Iron nitride materials and magnets including iron nitride materials

Patent metadata

Field	Value
Publication number	US-10504640-B2
Application number	US-201414900944-A
Country	US
Kind code	B2
Filing date	Jun 24, 2014
Priority date	Jun 27, 2013
Publication date	Dec 10, 2019
Grant date	Dec 10, 2019

Abstract

The disclosure describes magnetic materials including iron nitride, bulk permanent magnets including iron nitride, techniques for forming magnetic materials including iron nitride, and techniques for forming bulk permanent magnets including iron nitride.

First claim

What is claimed is:

1. A method comprising:
heating a mixture including iron and nitrogen to form a molten iron nitride-containing material and thereby forming the molten iron nitride-containing material; and
casting, quenching, and pressing the molten iron nitride-containing material to form a workpiece including at least one Fe 8 N phase domain.

2. The method of claim 1 , wherein casting, quenching, and pressing comprises continuously casting, quenching, and pressing the molten iron nitride-containing material to form a workpiece having a dimension that is longer than other dimensions of the workpiece.

3. The method of claim 1 , further comprising:
milling, in a bin of a rolling mode milling apparatus, a stirring mode milling apparatus, or a vibration mode milling apparatus, an iron-containing raw material in the presence of a nitrogen source to generate a powder including iron nitride, and
wherein heating the mixture including iron and nitrogen comprises heating the powder including iron nitride.

4. The method of claim 3 , wherein the nitrogen source comprises at least one of ammonium nitrate, an amide-containing material, or a hydrazine-containing material.

5. The method of claim 4 , wherein the at least one of the amide-containing or hydrazine-containing material comprises at least one of a liquid amide, a solution containing an amide, a hydrazine, or a solution containing hydrazine.

6. The method of claim 4 , wherein the at least one of the amide-containing or hydrazine-containing material comprises at least one of carbamide, methanamide, benzamide, or acetamide.

7. The method of claim 3 , wherein the iron-containing raw material comprises substantially pure iron.

8. The method of claim 3 , further comprising adding a catalyst to the iron-containing raw material.

9. The method of claim 8 , wherein the catalyst comprises at least one of nickel or cobalt.

10. The method of claim 3 , wherein the iron-containing raw material comprises a powder with an average diameter of less than about 100 μm.

11. The method of claim 3 , wherein the powder including iron nitride comprises at least one of FeN, Fe 2 N, Fe 3 N, Fe 4 N, Fe 2 N 6 , Fe 8 N, Fe16N 2 , or FeN x , wherein x is in the range of from about 0.05 to about 0.5.

12. The method of claim 3 , further comprising milling an iron precursor to form the iron-containing raw material.

13. The method of claim 12 , wherein the iron precursor comprises at least one of Fe, FeCl 3 , Fe 2 O 3 , or Fe 3 O 4 .

14. The method of claim 12 , wherein milling the iron precursor to form the iron-containing raw material comprises milling the iron precursor in the presence of at least one of Ca, Al, or Na under conditions sufficient to cause an oxidation reaction between the at least one of Ca, Al, or Na and oxygen present in the iron precursor.

15. The method of claim 3 , further comprising melting spinning an iron precursor to form the iron-containing raw material.

16. The method of claim 15 , wherein melting spinning the iron precursor comprises:
forming molten iron precursor;
cold rolling the molten iron precursor to form a brittle ribbon of material;
heat treating the brittle ribbon of material; and
shattering the brittle ribbon of material to form the iron-containing raw material.

17. The method of claim 1 , wherein a dimension of the workpiece including at least one Fe 8 N phase domain is less than about 50 millimeters in at least one axis.

18. The method of claim 1 , wherein the molten iron nitride-containing material includes an iron atom-to-nitrogen atom ratio of about 8:1.

19. The method of claim 1 , wherein the molten iron-nitride containing material includes at least one ferromagnetic or nonmagnetic dopant.

20. The method of claim 19 , wherein the at least one ferromagnetic or nonmagnetic dopant comprises at least one of Sc, Ti, V, Cr, Mn, Co, Ni, Cu, Zn, Zr, Nb, Mo, Ru, Rh, Pd, Ag, Cd, Pt, Au, Sm, C, Pb, W, Ga, Y, Mg, Hf, or Ta.

21. The method of claim 19 , wherein the molten iron-nitride containing material comprises less than about 10 atomic percent of the at least one ferromagnetic or nonmagnetic dopant.

22. The method of claim 1 , wherein the molten iron-nitride containing material further comprises at least one phase stabilizer.

23. The method of claim 22 , wherein the at least one phase stabilizer comprises at least one of B, Al, C, Si, P, O, Co, Cr, Mn, or S.

24. The method of claim 22 , wherein the molten iron-nitride containing material comprises between about 0.1 atomic percent and about 15 atomic percent of the at least one phase stabilizer.

25. The method of claim 1 , wherein heating the mixture including iron and nitrogen to form the molten iron nitride-containing material comprises heating the mixture at a temperature greater than about 1500° C.

26. The method of claim 1 , wherein continuously casting, quenching, and pressing the molten iron nitride-containing material comprises casting the molten iron nitride-containing material at a temperature in the range of from about 650° C. to about 1200° C.

27. The method of claim 1 , wherein continuously casting, quenching, and pressing the molten iron nitride-containing material comprises quenching the iron nitride-containing material to a temperature above about 650° C.

28. The method of claim 1 , wherein continuously casting, quenching, and pressing the molten iron nitride-containing material comprises pressing the iron nitride-containing material at a temperature below about 250° C. and a pressure in the range of from about 5 tons to about 50 tons.

29. The method of claim 1 , further comprising straining and post-annealing the workpiece including at least one Fe 8 N phase domain to form a workpiece including at least one Fe 16 N 2 phase domain.

30. The method of claim 29 , wherein straining and post-annealing the workpiece including at least one Fe 8 N phase domain reduces the dimension of the workpiece.

31. The method of claim 30 , wherein the dimension of the workpiece including at least one Fe 16 N 2 phase domain in the at least one axis following straining and post-annealing is less than about 0.1 mm.

32. The method of claim 29 , wherein, after straining and post-annealing, the workpiece consists essentially of a single Fe 16 N 2 phase domain.

33. The method of claim 29 , wherein straining the workpiece including at least one Fe 8 N phase domain comprises exerting a tensile strain on the workpiece in the range of from about 0.3% to about 12%.

34. The method of claim 33 , wherein the tensile strain is applied in a direction substantially parallel to at least one <001> crystal axis in the workpiece including at least one Fe 8 N phase domain.

35. The method of claim 29 , wherein post-annealing the workpiece including at least one Fe 8 N phase domain comprises heating the workpiece including at least one Fe 8 N phase domain to a temperature in the range of from about 100° C. to about 250° C.

36. The method of claim 29 , wherein the workpiece including at least one Fe 16 N 2 phase domain is characterized as being magnetically anisotropic.

37. The method of claim 36 , wherein the energy product, coercivity and saturation magnetization of the workpiece including at least

Assignees

• Univ Minnesota
• Wang Jian Ping
• Jiang Yanfeng

Inventors

• Wang Jian-Ping
• Jiang Yanfeng

Classifications

• H01F1/086

  sintered · CPC title

• B22F9/04

  starting from solid material, e.g. by crushing, grinding or milling ({C22C1/1084 takes precedence}; crushing, grinding or milling, in general, see the relevant subclasses, e.g. B02C) · CPC title

• C22C2202/02

  Magnetic · CPC title

• H01F41/02 Primary

  for manufacturing cores, coils, or magnets (H01F41/14 takes precedence; for dynamo-electric machines H02K15/00) · CPC title

• H01F1/047 Primary

  Alloys characterised by their composition · CPC title