least one first transfer vessel is determined volumetrically.

3. The method of claim 1 , further comprising adjusting a quantity of condensable mineralizer composition within the at least one first transfer vessel by passing purge gas over the condensable mineralizer composition within the at least one first transfer vessel, or by partially evacuating the condensable mineralizer composition within the at least one first transfer vessel.

4. The method of claim 1 , wherein the condensable mineralizer composition comprises fluorine.

5. The method of claim 4 , wherein the condensable mineralizer composition comprises HF, which is subsequently reacted with added NH 3 to form at least one of NH 4 F and NH 5 F 2 .

6. The method of claim 4 , further comprising transferring a second mineralizer composition comprising at least one of chlorine, bromine, or iodine to the receiving vessel.

7. The method of claim 1 , further comprising transferring at least a portion of the condensable mineralizer composition from the at least one first transfer vessel to a second transfer vessel.

8. The method of claim 1 , further comprising passing the condensable mineralizer composition through a point-of-use purifier, performing at least a second vapor phase transfer and a second condensation, or a combination thereof.

9. The method of claim 1 , further comprising exposing the condensable mineralizer composition to a getter in the at least one first transfer vessel.

10. The method of claim 1 , wherein the condensable mineralizer composition within the receiving vessel comprises a total oxygen content less than about 100 parts per million (ppm) by weight.

11. The method of claim 10 , wherein the condensable mineralizer composition within the receiving vessel comprises a total oxygen content less than about 5 parts per million (ppm) by weight.

12. The method of claim 1 , further comprising evacuating the manifold.

13. The method of claim 12 , wherein evacuating is carried out at least in part through a trap comprising a basic composition.

14. The method of claim 12 , wherein evacuating is carried out at least in part using a molecular drag pump.

15. The method of claim 1 , wherein at least one transfer vessel comprises a transparent plastic or a translucent plastic.

16. The method of claim 1 , wherein at least one transferring operation is carried out at a vapor pressure of the condensable mineralizer composition greater than one atmosphere.

17. The method of claim 1 , wherein transferring the condensable mineralizer composition to the receiving vessel is performed predominantly in a liquid phase.

18. 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.

19. The method of claim 18 , further comprising forming a semiconductor structure on the group III metal nitride wafer, the semiconductor structure comprising an In x Al y Ga 1-x-y N active layer, wherein 0≦x, y, and x+y≦1.

20. The method of claim 19 , further comprising incorporating the semiconductor structure into a device, the device comprising at least one of a light emitting diode, a laser diode, a photodetector, an avalanche photodiode, a transistor, a rectifier, a thyristor, a transistor, a rectifier, a Schottky rectifier, a thyristor, a p-i-n diode, a metal-semiconductor-metal diode, high-electron mobility transistor, a metal semiconductor field effect transistor, a metal oxide field effect transistor, a power metal oxide semiconductor field effect transistor, a power metal insulator semiconductor field effect transistor, a bipolar junction transistor, a metal insulator field effect transistor, a heterojunction bipolar transistor, a power insulated gate bipolar transistor, a power vertical junction field effect transistor, a cascade switch, an inner sub-band emitter, a quantum well infrared photodetector, a quantum dot infrared photodetector, a solar cell, and a diode for a photoelectrochemical water splitting and hydrogen generation device.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 23, 2017
From: SORAA, INC.
To: SLT TECHNOLOGIES, INC.
Reel/Frame 044636/0918 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 23, 2014
From: ALEXANDER, ALEX; NINK, JOHN W., JR.; D'EVELYN, MARK P.
To: SORAA, INC.
Reel/Frame 034023/0364 →
CONFIRMATORY LICENSE Recorded Aug 6, 2014
From: SORAA, INC.
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 033481/0681 →
Continuity (1)
Provisional Application 61707689 · Sep 28, 2012