Synthesis of ordered L10-type FeNi nanoparticles
View Patent ↗Particles of iron and nickel are added to a flowing plasma stream which does not chemically alter the iron or nickel. The iron and nickel are heated and vaporized in the stream, and then a cryogenic fluid is added to the stream to rapidly cause the formation of nanometer size particles of iron and nickel. The particles are separated from the stream. The particles are preferably formed as single crystals in which the iron and nickel atoms are organized in a tetragonal L1 0 crystal structure which displays magnetic anisotropy. A minor portion of an additive, such as titanium, vanadium, aluminum, boron, carbon, phosphorous, or sulfur, may be added to the plasma stream with the iron and nickel to enhance formation of the desired crystal structure.
1. A method of forming small particles with permanent magnet properties and consisting essentially of iron and nickel, and optionally one or more additive elements (A) selected from the group consisting of titanium, vanadium, aluminum, boron, carbon, phosphorous, and sulfur in accordance with the formula, (Fe 100−x Ni x ) 100−y A y , where x equals weight percent of nickel in combination with iron and has a value in the range of 25-67 weight percent, and y equals weight percent of an additive A incorporated with the combination of iron and nickel, and has a value of no more than fifteen weight percent; the method comprising:
adding iron and nickel atoms and, optionally, atoms of an additive A into a flowing process stream, which is initially a plasma stream, to produce a vapor in the process stream comprising a mixture of the added atoms, the plasma being formed of a material that is not condensable to a liquid at a temperature above 25° C.; thereafter
adding a quench fluid, initially at a temperature below about 100K, into the process stream, the quench fluid mixing with the process stream and being added in an amount to quench the iron, nickel, and additive atoms of the vapor in the process stream to form particles of the iron, nickel, and additive atoms at a temperature below about 300° C., the particles having a size of about 250 nanometers or smaller;
separating the particles from the process stream; and, if the formed and separated particles are not fully crystallized to a tetragonal L1 0 crystal structure, then
heating the separated particles such that the iron, nickel, and A are arranged in a tetragonal L1 0 crystal structure.
2. A method as stated in claim 1 in which the plasma is formed from an inert gas or a gas that is not reactive with the iron, nickel, or A atoms in the plasma.
3. A method as stated in claim 1 in which the quench fluid composition is one of argon, helium, or nitrogen, and is added to the process stream as a cryogenic fluid.
4. A method as stated in claim 1 in which the flowing process stream is directed in a flow path with a perimeter or perimeters, and iron and nickel atoms are added separately into the processing stream at more than one location around the perimeter and along the flow path of the process stream.
5. A method as stated in claim 1 in which the process stream is directed in a flow path with a perimeter and the quench fluid is added to the process stream at more than one location around the perimeter of the flow path of the process stream.
6. A method as stated in claim 1 in which the process stream is directed in a flow path with a perimeter and the process steam is caused to converge after the addition of the quench fluid to concentrate the formed particles for their separation from the process stream.
7. A method as stated in claim 1 in which x has a value in the range of 45 to 55 weight percent nickel.
8. A method as stated in claim 1 in which x has a value in the range of 25 to 39 weight percent nickel.
9. A method as stated in claim 1 in which the iron, nickel, and additive A are mixed in an alloy before being added to the process fluid.
10. A method as stated in claim 1 in which the separated particles with the tetragonal L1 0 crystal structure are subjected to a combination of consolidation and magnetization to form an article having permanent magnet properties.
11. A method as stated in claim 1 in which heating of the separated particles is done in combination with one or more of (a) the application of pressure to the particles, (b) the application of a magnetic field to the particles, and (c) mechanical working of the particles.
12. A method of forming small particles with permanent magnet properties and consisting essentially of iron and nickel, and optionally one or more additive elements (A) selected from the group consisting of titanium, vanadium, aluminum, boron, carbon, phosphorous, and sulfur in accordance with the formula, (Fe 100−x Ni x ) 100−y A y where x equals weight percent of nickel in combination with iron and has a value in the range of 25-67 weight percent, and y equals weight percent of an additive A incorporated with the combination of iron and nickel, and has a value of no more than fifteen weight percent; the method comprising:
adding iron and nickel atoms and, optionally, atoms of an additive A into a flowing process stream which is directed in a flow path with one or more perimeters, the process stream initially being a plasma stream, to produce a vapor in the process stream comprising a mixture of the added atoms, the plasma being formed of a material that is not condensable to a liquid at a temperature above 25° C., the iron and nickel atoms being added separately into the processing stream at more than one location around the perimeter and along the flow path of the process stream; thereafter
adding a quench fluid, initially at a temperature below about 100K, into the process stream, the quench fluid being added to the process stream at more than one location around the perimeter of the flow path of the process stream, the quench fluid mixing with the process stream and being added in an amount to quench the iron, nickel, and additive atoms of the vapor in the process stream to form particles of the iron, nickel, and additive atoms at a temperature below about 300° C., the particles having a size of about 250 nanometers or smaller;
separating the particles from the processing stream; and, if the formed and separated particles are not fully crystallized to a tetragonal L1 0 crystal structure, then
heating the separated particles such that the iron, nickel, and A are arranged in a tetragonal L1 0 crystal structure.
13. A method as stated in claim 12 in which the plasma is formed from an inert gas or a gas that is not reactive with the iron, nickel, or A atoms in the plasma.
14. A method as stated in claim 12 in which the quench fluid composition is one of argon, helium, or nitrogen, and is added to the process stream as a cryogenic liquid.
15. A method as stated in claim 12 in which the process stream is directed in a flow path with a perimeter and the process steam is caused to converge after the addition of the quench fluid to concentrate the formed particles for their separation from the process stream.
16. A method as stated in claim 12 in which x has a value in the range of 45 to 55 weight percent nickel.
17. A method as stated in claim 12 in which x has a value in the range of 25 to 39 weight percent nickel.
18. A method as stated in claim 12 in which the iron, nickel, and additive A are mixed in an alloy before being added to the process fluid.
19. A method as stated in claim 12 in which the separated particles with the tetragonal L1 0 crystal structure are subjected to a combination of consolidation and magnetization to form an article having permanent magnet properties.
20. A method as stated in claim 12 in which heating of the separated particles is done in combination with one or more of (a) the application of pressure to the particles, (b) the application of a magnetic field to the particles, and (c) mechanical working of the particles.