JP3505261B2 - Sm-Co permanent magnet material, permanent magnet and method for producing the same - Google Patents

Description

Detailed Description of the Invention

[0001]

The present invention relates to Sm, Fe, Cu, Z
Sm-Co based permanent magnet material containing r and Co as essential components and a method for producing the same, Sm-Co based sintered permanent magnet using this material as a raw material and having excellent magnetic properties, Sm-C
The present invention relates to an o-type bonded permanent magnet and manufacturing methods thereof.

[0002]

2. Description of the Related Art Conventionally, when a metal (including alloy) solidifies, the obtained crystal grows in a dendritic form when the temperature gradient in the metal liquid in front of the solid-liquid interface is small and the crystal growth rate is high. It is known that this is easy to do, and this dendrite form crystal is called dendrite or dentrite. It is known that this dendrite forms a substructure of columnar crystals. The part that serves as the trunk of dendrites is called the primary branch (arm), and it grows into columns within one columnar crystal. There are many parallel branches. The distance between the branches is called the distance between the dendrite primary arms, and it is known that the distance can be measured based on a microscopic photograph of a vertical section. However, it is not known how the distance between the dendrite primary arms affects magnet performance and magnet manufacturing conditions. The X-ray orientation degree f value is known as an index indicating the crystal orientation degree of a metal (Sato et al .: "Crystal orientation degree and sintered magnet characteristics of Nd-Fe-B system liquid quenched alloy", Tokin Technikal Review No. 15 P
29 (1989)). However, in conventional Sm-Co magnets, X
At present, there is no known material having a high degree of linear orientation f of 80 or more.

In the method for producing a sintered magnet for an Sm-Co magnet, the alloy ingot having the adjusted composition is crushed to 1 to 5 μm,
After pressure forming in a magnetic field of 8 to 15 KOe / cm ² , the temperature exceeds 1150 ° C. and 1350 ° C. in a pure argon stream.
Less than 2 hours, usually at 1200 ℃
Sintering is performed within the time and solution treatment is performed. Then 80
A set temperature is selected from a temperature range of 0 to 900 ° C., the set temperature is controlled to ± 2 ° C., an aging treatment is performed for about 8 hours, and a grinding process is performed to obtain dimensional accuracy when the magnet performance is obtained, After that, it is generally magnetized to obtain a product magnet.

In the case of the above-mentioned sintered magnet, the quality of the orientation during pressure molding in a magnetic field directly determines the degree of anisotropy, and if the orientation is poor, the magnet characteristics of the magnet material cannot be fully extracted. become. It is considered that this degree of orientation has a large factor in the uniformity of the crystal structure of the magnet powder and the uniformity of the particle size. Also in the manufacturing method, in the conventional method, the sintering temperature of the sintering process is as high as about 1200 ° C., and the sintering time is long, which requires a great energy cost. It adversely affects the magnetic properties of the obtained sintered magnet. Furthermore, for aging treatment, the set temperature is ±
The actual situation is that good magnetic properties cannot be obtained unless the temperature is strictly controlled within the range of 2 ° C., which requires advanced aging treatment equipment.

On the other hand, in the method for producing a bonded magnet in an Sm-Co type magnet, the alloy ingot having its structure adjusted is subjected to solution treatment in an argon stream at 1100 to 1300 ° C. for 15 to 30 hours, and then 800 to. A set temperature is selected from the temperature range of 900 ° C., the set temperature is controlled to ± 2 ° C., and an aging treatment is performed for about 8 hours. Then, the obtained alloy ingot was mixed with 10
8 to 15 KOe / cm after crushing to ~ 30 μm and mixing and kneading 1 to 5% by volume of resin such as epoxy resin and nylon resin.
^It is a general method to perform compression molding in a magnetic field of ^{2 at} a press pressure of 1 to 5 t / cm ² to obtain a molded body, shape-grind the obtained molded body, and magnetize it to obtain a product magnet. .

However, in the above-mentioned conventional bonded magnet, the grain size of the magnet powder is 1 because the structure in the magnet grain is not uniform.
When the grain size is as coarse as 0 to 30 μm, the degree of orientation, and hence the anisotropy, are immediately adversely affected, which causes deterioration of magnetic properties. Further, solution treatment and aging treatment also require a long time at a high temperature as in the case of the sintered magnet, and further, the temperature control of the aging treatment is strict, and the aging treatment equipment is expensive.

[0007]

SUMMARY OF THE INVENTION Therefore, an object of the present invention is to provide a permanent magnet having a uniform structure with excellent magnetic properties, and to lower the temperature condition during the production of the permanent magnet. The present invention is to provide a novel Sm-Co based permanent magnet material that can set the treatment time to a short time and can easily control the conditions at the time of manufacturing, and a method for manufacturing the same. Another object of the present invention is an Sm-Co based sintered permanent magnet having excellent magnet characteristics and S.
An object is to provide an m-Co based bonded permanent magnet. Another object of the present invention is to set the temperature condition at the time of manufacture to a low temperature and the treatment time to a short time, and to easily control the conditions at the time of manufacture, and to obtain excellent magnet characteristics. An object of the present invention is to provide a method for producing the obtained Sm-Co based sintered permanent magnet and Sm-Co based bonded permanent magnet.

[0008]

According to the present invention, Sm5
20-30 wt% rare earth metal containing 0 wt% or more, Fe
10 to 25% by weight, Cu 2 to 7% by weight, Zr 0.5 to 4
A permanent magnet material whose main component is an alloy composition consisting of wt% and the remaining amount of Co, and the material has a minor axis length of 10 to 200.
The crystal structure contains 90% by volume or more of columnar grains having a long axis length of 50 to 500 μm and the dendritic primary arms that are substructures of the columnar grains have an interval of 0.5 to
There is provided an Sm-Co based permanent magnet material, which comprises 80% by volume or more of a crystal having a size of 20 μm and has an X-ray orientation degree f value according to the following mathematical formula 2 of f ≧ 80.

[0009]

[Equation 2]

Further, according to the present invention, the alloy melt containing the above alloy composition as a main component is subjected to a subcooling of 10 to 10 by a single roll method.
Over 500 ℃, cooling rate over 500 ℃ / sec, 10,000 ℃
The above-mentioned S characterized by being uniformly solidified and cast into a strip having a thickness of 0.1 to 0.7 mm under a cooling condition of less than 1 / second.
A method for manufacturing an m-Co based permanent magnet material is provided.

Further, according to the present invention, there are provided an Sm-Co based sintered permanent magnet and an Sm-Co based bonded permanent magnet obtained by using the Sm-Co based permanent magnet material as a raw material. Furthermore, according to the present invention, the Sm—Co based permanent magnet material is finely pulverized, compression-molded in a magnetic field, sintered in a non-oxidizing atmosphere at 1000 to 1250 ° C. for 1 to 2 hours, and then 800 Select the set temperature from the temperature range of ~ 900 ℃,
There is provided a method for producing the Sm-Co based sintered permanent magnet, which is characterized in that the aging treatment is performed for 5 to 10 hours while controlling the set temperature to ± 5 ° C. Further, according to the present invention, the Sm-Co
1000-based permanent magnet material in a non-oxidizing atmosphere
After heat solution treatment at ~ 1200 ° C for 0.1 to 5 hours,
A preset temperature is selected from a temperature range of 800 to 900 ° C., the preset temperature is controlled to ± 5 ° C., an aging treatment is performed for 5 to 10 hours, and then the powder is pulverized to obtain a magnet powder having a particle diameter of 10 to 30 μm.
There is provided a method for producing the Sm-Co based bonded permanent magnet, which comprises mixing and kneading the magnet powder and a resin of 1 to 3% by volume and molding the mixture in a magnetic field.

The present invention will be described in more detail below. The Sm-Co based permanent magnet material of the present invention contains a specific alloy composition as a main component, and has a specific crystal structure and a crystal orientation degree. In this case, the main component is not particularly limited as long as it is contained in an amount that achieves the desired object of the present invention, but is usually 95% by weight or more, preferably 9% by weight based on the total amount of the magnetic material.
It means 7% by weight or more. The main component of the alloy composition is S
20 to 30 wt% of rare earth metal containing 50 wt% or more of m,
Fe 10-25 wt%, Cu 2-7 wt%, Zr0.5
˜4 wt% and Co balance. The rare earth metal other than Sm is not particularly limited, and La,
Examples thereof include Nd, Ce, Pr, Sc and Gd. When the content of Sm in the rare earth metal is less than 50% by weight, physical properties as a magnet cannot be imparted.

In addition to the above-mentioned main components, the permanent magnet material of the present invention further contains Ti, Bi, Nb, Cr, W, Al, Ge, Si and N, as long as it does not affect the desired purpose.
In addition to 3 wt% or less of i, V, Ta, Mo, Mn, Sb, Sn or a mixture thereof, other impurities that are inevitably contained in the normal production may be contained.

The Sm-Co based permanent magnet material of the present invention has a minor axis length of 10 to 200 μm, preferably 10 to 100 μm.
m, major axis length 50 to 500 μm, preferably 70 to 50
90 μm or more of 0 μm columnar grains are contained in the crystal structure, and the interval between the dendritic primary arms that are substructures of the columnar grains is 0.5 to 20 μm, preferably 0.5 to 10 μm. Contains 80% by volume or more of crystals. The minor axis and major axis lengths of the columnar grains are out of the above range, and 90
When the content is less than the volume%, the degree of uniform structure is low and excellent magnet characteristics cannot be imparted to the obtained magnet.
On the other hand, when the distance between the dendrite primary arms is outside the above range, and when the dendrites are less than 80% by volume,
When manufacturing a permanent magnet using this permanent magnet material,
Sintering and solution treatment cannot be performed easily at low temperature in a short time, and it becomes difficult to prevent oxidation that deteriorates magnetic properties. The interval between the dendritic primary arms that are sub-structures of the columnar grains is described in detail in "Casting and solidification; Lecture / Modern Metallurgical Materials 10: Published by The Japan Institute of Metals, p91-97 (1992)". Therefore, it can be measured and evaluated based on the microstructure photograph of the vertical section.

Further, the Sm-Co based permanent magnet material of the present invention has the above-mentioned specific columnar crystal and has a high degree of crystal orientation.
That is, the X-ray orientation degree f value shown by the above-mentioned mathematical expression 2 which is an orientation degree index is f ≧ 80. The X-ray orientation degree f-value is Sato et al .: "Crystal orientation degree and sintered magnet characteristics of Nd-Fe-B system liquid quenched alloy" (Tokin Technikal Review No. 15, P29 (198).
9)). In the above mathematical formula 2, the value of the intensity of the diffracted X-ray can be measured by the usual powder X-ray diffraction method. When this f value is less than 80, the crystallinity in the magnet material particles is poor, and the anisotropy when the magnet is used is reduced. When f ≧ 80, a high-performance anisotropic bonded permanent magnet can be obtained even when used in a bonded permanent magnet having a large powder particle diameter.

In the method for producing the Sm-Co based permanent magnet material of the present invention, first, an alloy melt containing the alloy composition as a main component is prepared. This alloy melt may contain 3% by weight or less of the above-mentioned other metal other than the above-mentioned main component. To prepare the alloy melt, for example, the vacuum melting furnace method,
It can be obtained by a high frequency melting furnace method or the like, preferably using a crucible or the like in an inert gas atmosphere or the like.

Next, in the method for producing the Sm-Co based permanent magnet material of the present invention, the degree of supercooling of the alloy melt is 10 to 500.
° C, preferably by increasing the ratio of the length of the obtained columnar crystal in the major axis direction and the length in the minor axis direction to improve the degree of anisotropy,
Further, in order to improve the magnetic properties of the permanent magnet obtained by improving the dispersibility of the phase rich in rare earth metal, the lower limit of the degree of supercooling is adjusted to 100 ° C. In this case, the degree of supercooling is a value of (melting point of alloy)-(actual temperature of alloy melt below melting point). More specifically, "supercooling" is the temperature at which the alloy melt does not actually solidify even when the alloy melt is cooled to reach the melting point of the alloy, and the temperature is further lowered. It is a phenomenon in which a fine solid phase, that is, crystals are formed and solidification occurs for the first time. Such supercooling degree control is performed, for example, by controlling the temperature of the alloy melt prepared by using the above-mentioned crucible or the like, and by appropriately adjusting the time and speed for leading to a single roll for solidification. be able to.

In the method for producing a permanent magnet material of the present invention, the cooling rate is preferably more than 500 ° C./sec and 10,000 ° C./sec or less, preferably 1000 to 5000 ° C./sec in an inert gas atmosphere. Under the conditions, the alloy casting having a controlled subcooling degree having a thickness of 0.1 to 0.7 mm, preferably 0.1 to 0.
A 5 mm strip is uniformly solidified and cast. The cooling rate and thickness can be controlled, for example, by adjusting the number of rotations of the roll, the surface temperature, the ambient temperature, or the amount of the alloy melt supplied to the roll. If the cooling rate and thickness are out of the specified ranges, the desired crystal structure and high degree of orientation cannot be obtained. In addition, the single roll is adopted because when a twin roll or a rotating disk is used, it is difficult to control the crystal growth direction and the cooling rate, the desired crystal structure cannot be obtained, and the durability of the apparatus itself is poor. This is because the single roll method makes it easy to control the conditions of such an alloy melt. The Sm-Co based sintered permanent magnet and the Sm-Co based bonded permanent magnet of the present invention are both obtained by using the Sm-Co based permanent magnet material as a raw material, and preferably obtained by the production method described later. You can

In the method for producing the Sm-Co based sintered permanent magnet of the present invention, first, the Sm-Co based permanent magnet material is finely pulverized. This fine pulverization can be carried out, for example, by roughly pulverizing with a crusher and then pulverizing with a wet ball mill or the like in an inert gas stream, preferably to 1 to 5 μm.

Next, the finely ground product is preferably 8 to 1
In an applied magnetic field of 5 kOe, compression molding is performed using, for example, a magnetic field press. Subsequently, the obtained compression molded product is 1000 to 1250 ° C., preferably 1150 to 1250 ° C., for 1 to 2 hours in a non-oxidizing atmosphere such as a high-purity argon gas stream that is vacuum-substituted using a vacuum heating furnace or the like. Sinter.
Sintering by the conventional method is at about 1300 ° C for more than 2 hours and 5
In the production method of the present invention, 80% by volume of crystals having a dendrite primary arm interval of 0.5 to 20 μm, which is a substructure of the columnar crystals, is used in the production method of the present invention.
Since the permanent magnet material contained above is used, sintering
The low temperature can be performed in a short time, and the cost can be reduced. It also makes it possible to prevent oxidation that deteriorates magnetic properties.

Subsequently, after sintering, the material is rapidly cooled to 800 to 900 ° C.
Preferably, the set temperature is selected from the temperature range of 830 to 850 ° C., the set temperature is controlled to ± 5 ° C., and the aging treatment is performed for 5 to 10 hours. The temperature setting of this aging treatment is very delicate due to the non-uniformity of the temperature distribution of the furnace in the conventional method, and the performance could not be improved unless it was controlled to about ± 2 ° C. High Sm-C
When an o-based permanent magnet material is used, high magnet characteristics can be obtained even by temperature control of ± 5 ° C, and temperature control is easy.

Next, the obtained magnet material after aging treatment is
Similar to the conventional method, a sintered permanent magnet can be obtained by a known method such as a method of magnetizing after grinding to obtain dimensional accuracy.

In the method of manufacturing the Sm-Co based bonded permanent magnet of the present invention, the Sm-Co based permanent magnet material is first vacuum-replaced using, for example, a high vacuum heating furnace or the like, and a non-oxidizing atmosphere such as an argon gas stream is used. Inside, 1000-1200
Heat solution treatment is performed at 0 ° C. for 0.1 to 5 hours. By this heat solution treatment, the crystal grain size is preferably 50 to 700 μm for the short axis length and 300 to 1000 μ for the long axis length.
It is desirable to set m. In the conventional method, a permanent magnet material containing 80% by volume or more of crystals having a dendrite primary arm spacing of 0.5 to 20 μm, which is a substructure of the columnar crystals, is not used as a raw material. It takes 15 to 30 hours.

Next, 800 to 900 ° C., preferably 83
A set temperature is selected from a temperature range of 0 to 850 ° C., the set temperature is controlled to ± 5 ° C., and an aging treatment is performed for 5 to 10 hours.
In the conventional method, the temperature setting of the aging treatment could not be improved unless it was controlled to about ± 2 ° C. in the same manner as in the sintered permanent magnet, but the Sm-Co system having high texture uniformity in the present invention was not achieved. When using a permanent magnet material, high magnet characteristics can be obtained even by temperature control of ± 5 ° C, and temperature control is easy.

Subsequently, the obtained ingot is crushed with a crusher, a disc mill or the like to preferably 10 to 30 μm,
Epoxy resin, nylon resin etc
~ 3% by volume, knead well, preferably 8-15
A desired bonded permanent magnet can be obtained by performing a molding process such as compression molding or injection molding with a press pressure of 1 to ⁵ t / cm ² in an applied magnetic field of kOe. At this time, the ingot can be pulverized by coarse pulverization of 10 to 30 μm as in the conventional method. Even with such coarse pulverization,
When the Sm—Co based permanent magnet material having a high degree of crystal orientation with an X-ray orientation degree f value of f ≧ 80 is used as a raw material,
It is possible to obtain a bonded permanent magnet having a high degree of anisotropy by magnetic field molding even with coarse particles without adversely affecting the degree of orientation or anisotropy as in the conventional case.

[0026]

In the Sm-Co based sintered or bonded permanent magnet of the present invention and the method for producing the same, the permanent magnet material of the present invention having a specific crystal structure and a high degree of orientation is used as a raw material. Is easy to sinter, has excellent magnetic properties such as residual magnetic flux density and coercive force, and exhibits particularly excellent anisotropy. Further, in a bonded magnet, the solution treatment of the alloy ingot is easy, the orientation of the obtained magnet powder is good, and even if it is coarse particles, it is excellent in the degree of anisotropy, and the residual magnetic flux density, coercive force, etc. Excellent magnet characteristics. Therefore, it is expected to be applied to the fields in which excellent magnetic properties are required. Further, the Sm-Co based permanent magnet material of the present invention is extremely effective as a raw material for such a permanent magnet, and is also useful for cost reduction in manufacturing.

[0027]

EXAMPLES The present invention will be described in more detail with reference to Examples and Comparative Examples below, but the present invention is not limited thereto.

[0028]

Example 1 Sm 23.5 parts by weight, Co 51.0 parts by weight, Fe 19.0 parts by weight, Cu 4.0 parts by weight and Zr
A metal mixture having a composition of 2.5 parts by weight was melted in a vacuum high frequency induction melting furnace in an argon atmosphere at a supercooling degree of 150.
C. and a cooling rate of 800 to 1000.degree. C./sec. Were used to cast into a band-shaped ingot having a thickness of 0.4 mm using a single roll casting device. The obtained strip-shaped ingot was observed with a scanning electron microscope manufactured by JEOL Ltd., and the shape of columnar grains and the dendrite primary arm interval were measured. In this scanning electron micrograph, a photograph for measuring the primary arm spacing of the dendrite is shown in FIG. 1, and a photograph for measuring the shape of columnar grains is shown in FIG. A powder X-ray diffraction pattern was prepared from the same strip-shaped ingot using an X-ray diffractometer manufactured by Rigaku Electric Co., and the X-ray orientation degree f value was calculated from the diffraction intensity. The results are shown in Table 1.

[0029] Then after rough grinding the strip ingot with a crusher, then pulverized to an average particle size 4μm in a wet ball mill, a 10 × 10 × 10 mm square at a press pressure of 2t / cm ² in an applied magnetic field of 12KOe this powder A large number of green compacts were formed. The green compact thus obtained was sintered in a vacuum heating furnace in a high-purity argon stream at 1200 ° C. for 2 hours. Subsequently, after a large amount of argon gas was flowed to quench the cooling, 830-
The temperature was changed in increments of 5 ° C. between 880 ° C., aging treatment was performed for 8 hours at each temperature, and grinding and magnetization were performed to obtain a sintered permanent magnet. The magnetic characteristics of each sintered permanent magnet were measured with a direct current magnetization measuring device manufactured by Toei Industry Co., Ltd. The results are shown in Table 2 and FIG.

[0030]

[Comparative Example 1] A columnar grain shape and a dendrite shape were obtained in the same manner as in Example 1 except that the metal mixture having the same composition as in Example 1 was formed into a slab having a thickness of 40 mm by a conventional die casting method. The dendrite primary arm interval was measured, and the X-ray orientation degree f value was calculated. The results are shown in Table 1. Then, the obtained ingot was formed into a powder compact in the same manner as in Example 1, followed by sintering, aging treatment, grinding and magnetization treatment to obtain a sintered permanent magnet. The magnetic property results are shown in Table 2 and FIG.

[0031]

[Table 1]

[0032]

[Table 2]

[0033]

Example 2 Sm 24.5 parts by weight, Co 47.5 parts by weight, Fe 21.0 parts by weight, Cu 5.0 parts by weight and Zr
Using a device similar to that of Example 1, 2.0 parts by weight of the metal mixture was used, and the degree of supercooling was 150 ° C. and the cooling rate was 1000 to 20.
It was cast into a strip-shaped ingot having a thickness of 0.3 mm under the condition of 00 ° C / sec. With respect to the obtained strip-shaped ingot, the shape of columnar grains and the dendrite primary arm spacing were measured in the same manner as in Example 1, and the X-ray orientation degree f value was calculated. The results are shown in Table 3. Next, the strip-shaped ingot was subjected to solution treatment at 1150 ° C. in an argon stream in a vacuum heating furnace, and then rapidly cooled in the argon stream. A sample was prepared by changing the solution treatment time from 0 to 20 hours, and all of them were subjected to 86
Aged at 5 ° C. for 8 hours. At this time, the optimum solution time is 4
The size of the columnar crystals when the time was taken was measured. The results are shown in Table 3.
Shown in.

Next, each sample was ground to an average particle size of 30 μm, 2% by volume of epoxy resin was added, mixed and kneaded, and then 10 K.
After orienting with an applied magnetic field of Oe, pressure molding is performed,
Further, it was ground and magnetized to obtain a bonded permanent magnet. The magnetic characteristics of the obtained bonded permanent magnet were measured in the same manner as in Example 1. The results are shown in Table 4 and FIG.

After solution treatment for 4 hours, which is the optimum solution treatment time, the temperature is changed by 5 ° C. between 840 and 880 ° C., aging treatment is carried out for 8 hours at each temperature, and then pulverization is carried out in the same manner as described above. The epoxy resin was mixed and kneaded, oriented and molded, and then ground and magnetized to prepare a bonded permanent magnet. The magnetic characteristics of each of the obtained bonded permanent magnets were measured in the same manner as in Example 1. The results are shown in Table 5 and FIG.

[0036]

Comparative Example 2 A metal mixture having the same composition as in Example 2 was cast by the die casting method in the same manner as in Comparative Example 1 to obtain a 40 mm thick ingot. With respect to the obtained ingot, the shape of columnar crystal grains and the spacing between dendrite primary arms were measured in the same manner as in Example 1, and the X-ray orientation degree f value was calculated. The results are shown in Table 3. Then, in the same manner as in Example 2, a sample was prepared by changing the solution treatment time from 0 to 20 hours, and all the ingots were simultaneously aged at 865 ° C. for 8 hours. At this time, the size of the columnar crystals was measured when the optimum solution time was 16 hours. The results are shown in Table 3.

Next, each sample was treated in the same manner as in Example 2 to obtain a bonded permanent magnet. The magnetic characteristics of the obtained bonded permanent magnet were measured in the same manner as in Example 1. The results are shown in Table 4.
And shown in FIG.

After solution treatment for 16 hours, which is the optimum solution treatment time, the temperature was changed by 5 ° C between 840 and 880 ° C, and the aging treatment was performed for 8 hours at each temperature.
Bond permanent magnets were prepared in the same manner as in. The magnetic characteristics of each of the obtained bonded permanent magnets were measured in the same manner as in Example 1. The results are shown in Table 5 and FIG.

[0039]

[Table 3]

[0040]

[Table 4]

[0041]

[Table 5]

[0042]

Examples 3 to 6 The composition of the metal mixture was Sm 24.5 parts by weight, Co 47.4 parts by weight, Fe 21.0 parts by weight, Cu.
5.0 parts by weight, Zr 2.0 parts by weight and V 0.10 parts by weight (Example 3), Sm 24.5 parts by weight, Co 47.45 parts by weight, Fe 21.0 parts by weight, Cu 5.0 parts by weight, Zr
2.0 parts by weight and Si 0.05 parts by weight (Example 4), S
m24.5 parts by weight, Co47.4 parts by weight, Fe21.0
Parts by weight, Cu 5.0 parts by weight, Zr 2.0 parts by weight and Ti
0.10 parts by weight (Example 5) or Sm24.5 parts by weight,
Co 47.45 parts by weight, Fe 21.0 parts by weight, Cu 5.
It was cast into a strip ingot having a thickness of 0.3 mm in the same manner as in Example 2 except that 0 parts by weight, 2.0 parts by weight of Zr, and 0.05 parts by weight of Bi (Example 6) were used instead. With respect to the obtained strip-shaped ingot, the shape of columnar grains and the dendrite primary arm spacing were measured in the same manner as in Example 1, and the X-ray orientation degree f value was calculated. The results are shown in Table 6.

Next, the strip-shaped ingot was subjected to solution treatment at 1150 ° C. for 4 hours in an argon stream in a vacuum heating furnace, and then rapidly cooled in the argon stream. Subsequently, after aging treatment at 855 ° C. for 8 hours, pulverization, epoxy resin mixing and kneading, magnetic field orientation, pressure molding were performed in the same manner as in Example 2, and further grinding and magnetization treatment were performed to obtain a bonded permanent magnet. . The magnetic characteristics of the obtained bonded permanent magnet were measured in the same manner as in Example 1. The results are shown in Table 7.

[0044]

Comparative Example 3 A metal mixture having the same composition as in Example 2 was cast by a die casting method in the same manner as in Comparative Example 1 to obtain a 40 mm thick ingot. With respect to the obtained ingot, the shape of columnar crystal grains and the spacing between dendrite primary arms were measured in the same manner as in Example 1, and the X-ray orientation degree f value was calculated. The results are shown in Table 6. Then, the ingot is heated to a temperature of 1150 ° C., 16
A bond permanent magnet was obtained in the same manner as in Example 3 except that the solution treatment was performed for 8 hours and then the aging treatment was performed at 865 ° C. for 8 hours.
The magnetic characteristics of the obtained bonded permanent magnet were measured in the same manner as in Example 1. The results are shown in Table 7.

[0045]

[Table 6]

[0046]

[Table 7]

[Brief description of drawings]

FIG. 1 is a scanning electron micrograph for measuring a dendrite primary arm interval of a strip ingot prepared in Example 1.

2 is a scanning electron micrograph for measuring the columnar grain shape of the strip-shaped ingot prepared in Example 1. FIG.

FIG. 3 is a graph showing the relationship between aging treatment and magnet characteristics in Example 1 and Comparative Example 1.

FIG. 4 is a graph showing the relationship between aging treatment and magnet characteristics in Example 2 and Comparative Example 2.

FIG. 5 is a graph showing the relationship between aging treatment and magnet characteristics in Example 2 and Comparative Example 2.

─────────────────────────────────────────────────── ─── Continuation of the front page (56) Reference JP-A-6-128703 (JP, A) JP-A-4-371555 (JP, A) JP-A-4-308054 (JP, A) JP-A-5- 295489 (JP, A) JP-A-3-247729 (JP, A) (58) Fields investigated (Int.Cl. ⁷ , DB name) C22C 19/07 H01F 1/04-1/08

Claims (7)

(57) [Claims] 1. A rare earth metal containing samarium (Sm) in an amount of 50% by weight or more, 20 to 30% by weight, and iron (Fe), 10 to 25.
% By weight, 2 to 7% by weight of copper (Cu), zirconium (Z
r) A permanent magnet material whose main component is an alloy composition consisting of 0.5 to 4% by weight and the balance of cobalt (Co), and the material has a minor axis length of 10 to 200 μm and a major axis length of 50 to 50.
A crystal having a grain structure of 0 μm in an amount of 90% by volume or more in the crystal structure and having a dendrite primary arm which is a substructure of the columnar grain and has an interval of 0.5 to 20 μm.
X-ray orientation degree f that includes 0% by volume or more and is in accordance with the following mathematical formula 1
A Sm—Co based permanent magnet material having a value of f ≧ 80. [Equation 1] 2. The permanent magnet material further comprises titanium (T
i), bismuth (Bi), niobium (Nb), chromium (Cr),
Tungsten (W), Aluminum (Al), Germanium
(Ge), silicon (Si), nickel (Ni), vanadium
(V), tantalum (Ta), molybdenum (Mo), manganese
(Mn), antimony (Sb), tin (Sn) or a mixture thereof is contained in an amount of 3% by weight or less.
The Sm-Co based permanent magnet material described. 3. The method for producing an Sm—Co based permanent magnet material according to claim 1, wherein the rare earth metal containing 50% by weight or more of samarium (Sm) is 20 to 30% by weight, and the iron (Fe) is 10.
˜25% by weight, copper (Cu) 2 to 7% by weight, zirconium (Zr) 0.5 to 4% by weight, and cobalt (Co) balance as the main component of the alloy melt, and the single roll method is used. By supercooling degree of 10 to 500 ° C. and cooling rate of more than 500 ° C./sec and 10,000 ° C./sec or less, it is possible to uniformly solidify and cast into a strip of 0.1 to 0.7 mm in thickness. A method for producing a characteristic Sm-Co based permanent magnet material. 4. A Sm—Co based sintered permanent magnet obtained by using the Sm—Co based permanent magnet material according to claim 1 as a raw material. 5. A method for producing a Sm—Co based sintered permanent magnet according to claim 4, wherein the Sm—Co based permanent magnet material according to claim 1 is pulverized and then compression molded in a magnetic field. Sintering at 1000 to 1250 ° C. for 1 to 2 hours in a non-oxidizing atmosphere, then select a set temperature from a temperature range of 800 to 900 ° C., control at the set temperature ± 5 ° C., and perform aging treatment for 5 to 10 hours. A method for producing an Sm-Co based sintered permanent magnet, comprising: 6. An Sm-C obtained by using, as a raw material, the Sm-Co based permanent magnet material according to claim 1 and a resin of 1 to 3% by volume.
o type bond permanent magnet. 7. A method for producing Sm-Co based bonded permanent magnet according to claim 6, the Sm-Co based permanent magnet material according to claim 1, in a non-oxidizing atmosphere 1000-1
After heat solution treatment at 200 ° C. for 0.1 to 5 hours, 80
Select a set temperature from a temperature range of 0 to 900 ° C., control the set temperature to ± 5 ° C., and perform aging treatment for 5 to 10 hours,
Then, the powder is pulverized to obtain a magnet powder having a particle size of 10 to 30 μm, and the magnet powder and a resin of 1 to 3% by volume are mixed and kneaded, and the mixture is molded in a magnetic field. Manufacturing method.