JPH08181009A - Permanent magnet and its manufacturing method - Google Patents

Abstract

PURPOSE: To achieve a high coercive force and a high energy product in a deposition hardening type magnet. CONSTITUTION: A permanent magnet consists of 23-27% R (R is one type out of rare earth metals containing Y), 3-6 %(6 is not included) Cu, 10-25% Fe, 1.5-4% Zr, and virtually Co for the remainder in terms of weight percentage. The alloy contains an intermetallic compound which mainly consists of rare earth cobalt. The intermetallic compound has a fine structure and Zr-containing sheet-shaped phase exists in parallel to a surface (c) of the crystal of the intermetallic compound.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a rare earth cobalt magnet, and more specifically, it is mainly composed of R (where R is at least one of rare earth metals containing Y) -cobalt intermetallic compound, Cu, Fe, or Zr
The present invention relates to the added specific composition of R ₂ Co ₁₇ system precipitation hardening permanent magnet.

[0002]

It has been well known for a long time that many intermetallic compounds exist between rare earth metals and Co.
It has been pointed out that among the metal compounds, the ferromagnetic compound centered on RCo ₅ has an extremely large magnetocrystalline anisotropy and a high saturation magnetic flux density, and is therefore an excellent permanent magnet. With this as a trigger, many researches have since led to the industrialization of rare earth cobalt magnets, which have much higher characteristics than conventional magnets. Among the RCo ₅ alloys, SmCo ₅ has a high coercive force ( _i H _c ) up to 30 KOe, and the maximum energy product {(BH) m} reaches 25 MGOe.

On the other hand, the R ₂ Co ₁₇ type alloy which is a precipitation hardening type permanent magnet has a small ratio of R to Co, is inexpensive, has a high saturation magnetic flux density, and has a high energy product. Since then, many studies have shown that Cu, Fe, Z
The maximum energy product is 3 in the specific composition with r added.
The characteristic of 0MGOe is obtained. For example,
In Japanese Patent No. 46575 (hereinafter referred to as Conventional Example 1), 24
~ 28 wt% rare earth metal R, 1-5 wt% copper Cu,
1 to 35 wt% iron Fe, 0.5 to 6 wt% (M = N
b, Zr, Ta, Hf, Ti, V), and 22-73.
A precipitation hardening permanent magnet containing 5 wt% of Co and having a cell structure with a cell distance of 500 angstroms or more as a microstructure is shown. In addition, Japanese Patent Publication 2-524
No. 13 (hereinafter referred to as Conventional Example 2) describes Ce-Co.
-Cu-Zr-Fe system, Ce-Sm-Co-Cu-Zr
-Fe system (however, Sm is 80% of the total weight of Ce and Sm)
% Or less), the zirconium-containing phases are parallel to the c-plane of the crystal, and the mutual average sensation is less than 5000 angstroms.

[0004]

By the way, R ₂ CO ₁₇
The RCo ₅ phase and the R ₂ Co ₁₇ phase are separated into two phases by aging, and the alloys show a favorable magnetic characteristic by magnetic hardening.
Further, it is known that the R ₂ Co ₁₇ type alloy has a cell structure as a fine structure. In the cell structure, the boundaries between the cells are clearly distinguished, and from the analysis result of the electron beam diffraction pattern, it is found that the inside of the cell has a 2/17 phase of a rhombohedral structure and the cell boundary has a 1/5 phase of a hexagonal structure. Has been done.

In Conventional Example 1, it has been known that the coercive force of the R ₂ Co ₁₇ alloy is due to the size of this cell structure. In the system in which Cu, Fe and Zr were added to R ₂ Co ₁₇ , the aging time was lengthened and the cell size was coarsened, and the coercive force became maximum when the cell diameter size became about 700 Å, and the aging time was further increased. It is said that the coercive force decreases as the cell diameter increases as the cell length increases. The value of this limit has been shown to be around 6000 Angstroms. However, in Conventional Example 1, no phase structure other than the RCo ₅ phase and the R ₂ Co ₁₇ phase was mentioned.

Further, in the R ₂ Co ₁₇ type alloy containing Ce as an essential component of Conventional Example 2, the zirconium-containing phase is described, and the average spacing between the zirconium-containing phases parallel to the c-plane where the characteristics deteriorate is described. The upper limit is 5000
It is said to be Angstrom. However, only the phase structure of the zirconium-containing phase within the composition range containing Ce is described, and the details of the phase structure not containing Ce and other phase structures are not shown at all.

Therefore, the technical problem of the present invention is to consider a fine structure in a rare earth cobalt-based precipitation hardening type magnet containing Sm as a rare earth as a main component, and to provide a permanent magnet capable of achieving a high coercive force and a high energy product. It is to provide the manufacturing method.

[0008]

The present invention provides, by weight percentage, 23 to 27% of R (where R is at least one of rare earth metals containing Y) and 3 to 6% (6 is not included). ) C
An alloy having a composition of u, 10 to 25% Fe, 1.5 to 4% Zr, and the balance substantially Co, the alloy containing an intermetallic compound mainly containing rare earth cobalt. , A cell structure as a fine structure, in which the inside of the cell has a main component phase of R ₂ Co ₁₇ , and the cell boundary portion has a phase containing RCo ₅ as a main component and the c-plane of the crystal of the intermetallic compound Is characterized by having a microstructure surrounded by two phases in parallel with the Zr-containing plate-like phase.

The reason for limiting the composition of the permanent magnet of the present invention is as follows. When R, which is at least one of rare earth metals including Y, exceeds 27 wt%, the saturation magnetic flux density (Br) decreases. Further, when R is less than 23 wt%, a constant coercive force ( _i H _c ) can be obtained, but the squareness of the demagnetization curve is poor and the magnetic properties are deteriorated. Also, Cu
This is because if the amount is less than 3 wt%, _i H _c is low, and if it is 6 wt% or more, the Curie point and Br decrease. Also, F
Regarding the amount of e, when the content is less than 10 wt%, Br decreases, and 3
Because _i H _c decreases exceeds 5 wt%. Furthermore, _i H _c and the energy product {(BH) m} decrease when the Zr amount is outside the range of 1.5 to 4 wt%.

The permanent magnet of the present invention having such a composition has a cell structure whose fine structure can be observed with a transmission electron microscope. In this cell structure, the inside of the cell is R-shaped.
_{It has} the main component phase of ₂ Co ₁₇ and the cell boundary is RCo ₅
The cell has a microstructure surrounded by two phases, a phase containing as a main component and a Zr-containing plate-like phase, and the distance between the cell centers of adjacent cells is less than 500 angstroms. Desirably, the distance between the cell centers is in the range of 200 to 400 angstroms.

In the present invention, whether or not it has the above cell structure can be easily observed and verified by a scanning electron microscope or a transmission electron microscope.

Such a structure The permanent magnet of the present invention is manufactured as follows. So that it has the composition shown above,
Each raw material is blended and melted in a high-frequency melting furnace in a vacuum of 1 × 10 ^-2 Torr or less to obtain a master alloy ingot. Next, the mother alloy ingot thus obtained is roughly crushed and then finely crushed in an inert atmosphere using a jet mill or the like to obtain a powder having an average particle size of 1 to 5 μm. This powder is 7-22KO
0.5 ~ in the direction perpendicular to or parallel to the magnetic field in the magnetic field of e
Press molding is performed with a pressing force of 2.0 ton / cm ² . Then, the molded body was placed in a vacuum of 1 × 10 ^-2 Torr or less,
Alternatively, sintering is performed at a temperature of 1150 to 1250 ° C. in an inert atmosphere or a combination thereof, and solution treatment is performed at a temperature 10 to 50 ° C. lower than the sintering temperature in the atmosphere. After the solution treatment, it is rapidly cooled at a cooling rate of 60 ° C./min or more. After the rapid cooling, the aging treatment is performed by heating and holding at a temperature of 700 to 870 ° C. for 1 hour or more in a vacuum of 1 × 10 ⁻² Torr or less or in an inert atmosphere.

In the present invention, all of the melting, pulverizing, sintering and solution treatment are performed in a vacuum or in an inert atmosphere so that the carbon content in the alloy is 700 ppm or less and the oxygen content is Can be suppressed to 3000 ppm or less as much as possible, and a permanent magnet having excellent magnetic characteristics can be obtained.

By the manufacturing process as described above, the magnetic hardening is performed and the permanent magnet of the present invention is obtained.

Incidentally, the permanent magnet of the present invention can be widely used in watches, electric motors, measuring instruments, communication devices, computer terminals, speakers, video disks, and various other parts.

[0016]

In the present invention, in addition to the cell structure found in the fine structure of the precipitation hardening magnet, a Zr-containing plate-like phase is precipitated parallel to the c-plane of the crystal of the rare earth cobalt intermetallic compound,
Not only the domain wall pinning effect at the cell boundary but also the domain wall pinning effect due to the plate-like phase is provided to obtain high coercive force and high energy product.

[0017]

EXAMPLES Examples of the present invention will be described below.

Example 1 First, 6 shown in Table 1 below.
Each raw material is blended so as to form an alloy with different composition,
^In a vacuum of ^-2 Torr or less, 6 types of master alloy ingots were obtained by melting in a high frequency melting furnace. These master alloy ingots were roughly crushed and finely crushed in an inert atmosphere with a jet mill to give an average particle size of 4 μm. Of powder was obtained. This powder was press-molded in a magnetic field of 15 KOe under a pressure of 1.0 ton / cm ² to obtain a molded body. The molded body thus obtained is sintered at a temperature of 1200 to 1250 ° C. in a vacuum of 1 × 10 ⁻² Torr or less and in an inert atmosphere, and then solution heat treated at 1180 to 1230 ° C. Then, it was rapidly cooled at a cooling rate of 100 ° C./min. After quenching,
Isothermal aging treatment was performed by heating and holding at 800 ° C. for 300 minutes in an inert atmosphere.

When the six types of permanent magnets magnetically hardened in this way were observed by a transmission electron microscope, they had a cell structure as a fine structure, the inside of the cell had an R ₂ CO ₁₇ phase, and the cell boundary portion was It was confirmed to have a fine structure surrounded by two phases, an RCo ₅ phase and a Zr-containing plate-like phase. In addition, when the magnetic characteristics of each permanent magnet material were measured, the results shown in Table 1 below were obtained.

[0020]

[Table 1] As is apparent from Table 1, the permanent magnet according to the first embodiment of the present invention, Br for practical use, _i H _c, it can be seen that with the (BH) m.

(Example 2) Sm 25.9 wt%, Cu
4.5wt%, Fe15.0wt%, Zr3.1wt%
The alloy having the composition consisting of and the balance Co was subjected to melting, crushing, molding, sintering and solution treatment in the same manner as in Example 1.

Next, the aging treatment was carried out in an inert atmosphere at an isothermal aging temperature of 800 ° C. within the range of 5 types of isothermal aging times shown in Table 2 below, a minimum of 6 minutes and a maximum of 900 minutes. The results are shown in Table 2 below.

[0023]

[Table 2] Next, using a transmission electron microscope equipped with an energy dispersive X-ray analyzer, the microstructures of the test materials having different coercive forces were observed to identify the Zr-containing plate phase. It was confirmed that it has a cell structure as a fine structure, the inside of the cell has an R ₂ Co ₁₇ phase, and the cell boundary has a fine structure surrounded by two phases, an RCo ₅ phase and a Zr-containing plate-like phase. Was done.

Photographs (a-plane of crystal) of the microstructures of the permanent magnets of the test materials 9 and 11 according to the present invention are shown in FIGS. 1 and 2, respectively.
Nanostructure photographs showing the lattice image at that time are shown in FIGS. 3 and 4, respectively. From the picture, the distance between the cell centers of adjacent cells is 1
It is from 00 to 400 angstroms. It can be seen that there is a relationship in which the coercive force _i H _c also increases as the isothermal aging time increases. The Zr-containing plate-like phase is perpendicular to the c-axis direction, that is, c
There are many parallel to the surface. The results of energy dispersive X-ray analysis of the Zr-containing plate-like phase and the R ₂ Co ₁₇ phase inside the cell are shown in FIGS. 5 and 6, respectively.

As shown in FIG. 5, a large amount of Zr is detected in the portion where the Zr-containing plate-like phase is present, but almost no Zr is detected in the R ₂ Co ₁₇ phase inside the cell shown in FIG. .

(Example 3) Sm 25.7 wt%, Cu
4.3wt%, Fe14.9wt%, Zr3.0wt%
The alloy having a composition of Co and the balance Co was melted, pulverized, molded, sintered, solution-treated, and aged in the same manner as in Example 1. Also, the gas content of each permanent magnet material was measured. The results are shown in Table 3 below together with the magnetic properties.

[0027]

[Table 3] As shown in the results of Table 3 above, the permanent magnet according to Example 3 of the present invention has a carbon content of 700 ppm or less and an oxygen content of 3000 pp.
m when: Br for practical use, _i H _c, show the (BH) m, it can be seen that a very high squareness ratio.

Example 4 Sm 25.8 wt%, Cu
4.5wt%, Fe15.0wt%, Zr3.0wt%
The alloy having the composition consisting of and the balance Co was subjected to melting, crushing, molding, sintering and solution treatment in the same manner as in Example 1. Then, rapid cooling after the solution treatment was performed at five types of cooling rates shown in Table 4 below at a temperature of 30 ° C to 300 ° C / min. After quenching, isothermal aging treatment was performed by heating and holding at 800 ° C. for 300 minutes in an inert atmosphere. The results are shown in Table 4 below.

[0029]

[Table 4] As shown in the results of Table 4 above, the permanent magnet according to Example 4 of the present invention shows Br, _i H _c , (BH) m that are practically used when the quenching rate after solution heat treatment is 60 ° C./min or more, It can be seen that it exhibits an extremely high squareness ratio.

[0030]

As described above, according to the present invention, by melting, finely pulverizing, sintering, solutionizing, quenching and isothermal aging, a cell structure is formed as a fine structure, and the inside of the cell is It has the main component phase of R ₂ Co ₁₇ and the cell boundary is RCo
Provided are a permanent magnet having a fine structure surrounded by two phases, a phase containing ₅ as a main component and a Zr-containing plate-like phase, and having excellent magnetic properties such as high coercive force and high energy product, and a manufacturing method thereof. Became possible.

[Brief description of drawings]

FIG. 1 is a transmission electron micrograph showing a metal structure of a permanent magnet having a fine structure according to Example 2 of the present invention.

FIG. 2 is a transmission electron micrograph showing a metal structure of a permanent magnet having a fine structure according to Example 2 of the present invention.

FIG. 3 is a transmission electron micrograph showing a metal structure for explaining a nanostructure of the permanent magnet of FIG.

4 is a transmission electron micrograph showing a metal structure for explaining a nanostructure of the permanent magnet of FIG.

5 is an energy dispersion analysis diagram of the Zr-containing plate-like phase and the R ₂ Co ₁₇ phase inside the cell of the permanent magnet of FIG. 1, respectively.

FIG. 6 is an energy dispersion analysis diagram of the Zr-containing plate-like phase and the R ₂ Co ₁₇ phase inside the cell of the permanent magnet of FIG. 2 respectively.

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[Procedure amendment]

[Submission date] February 3, 1995

[Procedure Amendment 1]

[Document name to be amended] Statement

[Name of item to be corrected] Claim 4

[Correction method] Change

[Correction content]

[Procedure Amendment 2]

[Document name to be amended] Statement

[Correction target item name] 0001

[Correction method] Change

[Correction content]

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a rare earth cobalt magnet, and more specifically, it is mainly composed of R (where R is at least one of rare earth metals containing Y) -cobalt intermetallic compound, Mainly Cu, Fe, and Zr
The present invention relates to the added specific composition of R ₂ Co ₁₇ based precipitation hardening permanent magnet.

[Procedure 3]

[Document name to be amended] Statement

[Name of item to be corrected] 0003

[Correction method] Change

[Correction content]

On the other hand, the R ₂ Co ₁₇ type alloy which is a precipitation hardening type permanent magnet has a small ratio of R to Co, is inexpensive, has a high saturation magnetic flux density, and has a high energy product. Since then, many studies have shown that Cu, Fe,
In the specific composition to which Zr is added, the characteristic of 30 MGOe is obtained at the maximum energy product. For example, Japanese Examination 1
-46575 (hereinafter, referred to as Conventional Example 1), 2
4 to 28 wt% rare earth metal R, 1 to 5 wt% copper C
u, 1 to 35 wt% iron Fe, 0.5 to 6 wt% (M
= Nb, Zr, Ta, Hf, Ti, V), and 22 to 7
A precipitation hardening permanent magnet containing 3.5 wt% Co and having a cell structure with a cell distance of 500 angstroms or more as a microstructure is shown. In addition, Japanese Patent Fair 2-5
No. 2413 (hereinafter referred to as Conventional Example 2) describes Ce-
Co-Cu-Zr-Fe system, Ce-Sm-Co-Cu-
In a Zr-Fe system (however, Sm is 80% or less of the total weight of Ce and Sm) permanent magnets whose zirconium-containing phases are parallel to the c-plane of the crystal and whose average interval is 5000 angstroms or less. A magnet is shown.

[Procedure amendment 4]

[Document name to be amended] Statement

[Correction target item name] 0007

[Correction method] Change

[Correction content]

[0007] Therefore, the technical problem of the present invention is a rare earth cobalt-based precipitation hardenable magnet composed mainly of Sm as the rare earth, consider the microstructure, a permanent magnet makes it possible high coercivity, and high energy product It is to provide the manufacturing method.

[Procedure Amendment 5]

[Document name to be amended] Statement

[Correction target item name] 0009

[Correction method] Change

[Correction content]

The reason for limiting the composition of the permanent magnet of the present invention is as follows. When R, which is at least one of rare earth metals including Y, exceeds 27 wt%, the saturation magnetic flux density (Br) decreases. Further, if R is less than 23 wt%, a constant coercive force ( _i H _c ) can be obtained, but the squareness of the demagnetization curve is poor and the magnetic properties are deteriorated. Also, Cu
This is because if the amount is less than 3 wt%, _i H _c is low, and if it is 6 wt% or more, the Curie point and Br are lowered. Also, F
With regard to e amount, Br decreases is less than 10 wt%, 2
5 exceeds wt% when _i H _c is lowered. Furthermore, when the Zr amount is outside the range of 1.5 to 4 wt%, _i H _c and the energy product {(BH) m} decrease.

[Procedure correction 6]

[Document name to be amended] Statement

[Correction target item name] 0012

[Correction method] Change

[Correction content]

The permanent magnet of the present invention having such a structure is manufactured as follows. The respective raw materials are blended so as to have the composition shown above, and melted in a high frequency melting furnace in a vacuum of 1 × 10 ⁻² Torr or less to obtain a master alloy ingot. Next, the obtained master alloy ingot is roughly pulverized and further finely pulverized in an inert atmosphere using a jet mill or the like to obtain a powder having an average particle size of 1 to 5 μm. 7 to this powder
Vertical to the magnetic field in a magnetic field of 22KOe, or press formed shape <br/> by pressure of 0.5 to 2.0 t / cm ² in a parallel direction. Then, the compact is sintered at a temperature of 1150 to 1250 ° C. in a vacuum of 1 × 10 ⁻² Torr or less, in an inert atmosphere, or in an atmosphere of a combination thereof, and the sintering temperature in the atmosphere is higher than the sintering temperature. Also, the solution treatment is performed at a temperature lower by 10 to 50 ° C. After the solution treatment, it is rapidly cooled at a cooling rate of 60 ° C./min or more. After quenching, 1 × 10 ⁻² To
700 to 87 in a vacuum below rr or in an inert atmosphere
Aging treatment is performed by heating and holding at a temperature of 0 ° C. for 1 hour or more.

[Procedure Amendment 7]

[Document name to be amended] Statement

[Correction target item name] 0018

[Correction method] Change

[Correction content]

(Example 1) First, as shown in Table 1 below, each raw material was blended so as to form an alloy of six kinds of compositions of Sm, Ce, Cu, Fe, Zr, and Co, and 1 x 10
-In a vacuum below ² Torr, 6 kinds of master alloy ingots were obtained by melting in a high frequency melting furnace. These master alloy ingots were coarsely crushed and finely crushed in an inert atmosphere with a jet mill to obtain an average particle size of 4 μm. Of powder was obtained. The press forming shape by the pressurizing force of the powder in a magnetic field of 15 kOe 1.0 tons / cm ² to obtain a molded body. The compact thus obtained is sintered at a temperature of 1200 to 1250 ° C. in a vacuum of 1 × 10 ⁻² Torr or less and in an inert atmosphere, and then solution heat treated at 1180 to 1230 ° C. Then, it was rapidly cooled at a cooling rate of 100 ° C./min. After quenching, isothermal aging treatment was performed by heating and holding at 800 ° C. for 300 minutes in an inert atmosphere.

[Procedure Amendment 8]

[Document name to be amended] Statement

[Correction target item name] 0020

[Correction method] Change

[Correction content]

[0020]

[Table 1] As is apparent from Table 1, the permanent magnet according to the first embodiment of the present invention, Br for practical use, i H _c, it can be seen that with the _(BH) m.

[Procedure Amendment 9]

[Document name to be amended] Statement

[Correction target item name] 0021

[Correction method] Change

[Correction content]

(Example 2) Sm 25.9 wt%, Cu
4.5wt%, Fe15.0wt%, Zr3.1wt%
And per alloys having compositions the balance Co, dissolved in the same manner as in Example 1, grinding, forming shapes and successively subjected to sintering and solution treatment.

[Procedure Amendment 10]

[Document name to be amended] Statement

[Correction target item name] 0028

[Correction method] Change

[Correction content]

Example 4 Sm 25.8 wt%, Cu
4.5wt%, Fe15.0wt%, Zr3.0wt%
And per alloys having compositions the balance Co, dissolved in the same manner as in Example 1, grinding, forming shapes and successively subjected to sintering and solution treatment. Then, rapid cooling after the solution treatment was performed at five types of cooling rates shown in Table 4 below at a temperature of 30 ° C to 300 ° C / min. After quenching, isothermal aging treatment was performed by heating and holding at 800 ° C. for 300 minutes in an inert atmosphere. The results are shown in Table 4 below.

Claims (4)

[Claims] 1. A weight percentage of R of 23 to 27% (R is at least one of rare earth metals including Y) and 3 to 6%.
An alloy consisting of Cu (not including 6), 10 to 25% Fe, 1.5 to 4% Zr, and the balance being substantially Co, said alloy being mainly composed of rare earth cobalt. A permanent magnet containing an intermetallic compound and having a fine structure, wherein a Zr-containing plate-like phase is present in the fine structure parallel to the c-plane of the crystal of the intermetallic compound. 2. The permanent magnet according to claim 1, wherein the fine structure has a cell structure, and in the cell structure, the inside of the cell has a main component phase of R ₂ Co ₁₇ and the cell boundary portion includes RCo ₅ . A permanent magnet having a fine structure surrounded by two phases, a phase as a main component and the plate-like phase. 3. The permanent magnet according to claim 1, wherein the carbon content in the alloy is at most 700 ppm and the oxygen content is at most 3000 ppm. 4. By weight percentage, 23 to 27% R (R is at least one of rare earth metals including Y) and 3 to 6%.
(However, 6 is not included) Cu and 10 to 25% Fe,
A method for producing a permanent magnet having an alloy composition of 1.5 to 4% Zr and the balance substantially Co, in which raw materials are blended so as to have the alloy composition, and at most 1 a dissolution step of dissolving at × 10 ^-2 Torr in a vacuum to obtain a mother alloy ingot, and coarsely pulverized to obtain a coarsely pulverized powder was coarsely grinding the resulting mother alloy ingot,
A fine pulverizing step of finely pulverizing the coarsely pulverized powder in an inert atmosphere to obtain a finely pulverized powder having an average particle size of 1 to 5 μm; and the finely pulverized powder in a magnetic field of 7 to 22 KOe in a direction perpendicular to or parallel to the magnetic field. In a direction of 0.5 to 2.0 ton / cm ² to obtain a compact, and the compact is subjected to a vacuum of 1 × 10 ^-2 Torr at most, in an inert atmosphere, and A sintering step of sintering at a sintering temperature of 1150 to 1250 ° C. to obtain a sintered body in any of the atmospheres of these combinations, and a temperature of 10 times higher than the sintering temperature in the atmosphere. A solution treatment step of heat treatment at a temperature lower by ~ 50 ° C, and at least 60 ° C / after the solution treatment step.
A quenching step of quenching at a cooling rate of a minute, and after the quenching step, heating and holding at a temperature of 700 to 870 ° C. for at least 1 hour in a vacuum or an inert atmosphere of at most 1 × 10 ⁻² Torr and aging. A method of manufacturing a permanent magnet, comprising: an aging treatment step of treating.