JP7419127B2 - Powder magnetic core and its manufacturing method - Google Patents
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- 238000004519 manufacturing process Methods 0.000 title description 15
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- 239000002245 particle Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 13
- 239000013078 crystal Substances 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 5
- 238000000635 electron micrograph Methods 0.000 claims description 4
- 239000011162 core material Substances 0.000 description 66
- 230000035699 permeability Effects 0.000 description 33
- 229910045601 alloy Inorganic materials 0.000 description 32
- 239000000956 alloy Substances 0.000 description 32
- 239000002159 nanocrystal Substances 0.000 description 23
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- 239000011812 mixed powder Substances 0.000 description 21
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- 238000002844 melting Methods 0.000 description 10
- 230000008018 melting Effects 0.000 description 10
- 238000009692 water atomization Methods 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 230000004907 flux Effects 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
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- 229910000604 Ferrochrome Inorganic materials 0.000 description 5
- 238000000889 atomisation Methods 0.000 description 5
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- 230000000694 effects Effects 0.000 description 3
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- 239000006247 magnetic powder Substances 0.000 description 3
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- 229910000592 Ferroniobium Inorganic materials 0.000 description 2
- 229910008458 Si—Cr Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910017060 Fe Cr Inorganic materials 0.000 description 1
- 229910002544 Fe-Cr Inorganic materials 0.000 description 1
- 229910017082 Fe-Si Inorganic materials 0.000 description 1
- 229910017133 Fe—Si Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
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- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- NRGIRRZWCDKDMV-UHFFFAOYSA-H cadmium(2+);diphosphate Chemical compound [Cd+2].[Cd+2].[Cd+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O NRGIRRZWCDKDMV-UHFFFAOYSA-H 0.000 description 1
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- CPSYWNLKRDURMG-UHFFFAOYSA-L hydron;manganese(2+);phosphate Chemical compound [Mn+2].OP([O-])([O-])=O CPSYWNLKRDURMG-UHFFFAOYSA-L 0.000 description 1
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- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
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- 229960002261 magnesium phosphate Drugs 0.000 description 1
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- 229910052748 manganese Inorganic materials 0.000 description 1
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- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
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- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
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Description
本発明は、圧粉磁心及びその製造方法に関する。 The present invention relates to a powder magnetic core and a method for manufacturing the same.
数ｋＨｚから数百ｋＨｚまでの領域に用いられるリアクトル用の磁心として圧粉磁心がある。圧粉磁心は、磁性粉末の表面を絶縁処理したのち加工成形したもので、絶縁処理により渦電流損失の発生が抑制されている。 There is a powder magnetic core as a magnetic core for a reactor used in the range from several kHz to several hundred kHz. A powder magnetic core is formed by processing and molding the surface of magnetic powder after insulating it, and the insulation treatment suppresses the occurrence of eddy current loss.
特に、急速に普及しはじめたハイブリッド自動車では、大出力の電気モータを有しており、これを駆動する電源回路には高電圧大電流に耐えうるリアクトルが必要になる。このリアクトルには小型化、低騒音化、低損失化、耐久性の要求が強く、リアクトルに用いられる磁心材の特性としては、高い飽和磁束密度Ｂｓに加えて高い透磁率μが要求される。 In particular, hybrid vehicles, which are rapidly becoming popular, have high-output electric motors, and the power supply circuit that drives them requires a reactor that can withstand high voltage and large current. There are strong requirements for this reactor to be compact, low noise, low loss, and durable, and the magnetic core material used in the reactor is required to have a high magnetic permeability μ in addition to a high saturation magnetic flux density Bs.
大電流用のリアクトル磁心として前述の圧粉磁心を用いたものがある。低損失が求められる圧粉磁心には、アモルファス混合粉末やナノ結晶混合粉末が用いられる（特許文献１参照）。しかしながら、アモルファス混合粉末等の初透磁率は、温度に対して負の係数を有するため、従来のリアクトルやモータコア等の磁性部品の導体に大電流を流した際にジュール熱が発生し、リアクトルの飽和磁束密度ＢｓやインダクタンスＬの磁気性能が悪化してしまう問題があった。 There are reactor cores for large currents that use the powder core described above. Amorphous mixed powder and nanocrystalline mixed powder are used for powder magnetic cores that require low loss (see Patent Document 1). However, since the initial magnetic permeability of amorphous mixed powder has a negative coefficient with respect to temperature, Joule heat is generated when a large current is passed through the conductor of magnetic parts such as conventional reactors and motor cores, which causes There was a problem that the magnetic performance of the saturation magnetic flux density Bs and the inductance L deteriorated.
また、アモルファス混合粉末等を用いたリアクトルにおいても、その組成に依存して透磁率が温度に対して負の係数を有する場合があり、同様にインダクタンスＬが低下する問題があった。 Further, even in a reactor using an amorphous mixed powder or the like, the magnetic permeability may have a negative coefficient with respect to temperature depending on the composition, and there is a problem that the inductance L similarly decreases.
さらには、上述したアモルファス混合粉末等では、絶対的な透磁率が不十分であり、インダクタＬを大きくすることができず、コイルの巻き数増大に伴ってリアクトルは必然的に大型化してしまうという問題があった。 Furthermore, the above-mentioned amorphous powder mixture has insufficient absolute magnetic permeability, making it impossible to increase the inductor L, and as the number of coil turns increases, the reactor inevitably becomes larger. There was a problem.
本発明は、特に高透磁率であって、リアクトル等の磁性部品の小型化に寄与することができる圧粉磁心及びその製造方法を提供することを目的とする。 An object of the present invention is to provide a powder magnetic core that has particularly high magnetic permeability and can contribute to downsizing of magnetic components such as reactors, and a method for manufacturing the same.
上記目的を達成すべく、本発明者らは鋭意検討を行った。その結果、長径Ｌ１と短径Ｌ２との比（Ｌ１／Ｌ２）が１．１～５．０の範囲のナノ結晶粉末を準備し、このナノ結晶粉末に展性粉末を混合して混合粉末を得、その後、混合粉末を成型して圧粉体を形成し、当該圧粉体を含む圧粉磁心を製造することにより、この圧粉磁心（圧粉体）の成型方向と垂直な方向にナノ結晶粉末が配向、すなわち、ナノ結晶粉末の長軸が配向し、当該配向方向に高い透磁率を示すことを見出した。 In order to achieve the above object, the present inventors conducted extensive studies. As a result, nanocrystalline powder having a ratio of the major axis L1 to the minor axis L2 (L1/L2) in the range of 1.1 to 5.0 was prepared, and a malleable powder was mixed with this nanocrystalline powder to form a mixed powder. After that, by molding the mixed powder to form a green compact and manufacturing a powder magnetic core containing the green compact, nano-sized particles are formed in a direction perpendicular to the molding direction of this powder magnetic core (green compact). It has been found that the crystal powder is oriented, that is, the long axis of the nanocrystal powder is oriented, and exhibits high magnetic permeability in the oriented direction.
すなわち、本発明は、以下に示す通りである。
（１）長径Ｌ１と短径Ｌ２との比（Ｌ１／Ｌ２）が１．１～５．０の範囲のナノ結晶粉末と、展性粉末とからなる圧粉体を含み、前記圧粉体の成型方向に垂直な方向に対する当該ナノ結晶粉末の配向角が４５°未満である粉末の割合が６５～８５％であることを特徴とする、圧粉磁心。
成型
（２）前記展性粉末のビッカース硬さＨｖが５００以下であることを特徴とする、（１）に記載の圧粉磁心。
（３）前記圧粉体における前記展性粉末の割合が、１０～９０％であることを特徴とする、（１）又は（２）に記載の圧粉磁心。
（４）前記圧粉体における前記展性粉末の前記ナノ結晶粉末に対する粒径比が１以下であることを特徴とする、（１）～（３）のいずれか１つに記載の圧粉磁心。
（５）前記ナノ結晶粉末の結晶化度が２５％以上であることを特徴とする、（１）～（４）のいずれか１つに記載の圧粉磁心。
（６）前記ナノ結晶粉末の結晶粒径が４５ｎｍ以下であることを特徴とする、（１）～（５）のいずれか１つに記載の圧粉磁心。
（７）前記ナノ結晶粉末の組成が、原子％で、
Ｓｉ：０～１７％、
Ｂ：２～１５％、
Ｐ：０～１５％、
Ｃｒ＋Ｎｂ：０～５％、
Ｃｕ：０．２～２％、
残部：Ｆｅ＋不可避不純物であることを特徴とする、（１）～（６）のいずれか１つに記載の圧粉磁心。
（８）長径Ｌ１と短径Ｌ２との比（Ｌ１／Ｌ２）が１．１～５．０の範囲のナノ結晶粉末を準備する工程と、前記ナノ結晶粉末と展性粉末とを混合して混合粉末を調整する工程と、前記混合粉末を成型して圧粉体を形成し、当該圧粉体を含む圧粉磁心を製造する工程と、を含むことを特徴とする、圧粉磁心の製造方法。
（９）前記展性粉末のビッカース硬さＨｖが５００以下であることを特徴とする、（８）に記載の圧粉磁心の製造方法。
（１０）前記圧粉体における前記展性粉末の割合が、１０～９０％であることを特徴とする、（８）又は（９）に記載の圧粉磁心の製造方法。
（１１）前記圧粉体における前記展性粉末の前記ナノ結晶粉末に対する粒径比が１以下であることを特徴とする、（８）～（１０）のいずれか１つに記載の圧粉磁心の製造方法。
（１２）前記ナノ結晶粉末の結晶化度が２５％以上であることを特徴とする、（８）～（１１）のいずれか１つに記載の圧粉磁心の製造方法。
（１３）前記ナノ結晶粉末の結晶粒径が４５ｎｍ以下であることを特徴とする、（８）～（１２）のいずれか１つに記載の圧粉磁心の製造方法。
（１４）前記ナノ結晶粉末の組成が、原子％で、
Ｓｉ：０～１７％、
Ｂ：２～１５％、
Ｐ：０～１５％、
Ｃｒ＋Ｎｂ：０～５％、
Ｃｕ：０．２～２％、
残部：Ｆｅ＋不可避不純物であることを特徴とする、（８）～（１３）のいずれか１つに記載の圧粉磁心の製造方法。
That is, the present invention is as shown below.
(1) A compact comprising a nanocrystalline powder having a ratio of the major axis L1 to the minor axis L2 (L1/L2) in the range of 1.1 to 5.0 and malleable powder; A powder magnetic core, characterized in that the ratio of the powder in which the orientation angle of the nanocrystal powder with respect to the direction perpendicular to the molding direction is less than 45° is 65 to 85%.
Molding (2) The powder magnetic core according to (1), wherein the malleable powder has a Vickers hardness Hv of 500 or less.
(3) The powder magnetic core according to (1) or (2), wherein the proportion of the malleable powder in the powder compact is 10 to 90%.
(4) The powder magnetic core according to any one of (1) to (3), characterized in that the particle size ratio of the malleable powder to the nanocrystalline powder in the powder compact is 1 or less. .
(5) The dust core according to any one of (1) to (4), wherein the nanocrystalline powder has a crystallinity of 25% or more.
(6) The powder magnetic core according to any one of (1) to (5), wherein the nanocrystalline powder has a crystal grain size of 45 nm or less.
(7) The composition of the nanocrystal powder is in atomic %,
Si: 0-17%,
B: 2-15%,
P: 0-15%,
Cr+Nb: 0-5%,
Cu: 0.2-2%,
The powder magnetic core according to any one of (1) to (6), characterized in that the remainder: Fe + inevitable impurities.
(8) a step of preparing nanocrystalline powder having a ratio of major axis L1 to minor axis L2 (L1/L2) in a range of 1.1 to 5.0; and mixing the nanocrystalline powder and malleable powder. Manufacturing a powder magnetic core, comprising the steps of: adjusting a mixed powder; molding the mixed powder to form a green compact; and manufacturing a powder magnetic core containing the green compact. Method.
(9) The method for producing a powder magnetic core according to (8), wherein the malleable powder has a Vickers hardness Hv of 500 or less.
(10) The method for producing a powder magnetic core according to (8) or (9), wherein the proportion of the malleable powder in the powder compact is 10 to 90%.
(11) The powder magnetic core according to any one of (8) to (10), wherein a particle size ratio of the malleable powder to the nanocrystalline powder in the powder compact is 1 or less. manufacturing method.
(12) The method for producing a powder magnetic core according to any one of (8) to (11), wherein the nanocrystalline powder has a crystallinity of 25% or more.
(13) The method for producing a powder magnetic core according to any one of (8) to (12), wherein the nanocrystalline powder has a crystal grain size of 45 nm or less.
(14) The composition of the nanocrystal powder is in atomic %,
Si: 0-17%,
B: 2-15%,
P: 0-15%,
Cr+Nb: 0-5%,
Cu: 0.2-2%,
The method for producing a powder magnetic core according to any one of (8) to (13), wherein the remainder is Fe + inevitable impurities.
なお、一般的に圧粉体は複数の面を有する金型にナノ結晶粉末や展性粉末などの磁性粉と結合材を充填し、成型圧を加えて製造する。これらの面のうち、成型圧を加える面と、これに対向する金型の面を結ぶ方向に成型圧が加わる。言い換えると、これらの面に対応する圧粉体の外面のいずれかより圧粉体へ成型圧が加わっているので、一般にはその外面に垂直な方向が成型方向となる。おおむねナノ結晶粉末の長径が向いている方向に垂直な方向が成型方向となる。成型方向は磁路に垂直な方向とすることが一般的である。 Note that powder compacts are generally manufactured by filling a multi-sided mold with magnetic powder such as nanocrystalline powder or malleable powder and a binder, and applying molding pressure. Among these surfaces, molding pressure is applied in a direction connecting the surface to which molding pressure is applied and the opposing surface of the mold. In other words, since molding pressure is applied to the powder compact from any of the outer surfaces of the powder compact corresponding to these surfaces, generally the direction perpendicular to the outer surface is the direction of molding. The molding direction is approximately perpendicular to the direction in which the long axis of the nanocrystalline powder is facing. The molding direction is generally perpendicular to the magnetic path.
本発明によれば、特に高透磁率であって、リアクトル等の磁性部品の小型化に寄与することができる圧粉磁心及びその製造方法を提供することができる。 According to the present invention, it is possible to provide a powder magnetic core that has particularly high magnetic permeability and can contribute to downsizing of magnetic components such as reactors, and a method for manufacturing the same.
以下、本発明の詳細及びその他の特徴について、発明を実施するための形態に基づいて説明する。 Hereinafter, details and other features of the present invention will be explained based on the detailed description.
本発明で使用するナノ結晶粉末は、長径Ｌ１と短径Ｌ２との比（Ｌ１／Ｌ２）が１．１～５．０の範囲であることが好ましく、１．２～３．５の範囲であることが好ましい。ナノ結晶粉末の長径Ｌ１と短径Ｌ２との比（Ｌ１／Ｌ２）が上記範囲にあることで、圧粉磁心（圧粉体）の成型方向と垂直な方向にナノ結晶粉末が配向、すなわち、ナノ結晶粉末の長軸が配向し、当該配向方向に高い透磁率を示す。 The nanocrystalline powder used in the present invention preferably has a ratio of major axis L1 to minor axis L2 (L1/L2) in the range of 1.1 to 5.0, and preferably in the range of 1.2 to 3.5. It is preferable that there be. When the ratio (L1/L2) of the long axis L1 to the short axis L2 of the nanocrystal powder is within the above range, the nanocrystal powder is oriented in a direction perpendicular to the molding direction of the powder magnetic core (powder compact), that is, The long axis of the nanocrystalline powder is oriented and exhibits high magnetic permeability in the direction of orientation.
なお、上記比（Ｌ１／Ｌ２）が１．１未満であると、ナノ結晶粉末の配向性が劣化してしまい配向方向における透磁率が減少してしまう。また、上記比（Ｌ１／Ｌ２）が５．０を超えると、圧粉体中のナノ結晶粉末の充填性が減少し、圧粉体、すなわち圧粉磁心の密度が減少してしまうので、飽和磁束密度及び透磁率等の磁気特性が劣化してしまう。 Note that if the above ratio (L1/L2) is less than 1.1, the orientation of the nanocrystal powder will deteriorate and the magnetic permeability in the orientation direction will decrease. Furthermore, if the above ratio (L1/L2) exceeds 5.0, the filling properties of the nanocrystalline powder in the green compact decrease, and the density of the green compact, that is, the powder magnetic core, decreases, resulting in saturation. Magnetic properties such as magnetic flux density and magnetic permeability deteriorate.
また、本発明で使用する展性粉末は、上記ナノ結晶粉末よりも柔らかく、展性に優れていれば特に限定されないが、好ましくはビッカース硬さＨｖが５００以下、より好ましくは４５０未満、さらに好ましくは２５０未満である。これによって、展性粉末が、ナノ結晶粉末が、圧粉磁心（圧粉体）の成型方向と垂直な方向に配向しやすくする助剤として機能するようになるので、当該ナノ結晶粉末が、圧粉磁心（圧粉体）の成型方向と垂直な方向に配向し、すなわち、ナノ結晶粉末の長軸が配向して、当該配向方向に高い透磁率を示す。 Further, the malleable powder used in the present invention is not particularly limited as long as it is softer than the nanocrystalline powder and has excellent malleability, but preferably has a Vickers hardness Hv of 500 or less, more preferably less than 450, and even more preferably is less than 250. As a result, the malleable powder functions as an auxiliary agent that facilitates the orientation of the nanocrystalline powder in the direction perpendicular to the molding direction of the powder magnetic core (powder compact), so that the nanocrystalline powder is The nanocrystalline powder is oriented in a direction perpendicular to the molding direction of the powder magnetic core (powder compact), that is, the long axis of the nanocrystalline powder is oriented, and exhibits high magnetic permeability in the orientation direction.
なお、ビッカース硬さＨｖの下限値は特に限定されないが、例えば５０とすることができる。当該下限値より小さくても、最早ナノ結晶粉末の配向性に影響を与えず、透磁率の増大に寄与しない。 Note that the lower limit value of the Vickers hardness Hv is not particularly limited, but may be set to 50, for example. Even if it is smaller than the lower limit, it no longer affects the orientation of the nanocrystalline powder and does not contribute to an increase in magnetic permeability.
上述のような展性粉末としては、純鉄粉、カルボニル鉄粉、センダスト粉末、Ｆｅ－Ｎｉ粉末、Ｆｅ－Ｓｉ－Ｃｒ粉末、Ｆｅ－Ｓｉ粉末、Ｆｅ－Ｃｒ系軟磁性粉末等を用いることができる。 As the above-mentioned malleable powder, pure iron powder, carbonyl iron powder, sendust powder, Fe-Ni powder, Fe-Si-Cr powder, Fe-Si powder, Fe-Cr-based soft magnetic powder, etc. can be used. can.
圧粉体における展性粉末の割合は１０～９０％であることが好ましく、３０～７０％であることがより好ましい。展性粉末の割合が上記範囲であると、上述のように、展性粉末が、ナノ結晶粉末が、圧粉磁心（圧粉体）の成型方向と垂直な方向に配向しやすくする助剤として機能するようになるので、当該ナノ結晶粉末が、圧粉磁心（圧粉体）の成型方向と垂直な方向に配向し、すなわち、ナノ結晶粉末の長軸が配向して、当該配向方向に高い透磁率を示す。 The proportion of malleable powder in the compact is preferably 10 to 90%, more preferably 30 to 70%. When the proportion of the malleable powder is within the above range, the malleable powder acts as an auxiliary agent that makes it easier for the nanocrystalline powder to orient in the direction perpendicular to the molding direction of the powder magnetic core (powder compact), as described above. To function, the nanocrystalline powder is oriented in a direction perpendicular to the molding direction of the powder magnetic core (powder compact), that is, the long axis of the nanocrystalline powder is oriented, and the nanocrystalline powder is oriented in the direction of the orientation. Indicates magnetic permeability.
なお、展性粉末の割合が１０％未満であると、上記作用効果が小さくなり、十分な透磁率を得ることができない場合があり、９０％を超えると、配向により透磁率に寄与するナノ結晶粉末の割合が減少してしまい、同様に、十分な透磁率を得ることができない場合がある。 Note that if the proportion of malleable powder is less than 10%, the above-mentioned effects will be reduced and sufficient magnetic permeability may not be obtained. If it exceeds 90%, nanocrystals that contribute to magnetic permeability due to orientation The proportion of powder decreases, and it may also be impossible to obtain sufficient magnetic permeability.
上述した展性粉末の割合は、圧粉磁心の電子顕微鏡写真において５００μｍ×５００μｍの領域を画定し、当該領域における展性粉末のナノ結晶粉末に対する面積比から求めたものである。 The proportion of the malleable powder described above was determined by defining a region of 500 μm×500 μm in an electron micrograph of the powder magnetic core and determining the area ratio of the malleable powder to the nanocrystalline powder in the region.
また、展性粉末のナノ結晶粉末に対する粒径比（展性粉末の粒径／ナノ結晶粉末）は１以下であることが好ましく、さらには０．４５未満であることが好ましい。この場合、ナノ結晶粉末が、圧粉磁心（圧粉体）の成型方向と垂直な方向に配向しやすくなるので、当該ナノ結晶粉末が、圧粉磁心（圧粉体）の成型方向と垂直な方向に配向し、すなわち、ナノ結晶粉末の長軸が配向して、当該配向方向に高い透磁率を示す。 Further, the particle size ratio of the malleable powder to the nanocrystalline powder (particle size of the malleable powder/nanocrystalline powder) is preferably 1 or less, and more preferably less than 0.45. In this case, the nanocrystalline powder is easily oriented in a direction perpendicular to the molding direction of the powder magnetic core (powder compact), so that the nanocrystalline powder is oriented perpendicular to the molding direction of the powder magnetic core (powder compact). In other words, the long axes of the nanocrystalline powder are oriented, and exhibit high magnetic permeability in the orientation direction.
なお、上記粒径比の下限値は特に限定されないが、例えば０．０２とすることができる。当該下限値より粒径比を小さくしても、最早配向性に影響を及ぼさず、透磁率に影響を与えない。 Note that the lower limit of the particle size ratio is not particularly limited, but may be set to 0.02, for example. Even if the particle size ratio is made smaller than the lower limit value, it no longer affects the orientation and does not affect the magnetic permeability.
また、ナノ結晶粉末の結晶化度は２５％以上であることが好ましく、さらには３５％以上であることが好ましい。この場合、ｂｃｃ－Ｆｅ（－Ｓｉ）の結晶割合が増大するので、飽和磁束密度や透磁率などの磁気特性が良好となる。 Further, the degree of crystallinity of the nanocrystalline powder is preferably 25% or more, more preferably 35% or more. In this case, since the crystal proportion of bcc-Fe(-Si) increases, magnetic properties such as saturation magnetic flux density and magnetic permeability become better.
なお、ナノ結晶粉末の結晶化度の上限は特に限定されないが、例えば７０％である。当該上限値を超えて結晶化度が増大しても、最早磁気特性に影響を与えない。 Note that the upper limit of the crystallinity of the nanocrystalline powder is not particularly limited, but is, for example, 70%. Even if the crystallinity increases beyond the upper limit, it no longer affects the magnetic properties.
また、ナノ結晶粉末の結晶粒径は、４５ｎｍ以下であることが好ましく、３０ｎｍ以下であることがさらに好ましい。この場合、保磁力が小さくなるので、圧粉磁心としての磁気特性が良好となる。なお、１０ｎｍ未満としても最早保磁力の減少には影響を与えないので、当該値が下限値となる。 Further, the crystal grain size of the nanocrystalline powder is preferably 45 nm or less, more preferably 30 nm or less. In this case, since the coercive force becomes small, the magnetic properties as a powder magnetic core are improved. Note that even if it is less than 10 nm, it no longer affects the decrease in coercive force, so this value becomes the lower limit.
次に、本発明のナノ結晶粉末の組成成分について説明する。なお、特に断らない限り、以下に示す％は原子％である。 Next, the compositional components of the nanocrystalline powder of the present invention will be explained. Note that unless otherwise specified, the percentages shown below are atomic percentages.
Ｓｉ：０～１７％
Ｓｉは、ΔＴ（化合物析出温度とｂｃｃ－Ｆｅ（－Ｓｉ）析出温度の差）を拡大して安定的に熱処理を行うための元素である。Ｓｉが１７％を超えるとアモルファス形成能が低下し、非晶質を主相とする粉末を得ることが困難となり、熱処理後の軟磁気特性が劣化する。
Si: 0-17%
Si is an element for expanding ΔT (difference between compound precipitation temperature and bcc-Fe(-Si) precipitation temperature) to stably perform heat treatment. If Si exceeds 17%, the ability to form an amorphous layer decreases, making it difficult to obtain a powder having an amorphous main phase, and the soft magnetic properties after heat treatment deteriorate.
Ｂ：２～１５％
Ｂが２％未満であると、急冷によるアモルファス相の形成が困難になり、熱処理後の軟磁気特性が低下する。Ｂが１５％を超えると、融点が高くなり製造上好ましくなく、アモルファス形成能も低下して軟磁気特性が劣化するので好ましくない。
B: 2-15%
If B is less than 2%, it becomes difficult to form an amorphous phase by rapid cooling, and the soft magnetic properties after heat treatment deteriorate. If B exceeds 15%, the melting point becomes high, which is unfavorable in terms of manufacturing, and the ability to form an amorphous layer also decreases, resulting in deterioration of soft magnetic properties.
Ｐ：０～１５％
Ｐは、微細で均一なナノ結晶粉末を形成しやすく、良好な磁気特性を得るための元素である。Ｐが１５％を超えると、他のメタロイド元素とのバランスが悪くなり、アモルファス形成能が低下して、飽和磁束密度が低下する。
P: 0-15%
P is an element that easily forms fine and uniform nanocrystalline powder and provides good magnetic properties. When P exceeds 15%, the balance with other metalloid elements deteriorates, the ability to form an amorphous layer decreases, and the saturation magnetic flux density decreases.
Ｃｒ＋Ｎｂ：０～５％
Ｃｒは粉末表面に酸化膜を形成し、耐食性を向上させる作用がある。また、Ｎｂは、ナノ結晶化の際に、ｂｃｃ結晶粒の成長を抑制し、微細なナノ結晶粉末を形成させる作用がある。しかしながら、Ｃｒ及びＮｂを添加することで相対的にＦｅ量が減少し、飽和磁束密度が減少する。また、アモルファス形成能が低下してしまうため、５％以下であることが好ましい。
Cr+Nb: 0-5%
Cr forms an oxide film on the powder surface and has the effect of improving corrosion resistance. Furthermore, Nb has the effect of suppressing the growth of BCC crystal grains and forming fine nanocrystal powder during nanocrystallization. However, by adding Cr and Nb, the amount of Fe is relatively reduced, and the saturation magnetic flux density is reduced. Furthermore, since the ability to form an amorphous layer decreases, the content is preferably 5% or less.
Ｃｕ：０．２～２％
Ｃｕが０．２％未満ではナノ結晶化熱処理時のクラスター析出が少なく、均一なナノ結晶化が困難となる。一方、Ｃｕが２％を超えると、Ｃｕ量が過多となるため、アモルファス形成能が低下し、軟磁気特性が低下してしまう。
Cu: 0.2-2%
If Cu is less than 0.2%, there will be little cluster precipitation during nanocrystallization heat treatment, making uniform nanocrystalization difficult. On the other hand, when Cu exceeds 2%, the amount of Cu becomes excessive, so that the ability to form an amorphous layer decreases and the soft magnetic properties deteriorate.
不可避不純物
不可避不純物としては、Ｃｏ，Ｎｉ，Ｚｎ，Ｚｒ，Ｈｆ，Ｍｏ，Ｔａ，Ｗ，Ａｇ，Ａｕ，Ｐｄ，Ｋ，Ｃａ，Ｍｇ，Ｓｎ，Ｔｉ，Ｖ，Ｍｎ，Ａｌ，Ｓ，Ｃ，Ｏ，Ｎ，Ｂｉ，希土類元素から選ばれる少なくとも１種であることが好ましい。このような元素が含まれることにより、熱処理後において、均一なナノ結晶粉末を容易に得ることができる。
Unavoidable impurities Unavoidable impurities include Co, Ni, Zn, Zr, Hf, Mo, Ta, W, Ag, Au, Pd, K, Ca, Mg, Sn, Ti, V, Mn, Al, S, C, O , N, Bi, and rare earth elements. By including such elements, uniform nanocrystalline powder can be easily obtained after heat treatment.
なお、ナノ結晶粉末は、原料となる純鉄、フェロシリコン、フェロリン、フェロボロン、フェロクロム及び電解銅などを１２５０～１４５０℃の温度で溶解して粉末化して得ることができる。 Note that nanocrystalline powder can be obtained by melting and powdering raw materials such as pure iron, ferrosilicon, ferroline, ferroboron, ferrochrome, and electrolytic copper at a temperature of 1250 to 1450°C.
また、粉末化は、例えば、水アトマイズ法、ガスアトマイズ法、回転水流アトマイズ法、スプレー法、キャビテーション法、スパークエロージョン法等の各種粉末化法により行うことができるが、水アトマイズ法、ガスアトマイズ法、回転水流アトマイズ法等のアトマイズ法が好ましい。アトマイズ法は、母合金を高周波誘導加熱装置で溶解し、母合金の溶湯をノズルから高速で噴射してできた合金溶湯の流れに冷却媒体（液体又は気体）を衝突させて、合金溶湯を微細化すると共に急冷し、ナノ結晶粉末を得る方法である。かかる方法によれば、極めて微小なナノ結晶粉末を効率よく製造することができる。 Powderization can be performed by various powdering methods such as water atomization method, gas atomization method, rotary water flow atomization method, spray method, cavitation method, and spark erosion method, but water atomization method, gas atomization method, rotation An atomization method such as a water jet atomization method is preferred. In the atomization method, the mother alloy is melted using a high-frequency induction heating device, and the molten mother alloy is injected from a nozzle at high speed. A cooling medium (liquid or gas) is collided with the flow of the molten alloy, making the molten alloy fine. In this method, nanocrystalline powder is obtained by rapidly cooling the nanocrystalline powder. According to this method, extremely fine nanocrystalline powder can be efficiently produced.
なお、目的とするナノ結晶粉末を得るに際には、上述のように、例えばアトマイズ法で得た粉末を適宜、不活性雰囲気中で、所定の時間、例えば０～１８０分間、所定の温度、例えば３５０～６００℃で熱処理してもよい。なお、熱処理温度が０分というのは、昇温中に反応が終了してしまう場合を意味するものである。熱処理雰囲気は、粉末の表面酸化を抑制するためには不活性雰囲気が望ましいが、特定の目的のために大気等の酸化雰囲気や水素等の還元雰囲気でも可能である。 In addition, when obtaining the desired nanocrystal powder, as mentioned above, the powder obtained by, for example, the atomization method is suitably heated in an inert atmosphere for a predetermined time, for example, 0 to 180 minutes, at a predetermined temperature, For example, heat treatment may be performed at 350 to 600°C. Note that the heat treatment temperature of 0 minutes means that the reaction ends during the temperature increase. The heat treatment atmosphere is preferably an inert atmosphere in order to suppress surface oxidation of the powder, but for specific purposes, an oxidizing atmosphere such as air or a reducing atmosphere such as hydrogen may also be used.
本発明の圧粉磁心を得るには、上述のようにして得たナノ結晶粉末と展性粉末とを混合して混合粉末を調整し、その後、当該混合粉末を例えば１９０～２０００ＭＰａの成型圧力で成型して圧粉体を形成することによって、当該圧粉体から目的とする圧粉磁心を得ることができる。 In order to obtain the powder magnetic core of the present invention, a mixed powder is prepared by mixing the nanocrystalline powder obtained as described above and a malleable powder, and then the mixed powder is subjected to a molding pressure of, for example, 190 to 2000 MPa. By molding to form a powder compact, a desired powder magnetic core can be obtained from the compact.
このとき、圧粉体の成型方向に垂直な方向に対する当該ナノ結晶粉末の配向角が４５°未満である粉末の割合が６５～８５％、好ましくは７０～８０％である。したがって、特に高透磁率であって、リアクトル等の磁性部品の小型化に寄与することができる圧粉磁心及びその製造方法を提供することができる。 At this time, the proportion of the powder in which the orientation angle of the nanocrystal powder with respect to the direction perpendicular to the molding direction of the green compact is less than 45° is 65 to 85%, preferably 70 to 80%. Therefore, it is possible to provide a powder magnetic core that has particularly high magnetic permeability and can contribute to downsizing of magnetic components such as reactors, and a method for manufacturing the same.
なお、混合粉末を成型する際には、適宜、結合材を混合し、圧粉体を熱処理して当該結合材を硬化させ、当該結合材を介してナノ結晶粉末及び展性粉末を結合するようにすることもできる。 In addition, when molding the mixed powder, a binder is mixed as appropriate, the green compact is heat-treated to harden the binder, and the nanocrystal powder and malleable powder are bonded through the binder. It can also be done.
結着材としては、例えば、シリコーン系樹脂、エポキシ系樹脂、フェノール系樹脂、ポリアミド系樹脂、ポリイミド系樹脂、ポリフェニレンサルファイド系樹脂等の有機材料、リン酸マグネシウム、リン酸カルシウム、リン酸亜鉛、リン酸マンガン、リン酸カドミウムのようなリン酸塩、ケイ酸ナトリウムのようなケイ酸塩（水ガラス）等の熱硬化性無機材料等が挙げられる。 Examples of the binder include organic materials such as silicone resin, epoxy resin, phenol resin, polyamide resin, polyimide resin, and polyphenylene sulfide resin, magnesium phosphate, calcium phosphate, zinc phosphate, and manganese phosphate. , thermosetting inorganic materials such as phosphates such as cadmium phosphate, silicates (water glass) such as sodium silicate, and the like.
（実施例１～５及び比較例１～２）
工業純鉄、フェロシリコン、フェロリン、フェロボロン、及び電解銅からなる原料を所定の合金組成（Ｆｅ８１．９Ｓｉ４Ｂ７Ｐ６．５Ｃｕ０．６）になるように秤量し、不活性雰囲気中、高周波溶解を用いて１４５０℃にて溶解した。その後、溶解した合金溶湯を水アトマイズ法にて処理し、－６３μｍ、±９０μｍ、±１５０μｍ、±２５０μｍで分級し、合金粉末を作製した。
(Examples 1 to 5 and Comparative Examples 1 to 2)
Raw materials consisting of industrially pure iron, ferrosilicon, ferroline, ferroboron, and electrolytic copper were weighed to have a predetermined alloy composition (Fe 81.9 Si 4 B 7 P 6.5 Cu 0.6 ) and placed in an inert atmosphere. Melting was performed at 1450°C using medium and high frequency melting. Thereafter, the molten alloy was treated by water atomization and classified at −63 μm, ±90 μm, ±150 μm, and ±250 μm to produce alloy powder.
赤外線加熱装置を用いて、得られた合金粉末を不活性雰囲気中で加熱した。合金粉末を毎分３０℃の昇温速度で４４０℃まで加熱して２０分保持し、その後、空冷した。熱処理後の粉末（ナノ結晶粉末）をＸＲＤにより解析したところ、いずれの粉末も結晶化度は４５％、結晶粒径は３５ｎｍであった。 The obtained alloy powder was heated in an inert atmosphere using an infrared heating device. The alloy powder was heated to 440°C at a heating rate of 30°C per minute, held for 20 minutes, and then cooled in air. When the heat-treated powders (nanocrystalline powders) were analyzed by XRD, the crystallinity of each powder was 45% and the crystal grain size was 35 nm.
次いで、ナノ結晶粉末にビッカース硬さＨｖが３５０のＦｅ－Ｓｉ－Ｃｒ粉末（展性粉末）を３０質量％の割合で混合し、得られた混合粉末に対して質量比で３％となるように結合材を加え、攪拌混合した。ここでは、結合材として、シリコーン樹脂を使用した。 Next, Fe-Si-Cr powder (malleable powder) having a Vickers hardness Hv of 350 was mixed with the nanocrystal powder at a ratio of 30% by mass, so that the mass ratio was 3% with respect to the obtained mixed powder. The binder was added to the mixture and mixed by stirring. Here, silicone resin was used as the binding material.
次いで、目開き５００μｍのメッシュを用いて、結合材を混合した混合粉末の粒度調整を行い、造粒粉末を得た。この造粒粉末の２．０ｇを秤量し、金型に入れ、油圧式自動プレス機により圧力２９４ＭＰａにて成型し、外形１３ｍｍ、内径８ｍｍの円筒形状の圧粉体を製造した。 Next, the particle size of the mixed powder containing the binder was adjusted using a mesh with an opening of 500 μm to obtain a granulated powder. 2.0 g of this granulated powder was weighed, put into a mold, and molded using a hydraulic automatic press machine at a pressure of 294 MPa to produce a cylindrical green compact with an outer diameter of 13 mm and an inner diameter of 8 mm.
次いで、圧粉体を恒温槽内に入れて、大気中１５０℃にて２時間保持し、結合材を硬化させた。 Next, the green compact was placed in a constant temperature bath and held at 150° C. in the atmosphere for 2 hours to harden the binder.
作製した圧粉磁心の磁気特性評価として、インピーダンスアナライザを用いて、周波数１ＭＨｚにおける初透磁率μを測定した。また、電子顕微鏡を用いて圧粉磁心の断面観察を行い、ナノ結晶粉末の形状（長径Ｌ１と短径Ｌ２の比：Ｌ１／Ｌ２）における長径方向の、圧粉体の成型方向に垂直な方向に対してなす角度である配向角を測定した。具体的には、圧粉磁心を冷間樹脂中に埋め込み硬化し、圧粉磁心の磁路と垂直に研磨することで圧粉磁心の断面を作製した。ＥＤＸ（Ｅｎｅｒｇｙ Ｄｉｓｐｅｒｓｉｖｅ Ｘ－ｒａｙ ｓｐｅｃｔｒｏｐｙ：エネルギー分散型Ｘ線分析）による元素マッピングから、圧粉磁心断面におけるナノ結晶粉末を３０個以上ランダムに選択し、各粉末の長径Ｌ１と短径Ｌ２を測定するとともに、配向角を調べた。長径Ｌ１は、各粉末の中で最も長い線分となるところ、短径Ｌ２は、長径に対して垂直な線分のうち、最も長いところとした。 To evaluate the magnetic properties of the produced powder magnetic core, the initial magnetic permeability μ at a frequency of 1 MHz was measured using an impedance analyzer. In addition, the cross section of the powder magnetic core was observed using an electron microscope, and the direction perpendicular to the molding direction of the powder compact in the major axis direction in the shape of the nanocrystalline powder (ratio of major axis L1 to minor axis L2: L1/L2). The orientation angle, which is the angle made with respect to Specifically, a powder magnetic core was embedded in a cold resin and hardened, and a cross section of the powder magnetic core was prepared by polishing perpendicular to the magnetic path of the powder magnetic core. From elemental mapping using EDX (Energy Dispersive X-ray spectroscopy), randomly select 30 or more nanocrystal powders in the cross section of the dust core, and measure the major axis L1 and minor axis L2 of each powder. At the same time, the orientation angle was also investigated. The major axis L1 was the longest line segment in each powder, and the minor axis L2 was the longest line segment perpendicular to the major axis.
配向角は、Ｌ１／Ｌ２比が１．１以上となるナノ結晶粉末を対象に、成型方向に垂直な方向に対するＬ１の角度を約１００個について計測し、４５°未満となる粉末の割合を算出した。 For the orientation angle, measure the angle of L1 with respect to the direction perpendicular to the molding direction for approximately 100 nanocrystalline powders with an L1/L2 ratio of 1.1 or more, and calculate the proportion of powders with an orientation angle of less than 45°. did.
表１に、ナノ結晶粉末として、－６３μｍ、±９０μｍ、±１５０μｍ、±２５０μｍで分級した合金粉末を用いた場合の、圧粉磁心の磁気特性と粉末形状、配向角４５度未満の割合を示す。 Table 1 shows the magnetic properties of the dust core, the powder shape, and the proportion of orientation angles of less than 45 degrees when alloy powders classified at -63 μm, ±90 μm, ±150 μm, and ±250 μm are used as nanocrystal powder. .
これより、目開きが大きい篩で分級した粉末の方が、初透磁率及びＬ１／Ｌ２比が高く配向角４５度未満の割合が高いことが分かる。すなわち、異形状のナノ結晶粉末の長軸が、圧粉磁心の成型方向に垂直な方向に配向していることが分かる。また、Ｌ１／Ｌ２比が大きすぎる場合は、充填率が低下し、初透磁率が下がってしまった。 From this, it can be seen that the powder classified using a sieve with a large opening has a higher initial magnetic permeability and a higher L1/L2 ratio, and a higher proportion of the orientation angle is less than 45 degrees. That is, it can be seen that the long axis of the irregularly shaped nanocrystal powder is oriented in a direction perpendicular to the molding direction of the dust core. Moreover, when the L1/L2 ratio was too large, the filling rate decreased and the initial magnetic permeability decreased.
分級時の目開きが大きいほど異形状の粉末が多くなって、ナノ結晶粉末の長軸が、圧粉磁心の成型方向に垂直な方向に配向する理由は、アトマイズ時に、水で分断された合金溶湯が小さい場合には、表面張力で球状になりやすいが、大きい分断溶湯は球状化する前に凝固するためである。 The larger the opening during classification, the more irregularly shaped powder there is, and the long axis of the nanocrystalline powder is oriented in a direction perpendicular to the molding direction of the dust core. This is because when the molten metal is small, it tends to become spherical due to surface tension, but when the molten metal is large, it solidifies before it becomes spherical.
（実施例６～８及び比較例３）
工業純鉄、フェロシリコン、フェロリン、フェロボロン、フェロクロム及び電解銅からなる原料を所定の合金組成（Ｆｅ８１．４Ｓｉ２．５Ｂ６Ｐ８．５Ｃｒ１．０Ｃｕ０．６）になるように秤量し、不活性雰囲気中、高周波溶解を用いて１２５０～１５５０℃にて溶解した。その後、溶解した合金溶湯を水アトマイズ法にて処理し、－４５μｍで分級し、合金粉末を作製した。
(Examples 6 to 8 and Comparative Example 3)
Raw materials consisting of industrially pure iron, ferrosilicon, ferroline, ferroboron, ferrochrome, and electrolytic copper are made into a predetermined alloy composition (Fe 81.4 Si 2.5 B 6 P 8.5 Cr 1.0 Cu 0.6 ). and melted at 1250-1550°C using high frequency melting in an inert atmosphere. Thereafter, the molten alloy was treated by water atomization and classified at -45 μm to produce alloy powder.
赤外線加熱装置を用いて、得られた合金粉末を不活性雰囲気中で加熱した。合金粉末を毎分３０℃の昇温速度で４３０℃まで加熱して２０分保持し、その後、空冷した。熱処理後の粉末（ナノ結晶粉末）をＸＲＤにより解析したところ、いずれの粉末も結晶化度は４０％、結晶粒径は２４ｎｍであった。 The obtained alloy powder was heated in an inert atmosphere using an infrared heating device. The alloy powder was heated to 430°C at a heating rate of 30°C per minute, held for 20 minutes, and then cooled in air. When the heat-treated powders (nanocrystalline powders) were analyzed by XRD, the crystallinity of each powder was 40% and the crystal grain size was 24 nm.
次いで、ナノ結晶粉末にビッカース硬さＨｖが１１０のカルボニル鉄粉（展性粉末）を４０質量％の割合で混合し、得られた混合粉末に対して質量比で２．５％となるように結合材を加え、攪拌混合した。ここでは、結合材として、フェノール樹脂を使用した。 Next, carbonyl iron powder (malleable powder) having a Vickers hardness Hv of 110 was mixed with the nanocrystal powder at a ratio of 40% by mass, so that the mass ratio was 2.5% with respect to the obtained mixed powder. The binder was added and mixed by stirring. Here, phenol resin was used as the binding material.
次いで、目開き５００μｍのメッシュを用いて、結合材を混合した混合粉末の粒度調整を行い、造粒粉末を得た。この造粒粉末の２．５ｇを秤量し、金型に入れ、油圧式自動プレス機により圧力２９４ＭＰａにて成型し、外形１３ｍｍ、内径８ｍｍの円筒形状の圧粉体を製造した。次いで、圧粉体を恒温槽内に入れて、大気中１５０℃にて２時間保持し、結合材を硬化させた。 Next, the particle size of the mixed powder containing the binder was adjusted using a mesh with an opening of 500 μm to obtain a granulated powder. 2.5 g of this granulated powder was weighed, put into a mold, and molded using a hydraulic automatic press at a pressure of 294 MPa to produce a cylindrical green compact with an outer diameter of 13 mm and an inner diameter of 8 mm. Next, the green compact was placed in a constant temperature bath and held at 150° C. in the atmosphere for 2 hours to harden the binder.
次いで、実施例１等と同様に、作製した圧粉磁心の磁気特性評価として、インピーダンスアナライザを用いて、周波数１ＭＨｚにおける初透磁率μを測定した。また、電子顕微鏡を用いて圧粉磁心の断面観察を行い、ナノ結晶粉末の形状（長径Ｌ１と短径Ｌ２の比：Ｌ１／Ｌ２）及び配向角を測定した。 Next, in the same manner as in Example 1, the initial magnetic permeability μ at a frequency of 1 MHz was measured using an impedance analyzer to evaluate the magnetic properties of the produced powder magnetic core. In addition, a cross section of the dust core was observed using an electron microscope, and the shape of the nanocrystalline powder (ratio of major axis L1 to minor axis L2: L1/L2) and orientation angle were measured.
表２に、ナノ結晶粉末として、１２５０～１５５０℃で溶解した合金粉末を用いた場合の、初透磁率、Ｌ１／Ｌ２比及び配向角４５度未満の割合を示した。 Table 2 shows the initial magnetic permeability, L1/L2 ratio, and proportion of orientation angle of less than 45 degrees when alloy powder melted at 1250 to 1550° C. is used as nanocrystal powder.
表２から、溶解温度の低い粉末の方が、Ｌ１／Ｌ２比が大きく及び配向角４５度未満の割合が高く、初透磁率が高いことが分かる。これは溶解温度の低い方が合金溶湯が凝固するまでの時間が短くなり、表面張力によって球状化する前に凝固して異形状となり、ナノ結晶粉末の長軸が、圧粉磁心の成型方向に垂直な方向に配向するためである。 From Table 2, it can be seen that the powder with a lower melting temperature has a larger L1/L2 ratio, a higher proportion of orientation angles of less than 45 degrees, and a higher initial magnetic permeability. This is because the lower the melting temperature, the shorter the time it takes for the molten alloy to solidify, and the nanocrystalline powder solidifies into an irregular shape before it becomes spheroidized due to surface tension, and the long axis of the nanocrystalline powder is aligned with the molding direction of the dust core. This is because the orientation is perpendicular.
（実施例９～１５）
工業純鉄、フェロシリコン、フェロリン、フェロボロン、フェロニオブ、フェロクロム及び電解銅からなる原料を表３に示すような合金組成になるように秤量し、不活性雰囲気中、高周波溶解を用いて１４５０℃にて溶解した。その後、溶解した合金溶湯を水アトマイズ法にて処理し、－１５０μｍで分級し、合金粉末を作製した。
(Examples 9 to 15)
Raw materials consisting of industrially pure iron, ferrosilicon, ferroline, ferroboron, ferroniobium, ferrochrome, and electrolytic copper were weighed to give the alloy composition shown in Table 3, and heated at 1450°C using high frequency melting in an inert atmosphere. Dissolved. Thereafter, the molten alloy was treated by water atomization and classified at -150 μm to produce alloy powder.
赤外線加熱装置を用いて、得られた合金粉末を不活性雰囲気中で加熱した。合金粉末を毎分３０℃の昇温速度で４４０℃まで加熱して２０分保持し、その後、空冷した。次いで、ナノ結晶粉末に表３に示すようなビッカース硬さＨｖの粉末（展性粉末）を４０質量％の割合で混合し、得られた混合粉末に対して質量比で３％となるように結合材を加え、攪拌混合した。ここでは、結合材として、フェノール樹脂を使用した。 The obtained alloy powder was heated in an inert atmosphere using an infrared heating device. The alloy powder was heated to 440°C at a heating rate of 30°C per minute, held for 20 minutes, and then cooled in air. Next, a powder (malleable powder) having a Vickers hardness Hv as shown in Table 3 was mixed with the nanocrystal powder at a ratio of 40% by mass, so that the mass ratio was 3% with respect to the obtained mixed powder. The binder was added and mixed by stirring. Here, phenol resin was used as the binding material.
次いで、目開き５００μｍのメッシュを用いて、結合材を混合した混合粉末の粒度調整を行い、造粒粉末を得た。この造粒粉末の２．５ｇを秤量し、金型に入れ、油圧式自動プレス機により圧力７８０ＭＰａにて成型し、外形１３ｍｍ、内径８ｍｍの円筒形状の圧粉体を製造した。次いで、圧粉体を恒温槽内に入れて、不活性雰囲気中１６０℃にて４時間保持し、結合材を硬化させた。 Next, the particle size of the mixed powder containing the binder was adjusted using a mesh with an opening of 500 μm to obtain a granulated powder. 2.5 g of this granulated powder was weighed, put into a mold, and molded using a hydraulic automatic press machine at a pressure of 780 MPa to produce a cylindrical green compact with an outer diameter of 13 mm and an inner diameter of 8 mm. Next, the green compact was placed in a constant temperature bath and held at 160° C. for 4 hours in an inert atmosphere to harden the binder.
次いで、実施例１等と同様に、作製した圧粉磁心の磁気特性評価として、インピーダンスアナライザを用いて、周波数１ＭＨｚにおける初透磁率μを測定した。また、電子顕微鏡を用いて圧粉磁心の断面観察を行い、ナノ結晶粉末の形状（長径Ｌ１と短径Ｌ２の比：Ｌ１／Ｌ２）及び配向角を測定した。 Next, in the same manner as in Example 1, the initial magnetic permeability μ at a frequency of 1 MHz was measured using an impedance analyzer to evaluate the magnetic properties of the produced powder magnetic core. In addition, a cross section of the dust core was observed using an electron microscope, and the shape of the nanocrystalline powder (ratio of major axis L1 to minor axis L2: L1/L2) and orientation angle were measured.
表３から、添加粉末が軟らかい方が、Ｌ１／Ｌ２比が大きく及び配向角４５度未満の割合が高く、初透磁率が高いことが分かる。これは添加粉末が、ナノ結晶粉末が、圧粉磁心（圧粉体）の成型方向と垂直な方向に配向しやすくする助剤として機能するようになるので、当該ナノ結晶粉末が、圧粉磁心（圧粉体）の成型方向と垂直な方向に配向し、すなわち、ナノ結晶粉末の長軸が配向して、当該配向方向に高い透磁率を示すようになるためである。 Table 3 shows that the softer the additive powder, the larger the L1/L2 ratio, the higher the proportion of orientation angles of less than 45 degrees, and the higher the initial magnetic permeability. This is because the additive powder functions as an auxiliary agent that makes it easier for the nanocrystalline powder to orient in the direction perpendicular to the molding direction of the powder magnetic core (powder compact). This is because the nanocrystal powder is oriented in a direction perpendicular to the molding direction of the powder compact, that is, the long axis of the nanocrystal powder is oriented, and exhibits high magnetic permeability in the orientation direction.
（実施例１６～２２）
工業純鉄、フェロシリコン、フェロリン、フェロボロン、フェロニオブ、フェロカーボン、フェロクロム及び電解銅からなる原料を表４に示すような合金組成になるように秤量し、不活性雰囲気中、高周波溶解を用いて１４５０℃にて溶解した。その後、溶解した合金溶湯を水アトマイズ法にて処理し、－１５０μｍで分級し、合金粉末を作製した。
(Examples 16-22)
Raw materials consisting of industrially pure iron, ferrosilicon, ferroline, ferroboron, ferroniobium, ferrocarbon, ferrochrome, and electrolytic copper were weighed to give an alloy composition as shown in Table 4, and heated to 1450% by high-frequency melting in an inert atmosphere. Dissolved at ℃. Thereafter, the molten alloy was treated by water atomization and classified at -150 μm to produce alloy powder.
赤外線加熱装置を用いて、得られた合金粉末を不活性雰囲気中で加熱した。合金粉末を毎分３０℃の昇温速度で４４０℃まで加熱して２０分保持し、その後、空冷した。次いで、ナノ結晶粉末に表４に示すような粉末（展性粉末）を表４に示す割合で混合し、得られた混合粉末に対して質量比で１．５％となるように結合材を加え、攪拌混合した。ここでは、結合材として、フェノール樹脂を使用した。 The obtained alloy powder was heated in an inert atmosphere using an infrared heating device. The alloy powder was heated to 440°C at a heating rate of 30°C per minute, held for 20 minutes, and then cooled in air. Next, powders shown in Table 4 (malleable powders) were mixed with the nanocrystal powder in the proportions shown in Table 4, and a binder was added to the resulting mixed powder at a mass ratio of 1.5%. The mixture was added and mixed by stirring. Here, phenol resin was used as the binding material.
次いで、目開き５００μｍのメッシュを用いて、結合材を混合した混合粉末の粒度調整を行い、造粒粉末を得た。この造粒粉末の４．５ｇを秤量し、金型に入れ、油圧式自動プレス機により圧力２９４ＭＰａにて成型し、外形２０ｍｍ、内径１３ｍｍの円筒形状の圧粉体を製造した。次いで、圧粉体を恒温槽内に入れて、不活性雰囲気中１６０℃にて４時間保持し、結合材を硬化させた。 Next, the particle size of the mixed powder containing the binder was adjusted using a mesh with an opening of 500 μm to obtain a granulated powder. 4.5 g of this granulated powder was weighed, put into a mold, and molded using a hydraulic automatic press at a pressure of 294 MPa to produce a cylindrical green compact with an outer diameter of 20 mm and an inner diameter of 13 mm. Next, the green compact was placed in a constant temperature bath and held at 160° C. for 4 hours in an inert atmosphere to harden the binder.
次いで、実施例１等と同様に、作製した圧粉磁心の磁気特性評価として、インピーダンスアナライザを用いて、周波数１ＭＨｚにおける初透磁率μを測定した。また、電子顕微鏡を用いて圧粉磁心の断面観察を行い、ナノ結晶粉末の形状（長径Ｌ１と短径Ｌ２の比：Ｌ１／Ｌ２）及び配向角を測定した。さらには、展性粉末の添加割合を、圧粉磁心の電子顕微鏡写真において５００μｍ×５００μｍの領域を画定し、当該領域における展性粉末のナノ結晶粉末に対する面積比から求めた。 Next, in the same manner as in Example 1, the initial magnetic permeability μ at a frequency of 1 MHz was measured using an impedance analyzer to evaluate the magnetic properties of the produced powder magnetic core. In addition, a cross section of the dust core was observed using an electron microscope, and the shape of the nanocrystalline powder (ratio of major axis L1 to minor axis L2: L1/L2) and orientation angle were measured. Further, the addition ratio of the malleable powder was determined by defining a region of 500 μm×500 μm in an electron micrograph of the dust core, and determining the area ratio of the malleable powder to the nanocrystalline powder in the region.
表４から、圧粉体における展性粉末の割合が１０～９０％、特に３０～７０％であると、展性粉末が、ナノ結晶粉末が、圧粉磁心（圧粉体）の成型方向と垂直な方向に配向しやすくする助剤として機能するようになるので、当該ナノ結晶粉末が、圧粉磁心（圧粉体）の成型方向と垂直な方向に配向し、すなわち、ナノ結晶粉末の長軸が配向して、当該配向方向に高い透磁率を示すことが分かる。 From Table 4, when the proportion of malleable powder in the powder compact is 10 to 90%, especially 30 to 70%, the malleable powder and the nanocrystalline powder are different from each other in the molding direction of the powder magnetic core (powder compact). Since it functions as an auxiliary agent that facilitates orientation in the vertical direction, the nanocrystalline powder is oriented in the direction perpendicular to the molding direction of the powder magnetic core (powder compact), that is, the length of the nanocrystalline powder is It can be seen that the axes are oriented and high magnetic permeability is exhibited in the orientation direction.
（実施例２３～２８）
工業純鉄、フェロシリコン、フェロリン、フェロボロン、フェロニオブ、フェロカーボン、フェロクロム及び電解銅からなる原料を表５に示すような合金組成になるように秤量し、不活性雰囲気中、高周波溶解を用いて１４５０℃にて溶解した。その後、溶解した合金溶湯を水アトマイズ法にて処理し、－１５０μｍで分級し、合金粉末を作製した。
(Examples 23 to 28)
Raw materials consisting of industrially pure iron, ferrosilicon, ferroline, ferroboron, ferronniobium, ferrocarbon, ferrochrome, and electrolytic copper were weighed to give an alloy composition as shown in Table 5, and heated to 1450% by high-frequency melting in an inert atmosphere. Dissolved at ℃. Thereafter, the molten alloy was treated by water atomization and classified at -150 μm to produce alloy powder.
赤外線加熱装置を用いて、得られた合金粉末を不活性雰囲気中で加熱した。合金粉末を毎分３０℃の昇温速度で４４０℃まで加熱して２０分保持し、その後、空冷した。次いで、ナノ結晶粉末に粉末（展性粉末）を表５に示すような割合で混合し、得られた混合粉末に対して質量比で１．５％となるように結合材を加え、攪拌混合した。ここでは、結合材として、フェノール樹脂を使用した。 The obtained alloy powder was heated in an inert atmosphere using an infrared heating device. The alloy powder was heated to 440°C at a heating rate of 30°C per minute, held for 20 minutes, and then cooled in air. Next, powder (malleable powder) was mixed with the nanocrystal powder in the ratio shown in Table 5, and a binder was added to the resulting mixed powder so that the mass ratio was 1.5%, and the mixture was stirred. did. Here, phenol resin was used as the binding material.
次いで、目開き５００μｍのメッシュを用いて、結合材を混合した混合粉末の粒度調整を行い、造粒粉末を得た。この造粒粉末の４．５ｇを秤量し、金型に入れ、油圧式自動プレス機により圧力２９４ＭＰａにて成型し、外形２０ｍｍ、内径１３ｍｍの円筒形状の圧粉体を製造した。次いで、圧粉体を恒温槽内に入れて、不活性雰囲気中１６０℃にて４時間保持し、結合材を硬化させた。 Next, the particle size of the mixed powder containing the binder was adjusted using a mesh with an opening of 500 μm to obtain a granulated powder. 4.5 g of this granulated powder was weighed, put into a mold, and molded using a hydraulic automatic press at a pressure of 294 MPa to produce a cylindrical green compact with an outer diameter of 20 mm and an inner diameter of 13 mm. Next, the green compact was placed in a constant temperature bath and held at 160° C. for 4 hours in an inert atmosphere to harden the binder.
次いで、実施例１等と同様に、作製した圧粉磁心の磁気特性評価として、インピーダンスアナライザを用いて、周波数１ＭＨｚにおける初透磁率μを測定した。また、電子顕微鏡を用いて圧粉磁心の断面観察を行い、ナノ結晶粉末の形状（長径Ｌ１と短径Ｌ２の比：Ｌ１／Ｌ２）及び配向角を測定した。さらには、展性粉末の添加割合を、圧粉磁心の電子顕微鏡写真において５００μｍ×５００μｍの領域を画定し、当該領域における展性粉末のナノ結晶粉末に対する面積比から求めた。 Next, in the same manner as in Example 1, the initial magnetic permeability μ at a frequency of 1 MHz was measured using an impedance analyzer to evaluate the magnetic properties of the produced powder magnetic core. In addition, a cross section of the dust core was observed using an electron microscope, and the shape of the nanocrystalline powder (ratio of major axis L1 to minor axis L2: L1/L2) and orientation angle were measured. Further, the addition ratio of the malleable powder was determined by defining a region of 500 μm×500 μm in an electron micrograph of the dust core, and determining the area ratio of the malleable powder to the nanocrystalline powder in the region.
表５から、展性粉末のナノ結晶粉末に対する粒径比（展性粉末の粒径／ナノ結晶粉末）は１以下、特に０．４５未満の場合、ナノ結晶粉末が、圧粉磁心（圧粉体）の成型方向と垂直な方向に配向しやすくなるので、当該ナノ結晶粉末が、圧粉磁心（圧粉体）の成型方向と垂直な方向に配向し、すなわち、ナノ結晶粉末の長軸が配向して、当該配向方向に高い透磁率を示すようになる。 From Table 5, when the particle size ratio of malleable powder to nanocrystalline powder (particle size of malleable powder/nanocrystalline powder) is less than 1, especially less than 0.45, nanocrystalline powder The nanocrystalline powder is easily oriented in the direction perpendicular to the molding direction of the powder core (powder body), so the long axis of the nanocrystalline powder is oriented perpendicular to the molding direction of the powder magnetic core (powder compact). It becomes oriented and exhibits high magnetic permeability in the orientation direction.
以上、本発明のいくつかの実施形態を説明したが、これらの実施形態は例として掲示したものであり、発明の範囲を限定することは意図していない。これら新規な実施形態は、その他の様々な形態で実施されることが可能であり、発明の要旨を逸脱しない範囲で、種々の省略、置き換え、変更を行うことができる。これら実施形態やその変形は、発明の範囲や要旨に含まれるとともに、特許請求の範囲に記載された発明とその均等の範囲に含まれる。 Although several embodiments of the present invention have been described above, these embodiments are presented as examples and are not intended to limit the scope of the invention. These novel embodiments can be implemented in various other forms, and various omissions, substitutions, and changes can be made without departing from the gist of the invention. These embodiments and their modifications are included within the scope and gist of the invention, as well as within the scope of the invention described in the claims and its equivalents.
Claims (7)
前記圧粉体の成型方向に垂直な方向に対する当該ナノ結晶粉末の配向角が４５度未満である粉末の割合が６５～８５％であることを特徴とする、圧粉磁心。 A compact comprising nanocrystalline powder having a ratio of the major axis L1 to the minor axis L2 (L1/L2) in the range of 1.1 to 5.0 and malleable powder,
A powder magnetic core, characterized in that the ratio of the powder in which the orientation angle of the nanocrystalline powder with respect to the direction perpendicular to the molding direction of the powder compact is less than 45 degrees is 65 to 85%.
Ｓｉ：０～１７％、
Ｂ：２～１５％、
Ｐ：０～１５％、
Ｃｒ＋Ｎｂ：０～５％、
Ｃｕ：０．２～２％、
残部：Ｆｅ＋不可避不純物であることを特徴とする、請求項１～６のいずれか１項に記載の圧粉磁心。 The composition of the nanocrystalline powder is in atomic %,
Si: 0-17%,
B: 2-15%,
P: 0-15%,
Cr+Nb: 0-5%,
Cu: 0.2-2%,
The powder magnetic core according to any one of claims 1 to 6, wherein the remainder is Fe + inevitable impurities.
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| JP2015167183A (en) | 2014-03-04 | 2015-09-24 | Ｎｅｃトーキン株式会社 | Nanocrystal soft magnetic alloy powder and powder-compact magnetic core arranged by use thereof |
| WO2019065500A1 (en) | 2017-09-29 | 2019-04-04 | 株式会社トーキン | Method for manufacturing powder magnetic core, powder magnetic core, and inductor |
| JP2019057693A (en) | 2017-09-22 | 2019-04-11 | 株式会社村田製作所 | Composite magnetic material and coil component using the same |
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| JP2015167183A (en) | 2014-03-04 | 2015-09-24 | Ｎｅｃトーキン株式会社 | Nanocrystal soft magnetic alloy powder and powder-compact magnetic core arranged by use thereof |
| JP2019057693A (en) | 2017-09-22 | 2019-04-11 | 株式会社村田製作所 | Composite magnetic material and coil component using the same |
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