CN111261351B - High-coercivity SmCo5FeCo nano composite permanent magnetic material and preparation method thereof - Google Patents

High-coercivity SmCo5FeCo nano composite permanent magnetic material and preparation method thereof Download PDF

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CN111261351B
CN111261351B CN202010136812.4A CN202010136812A CN111261351B CN 111261351 B CN111261351 B CN 111261351B CN 202010136812 A CN202010136812 A CN 202010136812A CN 111261351 B CN111261351 B CN 111261351B
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alloy
magnetic material
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CN111261351A (en
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安士忠
李孝森
李武会
徐盼盼
殷婷
朱雁风
任凤章
宋克兴
马峥
吕贵红
肖滕龙
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Henan University of Science and Technology
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    • 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
    • H—ELECTRICITY
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    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
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    • 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
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/0551—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 in the form of particles, e.g. rapid quenched powders or ribbon flakes
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    • 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
    • H01F1/06—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 in the form of particles, e.g. powder
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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
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    • H01F1/08—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 in the form of particles, e.g. powder pressed, sintered, or bound together
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    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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    • H01F41/0266—Moulding; Pressing
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    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets

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Abstract

The invention belongs to the technical field of permanent magnet materials, and particularly relates to high-coercivity SmCo5a/FeCo nano composite permanent magnetic material and a preparation method thereof. SmCo of the present invention5the/FeCo nano composite permanent magnetic material is prepared from SmCo5alpha-Fe and SmCo5Mixing hard magnetic phase stabilizing components and performing thermal deformation treatment to obtain the SmCo5The hard magnetic phase stabilizing component is SmNi alloy and/or SmZn alloy; the mass of the alpha-Fe is SmCo5And 20 to 50% of the total mass of alpha-Fe. SmCo5The hard magnetic phase stabilizing component can stabilize SmCo5Of the present invention, thus the SmCo of the present invention5the/FeCo nano composite permanent magnetic material has high coercive force which is 4-6 times of the coercive force of a composite material which does not contain SmNi or SmZn alloy and is prepared under the same condition.

Description

High-coercivity SmCo5FeCo nano composite permanent magnetic material and preparation method thereof
Technical Field
The invention belongs to the technical field of permanent magnet materials, and particularly relates to a permanent magnet materialHigh-coercivity SmCo5a/FeCo nano composite permanent magnetic material and a preparation method thereof.
Background
SmCo5The material is a hard magnetic material, has a strong magnetocrystalline anisotropy field (40T) and a high coercive force (5-7T can be achieved in a laboratory), but has low saturation magnetization. While soft magnetic phases such as Fe, Co and FeCo alloys, etc., having high saturation magnetization, are compared to SmCo5The nano-composite material with the characteristics of high saturation magnetization, high remanence and high coercivity can be obtained hopefully in nano-size composite. But soft magnetic phase and SmCo5SmCo formed by recombination5SmCo when the content of the soft magnetic phase in the soft magnetic phase two-phase nano composite material is higher (more than or equal to 20 percent)5Compatibility is easy to convert into SmCo3、SmCo7And Sm2Co17A phase with lower iso-magnetocrystalline anisotropy, thereby enabling SmCo5The coercive force of the soft magnetic phase two-phase nano composite material is lower.
Disclosure of Invention
The invention aims to provide high-coercivity SmCo5The composite permanent magnetic material has high coercive force.
The object of the present invention is to provide a high coercive force SmCo5A preparation method of a/FeCo nano composite permanent magnetic material.
In order to achieve the purpose, the invention adopts the technical scheme that:
high-coercivity SmCo5a/FeCo nano composite permanent magnetic material made of SmCo5alpha-Fe and SmCo5Mixing hard magnetic phase stabilizing components, compacting, and thermally deforming to obtain SmCo5The hard magnetic phase stabilizing component is SmNi alloy and/or SmZn alloy; the mass of the alpha-Fe is SmCo5And 20 to 50% of the total mass of alpha-Fe.
SmCo5Being a hard magnetic phase, SmCo5Sm atoms and Ni atoms or Zn atoms in the hard magnetic phase stabilizing component enter SmCo by diffusion5In the crystal lattice of (2), SmCo can be improved5Stability of crystal structure, thereby suppressing SmCo5Phase inversion, so that the SmCo of the present invention5the/FeCo nano composite permanent magnetic material has higher coercive force. The coercive force of the nano composite material of the invention is prepared under the same condition and does not contain SmCo54-6 times of the composite material of the hard magnetic phase stabilizing component.
The magnetic properties of the nanocomposite permanent magnetic material of the invention, the SmCo, are further optimized by adjusting the quality of the raw materials used5The hard magnetic phase stabilizing component has a mass of SmCo5alpha-Fe and SmCo52.5-10% of the total mass of the hard magnetic phase stabilizing components; the mass percentage of Sm in the SmNi and SmZn alloy is 50-90%, and the balance is Ni or Zn. Further preferably, the SmCo5The hard magnetic phase stabilizing component has a mass of SmCo5alpha-Fe and SmCo52.5-7.5% of the total mass of the hard magnetic phase stabilizing components; the mass percentage of Sm in the SmNi and SmZn alloy is 83-88%, and the balance is Ni or Zn. When the Sm content in the SmNi and SmZn alloy is too low, the alloy can be used for SmCo5The phase stabilization effect is poor; meanwhile, a small amount of Ni or Zn in the alloy can promote the diffusion of atoms and stabilize SmCo5And (4) forming a phase.
High coercivity SmCo of the invention5The preparation method of the/FeCo nano composite permanent magnetic material adopts the technical scheme that:
the SmCo with high coercive force5The preparation method of the/FeCo nano composite permanent magnetic material comprises the following steps: SmCo is mixed5alpha-Fe and SmCo5Uniformly mixing the hard magnetic phase stabilizing components to obtain a mixture; and (3) pressing and forming the mixture, and then carrying out thermal deformation treatment.
The preparation method of the invention prepares SmCo5The hard magnetic phase stabilizing component is uniformly introduced into the hard magnetic phase SmCo5In order to stabilize the hard magnetic phase SmCo5The function of the structure. SmCo prepared by adopting preparation method of the invention5the/FeCo nano composite permanent magnetic material has higher compactness, and the main phase of the hard magnetic phase is SmCo with a strong magnetocrystalline anisotropy field5The phase has higher coercive force and better comprehensive magnetic performance. The preparation process is simple and feasible, and the cost is low.
The compactness of the nanocomposite material of the invention is further improved and the production time is shortened by optimizing the conditions of thermal Deformation treatment, preferably, the temperature (T) during the thermal Deformation treatment is 600-900 ℃, the Deformation amount (Reduction) is 30-90%, and the Deformation rate (Deformation rate) is 5%/min-100%/min. More preferably, the temperature during the thermal deformation treatment is 600 ℃, the deformation amount is 60%, and the deformation rate is 30%/min to 50%/min.
The SmNi or SmZn alloy being sized to enable the SmCo to be used5The size of the alpha-Fe raw material is matched. Preferably, SmCo5The alpha-Fe and the SmNi or the SmZn alloy are powder or alloy quick-setting thin strips. Wherein the SmNi or SmZn alloy powder can be obtained by crushing an alloy ingot. Preferably, the SmNi or SmZn alloy is an alloy rapid-hardening thin strip, and the thickness of the alloy rapid-hardening thin strip is 10-200 μm. The alloy grains in the alloy rapid-hardening thin strip are fine, which is beneficial to alloy and SmCo5And alpha-Fe. Meanwhile, compared with an ingot, the alloy rapid-hardening thin strip is more brittle, is easier to break, is convenient to mix uniformly, and saves mixing time.
Preferably, SmCo5The alpha-Fe and the powder have the particle size of less than 180 mu m. SmCo5The particle diameter of (b) may be the same as or different from that of the α -Fe particle.
In order to improve the mixing uniformity of the three raw materials, the mixing is ball milling mixing, the ball milling time is 4-24 hours, and the rotating speed is 300-700 r/min.
The pressure used during the compression molding is 0.8-1.2 GPa, the die used during the compression molding is stainless steel, and the temperature during the compression molding is room temperature. The pressing forming specifically comprises the following steps: pressing the mixture into thin slices (thickness/diameter is less than 0.4), and filling the thin slices into a steel pipe to obtain a green compact. The compact is used for subsequent hot deformation treatment.
High coercive force SmCo in the present invention5In the preparation method of the/FeCo nano composite permanent magnetic material, mixing, compression molding and thermal deformation treatment are carried out in a protective atmosphere. Preferably, the protective atmosphere is an argon atmosphere.
Drawings
FIG. 1 shows SmCo of the present invention5A preparation flow chart of a/FeCo nano composite permanent magnetic material;
FIG. 2 is the initial magnetization curve and hysteresis loop of the nanocomposite permanent magnetic material of example 1 of the present invention and the nanocomposite material of comparative example 1;
FIG. 3 is the initial magnetization curve and hysteresis loop of the nanocomposite permanent magnetic material of example 2 of the present invention and the nanocomposite material of comparative example 1;
FIG. 4 is the initial magnetization curve and hysteresis loop for the nanocomposite permanent magnetic material of example 3 of the present invention and the nanocomposite material of comparative example 1;
FIG. 5 is the initial magnetization curve and hysteresis loop for the nanocomposite permanent magnetic material of example 4 of the present invention and the nanocomposite material of comparative example 1;
FIG. 6 is a TEM (a) and a selected area electron diffraction pattern (b) of the nanocomposite of comparative example 1 of the present invention;
FIG. 7 is a TEM (a) and selected area electron diffraction pattern (b) of a nanocomposite permanent magnetic material of example 1 of the present invention;
FIG. 8 is a TEM (a) and selected area electron diffraction pattern (b) of a nanocomposite permanent magnetic material of example 3 of the present invention;
FIG. 9 is an XRD pattern of the nanocomposite permanent magnetic material of example 1 of the present invention and the nanocomposite material of comparative example 1;
fig. 10 is an XRD pattern of the nanocomposite permanent magnetic material of example 3 of the present invention and the nanocomposite material of comparative example 1.
Detailed Description
The present invention will be further described with reference to the following specific examples.
SmCo used in the following examples5The powder is prepared by the following method: calculating the simple substances Sm and Co with the purity of more than 99.5 percent according to the stoichiometric ratio of 1:5, adding more Sm with the mass of 5 percent of the simple substance Sm calculated according to the stoichiometric ratio during smelting, and smelting to obtain SmCo5Ingot casting SmCo5And (4) crushing the cast ingot, and sieving the crushed cast ingot with a 80-mesh sieve to obtain the product.
High coercive force SmCo5FeCo nano composite permanent magnetExamples of materials
Example 1
High coercive force SmCo of this example5the/FeCo nano composite permanent magnetic material is prepared from SmCo5The powder and the alpha-Fe powder (the powder after being sieved by a sieve of 80 meshes and a SmNi alloy rapid hardening thin strip (the thickness is 10-50 mu m)) are mixed and then subjected to thermal deformation treatment to obtain the alloy, wherein the mass of the alpha-Fe is SmCo 520 percent of the powder and the alpha-Fe powder by mass, and the mass of the SmNi alloy rapid-hardening thin strip is SmCo52.5 percent of the total mass of the powder, the alpha-Fe powder and the SmNi alloy rapid-hardening thin strip; the mass percent of Sm in the SmNi alloy rapid-hardening thin strip is 83 percent, and the balance is Ni.
Example 2
High coercive force SmCo of this example5the/FeCo nano composite permanent magnetic material is prepared from SmCo5The alloy material is prepared by mixing powder, alpha-Fe powder (powder after being sieved by a sieve of 80 meshes) and a SmNi alloy rapid-hardening thin strip (the thickness is 30-90 mu m) and then carrying out thermal deformation treatment on the mixture, wherein the mass of the alpha-Fe is SmCo 520 percent of the powder and the alpha-Fe powder by mass, and the mass of the SmNi alloy rapid-hardening thin strip is SmCo57.5 percent of the total mass of the powder, the alpha-Fe powder and the SmNi alloy rapid-hardening thin strip; the mass percent of Sm in the SmNi alloy rapid-hardening thin strip is 83 percent, and the balance is Ni.
Example 3
High coercive force SmCo of this example5the/FeCo nano composite permanent magnetic material is prepared from SmCo5The alloy material is prepared by mixing powder, alpha-Fe powder (powder sieved by a sieve of 80 meshes) and a SmZn alloy rapid-hardening thin strip (the thickness is 80-150 mu m) and then carrying out thermal deformation treatment on the mixture, wherein the mass of the alpha-Fe is SmCo 520 percent of the powder and the alpha-Fe powder by mass, and the mass of the SmCo alloy rapid-hardening thin strip is SmCo 55 percent of the total mass of the powder, the alpha-Fe powder and the SmZn alloy rapid-hardening thin strip; the mass percent of Sm in the SmZn alloy rapid-hardening thin strip is 88 percent, and the balance is Zn.
Example 4
High coercive force SmCo of this example5the/FeCo nano composite permanent magnetic material is prepared from SmCo5The alloy material is prepared by mixing powder, alpha-Fe powder (powder sieved by a sieve of 80 meshes) and a SmZn alloy rapid-hardening thin strip (the thickness is 140-200 mu m) and then carrying out thermal deformation treatment on the mixture, wherein the mass of the alpha-Fe is SmCo5Powder and alpha20% of Fe powder and SmCo alloy rapid-hardening thin strip57.5 percent of the total mass of the powder, the alpha-Fe powder and the SmZn alloy rapid-hardening thin strip; the mass percent of Sm in the SmZn alloy rapid-hardening thin strip is 88 percent, and the balance is Zn.
Example 5
High coercive force SmCo of this example5the/FeCo nano composite permanent magnetic material is prepared from SmCo5The alloy material is prepared by mixing powder, alpha-Fe powder (powder sieved by a sieve of 80 meshes) and a SmZn alloy rapid-hardening thin strip (the thickness is 10-80 mu m) and then carrying out thermal deformation treatment on the mixture, wherein the mass of the alpha-Fe is SmCo 530 percent of the powder and the alpha-Fe powder by mass, and the mass of the SmCo alloy rapid-hardening thin strip is SmCo5The total mass of the powder, the alpha-Fe powder and the SmZn alloy rapid-hardening thin strip is 10 percent; the mass percent of Sm in the SmZn alloy rapid-hardening thin strip is 50 percent, and the balance is Zn.
Example 6
High coercive force SmCo of this example5the/FeCo nano composite permanent magnetic material is prepared from SmCo5The alloy material is prepared by mixing powder, alpha-Fe powder (powder sieved by a sieve of 80 meshes) and a SmZn alloy rapid-hardening thin strip (the thickness is 70-160 mu m), and then carrying out thermal deformation treatment on the mixture, wherein the mass of the alpha-Fe is SmCo 540% of the powder and the alpha-Fe powder, and the mass of the SmCo alloy rapid-hardening thin strip is SmCo5The total mass of the powder, the alpha-Fe powder and the SmZn alloy rapid-hardening thin strip is 10 percent; the mass percent of Sm in the SmZn alloy rapid-hardening thin strip is 70 percent, and the balance is Zn.
Example 7
High coercive force SmCo of this example5the/FeCo nano composite permanent magnetic material is prepared from SmCo5The alloy material is prepared by mixing powder, alpha-Fe powder (powder after being sieved by a sieve of 80 meshes) and a SmZn alloy rapid-hardening thin strip (the thickness is 120-200 mu m) and then carrying out thermal deformation treatment on the mixture, wherein the mass of the alpha-Fe is SmCo 550 percent of the powder and the alpha-Fe powder by mass, and the mass of the SmCo alloy rapid-hardening thin strip is SmCo5The total mass of the powder, the alpha-Fe powder and the SmZn alloy rapid-hardening thin strip is 10 percent; the mass percent of Sm in the SmZn alloy rapid-hardening thin strip is 90%, and the balance is Zn.
Second, high coercive force SmCo5Examples of the preparation method of/FeCo nanocomposite permanent magnetic materials
High coercivity SmCo of the invention5The preparation process flow of the/FeCo nano composite permanent magnetic material is shown in figure 1, and comprises the following steps: firstly, the raw material (SmCo)5+ α -Fe + (smini or SmZn)) to be Ball-Milled and mixed (Ball milling) to obtain mixed powder (Milled powder), wherein the mixed powder is Amorphous powder containing a FeCo phase (amophorus + FeCo); then putting the mixed powder into a stainless Steel mold for compression molding (consolidation), firstly compressing to obtain a slice (the thickness/diameter is less than 0.4) in order to ensure the density, and then putting the slice into a stainless Steel sleeve (Steel Capsule or Capsule) to obtain a pressed compact; the green compact is then subjected to a Hot deformation treatment (Hot deformation) and after the Hot deformation treatment, a mechanical working (Machining) is carried out to cause the material (Sample) to fall out of the stainless steel sleeve. Ball milling, pressing and hot deformation were all performed under argon (oxygen content less than 5ppm) protection to reduce oxidation.
Example 8
The preparation process of this example gives a product corresponding to the high coercivity SmCo in example 15the/FeCo nano composite permanent magnetic material comprises the following steps:
(1) SmCo is mixed5Ball-milling the powder, the alpha-Fe powder and the SmNi alloy rapid-hardening thin strip in an all-directional planetary ball mill for 6 hours at the rotating speed of 500r/min by using argon as a ball-milling medium to obtain mixed powder;
the SmNi alloy rapid-hardening thin strip is prepared by the following method: firstly, carrying out electric arc melting to obtain a SmNi alloy cast ingot, and then preparing the SmNi alloy cast ingot into a quick-setting thin strip on vacuum quick-quenching equipment, wherein the specific process comprises the following steps: vacuum degree higher than 1 x 10-3Under the condition of Pa, the alloy ingot is heated and melted and then rapidly sprayed onto a water-cooled copper wheel with the rotating speed of 40m/s under pressure.
(2) Loading the mixed powder into a stainless steel die in an argon atmosphere, then applying a pressure of 1GPa to the powder along the axial direction at room temperature, firstly pressing to obtain a sheet (the thickness/diameter is 0.2-0.3), and then loading the sheet into a stainless steel sleeve to obtain a pressed compact (the outside is the stainless steel sleeve); and then carrying out thermal deformation treatment along the axial direction, wherein the thermal deformation temperature is 600 ℃, the deformation amount is 60%, the deformation rate is 30%/min, and removing the stainless steel sleeve after the thermal treatment is finished.
Example 9
The preparation process of this example gives a product corresponding to the high coercivity SmCo of example 25The specific process of the/FeCo nano composite permanent magnetic material is the same as that of example 8.
Example 10
The preparation process of this example gives a product corresponding to the high coercivity SmCo in example 35the/FeCo nano composite permanent magnetic material comprises the following steps:
(1) SmCo is mixed5Ball-milling the powder, the alpha-Fe powder and the SmZn alloy rapid-hardening thin strip in an all-directional planetary ball mill for 6 hours at the rotating speed of 500r/min by using argon as a ball-milling medium to obtain mixed powder;
the SmZn alloy rapid-hardening thin strip is prepared by the following method: firstly, carrying out electric arc melting to obtain a SmZn alloy cast ingot, and then preparing the SmZn alloy cast ingot into a quick-setting thin strip on vacuum quick-quenching equipment, wherein the specific process comprises the following steps: vacuum degree higher than 1 x 10-3Under the condition of Pa, the alloy ingot is heated and melted and then rapidly sprayed onto a water-cooled copper wheel with the rotating speed of 40m/s under pressure.
(2) Loading the mixed powder into a stainless steel die in an argon atmosphere, then applying a pressure of 1GPa to the powder along the axial direction at room temperature, firstly pressing to obtain a sheet (the thickness/diameter is 0.2-0.3), and then loading the sheet into a stainless steel sleeve to obtain a pressed compact (the outside is the stainless steel sleeve); and then carrying out thermal deformation treatment along the axial direction, wherein the thermal deformation temperature is 600 ℃, the deformation amount is 60%, the deformation rate is 50%/min, and removing the stainless steel sleeve after the thermal treatment is finished.
Example 11
The preparation process of this example gives a product corresponding to the high coercivity SmCo in example 45The specific process of the/FeCo nano composite permanent magnetic material is basically the same as that of the example 10, and the difference is only that: the deformation rate in the thermal deformation in the step (2) is 30%/min.
Example 12
The preparation process of this example produced a product corresponding to the high coercivity SmCo of example 55The specific process of the/FeCo nano composite permanent magnetic material is basically the same as that of the example 10 are identical, differing only in that: the time for ball milling in the step (1) is 4h, and the rotating speed is 700 r/min; in the step (2), a compact is obtained by applying a pressure of 1.2GPa to the powder, the temperature during thermal deformation is 700 ℃, the deformation amount is 30%, and the deformation rate is 5%/min.
Example 13
The preparation process of this example produced a product corresponding to the high coercivity SmCo of example 65The specific process of the/FeCo nano composite permanent magnetic material is basically the same as that of the example 10, and the difference is only that: the time for ball milling in the step (1) is 12 hours, and the rotating speed is 600 r/min; in the step (2), a compact is obtained by applying a pressure of 1.1GPa to the powder, the temperature during thermal deformation is 800 ℃, the deformation amount is 60 percent, and the deformation rate is 80 percent/min.
Example 14
The preparation process of this example produced a product corresponding to the high coercivity SmCo of example 75The specific process of the/FeCo nano composite permanent magnetic material is basically the same as that of the example 10, and the difference is only that: the time for ball milling in the step (1) is 24 hours, and the rotating speed is 300 r/min; in the step (2), a green compact is obtained by applying a pressure of 0.8GPa to the powder, the temperature during thermal deformation is 900 ℃, the deformation is 90%, and the deformation rate is 100%/min.
Thirdly, comparison example: without SmNi or SmZn alloys
Comparative example 1
SmCo of this comparative example5/soft magnetic phase nano composite material made of SmCo5Mixing the powder and alpha-Fe powder, and thermally deforming to obtain the final product, wherein the alpha-Fe is SmCo 520% of the powder and the alpha-Fe powder by mass, the specific preparation method is basically the same as that of example 8, and the differences are only that: and (2) adding SmNi alloy or SmZn alloy during ball milling in the step (1).
SmCo of this comparative example5When the soft magnetic phase nanocomposite material is prepared, a sample is prepared in the same batch as the samples in the embodiments 8-9, and is marked as a sample without introduction of the SmNi alloy (without SmNi); then, another sample was prepared in the same batch as the samples in examples 10 to 14, and was labeled as a sample without introduction of SmZn alloy (without SmZn).
Comparative example 2
SmCo of this comparative example5/soft magnetic phase nano composite material made of SmCo5Mixing the powder and alpha-Fe powder, and thermally deforming to obtain the final product, wherein the alpha-Fe is SmCo 530% of the powder and the alpha-Fe powder by mass, the specific preparation method is basically the same as that of example 12, and the differences are only that: and (2) adding SmNi alloy or SmZn alloy during ball milling in the step (1).
Comparative example 3
SmCo of this comparative example5/soft magnetic phase nano composite material made of SmCo5Mixing the powder and alpha-Fe powder, and thermally deforming to obtain the final product, wherein the alpha-Fe is SmCo 540% of the powder and α -Fe powder by mass, the specific preparation method is basically the same as in example 13, except that: and (2) adding SmNi alloy or SmZn alloy during ball milling in the step (1).
Comparative example 4
SmCo of this comparative example5/soft magnetic phase nano composite material made of SmCo5Mixing the powder and alpha-Fe powder, and thermally deforming to obtain the final product, wherein the alpha-Fe is SmCo 550% of the powder and the α -Fe powder by mass, the specific preparation method is basically the same as that of example 14, except that: and (2) adding SmNi alloy or SmZn alloy during ball milling in the step (1).
Fourth, test example
Test example 1
The magnetic properties of the nanocomposite permanent magnet materials of examples 1-7 and the nanocomposite materials of comparative examples 1-4 were tested, and the specific test procedure was as follows: at room temperature, testing an initial magnetization curve of 0-3T, and then measuring a hysteresis loop under the condition of 3T-3T, wherein a sample during testing is a cylinder with phi of 3mm multiplied by 3, and the sample during testing is along the axial direction of the cylinder. The initial magnetization curves and hysteresis loops of the materials of examples 1 to 4 and comparative example 1 are shown in fig. 2 to 5, respectively.
FIG. 2 is a hysteresis loop of a nanocomposite permanent magnetic material of example 1 of the present invention (with 2.5% SmNi) and a nanocomposite material of comparative example 1 (with without SmNi); FIG. 3 is a hysteresis loop of a nanocomposite permanent magnetic material of example 2 of the present invention (with 7.5% SmNi) and a nanocomposite material of comparative example 1 (with without SmNi); FIG. 4 is a hysteresis loop of a nanocomposite permanent magnetic material of example 3 of the present invention (with 5% SmZn) and a nanocomposite material of comparative example 1 (with without SmZn); FIG. 5 is a hysteresis loop of the nanocomposite permanent magnetic material of example 4 of the present invention (with 7.5% SmZn) and the nanocomposite material of comparative example 1 (wthout SmZn).
As can be seen from fig. 2 to 5, the coercive force of the nanocomposite of comparative example 1 when the SmNi alloy or the SmZn alloy was not introduced was only 1.24kOe (sample to which the SmNi alloy was not introduced) and 1.54kOe (sample to which the SmZn alloy was not introduced) (the sample to which the SmNi alloy was not introduced and the sample to which the SmZn alloy was not introduced were not prepared in the same lot, and thus the coercive force was different, but within the error allowance range). The coercive force of the nano composite permanent magnetic material in the embodiment 1 is 5.13kOe, which is 4.1 times of that of the nano composite material in the comparative example 1; the coercive force of the nanocomposite permanent magnetic material of example 2 was 7.29kOe, which was 5.9 times that of the nanocomposite material of comparative example 1; the coercive force of the nanocomposite permanent magnetic material of example 3 was 6.88kOe, which was 4.5 times that of the nanocomposite material of comparative example 1; the coercivity of the nanocomposite permanent magnetic material of example 4 was 8.37kOe, which is 5.4 times that of the nanocomposite material of comparative example 1. Meanwhile, as can be seen from fig. 2 to 5, the residual magnetization of the nanocomposite material of the present invention is also improved.
The test results also show that: the coercivity of the nanocomposite permanent magnetic material in example 5 was 5.08kOe, while the coercivity of the nanocomposite material in comparative example 2 was 1.02 kOe; the coercivity of the nanocomposite permanent magnetic material in example 6 was 4.98kOe, while the coercivity of the nanocomposite material in comparative example 3 was 0.96 kOe; the coercivity of the nanocomposite permanent magnetic material in example 7 was 4.57kOe, while the coercivity of the nanocomposite material in comparative example 4 was 0.89 kOe.
Test example 2
TEM tests were performed on the nanocomposite permanent magnetic materials in examples 1 and 3 and the nanocomposite material in comparative example 1, and the test results are shown in FIGS. 6 to 8. In which fig. 6 is a tem (a) and a selected area electron diffraction pattern (b) of the nanocomposite material of comparative example 1, the results show that the material has a grain size of about 10nm,from Sm2Co17And an alpha-FeCo phase. FIG. 7 shows TEM (a) and selected area electron diffraction patterns (b) of the nanocomposite permanent magnetic material of example 1, showing that the material has a grain size of about 10nm, and is formed by SmCo5、Sm2Co17And an alpha-FeCo phase. FIG. 8 shows TEM (a) and selected area electron diffraction patterns (b) of the nanocomposite permanent magnetic material of example 3, showing that the material has a grain size of about 10nm, and is formed by SmCo5、Sm2Co17And an alpha-FeCo phase.
The test results show that the SmNi or SmZn alloy has small influence on the grain size of the material after being introduced and can stabilize SmCo5And (4) phase(s).
Test example 3
XRD tests were performed on the nanocomposite permanent magnetic materials of examples 1 and 3 and the nanocomposite material of comparative example 1, and the results are shown in fig. 9 and 10.
FIG. 9 is an XRD pattern of the nanocomposite permanent magnetic material of example 1 (with 2.5 wt.% SmNi) and the nanocomposite material of comparative example 1 (with SmNi out); fig. 10 is an XRD pattern in the nanocomposite permanent magnetic material of example 3 (with 5 wt.% SmZn) and the nanocomposite material of comparative example 1 (with smot SmZn). XRD test results show that the main phase of the hard magnetic phase in the nano composite permanent magnetic material of the comparative example 1 is Sm2Co17Phase (instead of SmCo)5Phase), and the main phase of the hard magnetic phase in the nanocomposite permanent magnetic material of example 1 and example 3 is SmCo5The test results were in agreement with those in test example 2.

Claims (8)

1. High-coercivity SmCo5the/FeCo nano composite permanent magnetic material is characterized by comprising SmCo5alpha-Fe and SmCo5Mixing hard magnetic phase stabilizing components, compacting, and thermally deforming to obtain SmCo5The hard magnetic phase stabilizing component is SmNi alloy and/or SmZn alloy; the mass of the alpha-Fe is SmCo5And 20-50% of the total mass of alpha-Fe; the SmNi alloy or the SmZn alloy is an alloy rapid-hardening thin strip; the SmCo5The hard magnetic phase stabilizing component has a mass of SmCo5、α-Fe and SmCo5The hard magnetic phase stabilizing component accounts for 2.5-10% of the total mass, the mass percentage content of Sm in the SmNi and SmZn alloy is 50-90%, and the balance is Ni or Zn.
2. A high coercive force SmCo as claimed in claim 15The preparation method of the/FeCo nano composite permanent magnetic material is characterized by comprising the following steps of: SmCo is mixed5alpha-Fe and SmCo5Uniformly mixing the hard magnetic phase stabilizing components to obtain a mixture; and (3) pressing and forming the mixture, and then carrying out thermal deformation treatment.
3. High coercivity SmCo according to claim 25The preparation method of the/FeCo nano composite permanent magnetic material is characterized in that the temperature during thermal deformation treatment is 600-900 ℃, the deformation amount is 30-90%, and the deformation rate is 5%/min-100%/min.
4. High coercivity SmCo according to claim 25The preparation method of the/FeCo nano composite permanent magnetic material is characterized in that the SmCo nano composite permanent magnetic material is prepared by the method5The hard magnetic phase stabilizing component is an alloy rapid-hardening thin strip, and the thickness of the alloy rapid-hardening thin strip is 10-200 mu m.
5. High coercivity SmCo according to any one of claims 2 to 45The preparation method of the/FeCo nano composite permanent magnetic material is characterized in that the SmCo nano composite permanent magnetic material is prepared by the method5The alpha-Fe and the powder have the particle size of less than 180 mu m.
6. High coercivity SmCo according to any one of claims 2 to 45The preparation method of the/FeCo nano composite permanent magnetic material is characterized in that the mixing is ball milling mixing, the ball milling time is 4-24 hours, and the rotating speed is 300-700 r/min.
7. High coercivity SmCo according to any one of claims 2 to 45The preparation method of the/FeCo nano composite permanent magnetic material is characterized in that the pressure used in the compression molding is 0.8-1.2 GPa.
8. High coercivity SmCo according to any one of claims 2 to 45The preparation method of the/FeCo nano composite permanent magnetic material is characterized in that the mixing, the compression molding and the thermal deformation treatment are all carried out in a protective atmosphere.
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