Applied magnetic field synthesis and processing of iron nitride magnetic materials

Patent metadata

Field	Value
Publication number	US-12338536-B2
Application number	US-202117182857-A
Country	US
Kind code	B2
Filing date	Feb 23, 2021
Priority date	Jun 30, 2014
Publication date	Jun 24, 2025
Grant date	Jun 24, 2025

Abstract

A method may include annealing a material including iron and nitrogen in the presence of an applied magnetic field to form at least one Fe 16 N 2 phase domain. The applied magnetic field may have a strength of at least about 0.2 Tesla (T).

First claim

The invention claimed is:

1. A method comprising:
solutionizing a material including iron, nitrogen, and at least one dopant, in the presence of an applied magnetic field with a strength of at least about 0.2 T at a temperature of about 660° C. or more; and
after solutionizing the material, quenching the material;
annealing the material to form an iron nitride material with at least one Fe 16 N 2 phase domain, wherein the applied magnetic field has a strength of at least about 0.2 Tesla (T), wherein the at least one dopant comprises at least one of Al, Mn, La, Cr, Co, Ti, Ni, or a rare earth metal.

2. The method of claim 1 , wherein the strength of the magnetic field in the annealing step is greater than about 2.5 T.

3. The method of claim 1 , wherein the strength of the magnetic field in the annealing step is between about 8 T and about 10 T.

4. The method of claim 1 , wherein the strength of the magnetic field in the annealing step is greater than about 9 T.

5. The method of claim 1 , wherein annealing the material comprises heating the material at a temperature of between about 120° C. to about 200° C. for between about 10 hours and about 100 hours.

6. The method of claim 5 , wherein annealing the material comprises heating the material at a temperature between about 150° C. and about 160° C. for between about 10 hours and about 30 hours.

7. The method of claim 1 , wherein the material comprises at least one of a pellet, rod, thin film, nanoparticle, powder, or nanoscale powder.

8. The method of claim 1 , wherein the at least one dopant comprises at least one of B, C, P, Si, or O.

9. The method of claim 1 , wherein annealing the material in the presence of the applied magnetic field transforms an α′-Fe 8 N phase in the material to an α″-Fe 16 N 2 phase.

10. The method of claim 9 , wherein a transformation yield of the α′-Fe 8 N phase to the α″-Fe 16 N 2 phase is at least 70%.

11. The method of claim 1 , wherein, after annealing, the α″-Fe 16 N 2 phase in the material is at least 20% of the material by volume.

12. The method of claim 1 , wherein the applied magnetic field is applied in substantial alignment with a c axis of at least one iron crystal in the material.

13. The method of claim 1 , wherein solutionizing the material comprises solutionizing the material in the presence of an applied magnetic field with a strength of at least about 9 T magnetic field at about 750° C.

14. The method of claim 1 , wherein, prior to annealing the material, the concentration of nitrogen in the material is between about 8 atomic percent (at. %) and about 9 at. %.

15. A method comprising:
nitridizing a material including iron in the presence of an applied magnetic field to form an iron-nitride-containing material at a temperature of about 600° C. or more;
and annealing the iron-nitride-containing material in the presence of the applied magnetic field to form at least one Fe 16 N 2 phase domain, wherein the applied magnetic field has a strength of at least about 0.2 Tesla (T), wherein the iron-nitride-containing material comprises at least one dopant selected from Al, Mn, La, Cr, Co, Ti, Ni, or a rare earth metal in the iron nitride material.

16. The method of claim 15 , wherein the material including iron comprises an iron-based powder or iron-based nanoscale powder.

17. The method of claim 15 , wherein the material comprises at least one of an iron oxide, iron carbide, iron chloride, or iron-metal solid solution.

18. The method of claim 15 , wherein nitridizing the material and annealing the iron-nitride-containing material to form at least one Fe 16 N 2 phase domain occur in situ in the presence of the applied magnetic field.

19. The method of claim 15 , further comprising, prior to nitridizing the material, reducing the material in at least one of hydrogen, nitrogen, or ammonia gas, wherein reduction of the material occurs in situ in the presence of the applied magnetic field.

20. The method of claim 19 , wherein reducing the material comprises reducing a carbon-coated iron powder in hydrogen gas for about 1 hour at a temperature of between about 375° C. and about 425° C.

21. The method of claim 15 , wherein the strength of the high magnetic field is greater than about 2.5 T.

22. The method of claim 15 , wherein the strength of the high magnetic field is between about 8 T and about 10 T.

23. The method of claim 15 , wherein the strength of the high magnetic field is greater than about 9 T.

24. The method of claim 15 , wherein annealing the iron-nitride-containing material comprises heating the iron-nitride-containing material at a temperature of between about 100° C. to about 250° C. for between about 10 hours and about 100 hours.

25. The method of claim 15 , wherein the at least one dopant comprises at least one of B, C, P, Si, or O.

26. The method of claim 15 , wherein annealing the iron-nitride-containing material in the presence of the applied magnetic field transforms an α′-Fe 8 N phase in the iron-nitride-containing material to an α″-Fe 16 N 2 phase.

27. The method of claim 26 , wherein a transformation yield of the α′-Fe 8 N phase to the α″-Fe 16 N 2 phase is at least 70%.

28. The method of claim 15 , wherein, after annealing, the α″-Fe 16 N 2 phase in the iron-nitride-containing material is at least 20% of the iron-nitride-containing material by volume.

29. The method of claim 15 , wherein the applied magnetic field is applied in substantial alignment with a c axis of at least one iron crystal in the iron-nitride-containing material.

30. A workpiece comprising iron nitride material made by solutionizing a material including iron and nitrogen at a temperature of about 600° C. or more, and annealing the material in the presence of an applied magnetic field to form at least one Fe 16 N 2 phase domain, wherein the applied magnetic field has a strength of at least about 0.2 Tesla (T), wherein the iron and nitrogen containing material comprises at least one dopant selected from Al, Mn, La, Cr, Co, Ti, Ni, or a rare earth metal in the iron nitride material.

31. The work piece of claim 30 , wherein the workpiece is a pellet, rod, thin film, nanoparticle, powder, or nanoscale powder.

32. An article comprising a plurality of workpieces, wherein at least one workpiece of the plurality of workpieces comprise iron nitride material made by the method of claim 1 , and wherein the at least one workpiece is a pellet, rod, thin film, nanoparticle, powder, or nanoscale powder.

33. The article of claim 32 , wherein the workpieces are arranged so the <001> axes of the respective iron nitride materials are substantially aligned.

34. The article of claim 33 , wherein the article is an electric motor, a generator, a sensor, an actuator, a component of an automotive vehicle, or a component of a wind turbine.

Assignees

• Univ Minnesota
• Ut Battelle Llc

Inventors

• Brady Michael P
• Rios Orlando
• Jiang Yanfeng
• Ludtka Gerard M
• Bridges Craig A
• Wang Jian-Ping
• Zhang Xiaowei
• Allard Lawrence F
• Lara-Curzio Edgar

Classifications

• C01P2006/42

  Magnetic properties · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• H01F1/065

  obtained by a reduction · CPC title

• H01F1/047

  Alloys characterised by their composition · CPC title

• C22C38/00

  Ferrous alloys, e.g. steel alloys (cast-iron alloys C22C37/00) · CPC title