JPH10261515A - Anisotropic nanocomposite magnet and its manufacture - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a nanocomposite magnet having high magnetic characteristics by making it anisotropic and its manufacture. SOLUTION: The composite magnet has mutually adjacent hard and soft magnetic phases. Because of the magnetic exchange reaction, the entire system is of the nature of a hard magnetic material. The manufacturing process comprises at least step 1 for preparing a magnet material, step 4 for hot working this material into an anisotropic material, and step 6 for pulverizing the hot worked material, or a step of introducing D (at least one of C, P and N) in the material. The hot working step crystallizes the hard and soft magnetic phases and converting the hard magnetic phase into an anisotropic phase.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD The present invention relates to a nanocomposite magnet having magnetic anisotropy and a method for producing the same.

[0002]

2. Description of the Related Art In a mixed phase structure of a hard magnetic phase and a soft magnetic phase, when the size of the soft magnetic phase becomes about nanometers, the soft magnetic phase becomes soft magnetic by the magnetic exchange coupling between the hard magnetic phase and the soft magnetic phase. It is known that the rotation of the magnetization of a phase is suppressed, and the influence of the magnetic phase on the coercive force of the entire system is sufficiently reduced.

[0003] In such a magnet, the magnetization of the soft magnetic phase easily changes its direction by the action of the external magnetic field Ha. Therefore, when it is mixed with the hard magnetic phase, the magnetization curve of the entire system has a step in the second quadrant. Snake-shaped curve ". Further, if strong exchange coupling acts between the two, the magnetization reversal started in the soft magnetic phase easily propagates to the hard magnetic phase, so that the coercive force of the entire system is significantly reduced.

[0004] Such a permanent magnet material comprising a mixed layer of a hard magnetic phase and a soft magnetic phase is called a nanocomposite magnet material, and (1) reversibly springs back the magnetization, and (2) a relatively low magnetic field. It can be magnetized, (3) there is little change in magnetic properties with time, and (4) the magnetic properties do not deteriorate even if it is pulverized.

Another reason to pay attention to nanocomposite magnets is that a magnet ribbon having a high remanent magnetization of 0.8 T to 1.3 T isotropically has a very low rare earth content of about 5 at%. Thus, practical use of an isotropic bonded magnet that is easy to use at low cost is technically possible.

However, such conventional nanocomposite magnets are magnetically isotropic and do not have high magnetic properties, and therefore have a problem that their applications are limited. It has not been converted.

[0007]

SUMMARY OF THE INVENTION An object of the present invention is to provide a nanocomposite magnet having high magnetic properties by making it anisotropic, and a method for producing the same.

[0008]

This and other objects are attained by the present invention which is defined below as (1) to (21).

(1) In a nanocomposite magnet in which a hard magnetic phase and a soft magnetic phase are adjacent to each other and have the property of a hard magnetic material as a whole system due to magnetic exchange interaction, the magnetic anisotropy of the whole system becomes large. A nanocomposite magnet characterized by:

(2) The anisotropic nanocomposite magnet according to the above (1), which has a composition represented by the following formula (I).

Rx TM100-xy By (I) (where R is at least one of rare earth elements including Y, TM is a transition element, and x and y are each 3 at%.)
≦ x ≦ 8 at%, 12 at% ≦ y ≦ 25 at%. (3) The anisotropic nanocomposite magnet according to the above (1), which has a composition represented by the following formula (II).

Rx TM100-xy By (II) (where R is at least one of the rare earth elements including Y, TM is a transition element, and x and y are each 3 at%.)
≦ x ≦ 12 at%, 3 at% ≦ y ≦ 10 at%. (4) The anisotropic nanocomposite magnet according to any one of the above (1) to (3), wherein the hard magnetic phase is an R2 TM14B system and the soft magnetic phase is TM or a compound of TM and B. .

(5) The anisotropic nanocomposite magnet according to the above (1), comprising an element represented by the following formula (III):

R1xR2yFe100-xyz Coz Dw (III) (where R1 is at least one of rare earth elements including Y, R2 is at least one of Zr, Hf, Sc, and D is N, C, P At least one of
x, y, z and w are respectively 2 at% ≦ x ≦ 20 at%,
0.1at% ≦ y ≦ 20at%, 4at% ≦ x + y ≦ 20at
%, 0 at% ≦ z ≦ 40 at%, 0.1 at% ≦ w ≦ 30 at%
To be satisfied. (6) The hard magnetic phase is (Sm.Zr) 1 Fe7 N
q system, wherein the soft magnetic phase is Fe or Fe and D
(1) or (5), wherein q is 0.1 at% ≦ q ≦
Satisfies 10 at%. ).

(7) The anisotropic nanocomposite magnet according to (1), comprising an element represented by the following formula (IV).

Rx TM100-xy Dy (IV) (where R is at least one of rare earth elements including Y, TM is a transition element, D is at least one of N, C and P, and x , Y are respectively 3 at% ≦ x ≦ 11 at
%, 12 at% ≦ y ≦ 18 at%. (8) the hard magnetic phase is an R2 TM17D3 type,
(1) or (7) above, wherein the soft magnetic phase is TM.
The anisotropic nanocomposite magnet according to 1.

(9) The anisotropic nanocomposite magnet according to any one of (1) to (8), wherein the hard magnetic phase is made anisotropic by hot working.

(10) The anisotropic nanocomposite magnet according to any one of (1) to (9), wherein the degree of orientation of the easy axis of the hard magnetic phase is 70% or more.

(11) The anisotropic nanocomposite magnet according to any one of (1) to (10), wherein the magnetic energy product (BH) max is 13 MGOe or more.

(12) The anisotropic nanocomposite magnet according to any one of (1) to (11), wherein the magnet powder is a bonded magnet formed by bonding a magnet powder with a bonding resin.

(13) The hard magnetic phase and the soft magnetic phase are adjacent to each other, and when the anisotropic nanocomposite magnet having properties as a hard magnetic material as a whole system is produced by magnetic exchange interaction, the hard magnetic phase A method of making anisotropic nanocomposite magnets by hot working.

(14) When the hard magnetic phase and the soft magnetic phase are adjacent to each other and the anisotropic nanocomposite magnet having properties as a hard magnetic material as a whole system is produced by magnetic exchange interaction, the hot working is performed. A step of crystallizing the hard magnetic phase and the soft magnetic phase according to the method, and a step of making the hard magnetic phase anisotropic.

(15) A method for producing an anisotropic nanocomposite magnet according to any one of the above (2) to (4), wherein a step of preparing a magnet material and a step of hot working the magnet material are performed. And an anisotropic nanocomposite magnet, comprising the steps of: applying and anisotropizing; and pulverizing the hot-worked magnet.

(16) The method for producing an anisotropic nanocomposite magnet according to any one of the above (5) to (8), wherein a step of preparing a magnet raw material and a step of hot working the magnet raw material Performing the anisotropic process, pulverizing the hot-worked magnet, and adding D to the magnet material.
And a method of producing an anisotropic nanocomposite magnet.

(17) The method for producing an anisotropic nanocomposite magnet according to (16) above, wherein the step of introducing D is performed on magnet powder pulverized after hot working.

(18) The method for producing an anisotropic nanocomposite magnet according to (17), wherein the step of introducing D is performed by heat-treating the magnet powder in a gas containing D.

(19) The method for producing an anisotropic nanocomposite magnet according to any one of the above (13) to (18), wherein the hot working is performed in a state where the work is encapsulated in a capsule for preventing oxidation. .

(20) The hot working is performed at a working temperature of 300
The method for producing an anisotropic nanocomposite magnet according to any one of the above (13) to (19), which is carried out at a temperature of from to 1000 ° C.

(21) The hot working is performed at a working degree of 50 to 8
The method for producing an anisotropic nanocomposite magnet according to any one of the above (13) to (20), wherein the method is performed at 0%.

[0030]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, an anisotropic nanocomposite magnet according to the present invention and a method for producing the same will be described.

1. Nanocomposite magnet First, the nanocomposite magnet will be described.

In the nanocomposite magnet of the present invention, the soft magnetic phase 10 and the hard magnetic phase 11 are formed, for example, as shown in FIGS.
Alternatively, they exist in a pattern (model) as shown in FIG. 3, and the thickness and particle size of each phase exist at the nanometer level (for example, 1 to 100 nm). Then, the soft magnetic phase 10 and the hard magnetic phase 11 are adjacent to each other, and a magnetic exchange interaction occurs.

Since the magnetization of the soft magnetic phase changes its direction easily by the action of an external magnetic field, if it is mixed with the hard magnetic phase, the magnetization curve of the entire system becomes a "snaked curve" with a step in the second quadrant. . When the size of the soft magnetic phase is sufficiently smaller than the domain wall width, the magnetization of the soft magnetic material is sufficiently strongly constrained by the coupling with the magnetization of the surrounding hard magnetic material so that the entire system behaves as a hard magnetic material. Become.

Such a nanocomposite magnet has mainly the following features 1) to 5).

1) In the second quadrant of the magnetization curve, the magnetization reversibly springs back (also referred to as a "spring magnet" in this sense).

2) Magnetization can be performed with a relatively low magnetic field.

3) The temperature dependence of the magnetic properties is smaller than in the case of using only the hard magnetic phase.

4) Changes in magnetic properties with time are small.

5) Even if finely pulverized, the magnetic properties do not deteriorate.

2. Composition of anisotropic nanocomposite magnet The anisotropic nanocomposite magnet of the present invention preferably has any one of the following compositions. Less than,
Description will be given for each composition.

[Composition] Rx TM100-xy By (where R is at least one of rare earth elements including Y, TM is a transition element, and x and y are each 3 at%.)
≦ x ≦ 8 at%, 12 at% ≦ y ≦ 25 at%. R is a rare earth element, for example, Y, La, C
e, Pr, Nd, Pm, Sm, Eu, Gd, Tb, D
Examples thereof include y, Ho, Er, Tm, Yb, Lu, and misch metal, and one or more of these can be included.

The content of such a rare earth element is 3 to 8
at% is preferable, and 3 to 6 at% is more preferable. When the content of the rare earth element is in this range, higher magnetic properties can be obtained without increasing the cost.

Examples of the TM, ie, the transition metal, include Fe, Co, Ni, and the like.
Species or two or more species may be included. Among them, those containing Fe are more preferable.

The content of B is preferably from 12 to 25 at% because of its high ability to form an amorphous phase, particularly preferably from 15 to 20 at%.
Is preferred. When the content of B is less than 12 at%, the ability to form an amorphous phase is low.
2 A TM14B-based hard magnetic layer is not generated, and a cubic metastable layer having low magnetic anisotropy and Curie temperature is generated, and desired magnetic properties cannot be obtained.

TM occupies the balance of the above elements (R and B).

[Composition] Rx TM100-xy By (where R is at least one of rare earth elements including Y, TM is a transition element, and x and y are each 3 at%.)
≦ x ≦ 12 at%, 3 at% ≦ y ≦ 10 at%. R is a rare earth element, for example, Y, La, C
e, Pr, Nd, Pm, Sm, Eu, Gd, Tb, D
Examples thereof include y, Ho, Er, Tm, Yb, Lu, and misch metal, and one or more of these can be included.

The content of such a rare earth element is 3 to 1
2 at% is preferable, and 5 to 11 at% is more preferable. When the content of the rare earth element is in this range, higher magnetic properties can be obtained without increasing the cost.

The TM, that is, the transition metal includes, for example, Fe, Co, Ni and the like.
Species or two or more species may be included. Among them, those containing Fe are more preferable.

The content of B is preferably 3 to 10 at%,
Particularly, 4 to 7 at% is preferable. If the content of B is less than 3 at%, a high coercive force cannot be obtained due to the rhombohedral R-Fe system, and if it exceeds 10 at%, the nonmagnetic phase increases and the residual magnetic flux density decreases.

TM occupies the balance of the above elements (R and B).

[Composition] R1xR2yFe100-xyz Coz Dw (where R1 is at least one of rare earth elements including Y, R2 is at least one of Zr, Hf and Sc, and D is one of N, C and P) At least one,
x, y, z and w are respectively 2 at% ≦ x ≦ 20 at%,
0.1at% ≦ y ≦ 20at%, 4at% ≦ x + y ≦ 20at
%, 0 at% ≦ z ≦ 40 at%, 0.1 at% ≦ w ≦ 30 at%
To be satisfied. R1 is a rare earth element, for example, Y, La,
Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, D
Examples thereof include y, Ho, Er, Tm, Yb, Lu, and misch metal, and one or more of these can be included.

The content of R1 is 2 to 20 at%.
Is preferable, and 5 to 10 at% is more preferable. When the content of R1 is in this range, higher magnetic properties can be obtained without increasing the cost.

R2 is at least one of Zr, Hf and Sc. Such R2 element has the effect of replacing the rare earth element in the crystal with iron in the TbCu7 structure crystal composed of these alloy elements.
It has the effect that the axis contracts, the c-axis expands, and c / a increases. Therefore, the saturation magnetization and the residual magnetization are improved.

The content of R2 is 0.1 to 20.
at% is preferable, and 1 to 5 at% is more preferable. By setting the content in such a range, the above-described functions and effects are sufficiently exhibited.

Further, the content of Co is preferably 40 at% or less, more preferably 10 to 30 at%. When Co replaces a part of Fe, the Curie temperature is increased, the temperature characteristics are improved, and the coercive force is improved. However, the content of Co is 40 at%.
When the value exceeds, the coercive force starts to decrease.

Examples of D include N, C, P and the like, and one or more of these can be included. Among these, those containing N are more preferable. These elements mainly exist at interstitial positions of the hard magnetic phase, and have an effect of improving the Curie temperature, magnetization, and magnetic anisotropy of the magnet.

The content of D is preferably 0.1 to 30 at%, more preferably 5 to 20 at%. D content is 0.1
If it is less than at%, the effect of adding D as described above cannot be sufficiently obtained, and if it exceeds 22 at%, the magnetic properties deteriorate.

Fe occupies the balance of each of the above elements.

[Composition] Rx TM100-xy Dy (where R is at least one of rare earth elements including Y, TM is a transition element, D is at least one of N, C and P, and x and y are 3at% ≦ x ≦ 11at
%, 12 at% ≦ y ≦ 18 at%. R is a rare earth element, for example, Y, La, C
e, Pr, Nd, Pm, Sm, Eu, Gd, Tb, D
Examples thereof include y, Ho, Er, Tm, Yb, Lu, and misch metal, and one or more of these can be included.

The content of such a rare earth element is 3 to 1
1 at% is preferable, and 5 to 9 at% is more preferable. When the content of the rare earth element is in this range, higher magnetic properties can be obtained without increasing the cost.

The TM, ie, the transition metal includes, for example, Fe, Co, Ni and the like.
Species or two or more species may be included. Among them, those containing Fe are more preferable.

Examples of D include N, C, P and the like, and one or more of these can be included. Among these, those containing N are more preferable. These elements mainly exist at interstitial positions of the hard magnetic phase, and have an effect of improving the Curie temperature, magnetization, and magnetic anisotropy of the magnet.

The content of D is preferably 12 to 18 at%, more preferably 13 to 16 at%. D content is 12
If it is less than at%, the effect of adding D as described above cannot be sufficiently obtained, and if it exceeds 18 at%, the magnetic properties deteriorate.

TM accounts for the balance of the above elements (R and D).

In the above, the composition of the entire magnet has been described. Next, preferred examples of the respective compositions of the hard magnetic phase and the soft magnetic phase will be described.

In the case of the above composition Hard magnetic phase: R2 TM14B system Soft magnetic phase: TM or a compound of TM and B, especially TM3 B system In the above composition Hard magnetic phase: R2 TM14B system Soft magnetic phase: TM, especially α -Fe In the case of the above composition Hard magnetic phase: (Sm.Zr) 1 Fe7 Dq system (however,
q satisfies 0.1 at% ≦ q ≦ 10 at%. ) Soft magnetic phase: Fe, Fe and Co or Fe and D
(At least one of N, C and P, particularly preferably N) is used as the compound. Here, the content of D is preferably 1 to 30 at%, and
0 at% is more preferred. When the content of D is within the above range, the effect of stabilizing the TbCu7 structural crystal can be obtained.

In the case of the above composition Hard magnetic phase: R2 TM17D3 system Soft magnetic phase: TM, especially α-Fe Regarding Magnetic Anisotropy The anisotropic nanocomposite magnet of the present invention exhibits magnetic anisotropy as a whole system. The degree of the magnetic anisotropy is such that the degree of orientation of the easy axis (c axis) (reference numeral 12 in FIGS. 1 to 3) is 70%.
It is preferably at least 75%, more preferably at least 75%.

The degree of orientation of the easy axis (MA)
Is defined by the following equation:

M · A = Bx / √ (Bx2 + By2 + Bz
2) × 100 (%) (where Bx, By and Bz are x,
Indicates the residual magnetic flux density in the y and z directions. ) 4. Regarding magnetic properties Such anisotropic nanocomposite magnet of the present invention has extremely high magnetic properties.

That is, the magnetic energy product (BH) max
However, preferably 13 MGOe or more, more preferably 17 MGOe
That is all.

The coercive force iHc is preferably 4 kOe
More preferably, it is 7 kOe or more.

5. Shape of Magnet The anisotropic nanocomposite magnet of the present invention includes powdery (magnetic powder), ribbon-like, scale-like, and bonded magnets, sintered magnets, and cast ingots produced therefrom. Any form of magnet, such as a cast magnet obtained by processing the same, may be used.

6. Next, a method for producing an anisotropic nanocomposite magnet of the present invention will be described with reference to the drawings.

FIG. 4 is a schematic process diagram of a method for producing the composition and the anisotropic nanocomposite magnet having the composition according to the present invention. FIG. It is a schematic process drawing of a manufacturing method.

Hereinafter, the steps of each of these manufacturing methods will be sequentially described.

[Composition] Preparation of Magnet Raw Material Powder (Step 1) First, a predetermined amount of raw materials for each of the R, TM, and B elements is prepared. Each of these magnet raw materials preferably has a purity of 99.5% or more.

Next, the above-mentioned raw materials are directly melted in a crucible for ultra-quenching, for example, by high-frequency induction heating and melting. Alternatively, in order to eliminate non-uniform composition, it is preferable to melt the master alloy in an arc melting furnace or a high-frequency induction melting furnace as primary melting. In order to prevent the metal material from being oxidized at a high temperature, the dissolution must be performed in an inert gas atmosphere or in a vacuum (about 1 × 10 -1 to 1 × 10 -5 torr).

An amorphous structure is obtained from the molten metal by, for example, a rapid quenching method, or a structure in which a fine crystal phase is contained in the amorphous structure (hereinafter, these are collectively referred to as “amorphous structure” or “amorphous state”). Obtain a super-quenched ribbon.

Here, as the ultra-quenching method, a single-roll method or a twin-roll method in which a molten metal is sprayed onto a single-roll or twin-roll rotating at high speed is generally used. In addition, an atomizing method such as gas atomization is used. , Rotating disk method,
Any method such as a mechanical alloying (MA) method may be used. Among them, the super-quenching method is effective in improving the magnetic properties of the permanent magnet, particularly, the coercive force and the like, because the metal structure is refined.

The cooling rate may be any rate as long as the above structure can be obtained. However, if the cooling rate is too high,
It is not preferable because the quenched ribbon scatters and lowers the production efficiency. For example, when a Cu roll is used as the rapid quenching method, the roll surface peripheral speed that satisfies this condition is approximately 20 to
70 m / sec is preferred.

In addition, these ultra-quenching methods employ Ar and He in order to prevent deterioration of magnetic properties due to oxidation of raw materials.
It is preferably performed in an inert gas atmosphere such as

2. Pulverization (Step 2) The quenched ribbon having a width of about 0.1 to 10 mm and a thickness of about 10 to 500 μm obtained by the above method is roughly pulverized. At the time of pulverization, Ar, H
It is preferable to carry out in an atmosphere of an inert gas such as e, N2 or the like or in a vacuum, but in order to simplify the manufacturing process, the above-mentioned method of pulverizing while blowing the inert gas may be used.

The particle size of the pulverized magnet powder is not particularly limited, but a preferable range is, for example, about 1 to 5 μm, particularly about 50 to 500 μm. When the particle size is in this range, it is easier to fill the capsule in the next step.

3. Encapsulation (Step 3) Prevention of oxidation and temperature reduction during hot working of magnet raw material powder,
The magnet powder is encapsulated in a capsule for uniform processing. The capsule is composed of a metal container and a metal lid closing the inside thereof. After filling the metal container with the magnetic powder, the capsule is closed with the lid.

Here, the material of the metal container constituting the capsule is not particularly limited, but for example, general-purpose steel such as mild steel or stainless steel is preferable. By using such a material, hot workability and weldability at the time of attaching the lid can be improved. It is also preferable in that the manufacturing cost of a metal container or the like can be kept low.

The thickness of the metal container and the lid is such that the strength capable of withstanding the stress during hot working can be secured.

The filling of the metal raw material powder into the metal container is preferably performed, for example, while slightly applying vibration to the container.
Thereby, the magnet raw material powder can be filled at a higher density.

After the filling of the magnet raw material powder, the metal container and the lid are hermetically joined, for example, by welding to form a capsule. In order to prevent the magnet raw material powder from being oxidized by oxygen in the air due to heat at the time of welding, it is preferable to perform, for example, argon welding.

Next, the capsule is baked (heated) in a predetermined temperature range, for example, and vacuum-sucked through a vacuum suction opening formed in the container or the lid, and then the opening is sealed. The baking is performed by, for example, supplying heat from outside the capsule by a heating wire or the like. By this baking, moisture, gas and the like adsorbed on the surface of the magnet raw material powder in the capsule are removed.

The baking is preferably started after the degree of vacuum in the capsule becomes 10 -1 torr or less in order to minimize the oxidation of the magnet. The baking temperature is preferably in the range of 30 ° C., which is equal to or higher than room temperature, to 300 ° C., at which oxidation of the magnet alloy powder in a low vacuum cannot be ignored, but in consideration of handling after the baking step, the capsule temperature is excessively high. 80
It is preferably carried out at a temperature of from 200 to 200C, more preferably at a temperature of from 100 to 150C.

4. Hot working (Step 4) The capsule, the inside of which is maintained in a vacuum state as described above, is further heated to perform hot working.

By this hot working, the hard magnetic phase and the soft magnetic phase are crystallized and the hard magnetic phase is made anisotropic. That is, the hard magnetic phase and the soft magnetic phase are crystallized by the heat of hot working to form a mixed phase structure thereof, and the crystal grains of both phases are controlled to an optimal size, and priority is given to the two phases. By causing crystal grain growth, an anisotropic nanocomposite magnet is obtained.

Examples of the heating method include general heating methods such as radiation heating and high frequency heating. The working temperature in the hot working is preferably in a temperature range of 300 to 1000 ° C.,
500-700 degreeC is more preferable. Processing temperature is 300 ℃
If it is less than 30, the deformability of the capsule itself becomes small and processing becomes difficult. At a temperature higher than 1000 ° C., the crystal grain size of the magnet powder tends to increase during processing.

The working method may be any working method such as pressing, rolling, extrusion, drawing, etc., but rolling is particularly preferred in terms of excellent mass productivity.

The strain rate in hot working is 10 sec -1.
The lower limit is preferably about 0.1 to 5 sec-1. This prevents a decrease in magnetic performance due to coarsening of crystal grains during hot working, and also improves productivity.

In the hot rolling, it is preferable to return to the furnace during the working so as to prevent the temperature from dropping during the working and to make the working temperature uniform.

The degree of processing (total degree of processing) is not particularly limited. However, the degree of processing of the capsule height is preferably from 50 to 80%, and more preferably from 60 to 75% since the degree of orientation is highest. When the working degree exceeds 80%, the orientation of the preferentially grown crystal grains is likely to be disturbed by shear strain, and when it is less than 50%, the degree of orientation cannot be sufficiently improved.

In the present invention, heat treatment can be performed before or after the hot working as required. Thereby, the coercive force can be increased. The temperature of the heat treatment is preferably from 400 to 800C, more preferably from 500 to 700C. If this temperature is lower than 400 ° C., the effect of increasing the coercive force is poor, while if it is higher than 800 ° C., the coercive force may be lower than before the heat treatment.

In the method of manufacturing an anisotropic nanocomposite magnet according to the present invention, such a heat treatment may not be performed.

5. Removal (Step 5) After hot working, the workpiece is cooled together with the capsule. For example, when cooled to 100 ° C. or less, the capsule material is peeled off from the massed magnet, and a desired anisotropic nanocomposite magnet is removed from the capsule.

6. Pulverization (Step 6) The anisotropic nanocomposite magnet (mass) removed from the capsule is pulverized. The pulverization method is not particularly limited, and the pulverization is performed by, for example, a ball mill, a brown mill, a stamp mill, or the like.

In the pulverizing step, A is used to suppress oxidation of the powder.
It is preferably performed in an atmosphere of an inert gas such as r, He, N2 or the like or in a vacuum, but in order to simplify the manufacturing process,
The method of pulverizing while blowing the above-mentioned inert gas may be used. The average particle size after grinding is, for example, about 1 to 400 μm,
In particular, the thickness is preferably 10 to 200 μm.

The particle size distribution after pulverization may be uniform or may be dispersed to some extent. However, in the case of a bonded magnet described later, good moldability during magnet molding can be obtained with a small amount of binder resin. For this reason, it is preferable that the particle size of the powder is dispersed to some extent (varied). This makes it possible to further reduce the porosity after molding.

7. Molding of Magnet (Step 8) A resin made of a thermoplastic resin (for example, polyamide, PPS) or a thermosetting resin (for example, epoxy resin) is added to the magnet powder obtained through the above-mentioned Step 6, for example, from 1 to 10
After adding wt% and kneading, molding is performed in a magnetic field (or in a non-magnetic field). In the case of molding in a magnetic field, the applied magnetic field is, for example, 5-1.
5 kOe. The molding method is compression molding (press molding),
Either extrusion molding or injection molding may be used. For example, in the case of compression molding, the molding pressure is preferably from 5 to 10 t / cm2 from the viewpoint of improving mass productivity, and more preferably from 7 to 8 t / cm2 from the viewpoint of obtaining mold durability.

When the binder resin is a thermosetting resin, the molded body is subjected to heat treatment, preferably heat treatment in a nitrogen gas to cure the resin to obtain a bonded magnet.

The shape of the magnet is not particularly limited, and may be any shape such as a cylinder, a column, a flat plate, a curved plate, and a bar. For example, in the case of a cylindrical magnet, the anisotropic direction may be any of a horizontal direction, a vertical direction, and a radial direction.

[Composition] Preparation of Magnet Raw Material Powder (Step 1) Same as in the case of the above composition.

2. Pulverization (Step 2) Same as in the case of the above composition.

3. Encapsulation (Step 3) Same as in the above composition.

4. Hot working (Step 4) Same as in the case of the above composition.

5. Removal (Step 5) Same as in the case of the composition.

6. Grinding (Step 6) Same as in the case of the above composition.

7. Introduction of D (nitriding treatment) (Step 7) As a raw material composition, D is introduced into the powder after the above-mentioned pulverization step. For example, in the case of introducing nitrogen (N), for example,
The heat treatment is performed at a temperature of 200 to 720 ° C. for 1 to 100 hours in a nitrogen (N 2) gas atmosphere at a pressure of 0.1 kPa to 10 MPa. As a result, the raw material powder is nitrided.

[0114] As the atmosphere during the nitriding treatment, a nitrogen compound gas (a gas containing N) such as an ammonia gas or a laughing gas may be used instead of the nitrogen gas.

As a pre-process, 0.1 kPa to 10 kPa
High-efficiency nitridation can be performed by performing a heat treatment in a hydrogen gas atmosphere of MPa at a temperature of 100 to 700 ° K. or by using a gas in which hydrogen is mixed with nitrogen gas.

When D is C, the introduction is preferably carried out by carbonization using a gas containing C such as methane gas, similarly to the nitriding treatment. For example, the powder obtained in the step 6 is heat-treated in the gas containing C.

When D is P, the introduction is preferably carried out by introducing P as a raw material element during the alloy melting step (the first half of the step 1). For example, it is carried out by adding P or a compound of P.

By introducing D as described above, a magnet having desired characteristics can be manufactured.

8. Molding of magnet (Step 8) Same as in the case of the composition.

Although the method for producing the anisotropic nanocomposite magnet of the present invention has been described with reference to the drawings, the present invention is not limited to these.
At least one of 7, 8 may be omitted. Alternatively, an arbitrary step (for example, a heat treatment step) may be added before or after each of the steps 1 to 8.

Further, for example, the crystallization of the hard magnetic phase and the soft magnetic phase may be performed by performing a heat treatment step separately before the step 5 without performing the hot working.

The hot working may be performed continuously or intermittently a plurality of times. In this case, it is preferable that heat treatment be performed between hot working.

[0123]

Next, specific examples of the present invention will be described.

(Examples 1 to 5) [Composition] Purity of 99.
5% or more of Fe, Co, Nd, Pr, and B were weighed so that the total amount was 100 g. Place φ0.
It was placed in a transparent quartz tube provided with a 6 mm orifice and melted by high-frequency heating in an Ar gas atmosphere.
° C.

Thereafter, the molten metal was sprayed onto the Cu roll from the position where the gap between the bottom of the quartz tube and the Cu roll rotating at a peripheral speed of 40 m / sec was 0.5 mm, and the thickness was 30 to 30 mm.
A quenched ribbon 50 μm wide and 2-3 mm wide was obtained.

In order to confirm the microstructure of the obtained quenched ribbon, X-ray diffraction was performed using Cu-Kα at a diffraction angle of 20 ° to 60 °, and it was confirmed that the ribbon was in an amorphous state.

The quenched ribbon was coarsely pulverized by a raikai pulverizer so that the average particle diameter of the powder was about 200 μm, to obtain an alloy powder.

This alloy powder is filled in a metal container made of SS41 (JIS standard), which is a general-purpose steel that can be obtained at low cost, while applying light vibrations, and is made of the same material (SS41) as a container having an opening for vacuum suction. Manufactured by Capsule Co., Ltd.) and welded by argon welding to form a capsule.

Next, the capsule was placed in an electron beam welding chamber, and the inside of the capsule was evacuated from the opening. Vacuum suction was started when the degree of vacuum in the chamber became lower than 10 -1 torr, and the capsules were baked so that the maximum temperature was 150 ° C.
The opening was sealed by electron beam welding while maintaining the degree of vacuum in the chamber at 10 -4 torr.

This capsule was heated to 600 ° C. in the air, and hot-rolled at a total workability of 70% and a strain rate of 1 sec −1.

After the hot rolling, the temperature of the capsule was 100
After the temperature became lower than or equal to ° C., the capsule was removed from the workpiece, and the hot-processed magnet inside was taken out.

To confirm the phase constitution and anisotropy of the magnet, X-ray diffraction was performed at a diffraction angle of 20 ° to 60 ° using Cu-Kα. From the diffraction pattern, diffraction peaks of the (Nd.Pr) 2 (Fe.Co) 14B1 phase, which is a hard magnetic phase, and the Fe3B, .alpha.-Fe phases, which are soft magnetic phases, were confirmed.

In the diffraction peaks, the (006) diffraction peak in the c-axis direction of the (Nd.Pr) 2 (Fe.Co) 14B1 phase, which is a hard magnetic phase, is particularly strongly observed. It was confirmed that the anisotropy was imparted.

The anisotropic magnet was further pulverized by a raikai machine so that the maximum powder particle diameter ≦ 200 μm and the average powder particle diameter became 100 μm, and then the anisotropic magnet powder was formed into a bonded magnet by a compression molding method. At that time, 1.6 wt% of an epoxy resin was added as a binding resin. The molding was performed at a molding pressure of 7 t / cm2 in a magnetic field of 15 kOe applied during molding.

The obtained molded body was heated in a nitrogen gas atmosphere for one hour to cure the binding resin, thereby producing an anisotropic bonded magnet (cube: 10 mm × 10 mm × 10 mm).

The magnetic properties of the anisotropic bonded magnet were measured. The measurement was performed with a maximum magnetic field of 25 kOe using a direct current magnetic flux meter. The measurement results are shown in Table 1 together with the degree of orientation. As shown in the table, all of the magnets of Examples 1 to 5 have high magnetic properties, and particularly have sufficient anisotropy (high orientation degree).
As a result, a high (BH) max is obtained.

(Comparative Example 1) A quenched ribbon was produced under the same composition and production conditions as in Example 1, and then pulverized, encapsulated, and vacuum-sealed. Only partial heat treatment was performed. 100 capsules after processing
The capsule was removed when the temperature became lower than or equal to ° C., and the magnet inside was taken out.

In order to confirm the phase structure and anisotropy of the magnet, X-ray diffraction was performed at a diffraction angle of 20 ° to 60 ° using Cu-Kα. As a diffraction pattern, a hard magnetic phase of Nd2 Fe14B1 phase and a soft magnetic phase of Fe3 B, α
A diffraction peak of the -Fe phase was confirmed. However, in the magnet of Comparative Example 1, only the diffraction peak in the c-axis direction (006) was not particularly strongly observed, and it was confirmed that the crystal orientation of the hard magnetic phase was isotropically distributed. .

This magnet powder was pulverized in the same manner as in Example 1 and then converted into a bond magnet to obtain a bond magnet having the same shape and size.

The magnetic properties of the bonded magnet were measured with a direct current recording magnetometer at a maximum applied magnetic field of 25 kOe. The measurement results are shown in Table 1 as Comparative Example 1. As shown in the table, this magnet was not subjected to hot working and was not anisotropic, and thus had lower magnetic properties than Examples 1 to 5.

[0141]

[Table 1]

(Examples 6 to 10) [Composition] Purity was set to 99.
5% or more of Fe, Co, Nd, Pr, and B were weighed so that the total amount was 100 g. Place φ0.
It was placed in a transparent quartz tube provided with a 6 mm orifice and melted by high-frequency heating in an Ar gas atmosphere.
° C.

Thereafter, the molten metal was sprayed onto the Cu roll from the position where the gap between the bottom of the quartz tube and the Cu roll rotating at a peripheral speed of 40 m / sec was 0.5 mm, and the thickness was 30 to 30 mm.
A quenched ribbon 50 μm wide and 2-3 mm wide was obtained.

In order to confirm the structure of the obtained quenched ribbon, X-ray diffraction was performed at a diffraction angle of 20 ° to 60 ° using Cu-Kα, and it was confirmed that the ribbon was in an amorphous state.

The quenched ribbon was roughly pulverized by a raikai pulverizer so that the average particle diameter of the powder was about 280 μm, to obtain an alloy powder.

This alloy powder is filled in a metal container made of general-purpose steel and made of inexpensive material SS41 (according to JIS) while applying light vibration, and is made of the same material (SS41) as a container having a vacuum suction opening. Manufactured by Capsule Co., Ltd.) and welded by argon welding to form a capsule.

Next, the capsule was placed in an electron beam welding chamber, and the inside of the capsule was evacuated through the opening. Vacuum suction was started when the degree of vacuum in the chamber became lower than 10 -1 torr, and the capsules were baked so that the maximum temperature was 150 ° C.
The opening was sealed by electron beam welding while maintaining the degree of vacuum in the chamber at 10 -4 torr.

This capsule was heated to 600 ° C. in the air, and hot-rolled at a total workability of 65% and a strain rate of 2 sec −1.

After the hot rolling, the capsule temperature was 100
After the temperature became lower than or equal to ° C., the capsule was removed from the workpiece, and the hot-processed magnet inside was taken out.

In order to confirm the phase constitution and anisotropy of the magnet, X-ray diffraction was performed at a diffraction angle of 20 ° to 60 ° using Cu-Kα. From the diffraction pattern, diffraction peaks of the (Nd.Pr) 2 (Fe.Co) 14B1 phase as the hard magnetic phase and the α-Fe phase as the soft magnetic phase were confirmed.

In these diffraction peaks, a (006) diffraction peak in the c-axis direction of the (Nd.Pr) 2 (Fe.Co) 14B1 phase, which is a hard magnetic phase, is particularly strongly observed. It was confirmed that the anisotropy was imparted.

The anisotropic magnet was further pulverized by a raikai machine so that the maximum powder particle diameter ≦ 200 μm and the average powder particle diameter became 100 μm, and then the anisotropic magnet powder was formed into a bonded magnet by a compression molding method. At that time, 1.6 wt% of an epoxy resin was added as a binding resin. The molding was performed at a molding pressure of 7 t / cm2 in a magnetic field of 15 kOe applied during molding.

The obtained molded body was heated in a nitrogen gas atmosphere for one hour to cure the binding resin, thereby producing an anisotropic bonded magnet (cube: 10 mm × 10 mm × 10 mm).

The magnetic properties of the anisotropic bonded magnet were measured. The measurement was performed with a maximum magnetic field of 25 kOe using a direct current magnetic flux meter. The measurement results are shown in Table 1 together with the degree of orientation. As shown in the table, all of the magnets of Examples 1 to 5 have high magnetic properties, and particularly have sufficient anisotropy (high orientation degree).
As a result, a high (BH) max is obtained.

(Comparative Example 2) A quenched ribbon was produced under the same composition and production conditions as in Example 2, followed by pulverization, encapsulation, and vacuum sealing. Only partial heat treatment was performed. 100 capsules after processing
The capsule was removed when the temperature became lower than or equal to ° C., and the magnet inside was taken out.

In order to confirm the phase constitution and anisotropy of the magnet, X-ray diffraction was performed at a diffraction angle of 20 ° to 60 ° using Cu-Kα. As the diffraction patterns, diffraction peaks of the Nd2 Fe14B1 phase as the hard magnetic phase and the α-Fe phase as the soft magnetic phase were confirmed. However, in the magnet of Comparative Example 2, only the diffraction peak in the c-axis direction (006) was not particularly strongly observed, and it was confirmed that the crystal orientation of the hard magnetic phase was isotropically distributed. .

This magnet powder was pulverized in the same manner as in Example 2 and then converted into a bond magnet to obtain a bond magnet having the same shape and size.

The magnetic properties of the bonded magnet were measured by a direct current recording magnetometer at a maximum applied magnetic field of 25 kOe. The measurement results are shown in Table 2 as Comparative Example 2. As shown in the table, this magnet was not subjected to hot working and was not anisotropic, and thus had lower magnetic properties than Examples 6 to 10.

[0159]

[Table 2]

Examples 11 to 20 [Composition] Sm, Zr, Fe having a purity of 99.5% or more,
Co was weighed so that the total amount was 100 g using a predetermined amount of each. This was placed in a transparent quartz tube having an orifice of φ0.6 mm at the bottom, and melted by high frequency heating in an Ar gas atmosphere to set the temperature of the molten metal at 1300 ° C.

Thereafter, the molten metal was sprayed onto the Cu roll from the position where the gap between the bottom of the quartz tube and the Cu roll rotating at a peripheral speed of 40 m / sec was 0.5 mm, and the thickness was 30 to 30 mm.
A quenched ribbon 50 μm wide and 2-3 mm wide was obtained.

In order to confirm the microstructure of the obtained quenched ribbon, X-ray diffraction was performed using Cu-Kα at a diffraction angle of 20 ° to 60 °, and it was confirmed that the ribbon was in an amorphous state.

The quenched ribbon was roughly pulverized by a raikai pulverizer so that the average particle diameter of the powder was about 200 μm, to obtain an alloy powder.

This alloy powder is filled in a metal container made of material SS41 (according to JIS standard) while applying light vibration, covered with a cover made of material SS41 having a vacuum suction opening, and welded by argon welding. Into a capsule.

Next, the capsule was placed in an electron beam welding chamber, and the inside of the capsule was evacuated through the opening. From the time when the degree of vacuum in the chamber becomes lower than 10 -1 torr, the maximum temperature is 150 at the same time as vacuum suction.
The capsule was baked at a temperature of ℃, and the opening was sealed by electron beam welding while the degree of vacuum in the chamber was maintained at 10 -4 torr.

The capsule was heated to 650 ° C. in the atmosphere, and the working temperature was 650 ° C., the total working degree was 70%, and the strain rate was 1
Hot rolling was performed at sec-1.

After the hot rolling, the capsules were cooled to a temperature of 100 ° C. or less, and then the capsules were removed from the workpiece, and the hot-worked magnet inside was taken out.

The removed magnet was pulverized by a raikai machine so that the maximum powder particle size was less than 200 μm and the average powder particle size was 100 μm.

Next, as a step of introducing nitrogen (N),
The powder was subjected to a heat treatment at a temperature of 450 ° C. for 2 hours in a nitrogen gas atmosphere at a pressure of 1 MPa to perform nitriding of the powder.

The introduction of carbon (C) was carried out by a heat treatment at 450 ° C. for 2 hours in a methane gas atmosphere at a pressure of 1 MPa.

The introduction of phosphorus (P) was carried out by adding a compound of P to the molten alloy as a starting material.

After the nitriding treatment and the like, the composition of the magnet was analyzed. As a result, the compositions of Examples 11 to 20 in Table 3 were obtained.

Further, in order to confirm the phase constitution and anisotropy of the magnet, X-ray diffraction was performed at a diffraction angle of 20 ° to 60 ° using Cu-Kα. As diffraction patterns, diffraction peaks of the (Sm.R2) 1 (Fe.Co) 7 Nq phase as the hard magnetic phase and the .alpha.-Fe phase as the soft magnetic phase were confirmed.
In these diffraction peaks, a (002) diffraction peak in the c-axis direction of the (Sm.R2) 1 (Fe.Co) 7 Nq phase, which is a hard magnetic phase, is particularly strongly observed. It was confirmed that the impartation of sexual properties was performed.

This anisotropic magnet powder was formed into a cylindrical bonded magnet by a compression molding method. At that time, 1.6 wt% of an epoxy resin was added as a binding resin. The molding was performed at a molding pressure of 7 t / cm2 in an applied magnetic field of 15 kOe.

The obtained molded body was heated in a nitrogen gas atmosphere for one hour to cure the binding resin, thereby producing an anisotropic bonded magnet (cube: 10 mm × 10 mm × 10 mm).

The magnetic properties of this anisotropic bonded magnet were measured. The measurement was performed with a maximum magnetic field of 25 kOe using a direct current magnetic flux meter. The measurement results are shown in Table 3 together with the degree of orientation. As shown in the table, the magnets of Examples 11 to 20 all have high magnetic properties, and particularly, have high (BH) max due to sufficient anisotropy (high degree of orientation).

(Comparative Example 3) A quenched ribbon was produced under the same composition and production conditions as in Example 11, followed by pulverization, encapsulation, and vacuum sealing. Only partial heat treatment was performed. 100 capsules after processing
The capsule was removed when the temperature became lower than or equal to ° C., and the magnet inside was taken out.

The magnet was pulverized in the same manner as in Example 11 and subjected to a nitriding treatment.

Further, in order to confirm the phase structure and anisotropy of the magnet, X-ray diffraction was performed using Cu-Kα at a diffraction angle of 20 ° to 60 °. As the diffraction patterns, diffraction peaks of the (Sm.Zr) 1 (Fe.Co) 7 Nq phase as the hard magnetic phase and the .alpha.-Fe phase as the soft magnetic phase were confirmed.
However, in the magnet of this comparative example, only the diffraction peak in the c-axis direction (002) was not particularly strongly observed, and it was confirmed that the crystal orientation of the hard magnetic phase was isotropically distributed.

The magnet powder after nitriding was converted into a bond magnet in the same manner as in Example 11 to obtain a bond magnet having the same shape and size.

The magnetic properties of the bonded magnet were measured with a direct current recording magnetometer at a maximum applied magnetic field of 25 kOe. The measurement results are shown in Table 3 as Comparative Example 3. As shown in the table, this magnet was not subjected to hot working and was not anisotropic, and thus had lower magnetic properties than Examples 11 to 20.

[0182]

[Table 3]

(Examples 21 to 27) [Composition] Sm, Pr, Fe, with a purity of 99.5% or more
Co was weighed so that the total amount was 100 g using a predetermined amount of each. This was placed in a transparent quartz tube having an orifice of φ0.6 mm at the bottom, and melted by high frequency heating in an Ar gas atmosphere to set the temperature of the molten metal at 1300 ° C.

Thereafter, the molten metal was sprayed onto the Cu roll from the position where the gap between the bottom of the quartz tube and the Cu roll rotating at a peripheral speed of 40 m / sec was 0.5 mm, and the thickness was 30 to 30 mm.
A quenched ribbon 50 μm wide and 2-3 mm wide was obtained.

In order to confirm the microstructure of the obtained quenched ribbon, X-ray diffraction was performed at a diffraction angle of 20 ° to 60 ° using Cu-Kα, and it was confirmed that the ribbon was in an amorphous state.

The quenched ribbon was coarsely pulverized by a raikai pulverizer so that the average particle diameter of the powder was about 250 μm, to obtain an alloy powder.

This alloy powder was filled into a metal container made of material SS41 (according to JIS standard) while applying slight vibration, covered with a cover made of material SS41 having a vacuum suction opening, and welded by argon welding. Into a capsule.

Next, the capsule was placed in an electron beam welding chamber, and the inside of the capsule was evacuated from the opening. From the time when the degree of vacuum in the chamber becomes lower than 10 -1 torr, the maximum temperature is 150 at the same time as vacuum suction.
The capsule was baked at a temperature of ℃, and the opening was sealed by electron beam welding while the degree of vacuum in the chamber was maintained at 10 -4 torr.

This capsule was heated to 650 ° C. in the atmosphere, and the working temperature was 650 ° C., the total working degree was 75%, and the strain rate was 2
Hot rolling was performed at sec-1.

After the hot rolling, the capsules were cooled to a temperature of 100 ° C. or less, and then the capsules were removed from the workpiece, and the hot-worked magnet inside was taken out.

The removed magnet was pulverized by a raikai machine so that the maximum powder particle diameter was 200 μm and the average powder particle diameter was 100 μm.

Next, as a step of introducing nitrogen (N),
The powder was subjected to a heat treatment at a temperature of 440 ° C. for 2 hours in a nitrogen gas atmosphere at a pressure of 1 MPa to perform nitriding of the powder.

Further, introduction of carbon (C) and phosphorus (P)
Was introduced in the same manner as described above.

After the nitriding treatment and the like, the composition of the magnet was analyzed. As a result, the compositions of Examples 21 to 27 in Table 4 were obtained.

In order to confirm the phase structure and anisotropy of the magnet, X-ray diffraction was performed at a diffraction angle of 20 ° to 60 ° using Cu-Kα. As diffraction patterns, diffraction peaks of a (Sm.Pr) 2 (Fe.Co) 17D3 phase as a hard magnetic phase and an α-Fe phase as a soft magnetic phase were confirmed. The diffraction peak of (002) in the c-axis direction of the (Sm.Pr) 2 (Fe.Co) 17D3 phase, which is a hard magnetic phase, is particularly strongly observed in these diffraction peaks. Has been confirmed. This anisotropic magnet powder was formed into a bonded magnet by a compression molding method. At that time, 1.6 wt% of an epoxy resin was added as a binding resin. Molding was performed at a molding pressure of 7 t / cm 2 in a magnetic field of 15 kOe applied magnetic field.

The obtained molded body was heated in a nitrogen gas atmosphere for one hour to cure the binding resin, thereby producing an anisotropic bonded magnet (cube: 10 mm × 10 mm × 10 mm). The magnetic properties of the anisotropic bonded magnet were measured. The measurement was performed with a maximum magnetic field of 25 kOe using a direct current magnetic flux meter. The measurement results are shown in Table 4 together with the degree of orientation. As shown in the table, all of the magnets of Examples 21 to 27 have high magnetic properties, and particularly have high (BH) max due to sufficient anisotropy (high degree of orientation).

(Comparative Example 4) A quenched ribbon was produced under the same composition and production conditions as in Example 21, followed by pulverization, encapsulation, and vacuum sealing. Only partial heat treatment was performed. 100 capsules after processing
The capsule was removed when the temperature became lower than or equal to ° C., and the magnet inside was taken out.

This magnet was ground in the same manner as in Example 21 and subjected to nitriding.

In order to confirm the phase structure and anisotropy of the magnet, X-ray diffraction was performed using Cu-Kα at a diffraction angle of 20 ° to 60 °. As diffraction patterns, diffraction peaks of a (Sm.Pr) 2 (Fe.Co) 17D3 phase as a hard magnetic phase and an α-Fe phase as a soft magnetic phase were confirmed. However, in the magnet of this comparative example, only the diffraction peak in the c-axis direction (002) was not particularly strongly observed, and it was confirmed that the crystal orientation of the hard magnetic phase was isotropically distributed.

The magnet powder after nitriding was converted into a bond magnet in the same manner as in Example 21 to obtain a bond magnet having the same shape and the same size.

The magnetic properties of the bonded magnet were measured by a direct current recording magnetometer at a maximum applied magnetic field of 25 kOe. The measurement results are shown in Table 4 as Comparative Example 4. As shown in the table, since the magnet was not subjected to hot working and was not anisotropic, it had lower magnetic properties than Examples 21 to 27.

[0202]

[Table 4]

[0203]

As described above, according to the present invention, an anisotropic nanocomposite magnet can be provided, and high magnetic properties can be obtained. In particular, the anisotropy of nanocomposite magnets, which had been considered difficult to put into practical use, has been improved by using hot work that can be used industrially to nanocrystallize the hard magnetic phase and soft magnetic phase, and anisotropic the hard magnetic phase. Therefore, an anisotropic nanocomposite magnet having high magnetic properties can be obtained easily and inexpensively.

[Brief description of the drawings]

FIG. 1 is a view systematically showing an example of a macrostructure of an anisotropic nanocomposite magnet of the present invention.

FIG. 2 is a view systematically showing an example of the macrostructure of the anisotropic nanocomposite magnet of the present invention.

FIG. 3 is a view systematically showing an example of a macrostructure of the anisotropic nanocomposite magnet of the present invention.

FIG. 4 is a schematic process diagram of a method for producing an anisotropic nanocomposite magnet having the composition of the present invention.

FIG. 5 is a schematic process chart of a method for producing an anisotropic nanocomposite magnet having the composition of the present invention.

[Explanation of symbols]

 1 step (production of magnet raw material powder) 2 step (pulverization) 3 step (encapsulation) 4 step (hot working) 5 step (extraction) 6 step (pulverization) 7 step (introduction of D) 8 step (bond magnet ) 10 soft magnetic phase 11 hard magnetic phase 12 easy axis of magnetization (c axis)

Claims (21)

[Claims] 1. A nanocomposite magnet in which a hard magnetic phase and a soft magnetic phase are adjacent to each other and have properties as a hard magnetic material as a whole system due to magnetic exchange interaction, wherein the whole system exhibits magnetic anisotropy. A nanocomposite magnet characterized in that: 2. The anisotropic nanocomposite magnet according to claim 1, having a composition represented by the following formula (I). Rx TM100-xy By (I) (where R is at least one of rare earth elements including Y, TM is a transition element, and x and y are each 3 at%.)
≦ x ≦ 8 at%, 12 at% ≦ y ≦ 25 at%. ) 3. The anisotropic nanocomposite magnet according to claim 1, having a composition represented by the following formula (II). Rx TM100-xy By (II) (where R is at least one of rare earth elements including Y, TM is a transition element, and x and y are each 3 at%.)
≦ x ≦ 12 at%, 3 at% ≦ y ≦ 10 at%. ) 4. The anisotropic nanocomposite magnet according to claim 1, wherein said hard magnetic phase is an R2 TM14B system and said soft magnetic phase is TM or a compound of TM and B. 5. The anisotropic nanocomposite magnet according to claim 1, comprising an element represented by the following formula (III). R1xR2yFe100-xyz Coz Dw (III) (where R1 is at least one of rare earth elements including Y, R2 is at least one of Zr, Hf and Sc, and D is one of N, C and P) At least one,
x, y, z and w are respectively 2 at% ≦ x ≦ 20 at%,
0.1at% ≦ y ≦ 20at%, 4at% ≦ x + y ≦ 20at
%, 0 at% ≦ z ≦ 40 at%, 0.1 at% ≦ w ≦ 30 at%
To be satisfied. ) 6. The method according to claim 1, wherein the hard magnetic phase is (Sm.Zr) 1 F
e7 Nq system, wherein the soft magnetic phase is Fe or F
6. The anisotropic nanocomposite magnet according to claim 1, which is a compound of e and D (where q is 0.1 at% ≦ q ≦).
Satisfies 10 at%. ). 7. The anisotropic nanocomposite magnet according to claim 1, comprising an element represented by the following formula (IV). Rx TM100-xy Dy (IV) (where R is at least one of rare earth elements including Y, TM is a transition element, D is at least one of N, C, and P, and x and y are 3at% ≦ x ≦ 11at
%, 12 at% ≦ y ≦ 18 at%. ) 8. The method according to claim 1, wherein said hard magnetic phase is R2 TM17D3 and said soft magnetic phase is TM.
The anisotropic nanocomposite magnet according to 1. 9. The anisotropic nanocomposite magnet according to claim 1, wherein said hard magnetic phase is made anisotropic by hot working. 10. The anisotropic nanocomposite magnet according to claim 1, wherein the degree of orientation of the easy axis of the hard magnetic phase is 70% or more. 11. The magnetic energy product (BH) max is 13
The anisotropic nanocomposite magnet according to any one of claims 1 to 10, which has an MGOe or more. 12. The anisotropic nanocomposite magnet according to claim 1, which is a bonded magnet formed by bonding magnet powder with a bonding resin. 13. A hard magnetic phase and a soft magnetic phase are adjacent to each other to produce an anisotropic nanocomposite magnet having properties as a hard magnetic material as a whole system by magnetic exchange interaction. A method for producing an anisotropic nanocomposite magnet, comprising a step of making anisotropic by hot working. 14. A hard magnetic phase and a soft magnetic phase are adjacent to each other to produce an anisotropic nanocomposite magnet having properties as a hard magnetic material as a whole system by magnetic exchange interaction. A method for producing an anisotropic nanocomposite magnet, comprising a step of crystallizing the hard magnetic phase and the soft magnetic phase and making the hard magnetic phase anisotropic. 15. The method for producing an anisotropic nanocomposite magnet according to claim 2, wherein a step of producing a magnet material; and a step of subjecting the magnet material to hot working to obtain an anisotropic nanocomposite magnet. And a step of pulverizing the hot-worked magnet. 16. A method for producing an anisotropic nanocomposite magnet according to claim 5, wherein a step of producing a magnet raw material, and a step of subjecting the magnet raw material to hot working, A method for producing an anisotropic nanocomposite magnet, comprising: a step of making anisotropic; a step of crushing the hot-worked magnet; and a step of introducing the D into a magnet material. 17. The method for producing an anisotropic nanocomposite magnet according to claim 16, wherein the step of introducing D is performed on magnet powder pulverized after hot working. 18. The method for manufacturing an anisotropic nanocomposite magnet according to claim 17, wherein the step of introducing D is performed by heat-treating the magnet powder in a gas containing D. 19. The hot working is performed in a state where the work is encapsulated in an antioxidant capsule.
9. The method for producing an anisotropic nanocomposite magnet according to any one of 8. 20. The hot working is performed at a working temperature of 300 to 1
The method for producing an anisotropic nanocomposite magnet according to any one of claims 13 to 19, wherein the method is performed at 000 ° C. 21. The hot working is performed at a working ratio of 50 to 80%.
The method for producing an anisotropic nanocomposite magnet according to any one of claims 13 to 20, wherein the method is performed.