IP Library Granted Patent US 12,031,210
Granted Patent B2
US 12,031,210 · App. 16/988,217 · Granted Jul 9, 2024

System and method for atomic layer deposition of rare-earth oxides on optical grade materials for laser gain media

Inventors: John S. Miller (Walnut Creek, CA); Selim Elhadj (Livermore, CA); Thomas M. Spinka (Livermore, CA)
Assignee: Lawrence Livermore National Security, LLC
C23C16/45555C23C16/403C23C16/45536C23C16/45544C23C16/45553
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Quick Facts
Patent No.
US 12,031,210
App. No.
16/988,217
Granted
Jul 9, 2024
Kind
B2
Abstract

A method is disclosed for doping a quantity of powder particles. A container having a central chamber is initially charged with a quantity of powder particles. A quantity of precursor is sublimed to form a heated precursor. A quantity of carrier gas is mixed with the precursor to form a mixture of heated precursor/carrier gas. The central chamber is charged with the heated precursor/carrier gas and then moved to cause interaction of the powder particles with the heated precursor/carrier gas to form a first monolayer coating on the powder particles. The heated precursor/carrier gas is then removed from the central chamber and the central chamber is charged with a O2/O3 gas under a plasma. The central chamber is then further moved to produce interaction of the O2/O3 gas with the first monolayer coating on the powder particles to modify the first monolayer coating to create a different, single monolayer coating forming an oxide coating on the powder particles.

Claims (42)

1. A method for applying a doping material on a quantity of powder particles, comprising:

providing a controller;

providing a stationary container having:

an RF plasma generating subsystem disposed within the container and in communication with the controller;

a central chamber having a first port for receiving a heated, precursor/carrier gas, a second port forming a vacuum port for enabling the container to be placed in a vacuum condition, and a third port for receiving an O 2 /O 3 gas);

locating a rotatable metal cylinder within the central chamber of the container, the rotatable cylinder being rotatable independently of the container;

operatively coupling a rotation mechanism to the rotatable cylinder, the rotation mechanism being controlled via first control signals supplied from the controller;

charging the rotatable cylinder with a quantity of powder particles;

heating a quantity of precursor contained within a bubbler, the bubbler being independent of the container, to sublime the precursor;

controlling a temperature of the bubbler, and rotation of the rotatable cylinder, using the controller;

feeding a quantity of carrier gas into the bubbler and mixing the quantity of carrier gas with the heated precursor within the bubbler to form a mixture of heated precursor/carrier gas;

charging the central chamber with the heated precursor/carrier gas through the first port in the container;

using the rotation mechanism to cause rotational movement of the rotatable cylinder within the container while the container is held stationary to cause tumbling of the powder particles, to produce an interaction of the powder particles with the heated precursor/carrier gas within the rotatable cylinder to form a first monolayer coating on each of the powder particles;

removing the heated precursor/carrier gas from the central chamber by using second control signals supplied from the controller to control a vacuum pump, the vacuum pump being in communication with the stationary container and activated by the controller upon the expiration of a predetermined time period, the predetermined time period being indicative that the first monolayer coating on each of the powder particles has been fully formed;

charging the central chamber through the third port with a O 2 /O 3 gas), and into a plasma generating subsystem;

using the plasma generating subsystem to direct the O 2 /O 3 gas) under a plasma into the rotatable cylinder, the plasma generating subsystem further being controlled by the controller; and

causing further rotational movement of the rotatable cylinder while maintaining the container stationary, to cause further tumbling of the powder particles contained within the rotatable cylinder, to produce interaction of the O 2 /O 3 gas) with the first monolayer coating on each said powder particle to modify the first monolayer coating to create a different, single monolayer coating forming an oxide coating on each of the powder particles, wherein the different, single monolayer coating forms a dopant for the powder particles.

2. The method of claim 1 , wherein the oxide coating comprises at least one of a rare-earth oxide coating or an aluminum oxide coating.

3. The method of claim 1 , wherein heating a quantity of precursor comprises heating a quantity of optically active organometallic precursor.

4. The method of claim 3 , wherein heating a quantity of organometallic precursor comprises heating a quantity of Nd(TMHD) 3 material within the bubbler until the organometallic precursor sublimes.

5. The method of claim 1 , wherein:

heating a quantity of precursor within the bubbler comprises heating a quantity of Nd(TMHD) 3 material; and

producing interaction of the O 2 /O 3 gas) with the first monolayer coating produces a Nd 2 O 3 monolayer on each of the powder particles.

6. The method of claim 1 , further sintering the powder particles after creating the different monolayer coating on the powder particles.

7. The method of claim 1 , wherein mixing a quantity of carrier gas with the heated precursor comprises mixing a quantity of argon with the heated precursor inside the bubbler.

8. The method of claim 1 , wherein causing movement of the rotatable cylinder to cause interaction of the powder particles with the heated precursor/carrier gas comprises rotating the rotatable cylinder continuously.

9. The method of claim 1 , wherein causing further movement of the rotatable cylinder to produce interaction of the O 2 /O 3 gas) with the first monolayer coating on each powder particle comprises causing continuous rotation of the rotatable cylinder.

10. A method of doping a quantity of nano-powder particles, comprising:

filling a container having a central chamber with a quantity of nano-powder particles;

heating a quantity of optically active precursor to cause sublimation, to form a heated organometallic precursor;

mixing a quantity of carrier gas with the heated optically active precursor to form a mixture of heated precursor/carrier gas;

charging the central chamber with the heated precursor/carrier gas and causing rotation of the chamber to cause interaction of the nano-powder particles with the heated precursor/carrier gas to form a first monolayer coating on each of the nano-powder particles;

removing the heated precursor/carrier gas from the central chamber and charging the central chamber with a O 2 /O 3 gas) under a plasma;

causing further rotation of the central chamber to produce interaction of the O 2 /O 3 gas) with the first monolayer coating on each said nano-powder particle to modify the first monolayer coating to create a different, single monolayer coating forming a rare-earth oxide dopant coating on each of the nano-powder particles; and

sintering the nano-powder particles to incorporate the rare-earth oxide dopant coating into a crystal lattice structure using the nano-powder particles.

11. The method of claim 10 , wherein heating a quantity of optically active precursor to form an organometallic precursor comprises heating a quantity of Nd(TMHD) 3 material until the Nd(TMHD) 3 material sublimes.

12. The method of claim 10 , wherein heating a quantity of optically active precursor to form an organometallic precursor comprises heating a quantity of Nd(TMHD) 3 material; and

wherein producing interaction of the O 2 /O 3 gas) with the first monolayer coating produces a Nd 2 O 3 monolayer on each of the nano-powder particles.

13. The method of claim 10 , wherein causing rotation of the chamber to cause interaction of the nano-powder particles with the heated precursor/carrier gas comprises causing rotation of the chamber continuously.

14. The method of claim 10 , wherein causing further rotation of the central chamber to produce an interaction of the O 2 /O 3 gas) with the first monolayer coating on each nano-powder particle comprises causing rotation of the chamber continuously.

15. The method of claim 10 , wherein removing the heated precursor/carrier gas from the central chamber and charging the central chamber with a O 2 /O 3 gas) under a plasma comprises charging the central chamber with a plasma having a power level of 0 watts-300 watts.

16. The method of claim 10 , wherein removing the heated precursor/carrier gas from the central chamber and charging the central chamber with a O 2 /O 3 gas) under a plasma comprises charging the central chamber with a plasma having a power level between 0 and 200 watts.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 10, 2020
From: MILLER, JOHN S.; ELHADJ, SELIM; SPINKA, THOMAS M.
To: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
Reel/Frame 054324/0364 →
CONFIRMATORY LICENSE (SEE DOCUMENT FOR DETAILS) Recorded Aug 19, 2020
From: LAWRENCE LIVERMORE NATIONAL SECURITY, LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 053555/0858 →
Continuity (1)
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