JP4618557B2 - Soft magnetic alloy compact and manufacturing method thereof - Google Patents
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- 229910001004 magnetic alloy Inorganic materials 0.000 title claims description 55
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 239000000843 powder Substances 0.000 claims description 185
- 229910000808 amorphous metal alloy Inorganic materials 0.000 claims description 155
- 239000002245 particle Substances 0.000 claims description 67
- 230000009477 glass transition Effects 0.000 claims description 43
- 238000000465 moulding Methods 0.000 claims description 39
- 239000011248 coating agent Substances 0.000 claims description 32
- 238000000576 coating method Methods 0.000 claims description 32
- 239000012212 insulator Substances 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 18
- 238000009826 distribution Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 239000000243 solution Substances 0.000 description 14
- 229910004298 SiO 2 Inorganic materials 0.000 description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 13
- 229910052814 silicon oxide Inorganic materials 0.000 description 13
- 229910045601 alloy Inorganic materials 0.000 description 11
- 239000000956 alloy Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 239000000696 magnetic material Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 239000011162 core material Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 230000004907 flux Effects 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 230000020169 heat generation Effects 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000002923 metal particle Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 229910000851 Alloy steel Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000000113 differential scanning calorimetry Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000009689 gas atomisation Methods 0.000 description 2
- 238000001513 hot isostatic pressing Methods 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910001337 iron nitride Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000013526 supercooled liquid Substances 0.000 description 1
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- Powder Metallurgy (AREA)
- Soft Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Description
本発明は、軟磁性合金圧密体及びその製造方法に係り、更に詳細には、例えば電気自動車やハイブリッド車等のモーターの磁心として好適に用いることができる軟磁性合金圧密体及びその製造方法に関する。 The present invention relates to a soft magnetic alloy compact and a method for manufacturing the same, and more particularly to a soft magnetic alloy compact that can be suitably used as a magnetic core of a motor of, for example, an electric vehicle or a hybrid vehicle.
一般に、金属軟磁性材料は、高い飽和磁束密度と高透磁率とを有するが、電気抵抗率が低いため、渦電流損失が大きいことが知られている。一方、金属酸化物軟磁性材料は、金属軟磁性材料と比較して電気抵抗率は高く、渦電流損失は小さいが、飽和磁束密度が不十分であることが知られている。
このような事情から、双方の欠点を無くした軟磁性材料として、高い飽和磁束密度と高い電気抵抗率とを併有する複合軟磁性材料が開発されている。
In general, a metal soft magnetic material has a high saturation magnetic flux density and a high magnetic permeability, but is known to have a large eddy current loss because of its low electrical resistivity. On the other hand, it is known that the metal oxide soft magnetic material has higher electrical resistivity and smaller eddy current loss than the metal soft magnetic material, but the saturation magnetic flux density is insufficient.
Under such circumstances, a composite soft magnetic material having both a high saturation magnetic flux density and a high electric resistivity has been developed as a soft magnetic material that eliminates both drawbacks.
例えば、常温での成形が容易な金属については、表面を絶縁物で被覆した金属粒子を冷間プレス成形し、歪取り熱処理を実施した製品が実用化されている。
また、常温での成形が困難な合金については、絶縁性のバインダーと金属粒子を混合して射出成形やプレス成形する製品が実用化されている。
しかしながら、これらは密度が低く、良好な磁気特性が得られないという問題があり、熱間成形による高密度化と絶縁膜の絶縁性維持が望まれている。
For example, for metals that can be easily molded at room temperature, products in which metal particles whose surfaces are coated with an insulating material are cold press-molded and subjected to strain relief heat treatment have been put into practical use.
For alloys that are difficult to mold at room temperature, products that are injection molded or press molded by mixing an insulating binder and metal particles have been put to practical use.
However, these have a problem that the density is low and good magnetic properties cannot be obtained, and it is desired to increase the density by hot forming and maintain the insulating properties of the insulating film.
また、近年、モーター等の電気製品の小型化に伴い、これらの電気製品内の各種素子に用いられる磁心材料も小型化且つ高性能化が要求されており、従来用いられているフェライトなどの金属酸化物に替わって、磁束密度が高い鉄（Ｆｅ）にケイ素（Ｓｉ）やコバルト（Ｃｏ）、ニッケル（Ｎｉ）を含有させた高合金鋼を利用することが望まれている。
しかしながら、これら高合金鋼は金属であるため、上述したように金属酸化物と比較して電気抵抗率が低く、使用時の発熱量が多いという問題があり、モーターに使用した場合には、発熱によるロスが生じ、効率が低下することが知られている。
In recent years, along with miniaturization of electric products such as motors, magnetic core materials used for various elements in these electric products are also required to be miniaturized and high performance, and conventionally used metals such as ferrite. Instead of oxides, it is desired to use high alloy steel in which silicon (Si), cobalt (Co), and nickel (Ni) are contained in iron (Fe) having a high magnetic flux density.
However, since these high alloy steels are metals, there is a problem that the electrical resistivity is low as compared with metal oxides as described above, and there is a large amount of heat generated during use. It is known that the loss due to this occurs and the efficiency decreases.
かかる問題点を克服するために、軟磁性金属粒子に高抵抗軟磁性物質を被覆してプラズマ活性化焼結する製造方法が提案されている（特許文献１参照。）。
また、無機絶縁物を被覆した金属粉末を熱間成型する製造方法が提案されている（特許文献２参照。）。
更に、金属ガラス粉末に絶縁処理を施し、加圧成形して得られる圧粉磁心が提案されている（特許文献３参照。）。
In addition, a manufacturing method has been proposed in which metal powder coated with an inorganic insulator is hot-molded (see Patent Document 2).
Furthermore, a powder magnetic core obtained by subjecting metal glass powder to insulation treatment and press molding has been proposed (see Patent Document 3).
しかしながら、特許文献１に記載の従来技術においては、高抵抗軟磁性物質として各種フェライトや窒化鉄などが用いられており、これらは高温での焼結が可能である反面、必ずしも十分な電気絶縁性が得られないという問題があった。 However, in the prior art described in Patent Document 1, various ferrites, iron nitrides, and the like are used as high-resistance soft magnetic materials, which can be sintered at high temperatures, but are not necessarily sufficiently electrically insulating. There was a problem that could not be obtained.
また、特許文献２に記載の従来技術においては、絶縁皮膜として合金粉末より酸化物が不安定なものが使用されており、成形時に合金粉末が酸化され、磁気特性や絶縁性が劣化する問題が生じるおそれがあった。 Further, in the prior art described in Patent Document 2, an insulating film whose oxide is more unstable than the alloy powder is used, and the alloy powder is oxidized at the time of molding, and there is a problem that the magnetic properties and the insulation are deteriorated. There was a risk of it occurring.
更に、現状の高合金鋼は強度が高いため、成形温度が低い場合には緻密化が困難である一方、成形温度が高い場合には被覆した絶縁材が熱間成形中に合金と反応したり皮膜自体が変質して絶縁性を劣化させるという問題があった。
このような問題に対し、特許文献３に記載の従来技術においては、金属ガラスを用いることにより低温での圧密化に成功しているが、用いる原料粉末の配合により密度がばらついたり、皮膜同士の密着性が悪く十分な強度が得られない等の問題が生じることがあった。
Furthermore, because the current high alloy steel has high strength, it is difficult to densify when the forming temperature is low, whereas when the forming temperature is high, the coated insulating material may react with the alloy during hot forming. There was a problem that the coating itself was altered and the insulation was deteriorated.
For such problems, in the prior art described in Patent Document 3, the metal glass is used to achieve consolidation at a low temperature, but the density varies depending on the composition of the raw material powder used. In some cases, the adhesiveness is poor and sufficient strength cannot be obtained.
本発明は、このような従来技術の有する課題に鑑みてなされたものであり、その目的とするところは、例えば電気自動車やハイブリッド車等のモーターの磁心として好適に用いることができる軟磁性合金圧密体及びその製造方法を提供することにある。 The present invention has been made in view of such problems of the prior art, and an object thereof is to soften a soft magnetic alloy that can be suitably used as a magnetic core of a motor of, for example, an electric vehicle or a hybrid vehicle. It is in providing a body and its manufacturing method.
本発明者らは、上記目的を達成するために鋭意研究を重ねた。
まず、従来から電気抵抗の高抵抗化の指標として一般的に用いられている直流抵抗と、渦電流による発熱量の相関について調査した。
その結果、これらは一対一の相関関係にはなく、電気抵抗が劣っていても渦電流による発熱が抑制される場合があることを見出した。これは、直流抵抗が測定器両端子間の直線的な電気の導通に対する指標であるのに対し、渦電流による発熱量は、交番磁場方向に垂直な断面における環状の電気の導通に支配されるものであるためと推定される。
したがって、材料組織において、粒子が環状に短絡している状態を阻止するか又は可能な限り曲率が小さい環状の短絡に抑制することが渦電流による発熱を抑制するために効果的な手法であると推測される。
そこで、材料組織と渦電流による発熱量の相関について調査した。
その結果、絶縁物で被覆した粉末と被覆していない粉末とを混合しても、その配合比（体積率）によっては、電気抵抗が劣化しても渦電流による発熱などいわゆる渦電流損失が増大しない範囲があることを見出し、本発明を完成するに至った。
更に、この絶縁物で被覆していない粉末を所定の配合比（体積率）で混在させることによって、強度が向上することも見出した。
The inventors of the present invention have made extensive studies to achieve the above object.
First, we investigated the correlation between DC resistance, which has been conventionally used as an index for increasing electrical resistance, and the amount of heat generated by eddy current.
As a result, they found that they are not in a one-to-one correlation, and that heat generation due to eddy currents may be suppressed even if the electrical resistance is inferior. This is because the direct current resistance is an indicator for linear electrical conduction between both terminals of the measuring instrument, whereas the amount of heat generated by the eddy current is governed by annular electrical conduction in a cross section perpendicular to the alternating magnetic field direction. It is presumed that it is a thing.
Therefore, in the material structure, preventing the state where the particles are short-circuited in the ring or suppressing the short-circuit in the ring as small as possible is an effective technique for suppressing heat generation due to the eddy current. Guessed.
Therefore, the correlation between the material structure and the amount of heat generated by the eddy current was investigated.
As a result, even if the powder coated with the insulator and the powder not coated are mixed, depending on the mixing ratio (volume ratio), so-called eddy current loss such as heat generation due to eddy current increases even if the electrical resistance deteriorates. The present inventors have found that there is a range that does not, and have completed the present invention.
Furthermore, it has also been found that the strength is improved by mixing the powder not coated with the insulator at a predetermined blending ratio (volume ratio).
即ち、本発明の軟磁性合金圧密体は、少なくとも１種の非晶質合金粉末を加圧成形処理して成り、該非晶質合金粉末は、該非晶質合金粉末の全体積を基準として、５０〜９９体積％の非晶質合金粉末がその表面に絶縁物被膜を有しており、且つ１〜５０体積％の非晶質合金粉末がその表面に絶縁物被膜を有していない軟磁性合金圧密体であって、該非晶質合金粉末は、異なる粒度分布を有する該表面に絶縁物被膜を有していない非晶質合金粉末Ａと該表面に絶縁物被膜を有している非晶質合金粉末Ｂとから成り、該非晶質合金粉末Ａの平均粒径（ｒ Ａ ）と該非晶質合金粉末Ｂの平均粒径（ｒ Ｂ ）とが次式（１）
ｒ Ａ ／ｒ Ｂ ＜１…（１）
の関係を満足すると共に、該非晶質合金粉末Ｂのガラス転移温度を基準として、該非晶質合金粉末Ａのガラス転移温度が１０Ｋ以上低いことを特徴とする。
また、本発明の軟磁性合金圧密体は、少なくとも１種の非晶質合金粉末を加圧成形処理して成り、該非晶質合金粉末は、該非晶質合金粉末の全体積を基準として、５０〜９９体積％の非晶質合金粉末がその表面に絶縁物被膜を有しており、且つ１〜５０体積％の非晶質合金粉末がその表面に絶縁物被膜を有していない軟磁性合金圧密体であって、該非晶質合金粉末は、異なる粒度分布を有する該表面に絶縁物被膜を有していない非晶質合金粉末Ａと該表面に絶縁物被膜を有している非晶質合金粉末Ｂとから成り、該非晶質合金粉末Ａの平均粒径（ｒ Ａ ）と該非晶質合金粉末Ｂの平均粒径（ｒ Ｂ ）とが次式（２）
０．０５≦ｒ Ａ ／ｒ Ｂ ≦０．３…（２）
の関係を満足すると共に、該非晶質合金粉末Ｂのガラス転移温度を基準として、該非晶質合金粉末Ａのガラス転移温度が１０Ｋ以上低いことを特徴とする。
That is, the soft magnetic alloy compact of the present invention is formed by press-molding at least one amorphous alloy powder, and the amorphous alloy powder is 50% on the basis of the total volume of the amorphous alloy powder. Soft magnetic alloy in which ~ 99% by volume of amorphous alloy powder has an insulating film on its surface and 1-50% by volume of amorphous alloy powder has no insulating film on its surface The amorphous alloy powder, which is a compacted body, includes an amorphous alloy powder A having a different particle size distribution and having no insulator coating on the surface, and an amorphous alloy having an insulator coating on the surface The average particle size (r A ) of the amorphous alloy powder A and the average particle size (r B ) of the amorphous alloy powder B are expressed by the following formula (1).
r A / r B <1 (1)
And the amorphous alloy powder A has a glass transition temperature lower by 10 K or more on the basis of the glass transition temperature of the amorphous alloy powder B.
Further, the soft magnetic alloy compact of the present invention is formed by press-molding at least one amorphous alloy powder, and the amorphous alloy powder is 50% on the basis of the total volume of the amorphous alloy powder. Soft magnetic alloy in which ~ 99% by volume of amorphous alloy powder has an insulating film on its surface and 1-50% by volume of amorphous alloy powder has no insulating film on its surface The amorphous alloy powder, which is a compacted body, includes an amorphous alloy powder A having a different particle size distribution and having no insulator coating on the surface, and an amorphous alloy having an insulator coating on the surface The average particle size (r A ) of the amorphous alloy powder A and the average particle size (r B ) of the amorphous alloy powder B are expressed by the following formula (2).
0.05 ≦ r A / r B ≦ 0.3 (2)
And the amorphous alloy powder A has a glass transition temperature lower by 10 K or more on the basis of the glass transition temperature of the amorphous alloy powder B.
また、本発明の軟磁性合金圧密体の製造方法は、上記本発明の軟磁性合金圧密体を製造する方法であって、下記の工程（１）及び（２）を含むことを特徴とする。
（１）非晶質合金粉末の全体積を基準として、非晶質合金粉末の表面に絶縁物被膜を有していない粉末及び非晶質合金粉末の表面に絶縁物被膜を有している粉末を、それぞれの含有率が１〜５０体積％及び５０〜９９体積％となるように混合する工程
（２）（１）工程で得られた粉末を加圧成形処理する工程
Moreover, the manufacturing method of the soft magnetic alloy compact of this invention is a method of manufacturing the said soft magnetic alloy compact of this invention, Comprising: The following processes (1) and (2) are included, It is characterized by the above-mentioned.
(1) Based on the total volume of the amorphous alloy powder, a powder that does not have an insulator coating on the surface of the amorphous alloy powder and a powder that has an insulator coating on the surface of the amorphous alloy powder Step of mixing the powders obtained in steps (2) and (1) so that the respective contents are 1 to 50% by volume and 50 to 99% by volume
本発明によれば、非晶質合金粉末の全体積を基準として、非晶質合金粉末の表面に絶縁物被膜を有していない粉末及び非晶質合金粉末の表面に絶縁物被膜を有している粉末を、それぞれの含有率が１〜５０体積％及び５０〜９９体積％となるように混合し、得られた粉末を加圧成形処理することなどとしたため、電気自動車やハイブリッド車等のモーターの磁心として好適に用いることができる軟磁性合金圧密体及びその製造方法を提供することができる。 According to the present invention, on the basis of the total volume of the amorphous alloy powder, the surface of the amorphous alloy powder does not have an insulator coating and the surface of the amorphous alloy powder has an insulator coating. Are mixed so that the respective contents are 1 to 50% by volume and 50 to 99% by volume, and the obtained powder is subjected to pressure molding treatment, etc. It is possible to provide a soft magnetic alloy compact that can be suitably used as a magnetic core of a motor and a method for manufacturing the same.
以下、本発明の軟磁性合金圧密体について詳細に説明する。
上述の如く、本発明の軟磁性合金圧密体は、少なくとも１種の非晶質合金粉末を加圧成形処理して成るものである。
かかる非晶質合金粉末は、当該非晶質合金粉末の全体積を基準として、５０〜９９体積％の非晶質合金粉末がその表面に絶縁物被膜を有しており、且つ１〜５０体積％の非晶質合金粉末がその表面に絶縁物被膜を有していない。
このような構成とすることにより、優れた強度を有し、且つ渦電流損失を低減し得る軟磁性合金圧密体となる。
Hereinafter, the soft magnetic alloy compact of the present invention will be described in detail.
As described above, the soft magnetic alloy compact of the present invention is formed by pressure-molding at least one amorphous alloy powder.
Such amorphous alloy powder has 50 to 99 volume% of amorphous alloy powder having an insulating film on its surface, and 1 to 50 volume based on the total volume of the amorphous alloy powder. % Amorphous alloy powder does not have an insulator coating on its surface.
By adopting such a configuration, a soft magnetic alloy consolidated body having excellent strength and capable of reducing eddy current loss is obtained.
表面に絶縁物被膜を有する非晶質合金粉末の割合を５０体積％未満とする、換言すれば表面に絶縁物被膜を有していない非晶質合金粉末の割合を５０体積％超とすると、渦電流損失の低減効果が損われる場合が著しく増加する一方で、表面に絶縁物被膜を有する非晶質合金粉末の割合を９９体積％超とする、換言すれば表面に絶縁物被膜を有していない非晶質合金粉末の割合を１体積％未満とすると、所望する強度が得られない。
これは、絶縁物被膜の膜厚が不必要に厚い場合には所望の強度が得られず、所望の強度を得るためには膜厚を薄く保つことが有効であり、上述の如く絶縁物被膜を有していない非晶質合金粉末を混在させることにより、絶縁物被膜を有していない非晶質合金粉末の界面における絶縁物被膜の膜厚は、絶縁物被膜を有している非晶質合金粉末同士の界面における絶縁物被膜の膜厚の半分になり、好適な膜厚が形成され易いためと考えられる。また、強度をより向上させるためには、表面に絶縁物被膜を有していない非晶質合金粉末の割合を５体積％以上とすることが好ましく、１０体積％以上とすることが更に好ましい。
When the ratio of the amorphous alloy powder having an insulating film on the surface is less than 50% by volume, in other words, the ratio of the amorphous alloy powder having no insulating film on the surface is more than 50% by volume, While the effect of reducing eddy current loss is significantly increased, the ratio of amorphous alloy powder having an insulating film on the surface is more than 99% by volume, in other words, having an insulating film on the surface. If the proportion of the amorphous alloy powder that is not present is less than 1% by volume, the desired strength cannot be obtained.
This is because the desired strength cannot be obtained when the thickness of the insulating coating is unnecessarily thick, and it is effective to keep the thickness thin in order to obtain the desired strength. By mixing the amorphous alloy powder that does not have an insulating film, the thickness of the insulating film at the interface of the amorphous alloy powder that does not have the insulating film becomes amorphous. This is because the film thickness is half of the thickness of the insulating coating film at the interface between the alloy powders and a suitable film thickness is easily formed. In order to further improve the strength, the ratio of the amorphous alloy powder having no insulating coating on the surface is preferably 5% by volume or more, and more preferably 10% by volume or more.
また、本発明における加圧成形処理工程は、所望の圧密体が得られれば特に限定されるものではないが、例えば従来公知のホットプレスやプラズマ放電焼結、熱間静水圧焼結（ＨＩＰ）などの方法により行なうことができる。また、処理条件は、用いる非晶質合金粉末などの組成により異なるものと考えられ、特に限定されるものではないが、例えば成形圧力は５０ＭＰａ〜９８０ＭＰａ、好ましくは１００ＭＰａ〜５００ＭＰａ、成形温度は３５０〜６００℃、好ましくは３７０〜５００℃、より好ましくは４００〜５００℃で、アルゴン（Ａｒ）などの不活性ガス雰囲気や真空中の雰囲気とすればよい。また、ホットプレス法の場合には、典型的には成形圧力２００〜６００ＭＰａ、成形温度４００〜５００℃で、０．１Ｐａ以下の真空雰囲気とすればよく、プラズマ放電焼結法の場合には、典型的には成形圧力１００〜５００ＭＰａ、成形温度４００〜５００℃で、０．１Ｐａ以下の真空雰囲気とすればよく、ＨＩＰ法の場合には、典型的には成形圧力１００ＭＰａ〜１０００ＭＰａ、成形温度４５０〜５００℃とすればよい。
なお、放電プラズマ焼結装置を用いると、適度な導電性と局所的な高電気抵抗を有するため、効率的に軟磁性合金圧密体を作製することができる。
Further, the pressure molding treatment step in the present invention is not particularly limited as long as a desired compacted body is obtained. For example, conventionally known hot press, plasma discharge sintering, hot isostatic pressing (HIP) It can be performed by such a method. The processing conditions are considered to vary depending on the composition of the amorphous alloy powder to be used and are not particularly limited. For example, the molding pressure is 50 MPa to 980 MPa, preferably 100 MPa to 500 MPa, and the molding temperature is 350 to 500. An inert gas atmosphere such as argon (Ar) or a vacuum atmosphere may be used at 600 ° C., preferably 370 to 500 ° C., more preferably 400 to 500 ° C. In the case of the hot press method, typically, a molding pressure of 200 to 600 MPa, a molding temperature of 400 to 500 ° C., and a vacuum atmosphere of 0.1 Pa or less may be used. In the case of the plasma discharge sintering method, Typically, a molding pressure of 100 to 500 MPa, a molding temperature of 400 to 500 ° C., and a vacuum atmosphere of 0.1 Pa or less may be used. In the case of the HIP method, typically, a molding pressure of 100 MPa to 1000 MPa and a molding temperature of 450 are used. What is necessary is just to set it as -500 degreeC.
In addition, when a discharge plasma sintering apparatus is used, since it has moderate electroconductivity and local high electrical resistance, a soft-magnetic alloy compact can be produced efficiently.
また、本発明においては、加圧成形処理工程の成形温度が、上記少なくとも１種の非晶質合金粉末のガラス転移温度以上であることが望ましい。
このような工程を経ない場合、即ち成形温度が含有される非晶質合金粉末のガラス転移温度未満であると、非晶質合金粉末の特徴である良好な成形性が十分に発揮されず、高い強度が得られにくい。
In the present invention, it is desirable that the molding temperature in the pressure molding treatment step is equal to or higher than the glass transition temperature of the at least one amorphous alloy powder.
When such a step is not performed, that is, when the molding temperature is lower than the glass transition temperature of the amorphous alloy powder, the good formability characteristic of the amorphous alloy powder is not sufficiently exhibited, High strength is difficult to obtain.
更に、本発明においては、加圧成形処理工程の平均プレス歪速度が、０．０００１〜１Ｓ−１であることが好ましく、より好ましくは０．００５〜０．１Ｓ−１である。
平均プレス歪速度が１Ｓ−１を超えると絶縁物被膜の変形が非晶質合金粉末の変形に追随できずに被膜の破損が大きくないし多くなり、また非晶質合金粉末の変形抵抗自体が大きくなり金型と加圧成形処理装置（例えば、プラズマ放電焼結装置。）の負担が大きくなることがある一方、平均プレス歪速度が０．０００１Ｓ−１未満のように過度に遅すぎると生産性が損われることがある。
Further, in the present invention, the average press strain rate of pressure molding step is preferably from 0.0001～1S -1, more preferably 0.005~0.1S -1.
When the average press strain rate exceeds 1S- 1 , the deformation of the insulating film cannot follow the deformation of the amorphous alloy powder, resulting in large or large damage of the film, and the deformation resistance itself of the amorphous alloy powder is large. While the burden on the die and the pressure molding processing apparatus (for example, plasma discharge sintering apparatus) may increase, if the average press strain rate is too slow, such as less than 0.0001 S −1 , productivity will be increased. May be damaged.
更にまた、本発明においては、用いる非晶質合金粉末は、その平均粒径が５〜４００μｍであることが好ましく、１０〜３００μｍであることがより好ましく、１０〜２００μｍであることが更に好ましい。
これは、一般に、軟磁性体は、保磁力が低いほど透磁率が高くなり、そして、非晶質合金粉末を用いた軟磁性合金圧密体は、非晶質合金粉末の平均粒径が５μｍより小さくなると、混在する粒径が大きい粒子との接触面積が不足し、十分な強度向上効果が得られないことがあり、４００μｍを超えると、混在する極度に粒径が大きい粒子の空隙が大きくなり、密度向上効果が得られないことがある。
Furthermore, in the present invention, the amorphous alloy powder to be used preferably has an average particle size of 5 to 400 μm, more preferably 10 to 300 μm, still more preferably 10 to 200 μm.
Generally, the soft magnetic material has a higher magnetic permeability as the coercive force is lower, and the soft magnetic alloy compact using the amorphous alloy powder has an average particle diameter of the amorphous alloy powder of more than 5 μm. If it is smaller, the contact area with the mixed particles having a large particle size may be insufficient, and a sufficient strength improvement effect may not be obtained. If the particle size exceeds 400 μm, the voids of the extremely large particles having a large particle size increase. The density improving effect may not be obtained.
ここで、「平均粒径」は、粒度分布の平均値を表したものであるが、値が過度に乖離した粒径のものが混在したものを使用すると、調製した際に所望する磁気特性が得られない（低再現性）ことがある。そこで、サイズを基準としたときに、用いた非晶質合金粉末が１種類であるとは、粒度分布のピークが１つであり、平均粒径の±２０％の範囲内に全重量の８０％以上の粉末粒径がおさまることをいい、好ましくは±１５％の範囲内に全重量の８０％以上の粉末粒径がおさまることをいう。 Here, the “average particle size” represents the average value of the particle size distribution, but when a mixture of particles having particle sizes whose values are excessively different from each other is used, the desired magnetic properties when prepared are obtained. May not be obtained (low reproducibility). Therefore, when the size is used as a reference, the single amorphous alloy powder used means that there is one peak in the particle size distribution, and the total weight is within the range of ± 20% of the average particle size. % Means that the powder particle diameter is within 80% or more of the total weight within the range of ± 15%.
なお、一般に、軟磁性合金圧密体は、内部に生成した空隙によって密度が不足すると、十分な飽和磁束密度が得られないだけでなく、その空隙の増加と共に圧密体の強度も低下する。
そこで、上述したようにガラス転移領域の広い非晶質合金粉末を用いることにより、変形が容易であるため、より緻密化させることができる。
In general, when the density of a soft magnetic alloy compact is insufficient due to voids generated inside, not only a sufficient saturation magnetic flux density cannot be obtained, but also the strength of the compact decreases as the voids increase.
Therefore, by using an amorphous alloy powder having a wide glass transition region as described above, the deformation can be easily performed, so that it can be further densified.
また、軟磁性合金圧密体の磁気異方性は小さいことが好ましいので、用いる非晶質合金粉末は、その形状が球状であることが望ましく、このような球状の非晶質合金粉末は、例えばアトマイズ法により容易に作製することができるが、これらの形状や製法に限定されるものではない。 Further, since the magnetic anisotropy of the soft magnetic alloy compact is preferably small, the amorphous alloy powder to be used preferably has a spherical shape, and such a spherical amorphous alloy powder is, for example, Although it can be easily manufactured by an atomizing method, it is not limited to these shapes and manufacturing methods.
更に、用いる非晶質合金粉末の含有成分やその組成は特に限定されるものではないが、磁気特性が良好であり、広い低温度範囲（例えば３５０〜６００℃）で非晶質（ガラス）状態となるものが望ましい。例えば、次式（３）
ΔＴｘ＝Ｔｘ−Ｔｇ…（３）
（式中のＴｘは結晶化開始温度、Ｔｇはガラス転移温度を示す。）で表される過冷却液体領域の温度間隔ΔＴｘが２０Ｋ以上であるＦｅ、Ｎｉ又はＣｏ、及びこれらの任意の組合わせに係る金属元素を主成分とする非晶質合金粉末を用いることが好適である。
典型的には、Ｎｉ、Ｃｏ及びＳｉを含有したＦｅ基合金、いわゆる鉄心材料を好適に用いることができる。
なお、非晶質合金粉末としては含有成分やその組成が異なる複数の非晶質合金粉末を混在させたものを用いてもよい。また、本発明においては、第３種以上の非晶質合金粉末を含んでいてもよい。
Furthermore, the content and composition of the amorphous alloy powder to be used are not particularly limited, but it has good magnetic properties and is in an amorphous (glass) state in a wide low temperature range (for example, 350 to 600 ° C.). Is desirable. For example, the following formula (3)
ΔTx = Tx−Tg (3)
(Wherein Tx represents a crystallization start temperature and Tg represents a glass transition temperature) Fe, Ni or Co having a temperature interval ΔTx of 20 K or more in the supercooled liquid region, and any combination thereof It is preferable to use an amorphous alloy powder containing the metal element as a main component.
Typically, an Fe-based alloy containing Ni, Co and Si, that is, a so-called iron core material can be suitably used.
The amorphous alloy powder may be a mixture of a plurality of amorphous alloy powders having different components and compositions. In the present invention, the third or more amorphous alloy powder may be included.
更にまた、絶縁物被膜は、所望の絶縁性を有していれば、その成分や膜厚について特に限定されるものではないが、その成分としては、例えば酸化ケイ素（ＳｉＯ２）やアルミナ（Ａｌ２Ｏ３）、マグネシア（ＭｇＯ）などを適用することができ、また膜厚は、例えば０．０１〜２μｍ、好ましくは０．０５〜１μｍであればよい。 Furthermore, the insulating film is not particularly limited in terms of its component and film thickness as long as it has a desired insulating property. Examples of the component include silicon oxide (SiO 2 ) and alumina (Al 2 O 3 ), magnesia (MgO), or the like can be applied, and the film thickness may be, for example, 0.01 to 2 μm, preferably 0.05 to 1 μm.
また、本発明においては、非晶質合金粉末は、異なる粒度分布を有する上記表面に絶縁物被膜を有していない非晶質合金粉末Ａと上記表面に絶縁物被膜を有している非晶質合金粉末Ｂとから成り、該非晶質合金粉末Ａの平均粒径（ｒＡ）と該非晶質合金粉末Ｂの平均粒径（ｒＢ）とが次式（１）
ｒＡ／ｒＢ＜１…（１）
の関係を満足することが好ましく、次式（２）
０．０５≦ｒＡ／ｒＢ≦０．３…（２）
の関係を満足することがより好ましく、上記式（２）において、その上限値が０．２５であることが更に好ましく、０．２０であることが特に好ましい。
上述したように、用いる原料粉末は非晶質（ガラス）合金であるので、酸化物と比較して変形が容易であり、比較的緻密化が進行するが、各粉末の変形量が過剰となると透磁率が低くなることがある。
そこで、密度を向上させ得るという観点から、非晶質合金粉末Ａの平均粒径（ｒＡ）と非晶質合金粉末Ｂの平均粒径（ｒＢ）とが上記式（１）の関係を満足し、粉末の特性に応じた粒度分布を有することが好ましく、更には、それぞれの粉末の過剰な変形を抑制し得るという観点から上記式（２）の関係を満足することが好ましい。
このときは、絶縁物被膜を有していない粒径の小さいものが絶縁物被膜を有する粒径が大きいものの隙間に分散するので、軟磁性合金圧密体の全体に分散した状態となり、絶縁性を維持しつつ、密度を向上させることができる。
In the present invention, the amorphous alloy powder is composed of an amorphous alloy powder A having a different particle size distribution and not having an insulator coating on the surface, and an amorphous alloy having an insulator coating on the surface. The average particle size (r A ) of the amorphous alloy powder A and the average particle size (r B ) of the amorphous alloy powder B are expressed by the following formula (1):
r A / r B <1 (1)
It is preferable to satisfy the relationship:
0.05 ≦ r A / r B ≦ 0.3 (2)
It is more preferable that the above relationship is satisfied, and in the above formula (2), the upper limit value is more preferably 0.25, and particularly preferably 0.20.
As described above, since the raw material powder to be used is an amorphous (glass) alloy, it is easily deformed as compared with the oxide and relatively densified, but when the amount of deformation of each powder becomes excessive. Permeability may be low.
Therefore, from the viewpoint that the density can be improved, the average particle size (r A ) of the amorphous alloy powder A and the average particle size (r B ) of the amorphous alloy powder B satisfy the relationship of the above formula (1). It is preferable to have a particle size distribution according to the characteristics of the powder, and it is more preferable to satisfy the relationship of the above formula (2) from the viewpoint that excessive deformation of each powder can be suppressed.
At this time, since the small particle size without the insulating film is dispersed in the gaps with the large particle size having the insulating film, it becomes dispersed throughout the soft magnetic alloy compact, and the insulating property is reduced. The density can be improved while maintaining.
更に、本発明においては、非晶質合金粉末Ｂのガラス転移温度を基準として、非晶質合金粉末Ａのガラス転移温度が１０Ｋ以上低いことが好ましく、特に１０〜３０Ｋ低いことが好ましい。
このとき、平均粒径が相対的に小さい非晶質合金粉末Ａは、平均粒径が相対的に大きい非晶質合金粉末Ｂの隙間に分散して、密度を向上させつつ非晶質合金粉末Ｂ同士の接合を補助するような構造を形成する。このとき、上記のようなガラス転移温度の関係を有する場合には、加圧成形処理の際に非晶質合金粉末Ａが優先的に変形して、非晶質合金粉末Ｂと密着し、密度を向上させつつ絶縁物被膜の膜厚を薄い状態のままの接触面積を拡大させることができる。また、非晶質合金粉末Ｂの絶縁物被膜の破損を抑制することもできる。
Furthermore, in the present invention, the glass transition temperature of the amorphous alloy powder A is preferably 10 K or more lower, particularly preferably 10 to 30 K lower than the glass transition temperature of the amorphous alloy powder B.
At this time, the amorphous alloy powder A having a relatively small average particle size is dispersed in the gaps of the amorphous alloy powder B having a relatively large average particle size to improve the density and improve the density. A structure that assists the bonding between B is formed. At this time, in the case of having the glass transition temperature relationship as described above, the amorphous alloy powder A is preferentially deformed during the pressure forming process, and is in close contact with the amorphous alloy powder B. It is possible to increase the contact area while keeping the thickness of the insulating coating film thin. Moreover, damage to the insulating film of the amorphous alloy powder B can be suppressed.
また、本発明においては、非晶質合金粉末の全体積を基準として、非晶質合金粉末Ａの含有率が５０体積％以下である必要があるが、特に含有率が３０体積％以下では、絶縁物被覆した粉末を１００体積％にした場合と同等の発熱抑制効果が得られるため、３０体積％以下であることが好ましい。なお、２０体積％以下であることがより好ましい。 Further, in the present invention, the content of the amorphous alloy powder A needs to be 50% by volume or less based on the total volume of the amorphous alloy powder, and particularly when the content is 30% by volume or less, Since the heat generation suppressing effect equivalent to that obtained when the insulating-coated powder is 100% by volume is obtained, it is preferably 30% by volume or less. In addition, it is more preferable that it is 20 volume% or less.
更にまた、本発明においては、加圧成形処理工程の成形温度が、非晶質合金粉末Ａのガラス転移温度以上であり且つ非晶質合金粉末Ａの結晶化開始温度以下であると共に、当該加圧成形処理の平均プレス歪速度が０．０００１〜１Ｓ−１であることが好ましい、より好ましくは０．００５〜０．１Ｓ−１である。
このような工程を経た軟磁性合金圧密体は、加圧成形処理の際に、非晶質合金粉末Ａを非晶質合金粉末Ｂに優先して変形させることが可能となる。
Furthermore, in the present invention, the molding temperature in the pressure molding treatment step is not less than the glass transition temperature of the amorphous alloy powder A and not more than the crystallization start temperature of the amorphous alloy powder A. it is preferred that the average pressing strain rate of molding process is 0.0001~1S -1, more preferably 0.005~0.1S -1.
The soft magnetic alloy compact that has undergone such a process can deform the amorphous alloy powder A in preference to the amorphous alloy powder B during the pressure forming process.
次に、本発明の軟磁性合金圧密体の製造方法について詳細に説明する。
上述の如く、本発明の軟磁性合金圧密体の製造方法は、上記本発明の軟磁性合金圧密体を製造する方法であって、（１）非晶質合金粉末の全体積を基準として、非晶質合金粉末の表面に絶縁物被膜を有していない粉末及び非晶質合金粉末の表面に絶縁物被膜を有している粉末を、それぞれの含有率が１〜５０体積％及び５０〜９９体積％となるように混合する工程、（２）（１）工程で得られた粉末を加圧成形処理する工程、を含む製造方法である。
このような製造方法により作製された軟磁性合金圧密体は、優れた強度を有し、且つ渦電流損失を低減し得るものとなる。
Next, the manufacturing method of the soft magnetic alloy compact of this invention is demonstrated in detail.
As described above, the method for producing a soft magnetic alloy compact according to the present invention is a method for producing the above soft magnetic alloy compact according to the present invention. (1) Based on the total volume of amorphous alloy powder, The powders having no insulating film on the surface of the crystalline alloy powder and the powders having the insulating film on the surface of the amorphous alloy powder have a content of 1 to 50% by volume and 50 to 99, respectively. It is a manufacturing method including a step of mixing so as to be volume%, and a step of pressure-forming the powder obtained in steps (2) and (1).
The soft magnetic alloy compact manufactured by such a manufacturing method has excellent strength and can reduce eddy current loss.
更に、上記のような絶縁物被膜は、例えば以下の製造方法により形成することができる。即ち、非晶質合金粉末を絶縁物前駆体含有溶液に浸漬し、乾燥させて非晶質合金粉末表面に絶縁物前駆体を被覆担持させる。この過程は、被覆量と溶液濃度に応じて、浸漬、乾燥を繰り返すことができる。
次いで、この絶縁物前駆体を被覆担持した非晶質合金粉末を加熱して、絶縁物前駆体を焼成する。絶縁物前駆体は焼成中に、化学反応と溶解により絶縁物被膜に変化する。
Furthermore, the insulating film as described above can be formed, for example, by the following manufacturing method. That is, the amorphous alloy powder is immersed in an insulator precursor-containing solution and dried to coat and carry the insulator precursor on the surface of the amorphous alloy powder. In this process, immersion and drying can be repeated according to the coating amount and the solution concentration.
Next, the amorphous alloy powder coated and supported with the insulator precursor is heated to fire the insulator precursor. During firing, the insulator precursor changes into an insulator film due to chemical reaction and dissolution.
以下、本発明を実施例及び比較例により更に詳細に説明するが、本発明はこれら実施例に限定されるものではない。 EXAMPLES Hereinafter, although an Example and a comparative example demonstrate this invention further in detail, this invention is not limited to these Examples.
［非晶質合金粉末の準備］
鉄（Ｆｅ）、ガリウム（Ｇａ）、ホウ素（Ｂ）ケイ素（Ｓｉ）、鉄（Ｆｅ）−炭素（Ｃ）合金、鉄（Ｆｅ）−リン（Ｐ）合金を所定量秤量し、高周波溶解炉を用いてアルゴン（Ａｒ）ガス中で溶解した。そして、組成がＦｅ７６Ｇａ４Ｐ９．５Ｃ４Ｂ４Ｓｉ２．５となるインゴットを作製した。
得られたインゴットをアルゴン雰囲気、減圧（１０−３Ｐａ）下で溶解し、Ａｒガスで噴霧してガスアトマイズを行なった。
ガスアトマイズによって得られた粉末は、Ｘ線解析の結果、急冷された非晶質合金粉末となっていた。
得られた粉末は、平均粒径の±２０％以内におさまるように篩を用いて分級した。なお、粒度は、レーザ回折方式粒度分布測定装置で測定して決定した。また、ガラス転移温度は、示差走査熱量分析（ＤＳＣ解析）により白金坩堝を用いてＡｒ気流中で測定して決定した。
[Preparation of amorphous alloy powder]
A predetermined amount of iron (Fe), gallium (Ga), boron (B) silicon (Si), iron (Fe) -carbon (C) alloy, iron (Fe) -phosphorus (P) alloy is weighed, and a high-frequency melting furnace is used. And dissolved in argon (Ar) gas. Then, the composition was prepared an ingot to be Fe 76 Ga 4 P 9.5 C 4 B 4 Si 2.5.
The obtained ingot was melted under an argon atmosphere and reduced pressure (10 −3 Pa) and sprayed with Ar gas for gas atomization.
As a result of X-ray analysis, the powder obtained by gas atomization was a rapidly cooled amorphous alloy powder.
The obtained powder was classified using a sieve so as to be within ± 20% of the average particle size. The particle size was determined by measuring with a laser diffraction particle size distribution measuring device. Further, the glass transition temperature was determined by measurement in an Ar stream using a platinum crucible by differential scanning calorimetry (DSC analysis).
（実施例１）
平均粒径が２２５μｍ、ガラス転移温度が４６５℃の非晶質合金粉末１０ｇ当たり、５ｍＬのポリシザラン溶液（アクアミカ社製）を塗布し、ドライヤーで乾燥し、１００℃で１時間保持して、絶縁物である酸化ケイ素（ＳｉＯ２）の被膜を有する非晶質合金粉末を得た。
一方、平均粒径が４５μｍ、ガラス転移温度が４４０℃の非晶質合金粉末を用意し、それぞれの含有率が７５体積％及び２５体積％となるように混合した。なお、２種類の粉末の比重が同等とみなせたので、ここでは質量により測定した（以下の実施例及び比較例において同様。）。
この混合した粉末３ｇを秤量して、プレス面が外径３０ｍｍ、内径２０ｍｍである円環状の金型に充填し、１．６ＭＡ／ｍの磁場中で、成形温度は室温、成形圧力は０．０５ＧＰａで仮成形した。
得られた仮成形体を真空中でプラズマ放電焼結法により下記の要領で加圧成形処理して、本例の軟磁性合金圧密体を得た。
具体的には、一定の成形圧力０．０５ＧＰａを保持しつつ、昇温速度２５℃／分で室温から４５０℃まで昇温した。次いで、成形温度４５０℃で１分間保持した。更に、徐々に荷重を大きくして０．５ＧＰａまで５秒で到達させた。この間の平均プレス歪速度は０．１Ｓ−１であった。しかる後、荷重負荷を開放して冷却し、本例の軟磁性合金圧密体を得た（寸法：外径３０ｍｍ、内径２０ｍｍ、厚み４ｍｍ）。なお、冷却中も室温になるまで真空を保持した。
Example 1
5 g of polysizaran solution (Aquamica) is applied per 10 g of amorphous alloy powder having an average particle size of 225 μm and a glass transition temperature of 465 ° C., dried with a drier, and held at 100 ° C. for 1 hour. Amorphous alloy powder having a silicon oxide (SiO 2 ) coating was obtained.
On the other hand, amorphous alloy powders having an average particle size of 45 μm and a glass transition temperature of 440 ° C. were prepared and mixed so that the respective contents were 75% by volume and 25% by volume. In addition, since it was considered that the specific gravity of two types of powder was equivalent, it measured by mass here (same in the following Examples and Comparative Examples).
3 g of the mixed powder was weighed and filled in an annular mold having a press surface of 30 mm outer diameter and 20 mm inner diameter, in a magnetic field of 1.6 MA / m, the molding temperature was room temperature, and the molding pressure was 0. Temporary molding was performed at 05 GPa.
The obtained temporary molded body was subjected to pressure forming treatment in a vacuum by a plasma discharge sintering method in the following manner to obtain a soft magnetic alloy consolidated body of this example.
Specifically, the temperature was increased from room temperature to 450 ° C. at a temperature increase rate of 25 ° C./min while maintaining a constant molding pressure of 0.05 GPa. Subsequently, it was held at a molding temperature of 450 ° C. for 1 minute. Further, the load was gradually increased to reach 0.5 GPa in 5 seconds. The average press strain rate during this period was 0.1S- 1 . Thereafter, the load was released and cooled to obtain a soft magnetic alloy consolidated body of this example (dimensions: outer diameter 30 mm, inner diameter 20 mm, thickness 4 mm). Note that the vacuum was maintained during cooling until the temperature reached room temperature.
（実施例２）
平均粒径が３８０μｍ、ガラス転移温度が４６５℃の非晶質合金粉末１０ｇ当たり、５ｍＬのポリシザラン溶液（アクアミカ社製）を塗布し、ドライヤーで乾燥し、１００℃で１時間保持して、絶縁物である酸化ケイ素（ＳｉＯ２）の被膜を有する非晶質合金粉末を得た。
一方、平均粒径が５μｍ、ガラス転移温度が４４０℃の非晶質合金粉末を用意し、それぞれの含有率が５５体積％及び４５体積％となるように混合して用いた以外は、実施例１と同様の操作を繰り返し、本例の軟磁性合金圧密体を得た。
(Example 2)
Apply 5 mL of polysizaran solution (Aquamica) per 10 g of amorphous alloy powder with an average particle size of 380 μm and a glass transition temperature of 465 ° C., dry with a drier, and hold at 100 ° C. for 1 hour. Amorphous alloy powder having a silicon oxide (SiO 2 ) coating was obtained.
On the other hand, Examples were prepared except that amorphous alloy powders having an average particle diameter of 5 μm and a glass transition temperature of 440 ° C. were prepared and mixed so that the respective contents were 55% by volume and 45% by volume. The same operation as in No. 1 was repeated to obtain a soft magnetic alloy consolidated body of this example.
（実施例３）
平均粒径が１５０μｍ、ガラス転移温度が４６５℃の非晶質合金粉末１０ｇ当たり、５ｍＬのポリシザラン溶液（アクアミカ社製）を塗布し、ドライヤーで乾燥し、１００℃で１時間保持して、絶縁物である酸化ケイ素（ＳｉＯ２）の被膜を有する非晶質合金粉末を得た。
一方、平均粒径が２０μｍ、ガラス転移温度が４４０℃の非晶質合金粉末を用意し、それぞれの含有率が８０体積％及び２０体積％となるように混合して用いた以外は、実施例１と同様の操作を繰り返し、本例の軟磁性合金圧密体を得た。
(Example 3)
Apply 5 mL of polysizaran solution (manufactured by Aquamica) per 10 g of amorphous alloy powder with an average particle size of 150 μm and a glass transition temperature of 465 ° C., dry with a drier, and hold at 100 ° C. for 1 hour. Amorphous alloy powder having a silicon oxide (SiO 2 ) coating was obtained.
On the other hand, Examples were prepared except that amorphous alloy powders having an average particle size of 20 μm and a glass transition temperature of 440 ° C. were prepared and mixed so that the respective contents were 80% by volume and 20% by volume. The same operation as in No. 1 was repeated to obtain a soft magnetic alloy consolidated body of this example.
（実施例４）
平均粒径が２２５μｍ、ガラス転移温度が４７０℃の非晶質合金粉末１０ｇ当たり、５ｍＬのポリシザラン溶液（アクアミカ社製）を塗布し、ドライヤーで乾燥し、１００℃で１時間保持して、絶縁物である酸化ケイ素（ＳｉＯ２）の被膜を有する非晶質合金粉末を得た。
一方、平均粒径が４５μｍ、ガラス転移温度が４３５℃の非晶質合金粉末を用意し、それぞれの含有率が９０体積％及び１０体積％となるように混合して用い、仮成形処理を実施せず、加圧成形処理における成形温度を４６５℃とし、且つ平均歪速度を０．０５Ｓ−１とした以外は、実施例１と同様の操作を繰り返し、本例の軟磁性合金圧密体を得た。
Example 4
5 g of polysizaran solution (manufactured by Aquamica) is applied per 10 g of amorphous alloy powder having an average particle size of 225 μm and a glass transition temperature of 470 ° C., dried with a drier, and held at 100 ° C. for 1 hour. Amorphous alloy powder having a silicon oxide (SiO 2 ) coating was obtained.
On the other hand, an amorphous alloy powder having an average particle size of 45 μm and a glass transition temperature of 435 ° C. is prepared and mixed so that the respective contents are 90% by volume and 10% by volume, and a temporary forming process is performed. Otherwise, the same operation as in Example 1 was repeated except that the molding temperature in the pressure molding treatment was 465 ° C. and the average strain rate was 0.05 S −1 to obtain the soft magnetic alloy consolidated body of this example. It was.
（実施例５）
平均粒径が７５μｍ、ガラス転移温度が４６５℃の非晶質合金粉末１０ｇ当たり、５ｍＬのポリシザラン溶液（アクアミカ社製）を塗布し、ドライヤーで乾燥し、１００℃で１時間保持して、絶縁物である酸化ケイ素（ＳｉＯ２）の被膜を有する非晶質合金粉末を得た。
一方、平均粒径が８μｍ、ガラス転移温度が４４０℃の非晶質合金粉末を用意し、それぞれの含有率が７５体積％及び２５体積％となるように混合して用い、加圧成形処理における平均歪速度を０．３Ｓ−１とした以外は、実施例１と同様の操作を繰り返し、本例の軟磁性合金圧密体を得た。
(Example 5)
5 g of polysizaran solution (manufactured by Aquamica) is applied per 10 g of amorphous alloy powder having an average particle size of 75 μm and a glass transition temperature of 465 ° C., dried with a drier, held at 100 ° C. for 1 hour, and an insulator Amorphous alloy powder having a silicon oxide (SiO 2 ) coating was obtained.
On the other hand, an amorphous alloy powder having an average particle size of 8 μm and a glass transition temperature of 440 ° C. is prepared and mixed so that the respective contents are 75% by volume and 25% by volume. Except for setting the average strain rate to 0.3 S- 1 , the same operation as in Example 1 was repeated to obtain a soft magnetic alloy consolidated body of this example.
（実施例６）
平均粒径が１５０μｍ、ガラス転移温度が４６５℃の非晶質合金粉末１０ｇ当たり、５ｍＬのポリシザラン溶液（アクアミカ社製）を塗布し、ドライヤーで乾燥し、１００℃で１時間保持して、絶縁物である酸化ケイ素（ＳｉＯ２）の被膜を有する非晶質合金粉末を得た。
一方、平均粒径が２０μｍ、ガラス転移温度が４４０℃の非晶質合金粉末及び平均粒径が８μｍ、ガラス転移温度が４４０℃の非晶質合金粉末を用意し、それぞれの含有率が７５体積％、１５体積％及び１０体積％となるように混合して用い、加圧成形処理における平均歪速度を０．３Ｓ−１とした以外は、実施例１と同様の操作を繰り返し、本例の軟磁性合金圧密体を得た。
(Example 6)
Apply 5 mL of polysizaran solution (manufactured by Aquamica) per 10 g of amorphous alloy powder with an average particle size of 150 μm and a glass transition temperature of 465 ° C., dry with a drier, and hold at 100 ° C. for 1 hour. Amorphous alloy powder having a silicon oxide (SiO 2 ) coating was obtained.
On the other hand, an amorphous alloy powder having an average particle size of 20 μm and a glass transition temperature of 440 ° C. and an amorphous alloy powder having an average particle size of 8 μm and a glass transition temperature of 440 ° C. are prepared, and each content is 75 volumes. %, 15% by volume and 10% by volume, and the same operation as in Example 1 was repeated except that the average strain rate in the pressure molding treatment was 0.3S- 1 . A soft magnetic alloy compact was obtained.
（実施例７）
平均粒径が２２５μｍ、ガラス転移温度が４６５℃の非晶質合金粉末１０ｇ当たり、５ｍＬのポリシザラン溶液（アクアミカ社製）を塗布し、ドライヤーで乾燥し、１００℃で１時間保持して、絶縁物である酸化ケイ素（ＳｉＯ２）の被膜を有する非晶質合金粉末を得た。
一方、平均粒径が７５μｍ、ガラス転移温度が４４０℃の非晶質合金粉末を用意し、それぞれの含有率が７５体積％及び２５体積％となるように混合して用い、加圧成形処理における平均歪速度を０．００５Ｓ−１とした以外は、実施例１と同様の操作を繰り返し、本例の軟磁性合金圧密体を得た。
(Example 7)
5 g of polysizaran solution (Aquamica) is applied per 10 g of amorphous alloy powder having an average particle size of 225 μm and a glass transition temperature of 465 ° C., dried with a drier, and held at 100 ° C. for 1 hour. Amorphous alloy powder having a silicon oxide (SiO 2 ) coating was obtained.
On the other hand, an amorphous alloy powder having an average particle size of 75 μm and a glass transition temperature of 440 ° C. is prepared and mixed so that the respective contents are 75% by volume and 25% by volume. Except that the average strain rate was 0.005 S −1 , the same operation as in Example 1 was repeated to obtain a soft magnetic alloy consolidated body of this example.
（比較例５）
平均粒径が７５μｍ、ガラス転移温度が４６５℃の非晶質合金粉末１０ｇ当たり、５ｍＬのポリシザラン溶液（アクアミカ社製）を塗布し、ドライヤーで乾燥し、１００℃で１時間保持して、絶縁物である酸化ケイ素（ＳｉＯ２）の被膜を有する非晶質合金粉末を得た。
一方、平均粒径が７５μｍ、ガラス転移温度が４６５℃の非晶質合金粉末を用意し、それぞれの含有率が８０体積％及び２０体積％となるように混合して用い、加圧成形処理における平均歪速度を０．０５Ｓ−１とした以外は、実施例１と同様の操作を繰り返し、本例の軟磁性合金圧密体を得た。
( Comparative Example 5 )
5 g of polysizaran solution (manufactured by Aquamica) is applied per 10 g of amorphous alloy powder having an average particle size of 75 μm and a glass transition temperature of 465 ° C., dried with a drier, held at 100 ° C. for 1 hour, and an insulator Amorphous alloy powder having a silicon oxide (SiO 2 ) coating was obtained.
On the other hand, an amorphous alloy powder having an average particle size of 75 μm and a glass transition temperature of 465 ° C. is prepared and mixed so that the respective contents are 80% by volume and 20% by volume. A soft magnetic alloy consolidated body of this example was obtained by repeating the same operation as in Example 1 except that the average strain rate was 0.05 S- 1 .
（比較例１）
平均粒径が２２５μｍ、ガラス転移温度が４６５℃の非晶質合金粉末及び平均粒径が４５μｍ、ガラス転移温度が４４０℃の非晶質合金粉末を用意し、それぞれの含有率が７５体積％及び２５体積％となるように混合して用いた以外は、実施例１と同様の操作を繰り返し、本例の軟磁性合金圧密体を得た。
(Comparative Example 1)
An amorphous alloy powder having an average particle size of 225 μm and a glass transition temperature of 465 ° C. and an amorphous alloy powder having an average particle size of 45 μm and a glass transition temperature of 440 ° C. are prepared, and the respective contents are 75% by volume and A soft magnetic alloy consolidated body of this example was obtained by repeating the same operation as in Example 1 except that the mixture was used so as to be 25% by volume.
（比較例２）
平均粒径が２２５μｍ、ガラス転移温度が４６５℃の非晶質合金粉末１０ｇ当たり、５ｍＬのポリシザラン溶液（アクアミカ社製）を塗布し、ドライヤーで乾燥し、１００℃で１時間保持して、絶縁物である酸化ケイ素（ＳｉＯ２）の被膜を有する非晶質合金粉末を得た。
一方、平均粒径が４５μｍ、ガラス転移温度が４４０℃の非晶質合金粉末１０ｇ当たり、５ｍＬのポリシザラン溶液（アクアミカ社製）を塗布し、ドライヤーで乾燥し、１００℃で１時間保持して、絶縁物である酸化ケイ素（ＳｉＯ２）の被膜を有する非晶質合金粉末を得た。それぞれの含有率が７５体積％及び２５体積％となるように混合して用いた以外は、実施例１と同様の操作を繰り返し、本例の軟磁性合金圧密体を得た。
(Comparative Example 2)
5 g of polysizaran solution (Aquamica) is applied per 10 g of amorphous alloy powder having an average particle size of 225 μm and a glass transition temperature of 465 ° C., dried with a drier, and held at 100 ° C. for 1 hour. Amorphous alloy powder having a silicon oxide (SiO 2 ) coating was obtained.
On the other hand, 5 mL of polysizaran solution (manufactured by Aquamica) was applied per 10 g of amorphous alloy powder having an average particle diameter of 45 μm and a glass transition temperature of 440 ° C., dried with a dryer, and held at 100 ° C. for 1 hour. An amorphous alloy powder having a coating of silicon oxide (SiO 2 ) as an insulator was obtained. A soft magnetic alloy consolidated body of this example was obtained by repeating the same operation as in Example 1 except that the respective contents were mixed and used so as to be 75% by volume and 25% by volume.
（比較例３）
平均粒径が２２５μｍ、ガラス転移温度が４６５℃の非晶質合金粉末１０ｇ当たり、５ｍＬのポリシザラン溶液（アクアミカ社製）を塗布し、ドライヤーで乾燥し、１００℃で１時間保持して、絶縁物である酸化ケイ素（ＳｉＯ２）の被膜を有する非晶質合金粉末を得た。これのみを用いた以外は、実施例１と同様の操作を繰り返し、本例の軟磁性合金圧密体を得た。
(Comparative Example 3)
5 g of polysizaran solution (Aquamica) is applied per 10 g of amorphous alloy powder having an average particle size of 225 μm and a glass transition temperature of 465 ° C., dried with a drier, and held at 100 ° C. for 1 hour. Amorphous alloy powder having a silicon oxide (SiO 2 ) coating was obtained. Except using only this, the same operation as Example 1 was repeated and the soft magnetic alloy compact of this example was obtained.
（比較例４）
平均粒径が２０μｍ、ガラス転移温度が４６５℃の非晶質合金粉末１０ｇ当たり、５ｍＬのポリシザラン溶液（アクアミカ社製）を塗布し、ドライヤーで乾燥し、１００℃で１時間保持して、絶縁物である酸化ケイ素（ＳｉＯ２）の被膜を有する非晶質合金粉末を得た。これのみを用いた以外は、実施例１と同様の操作を繰り返し、本例の軟磁性合金圧密体を得た。
上記各例の軟磁性合金圧密体の仕様及び作製条件を表１に示す。
(Comparative Example 4)
Apply 5 mL of polysizaran solution (manufactured by Aquamica) per 10 g of amorphous alloy powder with an average particle size of 20 μm and a glass transition temperature of 465 ° C., dry with a drier, hold at 100 ° C. for 1 hour, and insulate Amorphous alloy powder having a silicon oxide (SiO 2 ) coating was obtained. Except using only this, the same operation as Example 1 was repeated and the soft magnetic alloy compact of this example was obtained.
Table 1 shows the specifications and production conditions of the soft magnetic alloy compacts of the above examples.
［性能評価］
上記各例の軟磁性合金圧密体の渦電流損失及び密度を下記の要領で測定した。得られた結果を表２に示す。
[Performance evaluation]
The eddy current loss and density of the soft magnetic alloy compacts of the above examples were measured as follows. The obtained results are shown in Table 2.
（渦電流損失）
周波数１ｋＨｚ、飽和磁束密度１Ｔの条件下で測定した。表中の結果は、比較例１の渦電流損失を基準値（１００）としたときの相対値である。
(Eddy current loss)
The measurement was performed under conditions of a frequency of 1 kHz and a saturation magnetic flux density of 1T. The results in the table are relative values when the eddy current loss of Comparative Example 1 is taken as the reference value (100).
（密度）
軟磁性合金圧密体の寸法及び質量から算出した。
(density)
It calculated from the size and mass of a soft magnetic alloy compact.
（強度）
プレス面が１０ｍｍ×１０ｍｍである金型に混合した粉末を４ｇ充填し、上記各例と同様の操作を行い、各例の軟磁性合金圧密体（寸法：１０ｍｍ×１０ｍｍ×５ｍｍ）を得た。得られた軟磁性合金圧密体から２ｍｍ×３ｍｍ×１０ｍｍの試験片をプレス面と平行に切り出し、３点曲げ試験に供し、抗折強度を測定した。得られた結果を表２に併記する。
(Strength)
4 g of powder mixed in a mold having a press surface of 10 mm × 10 mm was filled, and the same operation as in each of the above examples was performed to obtain a soft magnetic alloy compact (size: 10 mm × 10 mm × 5 mm) of each example. A 2 mm × 3 mm × 10 mm test piece was cut out from the obtained soft magnetic alloy compacted body in parallel with the press surface and subjected to a three-point bending test to measure the bending strength. The obtained results are also shown in Table 2.
表１及び表２より、本発明の範囲に属する実施例１〜７は、本発明外の比較例１〜５と比較して、優れた抗折強度を有し、且つ渦電流損失を低減し得ることが分かる。
更に、表１及び表２より、実施例１〜３及び実施例５〜７は、抗折強度が２５０ＭＰａ以上であり、渦電流損失が低減され得ることから、特に、電気自動車やハイブリッド車等のモーターの磁心として好適に用いることができることが分かる。
なお、実施例４からは、二種類の粉末粒子のガラス転移温度の差が大きいものを用いた方が強度がより向上することが分かり、比較例５からは、混合する粉末粒子の平均粒径が異なる方が密度が向上し易いことが分かる。
From Table 1 and Table 2, Examples 1 7 within the scope of the present invention, as compared with Comparative Example 1 to 5 of the outer present invention has excellent flexural strength, and to reduce the eddy current loss I know you get.
Furthermore, from Tables 1 and 2, Examples 1 to 3 and Examples 5 to 7 have a bending strength of 250 MPa or more, and eddy current loss can be reduced. It can be seen that the magnetic core of the motor can be suitably used.
In addition, from Example 4, it turns out that the intensity | strength improves more using the thing with a big difference of the glass transition temperature of two types of powder particles, From Comparative Example 5 , the average particle diameter of the powder particle to mix It can be seen that the density is easily improved when the difference is.
現時点においては、優れた抗折強度を有し、渦電流損失の低減させ得る観点から、実施例１や実施例３が最も良好な結果をもたらすものと思われる。 At the present time, from the viewpoint of having excellent bending strength and reducing eddy current loss, it seems that Example 1 and Example 3 give the best results.
Claims (8)
上記非晶質合金粉末は、該非晶質合金粉末の全体積を基準として、５０〜９９体積％の非晶質合金粉末がその表面に絶縁物被膜を有しており、且つ１〜５０体積％の非晶質合金粉末がその表面に絶縁物被膜を有していない軟磁性合金圧密体であって、
上記非晶質合金粉末は、異なる粒度分布を有する上記表面に絶縁物被膜を有していない非晶質合金粉末Ａと上記表面に絶縁物被膜を有している非晶質合金粉末Ｂとから成り、該非晶質合金粉末Ａの平均粒径（ｒ Ａ ）と該非晶質合金粉末Ｂの平均粒径（ｒ Ｂ ）とが次式（１）
ｒ Ａ ／ｒ Ｂ ＜１…（１）
の関係を満足し、
上記非晶質合金粉末Ｂのガラス転移温度を基準として、上記非晶質合金粉末Ａのガラス転移温度が１０Ｋ以上低いことを特徴とする軟磁性合金圧密体。 In a soft magnetic alloy compact formed by pressure-molding at least one amorphous alloy powder,
The amorphous alloy powder is based on the total volume of the amorphous alloy powder, 50 to 99% by volume of the amorphous alloy powder has an insulating film on its surface, and 1 to 50% by volume. amorphous alloy powder is a I軟 magnetic alloy compacts such have an insulator film on the surface of,
The amorphous alloy powder is composed of an amorphous alloy powder A having an insulating film on the surface and an amorphous alloy powder B having an insulating film on the surface having different particle size distributions. The average particle size (r A ) of the amorphous alloy powder A and the average particle size (r B ) of the amorphous alloy powder B are expressed by the following formula (1):
r A / r B <1 (1)
Satisfied with the relationship
A soft magnetic alloy compacted body characterized in that the glass transition temperature of the amorphous alloy powder A is 10K or more lower than the glass transition temperature of the amorphous alloy powder B.
上記非晶質合金粉末は、該非晶質合金粉末の全体積を基準として、５０〜９９体積％の非晶質合金粉末がその表面に絶縁物被膜を有しており、且つ１〜５０体積％の非晶質合金粉末がその表面に絶縁物被膜を有していない軟磁性合金圧密体であって、The amorphous alloy powder is based on the total volume of the amorphous alloy powder, 50 to 99% by volume of the amorphous alloy powder has an insulating film on its surface, and 1 to 50% by volume. The amorphous alloy powder is a soft magnetic alloy compact that does not have an insulator coating on its surface,
上記非晶質合金粉末は、異なる粒度分布を有する上記表面に絶縁物被膜を有していない非晶質合金粉末Ａと上記表面に絶縁物被膜を有している非晶質合金粉末Ｂとから成り、該非晶質合金粉末Ａの平均粒径（ｒThe amorphous alloy powder is composed of an amorphous alloy powder A having an insulating film on the surface and an amorphous alloy powder B having an insulating film on the surface having different particle size distributions. The average particle size of the amorphous alloy powder A (r ＡA ）と該非晶質合金粉末Ｂの平均粒径（ｒ) And the average particle size of the amorphous alloy powder B (r ＢB ）とが次式（２）) And the following formula (2)
０．０５≦ｒ0.05 ≦ r ＡA ／ｒ/ R ＢB ≦０．３…（２）≦ 0.3 (2)
の関係を満足し、Satisfied with the relationship
上記非晶質合金粉末Ｂのガラス転移温度を基準として、上記非晶質合金粉末Ａのガラス転移温度が１０Ｋ以上低いことを特徴とする軟磁性合金圧密体。A soft magnetic alloy compacted body characterized in that the glass transition temperature of the amorphous alloy powder A is 10K or more lower than the glass transition temperature of the amorphous alloy powder B.
（１）非晶質合金粉末の全体積を基準として、非晶質合金粉末の表面に絶縁物被膜を有していない粉末及び非晶質合金粉末の表面に絶縁物被膜を有している粉末を、それぞれの含有率が１〜５０体積％及び５０〜９９体積％となるように混合する工程、
（２）（１）工程で得られた粉末を加圧成形処理する工程、
を含むことを特徴とする軟磁性合金圧密体の製造方法。 A method for producing a soft magnetic alloy compact according to any one of claims 1 to 7, comprising the following steps (1) and (2):
(1) Based on the total volume of the amorphous alloy powder, a powder that does not have an insulator coating on the surface of the amorphous alloy powder and a powder that has an insulator coating on the surface of the amorphous alloy powder Are mixed so that the respective contents are 1 to 50% by volume and 50 to 99% by volume,
(2) A step of pressure-molding the powder obtained in the step (1),
A method for producing a soft magnetic alloy compact, comprising:
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| JP2003193174A (en) * | 2001-12-27 | 2003-07-09 | Mitsubishi Materials Corp | METHOD FOR MANUFACTURING Fe-Si SOFT MAGNETIC SINTERED MATERIAL WITH HIGH DENSITY AND EXCELLENT MAGNETIC PERMEABILITY |
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