CN113025912A - Iron-nickel-based hard magnetic material and preparation method thereof - Google Patents
Iron-nickel-based hard magnetic material and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C33/04—Making ferrous alloys by melting
- C22C33/06—Making ferrous alloys by melting using master alloys
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
Abstract
The invention discloses an iron-nickel-based hard magnetic material, and belongs to the technical field of magnetic materials. The method comprises the following steps: mainly consists of elements Fe, Ni, P and Si, and the component of the iron-nickel-based hard magnetic material is FeaNibSicPdSaid FeaNibSicPdIs in a polycrystalline form; wherein a, b, c and d respectively represent the mole percentage of each element, 40-b-42, 16-c + d-20, c < d. The hard magnetic material provided by the invention adds a proper amount of Si into the Fe-Ni-P alloy, and the highest coercive force reaches 920 Oe.
Description
Technical Field
The invention belongs to the technical field of magnetic materials, and particularly relates to an iron-nickel-based hard magnetic material and a preparation method thereof.
Background
At present, the high-performance permanent magnet mainly comprises two main types, one is a rare earth permanent magnet material represented by neodymium iron boron and samarium cobalt, and the other is a permanent magnet material represented by iron platinum and cobalt platinum and provided with L10A permanent magnetic material of a crystal structure. Although the former is relatively acceptable in terms of cost compared to the latter, it still requires a large use of scarce resources, hindering sustainable development in the field of application and production of magnetic materials. Also having L10Structure, L10FeNi (figure 1) does not contain precious elements and shows excellent permanent magnetism with high magnetocrystalline anisotropy performance, however, the alloy of Fe and Ni elements tends to preferentially form A1-FeNi (figure 1) without permanent magnetism under the normal conditions of solidification and heat treatment, so that Fe and Ni atoms in the alloy generally do not have the capacity of sufficient diffusion rearrangement to form ordered phases, thereby exciting the low-temperature diffusion capacity of Fe and Ni atoms in the alloy and improving L10The thermal stability of the phases is very important for the preparation of iron-nickel based hard magnetic materials.
Disclosure of Invention
In order to solve the problems, the invention provides an iron-nickel-based hard magnetic material and a preparation method thereof, the hard magnetic material is prepared by adding a proper amount of Si into Fe-Ni-P alloy, and the highest coercive force is up to 920 Oe. The method provided by the invention mainly adopts the crystallization phase change of the iron-nickel-based amorphous alloy to synthesize the alloy containing L10-a FeNi iron nickel based permanent magnet.
The invention provides an iron-nickel-based hard magnetic material which mainly comprises elements of Fe, Ni, P and Si and consists of FeaNibSicPdSaid FeaNibSicPdIs in a crystalline form; wherein a, b, c and d respectively represent the mole percentage of each element, 40-b-42, 16-c + d-20, c < d.
Preferably, 2. ltoreq. c.ltoreq.4.
More preferably, the iron-nickel based hard magnetic material is Fe42Ni42Si2P14Or Fe40Ni40Si4P16。
The second purpose of the invention is to provide a preparation method of the iron-nickel-based hard magnetic material, which comprises the following steps:
s1, uniformly mixing the raw materials of an iron source, a nickel source, a silicon source and a phosphorus source, smelting for 15-20 min at 1100-1250 ℃ under the protection of inert gas to obtain an intermediate alloy, and then rapidly cooling the intermediate alloy in a melt form to obtain an amorphous alloy; the phosphorus source is a phosphorus-containing iron alloy or nickel alloy;
and S2, annealing the amorphous alloy obtained in the S1 at 300-450 ℃ for 0.5-2 h to obtain the crystalline iron-nickel-based hard magnetic material.
Preferably, the iron source is pure iron and/or iron phosphide.
Preferably, the nickel source is pure nickel and/or nickel phosphide.
Preferably, the phosphorus source is iron phosphide and/or nickel phosphide; the silicon source is pure silicon.
Preferably, the melt rapid cooling rate is 1x106～4x106℃/s。
More preferably, the melt is rapidly cooled by a single-roller melt-spinning method, which comprises the following steps:
heating and melting the intermediate alloy on a single-roller strip throwing machine, pressurizing at 1100-1200 ℃ to spray the melt onto a rotating copper roller, and throwing out the melt through the copper roller to obtain the amorphous alloy.
More preferably, the diameter of the copper roller is 55mm, and the rotating speed is 4000 r/min.
Compared with the prior art, the invention has the beneficial effects that:
the hard magnetic material provided by the invention adds a proper amount of Si into the Fe-Ni-P alloy, and the highest coercive force reaches 920 Oe.
The invention utilizes the crystallization phase change of the iron-nickel-based amorphous alloy to synthesize the alloy containing L10The process of FeNi Fe-Ni based permanent magnet, adding proper amount of Si into alloy, can make L10FeNi withstands higher temperatures without decomposition, thus allowing a more efficient synthesis at higher temperatures.
Drawings
FIG. 1 shows L10Schematic structure of-FeNi and A1-FeNi.
FIG. 2 is an amorphous XRD diffraction pattern of the Fe-Ni-based hard magnetic material provided in examples 1-2 and comparative example 2.
FIG. 3 is a hysteresis loop of the Fe-Ni based hard magnetic material provided in examples 1-2 and comparative examples 1-2.
FIG. 4 is a transmission electron microscope image of the annealed strip of Fe-Ni based hard magnetic material provided in example 1. Wherein, the graph a is the bright field image of the electron microscope, the graph b is the high resolution image and the selected area diffraction pattern of the marked crystal grain in the broken line frame in the graph a, the inner and outer layer broken lines in the graph b respectively represent L10-the positions of the FeNi (001) and (110) superlattices diffraction sites.
Detailed Description
In order to make the technical solutions of the present invention better understood and enable those skilled in the art to practice the present invention, the following embodiments are further described, but the present invention is not limited to the following embodiments.
The experimental methods and the detection methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
A preparation method of an iron-nickel-based hard magnetic material comprises the following steps:
s1, weighing 23.26g of pure nickel, 0.53g of pure silicon and iron phosphide (Fe)3P)26.21g, for a total of 50g, for use
S2, mixing and loading the raw materials weighed in the S1 into a cylindrical alumina crucible, then placing the crucible into an induction melting furnace, and firstly vacuumizing the melting furnace to 1x10-2Pa or less (up to 10)-3Pa magnitude), under the protection of inert gas, introducing argon of 0.5atm, then starting to electrify and heat the coil of the induction furnace, keeping the temperature between 1100 and 1250 ℃, waiting for 15 minutes to ensure that all the raw materials are fully melted and uniformly mixed, stopping heating, opening a cabin door of the smelting furnace after the alloy is naturally cooled to below 200 ℃ to form an alloy ingot, and taking out the alloy ingot to obtain Fe-Ni-Si-P intermediate alloy;
s3, crushing the Fe-Ni-Si-P intermediate alloy ingot obtained in S2 into small blocks, wherein the grain diameter of the small blocks is subject to the fact that the small blocks can be placed in a quartz tube with the inner diameter of 10mm without hindrance, the intermediate alloy obtained in S2 is made into an amorphous strip by a single-roller strip throwing method, wherein the diameter of a copper roller is 55mm, the rotating speed is 4000 revolutions per minute, the control line speed in an experiment is controlled to be more than 45 meters per second, the quartz tube with the inner diameter of 10mm and a sharp nozzle at the bottom end (the diameter of a round hole of the sharp nozzle is 0.5mm) is used for containing about 4g of alloy fragments and is fixed on a strip throwing machine, the alloy fragments are fully melted through induction heating, the melt is sprayed onto the rotating copper roller under the pressurization at the temperature of 1150 ℃ (the reading of an infrared thermometer), the thrown strip is collected by an external pipeline of the equipment, or the heating and; the alloy strip structure is confirmed by an X-ray diffraction method (as shown in figure 2), and the basis for determining the amorphous structure is that no obvious crystal diffraction peak is observed;
s4, annealing the amorphous ribbon made of S3 at 370 ℃ for 1h to obtain the Fe-containing amorphous ribbon42Ni42Si2P14The iron-nickel based hard magnetic material of (a); and then, placing the sealed quartz tube filled with the amorphous strip into a box furnace with preset temperature, preserving the temperature for a designed time, and taking out the sealed quartz tube.
Example 2
A preparation method of an iron-nickel-based hard magnetic material comprises the following steps:
s1, weighing raw materials of 0.54g of pure iron, 19.23g of pure nickel, 1.08g of pure silicon and iron phosphide (Fe)3P)24.86g, nickel phosphide (Ni)2P)4.29g, 50g in total for standby;
s2, mixing and loading the raw materials weighed in the S1 into a cylindrical alumina crucible, then placing the crucible into an induction melting furnace, and firstly vacuumizing the melting furnace to 1x10-2Pa or less (up to 10)-3Pa magnitude), under the protection of inert gas, introducing argon of 0.5atm, then starting to electrify and heat the coil of the induction furnace, keeping the temperature between 1100 and 1250 ℃, waiting for 15 minutes to ensure that all the raw materials are fully melted and uniformly mixed, stopping heating, opening a cabin door of the smelting furnace after the alloy is naturally cooled to below 200 ℃ to form an alloy ingot, and taking out the alloy ingot to obtain Fe-Ni-Si-P intermediate alloy;
s3, crushing the Fe-Ni-Si-P intermediate alloy ingot obtained in S2 into small blocks, wherein the grain diameter of the small blocks is subject to the fact that the small blocks can be placed in a quartz tube with the inner diameter of 10mm without hindrance, the intermediate alloy obtained in S2 is made into an amorphous strip by a single-roller strip throwing method, wherein the diameter of a copper roller is 55mm, the rotating speed is 4000 revolutions per minute, the control line speed in an experiment is controlled to be more than 45 meters per second, the quartz tube with the inner diameter of 10mm and a sharp nozzle at the bottom end (the diameter of a round hole of the sharp nozzle is 0.5mm) is used for containing about 4g of alloy fragments and is fixed on a strip throwing machine, the alloy fragments are fully melted through induction heating, the melt is sprayed onto the rotating copper roller under the pressurization at the temperature of 1150 ℃ (the reading of an infrared thermometer), the thrown strip is collected by an external pipeline of the equipment, or the heating and; the alloy strip structure is confirmed by an X-ray diffraction method (as shown in figure 2), and the basis for determining the amorphous structure is that no obvious crystal diffraction peak is observed;
s4, annealing the amorphous ribbon made of S3 at 370 ℃ for 1h to obtain the Fe-containing amorphous ribbon40Ni40Si4P16The iron-nickel based hard magnetic material of (a); and then, placing the sealed quartz tube filled with the amorphous strip into a box furnace with preset temperature, preserving the temperature for a designed time, and taking out the sealed quartz tube.
Comparative example 1
The same as example 1, except that the amorphous alloy Fe obtained in S342Ni42Si2P14Fe-Ni based amorphous material Fe is obtained without annealing treatment42Ni42Si2P14。
Comparative example 2
A preparation method of an iron-nickel-based hard magnetic material is different from the embodiment 1 in that a silicon source is not introduced, and comprises the following steps:
s1, weighing 21.02g of pure nickel and iron phosphide (Fe)3P)26.19g, nickel phosphide (Ni)2P)2.79g, 50g in total for standby;
s2, mixing the raw materials weighed in the S1 and filling the mixture into a cylinderPlacing the crucible into an induction smelting furnace, and vacuumizing the smelting furnace to 1x10-2Pa or less (up to 10)-3Pa magnitude), under the protection of inert gas, introducing argon of 0.5atm, then starting to electrify and heat the coil of the induction furnace, keeping the temperature between 1100 and 1250 ℃, waiting for 15 minutes to ensure that all the raw materials are fully melted and uniformly mixed, stopping heating, opening a cabin door of the smelting furnace after the alloy is naturally cooled to below 200 ℃ to form an alloy ingot, and taking out the alloy ingot to obtain Fe-Ni-P intermediate alloy;
s3, crushing the Fe-Ni-P intermediate alloy ingot obtained in S2 into small blocks, wherein the grain diameter of the small blocks is subject to the fact that the small blocks can be placed in a quartz tube with the inner diameter of 10mm without hindrance, the intermediate alloy obtained in S2 is made into an amorphous strip by a single-roller melt-spun method, wherein the diameter of a copper roller is 55mm, the rotating speed is 4000 revolutions per minute, the control line speed in the experiment is over 45 meters per second, the quartz tube with the inner diameter of 10mm and a sharp nozzle at the bottom end (the diameter of a round hole of the sharp nozzle is 0.5mm) is used for containing about 4g of alloy fragments and is fixed on a melt-spun machine, the alloy fragments are fully melted by induction heating, and the melt is pressurized to be sprayed onto the rotating copper roller (the cooling speed is about 1x106～4x106DEG C/s), collecting the thrown strip by an external pipeline of the equipment, or collecting the strip after closing a heating and copper roller rotating motor after the spraying is finished to obtain an amorphous strip; the alloy strip structure is confirmed by an X-ray diffraction method (as shown in figure 2), and the basis for determining the amorphous structure is that no obvious crystal diffraction peak is observed;
s4, annealing the amorphous ribbon made of S3 at 370 ℃ for 1h to obtain the Fe-containing amorphous ribbon42Ni42P16The iron-nickel based hard magnetic material of (a); and then, placing the sealed quartz tube filled with the amorphous strip into a box furnace with preset temperature, preserving the temperature for a designed time, and taking out the sealed quartz tube.
In order to illustrate various properties of the iron-nickel-based hard magnetic material prepared by the preparation method of the iron-nickel-based hard magnetic material provided in the embodiments 1 to 2, the relevant properties of the iron-nickel-based hard magnetic material are detected. See Table 1, and FIGS. 3-4.
FIG. 2 shows Fe provided in examples 1 to 2 and comparative example 242Ni42Si2P14、Fe40Ni40Si4P16And Fe42Ni42P16Amorphous XRD pattern of Fe-Ni based hard magnetic material; as can be seen from fig. 2, no distinct crystalline diffraction peak was observed, and the structure was determined to be amorphous.
FIG. 3 shows Fe provided in examples 1 to 2 and comparative examples 1 to 2, respectively42Ni42S2P14、Fe40Ni40Si4P16、Fe42Ni42P16Annealed strip and Fe42Ni42S2P14Hysteresis loop of amorphous strip. Table 1 shows Fe provided for examples 1 to 2 and comparative examples 1 to 2, respectively42Ni42S2P14、Fe40Ni40Si4P16、Fe42Ni42P16Annealed strip and Fe42Ni42S2P14Magnetic properties of the amorphous strip.
As can be seen from the intersection of the hysteresis loop and the abscissa in FIG. 3 and Table 1, the coercivity of comparative example 1 is 50Oe or less (lower than the effective measurement range of the test equipment), the highest coercivity of the Fe-Ni-P alloy series provided in comparative example 2 is about 734Oe, and the Fe-Ni-Si-P alloy series provided in examples 1 and 2 are the derived modified Fe component of the former42Ni42S2P14And Fe40Ni40Si4P16The highest coercivity of the two modified composition annealed strips reached 905Oe and 920Oe, respectively. The test result shows that the heat treatment plays an important role in improving the coercive force of the iron-nickel-based amorphous alloy, and meanwhile, the addition of Si increases L10The disorder degree of the chemical arrangement of the-FeNi structure is improved, and the L1 is improved0The thermal stability and the annealing tendency of FeNi are favorable for improving the coercive force of an annealed strip.
Table 1 is Fe42Ni42S2P14、Fe40Ni40Si4P16、Fe42Ni42P16Annealed strip and Fe42Ni42S2P14Magnetic properties of the amorphous strip.
FIG. 4 shows Fe provided in example 142Ni42Si2P14Transmission electron microscope atlas of annealed strip of iron-nickel based hard magnetic material. Wherein, the drawing a is electron microscope bright field image, the drawing b is high resolution image and its selective area diffraction pattern of the marked crystal grain in the upper left area circle frame in the drawing a, the inner and outer layer dotted lines in the drawing b respectively represent L10-the positions of the FeNi (001) and (110) superlattices diffraction sites. Due to the superlattice diffraction in the system as L10Characteristic diffraction signal of the FeNi phase, thus visually confirming Fe42Ni42S2P14L1 in iron-nickel annealed strip0Presence of phase, further elucidating Fe42Ni42S2P14The iron-nickel annealed strip is in a polycrystalline form.
In summary, conventional L10The difficulty of the synthesis of FeNi is that it is converted into disordered A1-FeNi at 320 ℃ and the iron-nickel atom lacks the diffusion capacity seriously below this temperature, thus increasing L10Phase stability is very important for the preparation of iron-nickel based hard magnetic materials. The invention utilizes Fe-Ni based amorphous alloy to synthesize L1 by crystallization0FeNi, so that iron and nickel atoms in the alloy have one-time diffusion rearrangement capacity at a lower temperature; simultaneously, a proper amount of Si is added into the alloy, and L1 is added0The disorder degree of the structure enhances L10The thermal stability of the FeNi phase, thus increasing the annealing temperature that can be tolerated for its synthesis. Higher annealing temperature can bring more sufficient iron-nickel atom rearrangement, and improve L10The content of FeNi in the alloy improves the coercive force of the iron-nickel-based hard magnetic material.
The theoretical analysis provided by the invention shows that Co, Mn and other soluble L1 are added into the iron-nickel-based hard magnetic material0The element of-FeNi can also play a similar effect to SiAnd (5) fruit.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, it is intended that such changes and modifications be included within the scope of the appended claims and their equivalents.
Claims (10)
1. The Fe-Ni-based hard magnetic material is characterized by mainly comprising elements Fe, Ni, P and Si, wherein the component of the Fe-Ni-based hard magnetic material is FeaNibSicPdSaid FeaNibSicPdIs in a polycrystalline form; wherein a, b, c and d respectively represent the mole percentage of each element, 40-b-42, 16-c + d-20, c < d.
2. An iron-nickel based hard magnetic material according to claim 1, characterized in that 2. ltoreq. c.ltoreq.4.
3. The Fe-Ni-based hard magnetic material of claim 2, wherein the Fe-Ni-based hard magnetic material is Fe42Ni42Si2P14Or Fe40Ni40Si4P16。
4. A method for preparing an iron-nickel based hard magnetic material according to any one of claims 1 to 3, comprising the steps of:
s1, uniformly mixing the raw materials of an iron source, a nickel source, a silicon source and a phosphorus source, smelting for 15-20 min at 1100-1250 ℃ under the protection of inert gas to obtain an intermediate alloy, and then rapidly cooling the intermediate alloy in a melt form to obtain an amorphous alloy; the phosphorus source is a phosphorus-containing iron alloy or nickel alloy;
and S2, annealing the amorphous alloy obtained in the S1 at 300-450 ℃ for 0.5-2 h to obtain the crystalline iron-nickel-based hard magnetic material.
5. A method of producing an iron-nickel based hard magnetic material according to claim 4, wherein the iron source is pure iron and/or iron phosphide.
6. A method of producing an iron-nickel based hard magnetic material according to claim 4, wherein the nickel source is pure nickel and/or nickel phosphide.
7. The method of claim 4, wherein the phosphorous source is iron and/or nickel phosphide; the silicon source is pure silicon.
8. The method of claim 4, wherein the melt rapid cooling rate is 1x106～4x106℃/s。
9. The method for preparing the iron-nickel-based hard magnetic material according to claim 8, wherein the melt is rapidly cooled by a single-roller melt-spinning method, and the method comprises the following specific steps:
heating and melting the intermediate alloy on a single-roller strip throwing machine, pressurizing at 1100-1200 ℃ to spray the melt onto a rotating copper roller, and throwing out the melt through the copper roller to obtain the amorphous alloy.
10. The method of claim 9, wherein the copper roller has a diameter of 55mm and a rotational speed of 4000 r/min.
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| CN115637394A (en) * | 2022-10-21 | 2023-01-24 | 西北工业大学 | Cobalt-reinforced iron-nickel-based hard magnetic alloy and preparation method thereof |
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| CN115026514A (en) * | 2022-05-25 | 2022-09-09 | 西安理工大学 | Preparation method of bidirectional threaded rod based on carbon alloy material |
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| CN115637394B (en) * | 2022-10-21 | 2023-11-07 | 西北工业大学 | Cobalt-reinforced iron-nickel-based hard magnetic alloy and preparation method thereof |
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