IP Library Granted Patent US 11,195,644
Granted Patent B2
US 11,195,644 · App. 15/129,439 · Granted Dec 7, 2021

Iron nitride magnetic material including coated nanoparticles

Inventors: Jian-Ping Wang (Shoreview, MN); Yanfeng Jiang (Minneapolis, MN); Craig A. Bridges (Knoxville, TN); Michael Brady (Oak Ridge, TN); Orlando Rios (Knoxville, TN); Roberta A. Meisner (Knoxville, TN); Lawrence F. Allard (Knoxville, TN); Edgar Lara-Curzio (Lenoir City, TN); Shihai He (Fremont, CA)
Assignees: REGENTS OF THE UNIVERSITY OF MINNESOTA; UT-BATTELLE, LLC; UNIVERSITY OF TENNESSEE RESEARCH FOUNDATION
H01F1/047B22F1/0018C22C38/001C22C38/002C23C14/0036C23C14/0605C23C14/165C23C14/185C23C14/3414C23C14/3464C23C14/566C23C14/568C23C14/5806C23C14/586H01F1/0054H01F1/065H01F41/0253C22C2202/02
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Quick Facts
Patent No.
US 11,195,644
App. No.
15/129,439
Granted
Dec 7, 2021
Kind
B2
Abstract

The disclosure describes techniques for forming nanoparticles including Fe 16 N 2 phase. In some examples, the nanoparticles may be formed by first forming nanoparticles including iron, nitrogen, and at least one of carbon or boron. The carbon or boron may be incorporated into the nanoparticles such that the iron, nitrogen, and at least one of carbon or boron are mixed. Alternatively, the at least one of carbon or boron may be coated on a surface of a nanoparticle including iron and nitrogen. The nano particle including iron, nitrogen, and at least one of carbon or boron then may be annealed to form at least one phase domain including at least one of Fe 16 N 2 , Fe 16 (NB) 2 , Fe 16 (NC) 2 , or Fe 16 (NCB) 2 .

Claims (35)

1. A method comprising:

directing an energized sputtering gas at a target comprising iron to form an iron vapor, wherein the energized sputtering gas comprises argon and diatomic nitrogen;

forming atomic nitrogen vapor from the diatomic nitrogen;

condensing iron atoms from the iron vapor and nitrogen atoms from the atomic nitrogen vapor to form a nanoparticle including iron and nitrogen;

coating a surface of the nanoparticle including iron and nitrogen with at least one of carbon or boron to form a coated nanoparticle wherein a thickness of a coating of the coated nanoparticle is between about 0.5 nanometers and about 50 nanometers, and wherein the nanoparticle defines a diameter between about 0.5 nm and about 200 nm; and

nitriding the nanoparticle to form the nanoparticle including iron, nitrogen, and at least one of carbon or boron; and

annealing the nanoparticle to form a permanent magnet comprising at least one Fe 16 N 2 phase domain

wherein the nanoparticle comprises an oxide dopant.

2. The method of claim 1 , wherein coating the surface of the nanoparticle including iron and nitrogen with at least one of carbon or boron comprises:

directing an energized sputtering gas at a target comprising the at least one of carbon or boron to form a vapor comprising atoms of the at least one of carbon or boron; and

condensing the atoms of the at least one of carbon or boron from the vapor to coat the surface of the nanoparticle including iron and nitrogen with at least one of carbon or boron.

3. The method of claim 1 , wherein the nanoparticle including iron and nitrogen further comprises at least one of iron nitride, iron carbide, iron boride, or iron carbo-boride.

4. The method of claim 1 , wherein forming the nanoparticle including iron and at least one of carbon or boron comprises:

forming a coating comprising at least one of carbon or boron on a surface of a nanoparticle comprising iron to form a coated nanoparticle.

5. The method of claim 4 , wherein forming the coating comprising at least one of carbon or boron on the surface of the nanoparticle comprising iron to form the coated nanoparticle comprises:

directing an energized sputtering gas at a target comprising the at least one of carbon or boron to form a vapor comprising atoms of the at least one of carbon or boron; and

condensing the atoms of the at least one of carbon or boron from the vapor to coat the surface of the nanoparticle including iron with at least one of carbon or boron.

6. The method of claim 4 , wherein a thickness of the coating is between about 0.5 nanometers and about 50 nanometers, and wherein the nanoparticle defines a diameter between about 0.5 nm and about 200 nm.

7. The method of claim 1 , wherein the nanoparticle including iron and at least one of carbon or boron further comprises at least one of iron nitride, iron carbide, iron boride, or iron carbo-boride.

8. The method of claim 1 , wherein nitriding the coated nanoparticle comprises exposing the coated nanoparticle to gaseous ammonia at a temperature between about 100° C. and about 200° C. for up to about 1 week.

9. The method of claim 1 , wherein annealing the nanoparticle to form the at least one Fe 16 N 2 phase domain comprises annealing the nanoparticle at a temperature between about 150° C. and about 250° C. for between about 20 hours and 48 hours.

10. The method of claim 1 , wherein the nanoparticle including iron, nitrogen, and at least one of carbon or boron comprises between about 0.5 at. % and about 11 at. % of the at least one of carbon or boron.

11. The method of claim 1 , wherein annealing the nanoparticle to form at least one Fe 16 N 2 phase domain also forms at least one phase domain comprising at least one of Fe 16 (NB) 2 , Fe 16 (NC) 2 , or Fe 16 (NCB) 2 .

12. A method comprising:

directing an energized sputtering gas at a target comprising iron to form an iron vapor, wherein the energized sputtering gas comprises argon and diatomic nitrogen;

forming atomic nitrogen vapor from the diatomic nitrogen;

condensing iron atoms from the iron vapor and nitrogen atoms from the atomic nitrogen vapor to form a nanoparticle including iron and nitrogen;

coating a surface of the nanoparticle including iron and nitrogen with at least one of carbon or boron to form a coated nanoparticle; and

wherein the nanoparticle includes between about 0.5 at. % and about 11 at. % of at least one of carbon or boron;

wherein a thickness of a coating of the coated nanoparticle is between about 0.5 nanometers and about 50 nanometers, and wherein the nanoparticle defines a diameter between about 0.5 nm and about 200 nm, and

annealing the coated nanoparticle to form a permanent magnet comprising at least one phase domain comprising at least one of Fe 16 N 2 , Fe 16 (NB) 2 , Fe 16 (NC) 2 , or Fe 16 (NCB) 2

wherein the coated nanoparticle comprises an oxide dopant.

13. The method of claim 12 , wherein annealing the coated nanoparticle to form the at least one Fe 16 N 2 phase domain comprises annealing the coated nanoparticle to form the at least one Fe 16 N 2 phase domain at a temperature between about 150° C. and about 250° C. for between about 20 hours and 48 hours.

14. The method of claim 12 , wherein nitriding the coated nanoparticle comprises exposing the nanoparticle to gaseous ammonia at a temperature between about 100° C. and about 200° C. for up to about 1 week.

15. The method of claim 12 , wherein the nanoparticle including iron, nitrogen, and between about 0.5 at. % and about 11 at. % of at least one of carbon or boron further comprises at least one of iron carbide, iron boride, or iron carbo-boride.

Assignments (10)
CONFIRMATORY LICENSE Recorded Nov 3, 2021
From: UNIVERSITY OF MINNESOTA
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 058004/0570 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 22, 2020
From: BRADY, MICHAEL P.; BRIDGES, CRAIG A.; RIOS, ORLANDO; ALLARD, LAWRENCE F., JR.; LARA-CURZIO, EDGAR
To: UT-BATTELLE, LLC
Reel/Frame 054729/0156 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 18, 2020
From: BRIDGES, CRAIG A.; BRADY, MICHAEL; RIOS, ORLANDO; ALLARD, LAWRENCE F., JR.; LARA-CURZIO, EGAR
To: UT-BATTELLE, LLC
Reel/Frame 054688/0550 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 18, 2020
From: MEISNER, ROBERTA A.
To: UNIVERSITY OF TENNESSEE RESEARCH FOUNDATION
Reel/Frame 054688/0565 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 23, 2020
From: HE, SHIHAI
To: REGENTS OF THE UNIVERSITY OF MINNESOTA
Reel/Frame 054149/0666 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 31, 2019
From: JIANG, YANFENG
To: REGENTS OF THE UNIVERSITY OF MINNESOTA
Reel/Frame 049329/0589 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 28, 2018
From: MEISNER, ROBERTA A.
To: UNIVERSITY OF TENNESSEE RESEARCH FOUNDATION
Reel/Frame 045064/0334 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 4, 2017
From: WANG, JIAN-PING
To: REGENTS OF THE UNIVERSITY OF MINNESOTA
Reel/Frame 044285/0567 →
CONFIRMATORY LICENSE Recorded Apr 4, 2017
From: UT-BATTELLE, LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 041837/0265 →
CONFIRMATORY LICENSE Recorded Dec 13, 2016
From: REGENTS OF THE UNIVERSITY OF MINNESOTA
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 040717/0726 →
Continuity (2)
Provisional Application 61971730 · Mar 28, 2014
Related Publication 20170186518A1 · Jun 29, 2017
Cited By (1)
US 12,740,328