JPH0368743A - Fe-based sintered magnetic core material and its manufacturing method - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION Technical Field of the Invention The present invention relates to a Fe-based sintered magnetic core material and a method for producing the same, and more particularly to a Fe-based sintered magnetic core for high frequency use having high saturation magnetic flux density and excellent soft magnetic properties. Regarding materials and their manufacturing methods.

Technical background of the invention and its problems As a magnetic core material used in place of the iron core of transformers and motors, a large magnetic flux density is immediately maintained even with a small applied magnetic field, and the area enclosed by the hysteresis loop is small, making it suitable for practical use. Materials with low power loss when subjected to
A so-called soft magnetic material is used.

Conventionally, as such soft magnetic materials, permalloy alloys such as molybdenum permalloy and hard permalloy, silicon steel plates, ferrite, Fe-based amorphous alloys, Co-based amorphous alloys, etc. have been mainly used. However, although permalloy alloys, Co-based amorphous alloys, and ferrites have excellent soft magnetic properties such as magnetic permeability, they have low saturation magnetic flux density, and silicon steel sheets and Fe-based amorphous alloys have high saturation magnetic flux density. The soft magnetic properties at high frequencies are inferior to those of permalloy alloys, Co-based amorphous alloys, ferrites, and the like. In particular, Fe-metalloid amorphous alloys (Fe
SiB-based, FePC-based, etc.) have large saturation magnetostriction, and Fe-transition metal-based amorphous alloys (F e Z r
Because the Curie temperature of the systems (e.g., magnetic core materials) is low, near room temperature, good soft magnetic properties were not achieved in any of the systems, and it could not be said that they had sufficient properties as magnetic core materials.

For this reason, it has been desired to develop a magnetic core material for high frequencies that has both good soft magnetic properties and high saturation magnetic flux density.

Purpose of the Invention The present invention has been made in view of the above-mentioned prior art, and has an object to provide a high-frequency Fe-based sintered magnetic core material having high saturation magnetic flux density and excellent soft magnetic properties. There is.

Summary of the Invention In order to achieve the above object, the Fe-based sintered magnetic core material according to the present invention has the following formula: 1-a a 100-x-y Mx Ny
M is TtsZr5HfSVSNbSTa, Cr.

N is at least one element selected from Mo, W, and Mn; N is at least one element selected from C and B; Y is composed of a magnetic component in which a: 0.2 or less x: 2 to 20 y: 2 to 20, or the magnetic component further contains a sintering aid, and Fe It is characterized in that at least a portion of the base sintered magnetic core material is crystallized. Further, in the present invention, the crystallinity of the Fe-based sintered magnetic core material is 10 to 100%.
It is preferable that

Further, the method for manufacturing the Fe-based sintered magnetic core material according to the present invention is performed using the formula '(FeS'a)100-+t-y Mx "y
-a, M is Tis Zr, Hf, V, Nb5Ta, Cr, M
o5W, is at least one or more elements selected from Mn, N is at least one or more elements selected from C, B, and the above a, x, y are a: o, 2 or less x: 2 to 20 y: mechanically crushing a mixed powder or alloy powder having a composition of 2 to 20, mechanically crushing the amorphous alloy powder, and forming the amorphous alloy powder into a magnetic core shape; , is characterized by including a heat treatment step of heat-treating an amorphous alloy powder compact formed into a magnetic core shape in a vacuum or an inert gas atmosphere to sinter it and crystallize at least a part of it. .

In the Fe-based sintered magnetic core material according to the present invention, Ti, Zr, Hf5V%Nb are added to the FeSi-based alloy material.
, Tas Cr, Mo, W, %Mn in a specific amount, and at least one element selected from C and B in a specific amount. , or the magnetic component further contains a sintering aid, and at least a part of the Fe-based sintered magnetic core material is crystallized,
An Fe-based sintered magnetic core material that has both high saturation magnetic flux density and good soft magnetic properties and can be used as a high-frequency magnetic core material can be obtained.

DETAILED DESCRIPTION OF THE INVENTION The Fe-based sintered magnetic core material and the manufacturing method thereof according to the present invention will be specifically described below.

The Fe-based sintered magnetic core material according to the present invention has a 100-x-y Mx Ny (Fe
It is composed of a magnetic component represented by St), or it is composed of a sintering aid in addition to the magnetic component.

In the above formula, M is Ti, Zr, or Hf5V.

At least one element selected from Nb5TaSCr, Mo, W, and Mn, among which Ti, Zr, and N
N is preferably at least one element selected from C and B, and N is preferably at least one element selected from C and B.

Further, in the above formula, a, x, and y are in the following ranges.

a: 0.2 or less, preferably 0.06 to 0.14 x: 2 to
20 preferably 6 to 12 y: 2 to 20 preferably 6 to 12 A sintering aid is added to this magnetic component as necessary to form the Fe-based sintered magnetic core material according to the present invention. In order to realize high frequency characteristics, the sintering aid is preferably an insulator, such as 5bBi.

B1Se, BiS, B1Ge, B1Te.

It is preferable to use at least one kind selected from alloy powders of 5bTeSSbSeSSnSb.

In addition, the sintering aid is based on 100 parts by weight of the magnetic component.
It is desirable that it is added in an amount of 5 to 100 parts by weight, preferably 10 to 50 parts by weight.

The Fe-based sintered magnetic core material according to the present invention has the above composition,
At least a part of it is crystallized, and the degree of crystallinity is preferably 10 to 100%, particularly preferably 60 to 100%.

Note that the crystallinity in the present invention is determined by X-ray diffraction, and specifically, it is determined by X-ray diffraction in a completely crystallized state (X-ray diffraction intensity is saturated). This is the ratio of the X-ray diffraction intensity of the magnetic core material to be measured, expressed as a percentage, based on the intensity.

As described above, the magnetic components constituting the Fe-based sintered magnetic core material according to the present invention include FeS, Ti, and Zr5 in the FeS l-based alloy material.
HfSV, Nb, Ta5Cr, Mo.

A specific amount of at least one element selected from WSMn is added, and a specific amount of at least one element selected from CSB is added.

In the Fe-based sintered magnetic core material according to the present invention, FeS
Ti, Zr, Hf, and V as l-based alloy materials.

At least one element selected from Nb, Ta5Cr, Mo, W, and Mn is contained in an amount of 2 to 20 atomic%, preferably 6 to 12 atomic% based on the total number of atoms contained in the FeSi alloy material.
At least one element selected from C and B is added in an amount of 2 to 20 atom %, preferably 6 to 12 atom %, based on the total number of atoms contained in the FeS I alloy material. The resulting Fe-based sintered magnetic core material is composed of a magnetic component or further contains a sintering aid in addition to the magnetic component, and at least a part of it is crystallized. The saturation magnetic flux density of No. 4 is increased, and soft magnetic properties such as magnetic permeability are also improved.

The Fe-based sintered magnetic core material as described above is
, a 100-x-y Mx Ny system, (F
Tis Z is manufactured using the amorphous alloy powder as a raw material after creating an amorphous alloy powder, but Tis Z is produced by adding FeS to the alloy material.
r, HfSV, Nb, Ta, Cr
, Mo.

At least one element selected from WSMn, or at least one element selected from C and B,
If the amount is less than 2 atomic % based on the total number of atoms contained in the FeSi alloy material, it tends to be difficult to create an amorphous alloy powder.

Also, if either of these exceeds 20 atomic%,
Since the content of Fe, which is a ferromagnetic component, decreases relatively, the overall saturation magnetic flux density also tends to decrease. Therefore, as mentioned above, the content of both is preferably about 2 to 20 atom %, preferably about 6 to 12 atom %.

When St is dissolved in the ferromagnetic components F and e, the magnetocrystalline anisotropy constant and magnetostriction constant of the resulting Fe-based sintered magnetic core material decrease, resulting in improved soft magnetic properties. However, as the amount of added St increases, the saturation magnetic flux density and Curie temperature decrease. Therefore, it is desirable that the value of a be 0.2 or less, preferably 0.06 to 0.14.

In addition, the Fe-based sintered magnetic core material according to the present invention can be obtained by preparing an amorphous alloy powder and then adding a sintering aid thereto as necessary.
It is manufactured by molding into a magnetic core shape, heat-treating the obtained amorphous alloy powder compact, sintering it, and crystallizing at least a part of it, but the Fe-based sintered magnetic core material after sintering The crystallinity of is 10-100%, preferably 6
It is desirable that it is 0 to 100%. When the crystallinity of the Fe-based sintered magnetic core material is within this range, excellent soft magnetic properties are imparted to the Fe-based sintered magnetic core material.

Next, a method for manufacturing the Fe-based sintered magnetic core material according to the present invention will be explained.

The Fe-based sintered magnetic core material according to the present invention can be obtained by mechanically pulverizing a mixed powder or alloy powder represented by the following composition formula, and mechanically pulverizing the amorphous alloy powder. Manufactured by a manufacturing method including a molding step of molding into a magnetic core shape, and a heat treatment step of heat-treating the amorphous alloy powder compact molded into the magnetic core shape to sinter it and crystallize at least a part of it. be done.

1-a a 100-x-y MX Ny formula: (
(Fe St) However, M is Ti, Zr, Hf, VSNbSTa.

At least one element selected from C, Mo, W, and Mn, among which T l % Z r, Nb5
Preferably, it is at least one element selected from Ta, and N is at least one element selected from C and B.

In the above formula, alXsY is in the following range.

a: o, 2 or less preferably 0.06 to 0.14x: 2
-20 preferably 6-12 y: 2-20 preferably 6-12 In order to mechanically grind the mixed powder or alloy powder having the above composition, for example, mechanical alloying method or mechanical grinding method etc. can be adopted.

This mechanical pulverization is preferably carried out in a vacuum or in an inert gas atmosphere such as argon gas or nitrogen gas to such an extent that the mixed powder or alloy powder is not oxidized during pulverization.

Note that it is possible to create amorphous alloy powder using other methods such as liquid quenching, but in the case of liquid quenching,
Since it tends to be difficult to make a high melting point metal alloy system amorphous, it is particularly preferable to employ a mechanical crushing method in the present invention.

Next, the obtained amorphous alloy powder is molded into a magnetic core shape. The molding method may be any molding method as long as it can yield a molded article in the shape of a magnetic core. Note that when forming the amorphous alloy powder into a magnetic core shape, a sintering aid can be added to the amorphous alloy powder as necessary. The sintering aid is preferably an insulator in order to realize high frequency characteristics, such as 5bBi, BISe, 818%B
It is preferable that the powder is at least one selected from alloy powders of 1Ge, B1Te5SbTe, 5bSe, and 5nsb. The sintering aid is preferably added in an amount of 5 to 100 parts by weight, preferably 10 to 50 parts by weight, per 100 parts by weight of the amorphous alloy powder.

The Fe-based sintered magnetic core material according to the present invention is obtained by heat-treating the thus obtained amorphous alloy powder compact to sinter it and crystallize at least a portion thereof. The above heat treatment is preferably carried out in a vacuum to the extent that the amorphous alloy powder is not oxidized, or in an inert gas atmosphere such as argon gas or nitrogen gas after sufficient evacuation. Heat treatment temperature is 450-600℃,
The temperature is preferably 500 to 560°C, and the heat treatment time is preferably 0.2 to 3 hours, preferably 0.5 to 1 hour. Examples of the sintering method include pressureless sintering method,
Pressure sintering method (HP sintering method), hot isostatic pressure sintering method (H
For example, ordinary sintering methods such as IP sintering method) are exemplified.

The degree of crystallinity of the Fe-based sintered magnetic core material according to the present invention depends on the heat treatment temperature, heat treatment time, amount and type of sintering aid, etc., but is 10 to 100%, preferably 60 to 100%.
It is desirable that By performing heat treatment under such conditions, the amorphous alloy powder is sintered and partially or completely crystallized to produce the Fe-based sintered magnetic core material according to the present invention.

The Fe-based sintered magnetic core material according to the present invention has both a high saturation magnetic flux density and good soft magnetic properties, and can also be used as a high frequency magnetic core material.

Further, the Fe-based sintered magnetic core material according to the present invention has a small area surrounded by a hysteresis curve and has low power loss when put into practical use, so it can be preferably used in place of iron cores in transformers, motors, etc.

As described in detail, the Fe-based sintered magnetic core material according to the present invention has a FeSi-based alloy material with Tt.

Z", Hf, VSNbSTas Crs Mo, W.

A sintering aid is added as necessary to an amorphous alloy powder to which a specific amount of at least one element selected from Mn and at least one element selected from C and B is added. After adding, this is formed into a magnetic core shape, and the obtained amorphous alloy powder compact or amorphous alloy powder-containing compact is heat treated to sinter and crystallize at least a part of it. This makes it possible to provide an Fe-based sintered magnetic core material that has both high saturation magnetic flux density and excellent soft magnetic properties and is preferably used for high-frequency magnetic core materials.

[Examples] Hereinafter, the present invention will be further explained with reference to Examples, but the present invention is not limited to these Examples.

Example 1 FeSiC alloy powder with an average particle size of 10 μm has an average particle size of 5 μm.
The mixed powder obtained by adding μm Ti powder was amorphized by a mechanical alloying method in an argon gas atmosphere using a steel ball stirring type impact mill. Mechanical alloying was carried out at a rotational speed of 200 rpm for 25 hours. After adding 20 parts by weight of SbBi alloy powder as a sintering aid to the obtained amorphous alloy powder based on 100 parts by weight of the amorphous alloy powder, it was formed into a magnetic core shape and heated in an argon gas atmosphere. , and heat treated at 550° C. for 1 hour to produce a Fe-based sintered magnetic core material. The composition of the obtained Fe-based sintered magnetic core material was analyzed by plasma emission spectroscopy. Also measure power loss at a frequency of 100ktlz.

The measurement was carried out at a measurement magnetic field of 0.2 Tesla, and the saturation magnetic flux density was also measured. Furthermore, when the crystallinity of the obtained Fe-based sintered magnetic core material was measured by X-ray diffraction, it was found that at least a part of it was crystallized (crystallinity of 10% or more).

The results are shown in Table 1.

Examples 2-8 Zr, Hf, V, Nb instead of Ti powder.

The same operation as in Example 1 was performed except that each powder of T a % M O % W was used.

The results are shown in Table 1.

Example 9 The same operation as in Example 1 was performed except that Fe5iB alloy powder was used instead of FeSiC alloy powder.

The results are shown in Table 1.

Examples 10-16 Zr, Hf, V, Nb instead of Ti powder.

The same operation as in Example 9 was performed except that Ta, Mo, and W powders were used.

The results are shown in Table 1.

Comparative Examples 1 to 5 Silicon steel plate (FegaSt5B12
), permalloy alloy (Fe73Nb3si14Cu
Measuring the power loss of St B amorphous B10) e7B, 5 1 13.5 9 alloy, Co Fe Si B amorphous 87.5 4 16.5 12 alloy, M n -Z n ferrite, frequency 100 kHz, measuring magnetic field. The measurement was performed at 0.2 Tesla and the saturation magnetic flux density was measured.

The results are shown in Table 2.

From the above results, the Fe-based sintered magnetic core material according to the present invention is
It can be seen that this material has low power loss at high frequencies compared to conventional materials.

Claims (1)

[Claims] 1) Formula: (Fe_1_−_aSi_a)_1_0_0_
An Fe-based sintered magnetic core material having a composition represented by -_x_-_yM_xN_y, and at least a part of which is crystallized. [However, in the above formula, M is Ti, Zr, Hf, V, Nb, Ta, Cr, Mo
, W, and Mn; N is at least one element selected from C and B; and the above a, x, and y are a: 0.2 or less x: 2 to 20y: 2-20. ] 2) The crystallinity of the Fe-based sintered magnetic core material is 10 to 100.
% of the Fe-based sintered magnetic core material according to claim 1. 3) Formula: (Fe_1_−_aSi_a)_1_0_0_
-_x_yM_xN_y, M is Ti, Zr, Hf, V, Nb, Ta, Cr, Mo
, W, and Mn; N is at least one element selected from C and B; and the above a, x, and y are a: 0.2 or less x: 2 to 20 Y: A Fe-based sintered magnetic core material comprising a magnetic component of 2 to 20 and a sintering aid, and at least a part of which is crystallized. 4) The crystallinity of the Fe-based sintered magnetic core material is 10 to 100.
% of the Fe-based sintered magnetic core material according to claim 3. 5) The sintering aid according to any one of claims 3 and 4, wherein the sintering aid is added at a ratio of 5 to 100 parts by weight to 100 parts by weight of the magnetic component. Fe-based sintered magnetic core material described in . 6) The sintering aid is SbBi, BiSe, BiS, Bi
6. The Fe-based sintered magnetic core material according to claim 3, wherein the Fe-based sintered magnetic core material is at least one selected from alloy powders of Ge, BiTe, SbTe, SbSe, and SnSb. 7) Formula: (Fe_1_−_aSi_a)_1_0_0_
-_x_-_yM_xN_y, M is Ti, Zr, Hf, V, Nb, Ta, Cr, Mo
, W, and Mn; N is at least one element selected from C and B; and the above a, x, and y are a: 0.2 or less x: 2 to 20y: A step of mechanically crushing a mixed powder or alloy powder having a composition of 2 to 20 to create an amorphous alloy powder, and a forming step of shaping the obtained amorphous alloy powder into a magnetic core shape. and a heat treatment step of heat-treating the amorphous alloy powder compact formed into the shape of a magnetic core in a vacuum or an inert gas atmosphere to sinter it and crystallize at least a part of it. A method for producing a Fe-based sintered magnetic core material. 8) The Fe-based sintered magnetic core according to claim 7, wherein in the forming step, 5 to 100 parts by weight of a sintering aid is added to 100 parts by weight of the amorphous alloy powder. Method of manufacturing the material. 9) The sintering aid is SbBi, BiSe, BiS, Bi
9. The method for producing a Fe-based sintered magnetic core material according to claim 8, wherein the material is at least one selected from alloy powders of Ge, BiTe, SbTe, SbSe, and SnSb.