JP5382923B2 - Amorphous soft magnetic alloy powder, dust core and inductor - Google Patents
Amorphous soft magnetic alloy powder, dust core and inductor Download PDFInfo
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- JP5382923B2 JP5382923B2 JP2009111244A JP2009111244A JP5382923B2 JP 5382923 B2 JP5382923 B2 JP 5382923B2 JP 2009111244 A JP2009111244 A JP 2009111244A JP 2009111244 A JP2009111244 A JP 2009111244A JP 5382923 B2 JP5382923 B2 JP 5382923B2
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- 239000003638 chemical reducing agent Substances 0.000 claims description 42
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- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
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- Powder Metallurgy (AREA)
- Soft Magnetic Materials (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Description
本発明は低粒径かつ高飽和磁束密度を有する非晶質軟磁性合金粉末及びこれを用いた圧粉磁心並びにインダクタに関する。 The present invention relates to an amorphous soft magnetic alloy powder having a low particle size and a high saturation magnetic flux density, a dust core and an inductor using the same.
近年、各種電子機器の小型化、高機能化が進行しており、それに伴い、これら電子機器に内蔵されるコイル、トランスなどのインダクタ部品において、小型化と同時に大電流下におけるインダクタンスが求められている。これらの要求を満足させるには、磁心の高飽和磁束密度化と高周波域における損失特性を同時に向上させることが必要とされている。 In recent years, various electronic devices have been reduced in size and advanced in function. As a result, inductors such as coils and transformers incorporated in these electronic devices have been required to be downsized and have inductance under a large current. Yes. In order to satisfy these requirements, it is necessary to simultaneously increase the saturation magnetic flux density of the magnetic core and to improve the loss characteristics in the high frequency range.
高周波域で使用されるインダクタ部品における磁心材料としては、一般的にソフトフェライトや高珪素鋼、軟磁性金属粉末(純鉄粉、Fe-Si-Cr粉、Fe-Si粉、パーマロイ粉、鉄系非晶質粉など)などが挙げられる。 The core material of inductor components used in high frequency ranges is generally soft ferrite, high silicon steel, soft magnetic metal powder (pure iron powder, Fe-Si-Cr powder, Fe-Si powder, permalloy powder, iron-based material) Amorphous powder).
ソフトフェライトを用いた場合、比抵抗が高いことにより渦電流損失を小さくできるが、飽和磁束密度が低いという欠点を有している。また、高珪素鋼は薄板化して絶縁処理を施したものを積層することで高周波用磁心として用いられるが、加工できる形状が限定されることが難点であった。 When soft ferrite is used, eddy current loss can be reduced due to its high specific resistance, but it has the disadvantage of low saturation magnetic flux density. Moreover, although high silicon steel is used as a high frequency magnetic core by laminating thin silicon plates that have been subjected to insulation treatment, it has been difficult to limit the shapes that can be processed.
また、軟磁性金属粉末は樹脂等の絶縁材料と混合したものを圧縮成形して圧粉磁心として用いられている。圧粉磁心は粉末を絶縁性のある樹脂等で被覆することによって渦電流を低減することで損失特性を向上させる。更に、高い飽和磁束密度と形状自由度を有することから、軟磁性金属粉末を用いた圧粉磁心が盛んに利用されている。 Soft magnetic metal powder is used as a powder magnetic core by compression molding a mixture of an insulating material such as resin. The dust core improves the loss characteristics by reducing the eddy current by coating the powder with an insulating resin or the like. Furthermore, since it has a high saturation magnetic flux density and a high degree of freedom in shape, dust cores using soft magnetic metal powder are actively used.
軟磁性金属粉末を用いた圧粉磁心を高周波域で使用する場合、粒径を小さくすることで渦電流の発生をより低減できることが知られている。そこで、高周波域で使用可能な低粒径の軟磁性金属粉末として、平均粒径:約3μm〜10μmのカルボニル鉄粉が一般的に用いられている。しかし、カルボニル鉄粉は低粒径で、高い飽和磁束密度を持つ一方、結晶質であることから結晶磁気異方性や磁気歪みによりヒステリシス損失が増大してしまうことが問題とされている。 It is known that when a dust core using soft magnetic metal powder is used in a high frequency range, the generation of eddy current can be further reduced by reducing the particle size. Therefore, carbonyl iron powder having an average particle size of about 3 μm to 10 μm is generally used as a soft magnetic metal powder having a low particle size that can be used in a high frequency range. However, while carbonyl iron powder has a low particle size and high saturation magnetic flux density, it is problematic that hysteresis loss increases due to magnetocrystalline anisotropy and magnetostriction because it is crystalline.
そこで、特定方位の結晶構造を持たないことから結晶磁気異方性が無く、且つヒステリシス損失が小さく、高い飽和磁束密度を有する非晶質軟磁性合金粉末の圧粉磁心への適用が進められている。 Therefore, since it does not have a crystal structure of a specific orientation, there is no crystal magnetic anisotropy, hysteresis loss is small, and application of amorphous soft magnetic alloy powder having a high saturation magnetic flux density to a dust core has been promoted. Yes.
非晶質軟磁性合金粉末は製造時に104K/sec以上の高い急冷速度を必要とし、その製造は水アトマイズ法やガスアトマイズ法によるのみで、従来技術によって作製可能な粉末の平均粒径は10μm程度が限界である。 Amorphous soft magnetic alloy powder requires a high quenching rate of 10 4 K / sec or more at the time of production, and the production is only by the water atomization method or the gas atomization method. The average particle size of the powder that can be produced by the conventional technique is 10 μm. The degree is the limit.
一方で、特許文献1、2、3において、金属塩の水溶液とP系還元剤の水溶液を、錯化剤、pH調整剤およびpH緩衝剤の存在下で反応させることによる、平均粒径0.5μm〜10μmの球状非晶質粉末の製造方法が開示されている。しかしながら、これらの製造方法によって製造されるのはCo−Ni−P、Ni−P、Co−P非晶質合金粉末であり、その飽和磁束密度はFe基非晶質合金粉末と比較して遥かに低いものであると考えられる。 On the other hand, in Patent Documents 1, 2, and 3, an average particle size of 0.1 by reacting an aqueous solution of a metal salt and an aqueous solution of a P-based reducing agent in the presence of a complexing agent, a pH adjusting agent, and a pH buffering agent. A method for producing spherical amorphous powders of 5 μm to 10 μm is disclosed. However, these manufacturing methods produce Co—Ni—P, Ni—P, and Co—P amorphous alloy powders, and their saturation magnetic flux density is much higher than that of Fe-based amorphous alloy powders. It is thought that it is very low.
近年求められている電子部品の大電流化、高効率化に対し、特に、軟磁性合金粉末を用いた圧粉磁心において生じる、高周波領域における渦電流損失の増加による損失特性の悪化を低減する必要がある。 In order to increase the current and increase the efficiency of electronic components that have been demanded in recent years, it is necessary to reduce the deterioration of loss characteristics caused by the increase of eddy current loss in the high frequency region, especially in the powder magnetic core using soft magnetic alloy powder. There is.
そこで、本発明の課題は、従来技術による軟磁性合金粉末よりも粒径が小さく、非晶質構造であり、且つ高い飽和磁束密度(Bs)を有する非晶質軟磁性合金粉末を提供することにある。 Accordingly, an object of the present invention is to provide an amorphous soft magnetic alloy powder having a particle size smaller than that of the conventional soft magnetic alloy powder, an amorphous structure, and a high saturation magnetic flux density (Bs). It is in.
本発明はまた、上記の非晶質軟磁性合金粉末を用いた圧粉磁心、及び高周波域で低損失であるインダクタを提供しようとするものである。 Another object of the present invention is to provide a dust core using the amorphous soft magnetic alloy powder and an inductor having a low loss in a high frequency range.
本発明者らは、鉄塩、錯化剤、pH調整剤、分散剤及びP系還元剤を含む原料液を撹拌しながら、B系還元剤を含む還元液を滴下することを特徴とする液相還元法によって、Fe、B、Pのうち少なくともFe、Bから構成され、低粒径且つ高飽和磁束密度(Bs)である非晶質軟磁性合金粉末が得られることを見出し、本発明を完成するに至った。 The present inventors drop a reducing solution containing a B-based reducing agent while stirring a raw material solution containing an iron salt, a complexing agent, a pH adjusting agent, a dispersing agent and a P-based reducing agent. By the phase reduction method, it has been found that an amorphous soft magnetic alloy powder composed of at least Fe and B of Fe, B, and P, having a low particle size and a high saturation magnetic flux density (Bs) can be obtained. It came to be completed.
即ち、本発明によれば、平均粒径が0.01μm以上1.0μm以下の粒子あるいは微細粒子集合体粒子からなる、平均粒径が0.1μm以上5.0μm以下であることを特徴とする非晶質軟磁性合金粉末が得られる。 That is, according to the present invention, the average particle size is 0.1 μm or more and 5.0 μm or less composed of particles or fine particle aggregate particles having an average particle size of 0.01 μm or more and 1.0 μm or less. An amorphous soft magnetic alloy powder is obtained.
また、本発明によれば、上述の非晶質軟磁性合金粉末の組成は5重量%≦B≦10重量%、0重量%≦P≦5重量%で残部はFeからなることを特徴とする非晶質軟磁性合金粉末が得られる。 According to the present invention, the composition of the above-mentioned amorphous soft magnetic alloy powder is 5 wt% ≦ B ≦ 10 wt%, 0 wt% ≦ P ≦ 5 wt%, with the balance being Fe. An amorphous soft magnetic alloy powder is obtained.
また、本発明によれば、上述の非晶質軟磁性合金粉末と結合材との混合物を圧縮成型してなることを特徴とする圧粉磁心が得られる。本発明によれば更に、前記圧粉磁心とコイルとを組み合わせてなるインダクタが得られる。 In addition, according to the present invention, a powder magnetic core obtained by compression molding a mixture of the above-described amorphous soft magnetic alloy powder and a binder can be obtained. Further, according to the present invention, an inductor obtained by combining the dust core and the coil can be obtained.
本発明による非晶質軟磁性合金粉末は、鉄塩、錯化剤、pH調整剤、分散剤及びP系還元剤を含む原料液を撹拌しながら、B系還元剤を含む還元液を滴下する液相還元法に基づいて作製され、従来の水アトマイズ法により得られる金属粉末よりも粒径が小さく、Fe、B、Pのうち少なくともFe、Bから構成され、且つ高い飽和磁束密度(Bs)を有する非晶質軟磁性合金粉末である。更に、得られる非晶質軟磁性合金粉末を圧粉磁心に用いることで、渦電流損失が改善され、従来に比べて特に高周波域において低損失であるインダクタを提供することができる。 The amorphous soft magnetic alloy powder according to the present invention is a solution in which a reducing solution containing a B-based reducing agent is dropped while stirring a raw material solution containing an iron salt, a complexing agent, a pH adjusting agent, a dispersing agent and a P-based reducing agent. It is produced based on the liquid phase reduction method and has a smaller particle size than the metal powder obtained by the conventional water atomization method, and is composed of at least Fe and B among Fe, B and P, and has a high saturation magnetic flux density (Bs). An amorphous soft magnetic alloy powder having Furthermore, by using the obtained amorphous soft magnetic alloy powder for the powder magnetic core, the eddy current loss can be improved, and an inductor having a low loss especially in a high frequency region can be provided as compared with the prior art.
本発明における非晶質軟磁性合金粉末の製造工程は、原料となる鉄塩、錯化剤、分散剤及びP系還元剤を含む原料液及び、B系還元剤を含む還元液を得る原料製造工程、原料液にpH調整剤を投入することで所定のpHに調整するpH調整工程、原料液に対して撹拌しながら還元液を滴下することで非晶質軟磁性合金粉末を得る還元工程の組み合わせからなる。 The production process of the amorphous soft magnetic alloy powder in the present invention is a raw material production that obtains a raw material liquid containing an iron salt, a complexing agent, a dispersant and a P-based reducing agent as a raw material, and a reducing liquid containing a B-based reducing agent. A pH adjusting step for adjusting the pH by adding a pH adjusting agent to the raw material solution, and a reducing step for obtaining an amorphous soft magnetic alloy powder by dropping the reducing solution while stirring the raw material solution. Composed of a combination.
まず、前記原料製造工程においては、原料となる鉄塩、錯化剤、分散剤及びP系還元剤をそれぞれ秤量し、蒸留水と共にビーカー等の耐薬品性容器に投入し、これを撹拌しながら溶解することで原料液を製造する。更に、B系還元剤を秤量し、蒸留水と共に別の耐薬品性容器に投入し、撹拌しながら溶解することで還元液を製造する。 First, in the raw material manufacturing process, the iron salt, complexing agent, dispersing agent and P-based reducing agent as raw materials are weighed and put into a chemical resistant container such as a beaker together with distilled water, while stirring this. A raw material liquid is manufactured by dissolving. Furthermore, a B-type reducing agent is weighed, put into another chemical-resistant container together with distilled water, and dissolved with stirring to produce a reducing solution.
原料として使用可能な鉄塩としては、塩化鉄(II)、塩化鉄(III)、硝酸鉄(III)、硫酸鉄(II)、硫酸鉄(III)、酢酸鉄(II)、しゅう酸鉄(II)、硫酸鉄(II)アンモニウムなどが挙げられるが、同様な効果を奏するものであれば、これらに限定されるものではない。 Iron salts that can be used as raw materials include iron (II) chloride, iron (III) chloride, iron (III) nitrate, iron (II) sulfate, iron (III) sulfate, iron (II) acetate, iron oxalate ( II), ammonium iron (II) sulfate and the like, but are not limited to these as long as the same effect can be obtained.
原料として使用可能な錯化剤としては、塩化アンモニウム、クエン酸三ナトリウム、クエン酸カリウム、クエン酸、クエン酸鉄アンモニウム、酢酸ナトリウム、エチレングリコール、アンモニア水、ヒドラジンなどが挙げられるが、同様な効果を奏するものであれば、これらに限定されるものではない。 Complexing agents that can be used as raw materials include ammonium chloride, trisodium citrate, potassium citrate, citric acid, ammonium iron citrate, sodium acetate, ethylene glycol, ammonia water, hydrazine, etc., but the same effect However, the present invention is not limited to these.
原料として使用可能な分散剤としては、ポリビニルピロリドンが挙げられるが、同様な効果を奏するものであれば、これに限定されるものではない。 Examples of the dispersant that can be used as a raw material include polyvinyl pyrrolidone, but the dispersant is not limited thereto as long as the same effect can be obtained.
原料として使用可能な還元剤としては、P系還元剤として次亜リン酸ナトリウム、次亜リン酸、次亜リン酸アンモニウム、次亜リン酸カルシウム、亜リン酸などが挙げられる。また、B系還元剤としては水素化ホウ素ナトリウム、水素化ホウ素カリウム、ジメチルアミンボランなどが挙げられる。更に、これらの物質に加えてヒドラジンをP系還元剤と併用もしくは代替することができる。これらについても、同様な効果を奏するものであれば、これらに限定されるものではない。 Examples of the reducing agent that can be used as a raw material include sodium hypophosphite, hypophosphorous acid, ammonium hypophosphite, calcium hypophosphite, phosphorous acid and the like as P-based reducing agents. Examples of the B-based reducing agent include sodium borohydride, potassium borohydride, dimethylamine borane and the like. Furthermore, in addition to these substances, hydrazine can be used in combination with or replaced with a P-based reducing agent. These are not limited to these as long as the same effects can be obtained.
続いて、製造した原料液を耐薬品性容器内で撹拌しながらpH調整剤を投入することで、原料液を還元反応の開始に最適なpHに調整する、pH調整工程を行う。ここで、pH調整剤として使用可能な物質としては水酸化ナトリウム、アンモニア水などが挙げられるが、同様な効果を奏するものであれば、これらに限定されるものではない。 Subsequently, a pH adjusting step is performed in which the raw material liquid is adjusted to an optimum pH for the start of the reduction reaction by introducing a pH adjusting agent while stirring the produced raw material liquid in a chemical resistant container. Here, examples of the substance that can be used as the pH adjuster include sodium hydroxide and aqueous ammonia, but the substance is not limited to these as long as the same effect can be obtained.
続いて、pH調整後の原料液を撹拌しながら、別の耐薬品性容器内で調整した還元液を滴下することにより非晶質軟磁性合金粉末を製造する、還元工程を行う。還元工程では、原料液に滴下した還元液の作用により、原料液中に存在するFeイオンが還元され、このとき同時にP及びBも還元されることによってこれらの元素が析出し、Fe、P、Bを含む非晶質軟磁性合金粉末が生成される。 Subsequently, a reducing process is performed in which an amorphous soft magnetic alloy powder is produced by dropping a reducing solution adjusted in another chemical-resistant container while stirring the raw material solution after pH adjustment. In the reduction step, Fe ions existing in the raw material liquid are reduced by the action of the reducing liquid dropped on the raw material liquid, and at the same time, P and B are also reduced, thereby precipitating these elements, Fe, P, An amorphous soft magnetic alloy powder containing B is produced.
次いで、上記非晶質軟磁性合金粉末と結合材を混合し、圧縮成形することで圧粉磁心を製造し、更にこの圧粉磁心をコイルと組み合わせることでインダクタを製造することができる。このとき、圧粉磁心における結合材の含有量は絶縁性を確保する観点から1重量%以上、また著しい飽和磁束密度や透磁率の低下を避けるためには5重量%以下とするのが好ましい。また、圧縮成形時にステアリン酸などの潤滑剤を適宜添加してもよい。 Next, the above-mentioned amorphous soft magnetic alloy powder and a binder are mixed and compression-molded to produce a dust core, and further, this dust core is combined with a coil to produce an inductor. At this time, the content of the binder in the dust core is preferably 1% by weight or more from the viewpoint of ensuring insulation, and 5% by weight or less in order to avoid a significant decrease in saturation magnetic flux density and magnetic permeability. Further, a lubricant such as stearic acid may be appropriately added during compression molding.
ここで、上記非晶質軟磁性合金粉末と混合して用いる結合材としては熱硬化性樹脂が効果的であり、その樹脂の種類は圧粉磁心の用途や必要な耐熱性によって適宜選択することができる。好適に用いられる結合材の例としては、エポキシ樹脂、フェノール樹脂、シリコーン樹脂、ポリアミドイミド樹脂、不飽和ポリエステル樹脂、ジアリルフタレート樹脂、キシレン樹脂などが挙げられるが、同様な効果を奏するものであれば、これらに限定されるものではない。 Here, a thermosetting resin is effective as a binder used by mixing with the amorphous soft magnetic alloy powder, and the type of the resin should be appropriately selected according to the use of the dust core and the required heat resistance. Can do. Examples of binders that can be suitably used include epoxy resins, phenol resins, silicone resins, polyamideimide resins, unsaturated polyester resins, diallyl phthalate resins, xylene resins, and the like, as long as they have similar effects. However, it is not limited to these.
[実施例]
以下、本発明の実施例について具体的に説明する。まず、本発明の非晶質軟磁性合金粉末及びその製造方法の実施例について説明する。
[Example]
Examples of the present invention will be specifically described below. First, examples of the amorphous soft magnetic alloy powder of the present invention and the manufacturing method thereof will be described.
(実施例1)
鉄塩として塩化鉄(II)水和物を1.0mol/l(モル/リットル)、錯化剤として塩化アンモニウム及びクエン酸三ナトリウム水和物をそれぞれ1.5mol/l、0.8mol/l、分散剤としてポリビニルピロリドンを0.004mol/l、P系還元剤として次亜リン酸ナトリウム水和物を1.5mol/lの濃度となるようにそれぞれ秤量し、ガラス製容器内に蒸留水200mlと共に投入した。これを、室温において撹拌機により回転数:160rpm〜300rpmで60〜120分間撹拌することで原料液を作製した。
(Example 1)
Iron salt (II) chloride hydrate as an iron salt is 1.0 mol / l (mol / liter), and ammonium chloride and trisodium citrate hydrate as complexing agents are 1.5 mol / l and 0.8 mol / l, respectively. , Polyvinylpyrrolidone as a dispersant, 0.004 mol / l, sodium hypophosphite hydrate as a P-type reducing agent to a concentration of 1.5 mol / l, and 200 ml of distilled water in a glass container. I put it together. This was stirred at room temperature with a stirrer at a rotation speed of 160 rpm to 300 rpm for 60 to 120 minutes to prepare a raw material liquid.
次に、B系還元剤として水素化ホウ素ナトリウムを0.5mol/lの濃度となるように秤量し、原料液とは別のガラス製容器内に蒸留水150mlと共に投入し、これを室温において撹拌機により回転数:160〜300rpmで5〜10分間撹拌することで還元液を作製した。 Next, sodium borohydride as a B-based reducing agent is weighed so as to have a concentration of 0.5 mol / l, and is poured together with 150 ml of distilled water into a glass container separate from the raw material liquid, and stirred at room temperature. A reducing solution was prepared by stirring for 5 to 10 minutes at a rotational speed of 160 to 300 rpm with a machine.
次に、作製した原料液を室温において撹拌機により回転数:160〜300rpmで撹拌しながら、pH調整剤として30%水酸化ナトリウム水溶液を滴下することで、pH=10となるように調整した。 Next, while stirring the prepared raw material liquid at room temperature with a stirrer at a rotation speed of 160 to 300 rpm, a 30% aqueous sodium hydroxide solution was added dropwise as a pH adjuster to adjust to pH = 10.
次に、撹拌機により回転数:160〜300rpmで撹拌している原料液に対して、滴下装置を用いて滴下速度:200ml/hrで還元液の滴下を行った。また、滴下時においては超音波反応槽により超音波照射しながら滴下しても同様の効果が得られる。滴下終了後、原料液表面からの泡の発生が落ち着いた事を確認してから、析出した粉末を液中から分離し、得た粉末を水洗及びアルコール洗浄した後、不活性雰囲気中で乾燥することで非晶質軟磁性合金粉末を得た。 Next, with respect to the raw material liquid stirred at a rotation speed of 160 to 300 rpm with a stirrer, a reducing solution was dropped at a dropping rate of 200 ml / hr using a dropping device. In addition, the same effect can be obtained by dropping while applying ultrasonic waves in an ultrasonic reaction tank. After completion of dropping, after confirming that the generation of bubbles from the surface of the raw material liquid has settled, the deposited powder is separated from the liquid, and the obtained powder is washed with water and alcohol, and then dried in an inert atmosphere. Thus, an amorphous soft magnetic alloy powder was obtained.
(実施例2〜5、比較例1、2)
次に、B系還元剤である水素化ホウ素ナトリウムの濃度を0.05(比較例1)、0.10(実施例2)、1.00(実施例3)、1.50(実施例4)、2.00(実施例5)、3.00(比較例2)mol/lと変化させ、それ以外は上述した実施例1と同じ製造条件で作業を行い、非晶質軟磁性合金粉末を得た。
(Examples 2 to 5, Comparative Examples 1 and 2)
Next, the concentration of sodium borohydride as the B-based reducing agent was set to 0.05 (Comparative Example 1), 0.10 (Example 2), 1.00 (Example 3), 1.50 (Example 4). ), 2.00 (Example 5), 3.00 (Comparative Example 2) The amount was changed to mol / l, and the other conditions were the same as in Example 1 described above, and the amorphous soft magnetic alloy powder was used. Got.
続いて、得た非晶質軟磁性合金粉末について、ICP発光分析装置を用いた組成分析、BET比表面積計を用いた粒径の測定、振動試料型磁力計(VSM)を用いた飽和磁束密度(Bs)の測定、X線回折(XRD)を用いた結晶構造の同定を行った。実施例1から実施例5及び比較例1、2において得られた非晶質軟磁性合金粉末の組成、平均粒径、飽和磁束密度(Bs)及び結晶構造を表1に示した。 Subsequently, for the obtained amorphous soft magnetic alloy powder, composition analysis using an ICP emission analyzer, measurement of particle diameter using a BET specific surface area meter, saturation magnetic flux density using a vibration sample magnetometer (VSM) Measurement of (Bs) and identification of the crystal structure using X-ray diffraction (XRD) were performed. Table 1 shows the composition, average particle diameter, saturation magnetic flux density (Bs), and crystal structure of the amorphous soft magnetic alloy powders obtained in Examples 1 to 5 and Comparative Examples 1 and 2.
図1は、実施例1の非晶質軟磁性合金粉末における走査型電子顕微鏡(SEM)写真である。図1からわかるように、本発明において得られる非晶質軟磁性合金粉末は、粒子表面に微細粒子の境界が明確に存在する、粒径0.01μm以上1.0μm以下である2個以上の微細粒子の集合体から形成される粒子と、1個の粒子のみから形成される単粒子からなることを特徴としている。 1 is a scanning electron microscope (SEM) photograph of the amorphous soft magnetic alloy powder of Example 1. FIG. As can be seen from FIG. 1, the amorphous soft magnetic alloy powder obtained in the present invention has two or more particles having a particle diameter of 0.01 μm or more and 1.0 μm or less, in which fine particle boundaries are clearly present on the particle surface. It is characterized by comprising particles formed from an aggregate of fine particles and single particles formed from only one particle.
また、図2は、実施例1及び比較例1の非晶質軟磁性合金粉末におけるX線回折結果である。得られた粉末の結晶構造が結晶質か非晶質かの判定は、X線回折プロファイルにより行った。具体的には、結晶質の場合、析出した化合物の結晶構造に由来する鋭いピークが生じ、非晶質の場合は、結晶構造を有しないため、結晶質特有の鋭いピークは見られず、代わりに2θ=45°、80°の位置にブロードなピークが生じる。また、結晶質と非晶質とが混在する場合、結晶質の鋭いピークと非晶質のブロードなピークが共存したX線回折プロファイルが得られる。 FIG. 2 shows X-ray diffraction results for the amorphous soft magnetic alloy powders of Example 1 and Comparative Example 1. Whether the crystal structure of the obtained powder was crystalline or amorphous was determined by an X-ray diffraction profile. Specifically, in the case of crystalline, a sharp peak derived from the crystal structure of the precipitated compound is generated, and in the case of amorphous, since there is no crystal structure, a sharp peak peculiar to crystalline is not seen. A broad peak occurs at 2θ = 45 ° and 80 °. Further, when crystalline and amorphous are mixed, an X-ray diffraction profile in which a sharp peak of crystal and an amorphous broad peak coexist is obtained.
以上の判定基準を基に図2に示したX線回折プロファイルを見てみると、実施例1のX線回折プロファイルは非晶質特有のブロードなピークのみが見られることから、非晶質単相であると判断できる。一方、比較例1のX線回折プロファイルは非晶質特有のブロードなピークの他に、結晶質(α−Fe)の回折ピークが共存していることから、非晶質と結晶質の混相であると判断できる。 When looking at the X-ray diffraction profile shown in FIG. 2 on the basis of the above criteria, the X-ray diffraction profile of Example 1 shows only a broad peak peculiar to amorphous. It can be judged to be a phase. On the other hand, in the X-ray diffraction profile of Comparative Example 1, since the diffraction peak of crystalline (α-Fe) coexists in addition to the broad peak peculiar to amorphous, it is a mixed phase of amorphous and crystalline. It can be judged that there is.
表1に示されるように、B組成が4.80重量%である比較例1の非晶質軟磁性合金粉末の平均粒径が0.05μmであるのに対し、B組成が5.10重量%から10.18重量%の範囲である実施例1から実施例5の非晶質軟磁性合金粉末の平均粒径は0.15μmから4.75μmまでの範囲となった。一方、B組成が11.92重量%である比較例2の非晶質軟磁性合金粉末の平均粒径は6.00μmとなった。 As shown in Table 1, the average particle size of the amorphous soft magnetic alloy powder of Comparative Example 1 having a B composition of 4.80% by weight is 0.05 μm, whereas the B composition is 5.10% by weight. The average particle size of the amorphous soft magnetic alloy powders of Examples 1 to 5 in the range of 0.1% to 10.18% by weight was in the range of 0.15 μm to 4.75 μm. On the other hand, the average particle size of the amorphous soft magnetic alloy powder of Comparative Example 2 having a B composition of 11.92% by weight was 6.00 μm.
また、B組成が4.80重量%から11.92重量%の範囲である比較例1、実施例1から実施例5、比較例2の非晶質軟磁性合金粉末の飽和磁束密度(Bs)は、1.20Tから1.60Tまでの範囲となった。 Further, the saturation magnetic flux density (Bs) of the amorphous soft magnetic alloy powders of Comparative Example 1, Example 1 to Example 5, and Comparative Example 2 in which the B composition is in the range of 4.80 wt% to 11.92 wt%. Was in the range from 1.20T to 1.60T.
また、B組成が5.10重量%から10.18重量%の範囲である実施例1から実施例5の非晶質軟磁性合金粉末の結晶構造は非晶質であった。一方、B組成が4.80重量%である比較例1及び11.92重量%である比較例2から得た粉末の結晶構造は結晶質(α−Fe)と非晶質の混相であった。 Further, the amorphous soft magnetic alloy powders of Examples 1 to 5 having a B composition in the range of 5.10 wt% to 10.18 wt% were amorphous. On the other hand, the crystal structure of the powder obtained from Comparative Example 1 where the B composition is 4.80% by weight and Comparative Example 2 where the B composition is 11.92% by weight was a mixed phase of crystalline (α-Fe) and amorphous. .
上記結果より、B組成が5重量%以上10重量%以下となるようにB系還元剤である水素化ホウ素ナトリウム濃度を調整した還元液を滴下することにより、平均粒径が0.1μm以上5.0μm以下の範囲であり、且つ非晶質相のみから構成される、非晶質軟磁性合金粉末を得ることができる。 From the above results, by adding dropwise a reducing solution in which the concentration of sodium borohydride, which is a B-based reducing agent, is adjusted so that the B composition is 5 wt% or more and 10 wt% or less, the average particle size is 0.1 μm or more and 5 An amorphous soft magnetic alloy powder that is in the range of 0.0 μm or less and is composed of only an amorphous phase can be obtained.
(実施例1、6〜10、比較例3)
次に、P系還元剤である次亜リン酸ナトリウム水和物の濃度を0.00(実施例6)、0.10(実施例7)、0.50(実施例8)、1.50(実施例1)、2.00(実施例9)、3.00(実施例10)、4.00(比較例3)mol/lと変化させ、それ以外は上述した実施例1と同じ製造条件で作業を行い、非晶質軟磁性合金粉末を得た。
(Examples 1, 6 to 10, Comparative Example 3)
Next, the concentration of sodium hypophosphite hydrate as a P-based reducing agent was 0.00 (Example 6), 0.10 (Example 7), 0.50 (Example 8), 1.50. (Example 1), 2.00 (Example 9), 3.00 (Example 10), 4.00 (Comparative Example 3) The production was the same as Example 1 described above except that it was changed to mol / l. Work was performed under conditions to obtain amorphous soft magnetic alloy powder.
続いて、得た非晶質軟磁性合金粉末について、ICP発光分析装置を用いた組成分析、BET比表面積計を用いた粒径の測定、振動試料型磁力計(VSM)を用いた飽和磁束密度(Bs)の測定、X線回折(XRD)を用いた結晶構造の同定を行った。実施例1、実施例6〜10及び比較例3において得られた非晶質軟磁性合金粉末の組成、平均粒径、飽和磁束密度(Bs)及び結晶構造を表2に示した。 Subsequently, for the obtained amorphous soft magnetic alloy powder, composition analysis using an ICP emission analyzer, measurement of particle diameter using a BET specific surface area meter, saturation magnetic flux density using a vibration sample magnetometer (VSM) Measurement of (Bs) and identification of the crystal structure using X-ray diffraction (XRD) were performed. Table 2 shows the composition, average particle diameter, saturation magnetic flux density (Bs), and crystal structure of the amorphous soft magnetic alloy powders obtained in Example 1, Examples 6 to 10 and Comparative Example 3.
表2に示されるように、P組成が0.00重量%から4.73重量%の範囲である実施例1及び実施例6から実施例10の非晶質軟磁性合金粉末の平均粒径は0.12μmから4.00μmまでの範囲となった。一方、P組成が5.81重量%である比較例3の非晶質軟磁性合金粉末の平均粒径は5.80μmとなった。 As shown in Table 2, the average particle sizes of the amorphous soft magnetic alloy powders of Example 1 and Examples 6 to 10 in which the P composition is in the range of 0.00 wt% to 4.73 wt% are The range was from 0.12 μm to 4.00 μm. On the other hand, the average particle diameter of the amorphous soft magnetic alloy powder of Comparative Example 3 having a P composition of 5.81% by weight was 5.80 μm.
また、P組成が0.00重量%から5.81重量%の範囲である実施例1、実施例6から実施例10及び比較例3の非晶質軟磁性合金粉末の飽和磁束密度(Bs)は、1.45Tから1.60Tまでの範囲となった。 Further, the saturation magnetic flux density (Bs) of the amorphous soft magnetic alloy powders of Example 1, Examples 6 to 10 and Comparative Example 3 in which the P composition is in the range of 0.00 wt% to 5.81 wt%. Was in the range from 1.45T to 1.60T.
また、P組成が0.00重量%から4.73重量%の範囲である実施例1及び実施例6から実施例10の非晶質軟磁性合金粉末の結晶構造は非晶質であった。一方、P組成が5.81重量%である比較例3から得た粉末の結晶構造は結晶質(α−Fe)と非晶質の混相であった。 In addition, the crystal structures of the amorphous soft magnetic alloy powders of Example 1 and Examples 6 to 10 in which the P composition was in the range of 0.00 wt% to 4.73 wt% were amorphous. On the other hand, the crystal structure of the powder obtained from Comparative Example 3 having a P composition of 5.81% by weight was a mixed phase of crystalline (α-Fe) and amorphous.
上記結果より、P組成が0重量%以上5重量%以下となるようにP系還元剤である次亜リン酸ナトリウム水和物濃度を調整して原料液を作製することにより、平均粒径が0.1μm以上5.0μm以下の範囲であり、且つ非晶質相のみから構成される、非晶質軟磁性合金粉末を得ることができた。 From the above results, by preparing the raw material liquid by adjusting the concentration of sodium hypophosphite hydrate as the P-based reducing agent so that the P composition is 0 wt% or more and 5 wt% or less, the average particle size is An amorphous soft magnetic alloy powder having a range of 0.1 μm or more and 5.0 μm or less and composed only of an amorphous phase could be obtained.
(実施例1、実施例11〜17)
次に、原料として使用する鉄塩を塩化鉄(II)水和物、塩化鉄(III)水和物、硝酸鉄(III)水和物、硫酸鉄(II)水和物、硫酸鉄(III)水和物、しゅう酸鉄(II)水和物、酢酸鉄(II)、硫酸鉄(II)アンモニウムから選ばれる1種類の鉄塩とし、それ以外は上述した実施例1と同じ製造条件で作業を行い、非晶質軟磁性合金粉末を得た。
(Example 1, Examples 11-17)
Next, the iron salt used as a raw material is iron (II) chloride hydrate, iron (III) chloride hydrate, iron nitrate (III) hydrate, iron sulfate (II) hydrate, iron sulfate (III ) Hydrate, iron (II) oxalate hydrate, iron (II) acetate, iron (II) ammonium sulfate one kind of iron salt, except for the same production conditions as in Example 1 above Work was performed to obtain amorphous soft magnetic alloy powder.
(実施例1、実施例18〜31)
次に、使用する錯化剤を塩化アンモニウム、クエン酸三ナトリウム水和物、酢酸ナトリウム水和物、クエン酸水和物、クエン酸カリウム水和物、クエン酸鉄アンモニウム、エチレングリコール、ヒドラジン、アンモニア水から選ばれる2種類の錯化剤の組み合わせとし、それ以外は上述した実施例1と同じ製造条件で作業を行い、非晶質軟磁性合金粉末を得た。
(Example 1, Examples 18-31)
Next, the complexing agent used is ammonium chloride, trisodium citrate hydrate, sodium acetate hydrate, citric acid hydrate, potassium citrate hydrate, ammonium iron citrate, ethylene glycol, hydrazine, ammonia A combination of two kinds of complexing agents selected from water was used, and the other processes were performed under the same production conditions as in Example 1 to obtain amorphous soft magnetic alloy powder.
(実施例1、実施例32)
次に、使用するpH調整剤を30%水酸化ナトリウム、30%アンモニア水のいずれかとし、それ以外は上述した実施例1と同じ製造条件で作業を行い、非晶質軟磁性合金粉末を得た。
(Example 1, Example 32)
Next, the pH adjuster to be used is either 30% sodium hydroxide or 30% ammonia water, and the other processes are performed under the same production conditions as in Example 1 to obtain an amorphous soft magnetic alloy powder. It was.
(実施例1、実施例33〜39、比較例4)
次に、使用する還元剤として次亜リン酸ナトリウム水和物、次亜リン酸、次亜リン酸アンモニウム、次亜リン酸カルシウム、亜リン酸から選ばれる1種類のP系還元剤と、水素化ホウ素ナトリウム、水素化ホウ素カリウム、ジメチルアミンボランから選ばれる1種類のB系還元剤との組み合わせ、または上述したP系還元剤から選ばれる1種類の還元剤とヒドラジン、もしくは上述したB系還元剤から選ばれる1種類の還元剤とヒドラジンの組み合わせとし、それ以外は上述した実施例1と同じ製造条件で作業を行い、非晶質軟磁性合金粉末を得た。
(Example 1, Examples 33 to 39, Comparative Example 4)
Next, as a reducing agent to be used, one P-based reducing agent selected from sodium hypophosphite hydrate, hypophosphorous acid, ammonium hypophosphite, calcium hypophosphite, phosphorous acid, and borohydride From a combination of one type B reducing agent selected from sodium, potassium borohydride, dimethylamine borane, or one type of reducing agent selected from the P type reducing agent and hydrazine, or from the above B type reducing agent A combination of one selected reducing agent and hydrazine was used, and the other processes were performed under the same production conditions as in Example 1 to obtain amorphous soft magnetic alloy powder.
続いて、得た非晶質軟磁性粉末は実施例1の場合と同様にICP発光分析装置を用いた組成分析、BET比表面積計を用いた粒径の測定、振動試料型磁力計(VSM)を用いた飽和磁束密度(Bs)の測定、X線回折(XRD)を用いた結晶構造の同定を行った。表3には使用した鉄塩と得られた粉末の評価結果を、表4には使用した錯化剤の組み合わせと得られた粉末の評価結果を、表5には使用したpH調整剤の組み合わせと得られた粉末の評価結果を、表6には使用した還元剤の組み合わせと得られた粉末の評価結果を示した。なお、実施例11〜39及び比較例4における各原料の濃度は実施例1と同様とすることで、Fe:91.34重量%、B:7.86重量%、P:0.80重量%となるように試作を行った。また、得られた非晶質軟磁性合金粉末についてICP組成分析を行ったところ、いずれの粉末においても上記組成をほぼ再現する結果が得られた。 Subsequently, the obtained amorphous soft magnetic powder was subjected to composition analysis using an ICP emission analyzer, measurement of particle size using a BET specific surface area meter, vibration sample type magnetometer (VSM), as in Example 1. The saturation magnetic flux density (Bs) was measured using, and the crystal structure was identified using X-ray diffraction (XRD). Table 3 shows the evaluation results of the used iron salt and the obtained powder, Table 4 shows the combination of the complexing agent used and the evaluation result of the obtained powder, and Table 5 shows the combination of the pH adjusting agent used. Table 6 shows the evaluation results of the obtained powder and Table 6 shows the combination of reducing agents used and the evaluation result of the obtained powder. In addition, the density | concentration of each raw material in Example 11-39 and the comparative example 4 shall be the same as that of Example 1, Fe: 91.34 weight%, B: 7.86 weight%, P: 0.80 weight% A prototype was made so that Moreover, when the obtained amorphous soft magnetic alloy powder was subjected to ICP composition analysis, a result that almost reproduced the above composition was obtained in any powder.
表3に示されるように、使用する鉄塩のみを上記鉄塩に置き換えて試作を行った結果、実施例1、実施例11から実施例17で得た非晶質軟磁性合金粉末の平均粒径は0.8μmから1.5μmの範囲となった。 As shown in Table 3, as a result of trial manufacture by replacing only the iron salt to be used with the iron salt, the average grain size of the amorphous soft magnetic alloy powder obtained in Example 1 and Example 11 to Example 17 was obtained. The diameter was in the range of 0.8 μm to 1.5 μm.
また、表3に示されるように、使用する鉄塩のみを上記鉄塩に置き換えて試作を行った結果、実施例1、実施例11から実施例17で得た非晶質軟磁性合金粉末の結晶構造は全て非晶質単相となった。 Moreover, as shown in Table 3, as a result of trial manufacture by replacing only the iron salt to be used with the iron salt, the amorphous soft magnetic alloy powders obtained in Example 1 and Example 11 to Example 17 were obtained. The crystal structure was all amorphous single phase.
上記結果より、原料として使用する鉄塩を、塩化鉄(II)水和物、塩化鉄(III)水和物、硝酸鉄(III)水和物、硫酸鉄(II)水和物、硫酸鉄(III)水和物、しゅう酸鉄(II)水和物、酢酸鉄(II)、硫酸鉄(II)アンモニウムから選ばれる1種類の鉄塩とすることにより、平均粒径が0.1μm以上5.0μm以下の範囲で、P組成:0重量%以上5重量%以下、B組成:5重量%以上10重量%以下であり、且つ非晶質相のみで構成される、非晶質軟磁性合金粉末を得ることができた。 From the above results, the iron salt used as a raw material is iron (II) chloride hydrate, iron (III) chloride hydrate, iron nitrate (III) hydrate, iron sulfate (II) hydrate, iron sulfate (III) Hydrate, iron oxalate (II) hydrate, iron acetate (II), and iron (II) ammonium sulfate as one kind of iron salt, the average particle size is 0.1μm or more Amorphous soft magnetism in a range of 5.0 μm or less, P composition: 0% by weight to 5% by weight, B composition: 5% by weight to 10% by weight, and comprising only an amorphous phase Alloy powder could be obtained.
なお、表3に示した鉄塩から選ばれる2種類以上の鉄塩を組み合わせて使用した場合や、上記以外の鉄塩を使用した場合でも、同様な効果を奏するものであれば、それに限定されるものではない。 It should be noted that even when two or more types of iron salts selected from the iron salts shown in Table 3 are used in combination, or when iron salts other than those described above are used, the same effect can be obtained. It is not something.
表4に示されるように、使用する錯化剤のみを上記錯化剤から選ばれる2種類の物質に置き換えて試作を行った結果、実施例1、実施例18から実施例31で得た粉末の平均粒径は0.8μmから2.3μmの範囲となった。 As shown in Table 4, as a result of trial manufacture by replacing only the complexing agent to be used with two kinds of substances selected from the above complexing agents, powders obtained in Example 1 and Example 18 to Example 31 were obtained. The average particle size of was in the range of 0.8 μm to 2.3 μm.
また、表4に示されるように、使用する錯化剤のみを上記錯化剤から選ばれる2種類の物質に置き換えて試作を行った結果、実施例1、実施例18から実施例31で得た粉末の結晶構造は全て非晶質単相となった。 Further, as shown in Table 4, as a result of trial manufacture by replacing only the complexing agent to be used with two kinds of substances selected from the above complexing agents, the results obtained in Example 1 and Example 18 to Example 31 were obtained. The crystal structure of all the powders became an amorphous single phase.
上記結果より、使用する錯化剤を塩化アンモニウム、クエン酸三ナトリウム水和物、酢酸ナトリウム水和物、クエン酸水和物、クエン酸カリウム水和物、クエン酸鉄アンモニウム、エチレングリコール、ヒドラジン、アンモニア水から選ばれる2種類の錯化剤の組み合わせとすることにより、平均粒径が0.1μm以上5.0μm以下の範囲で、P組成:0重量%以上5重量%以下、B組成:5重量%以上10重量%以下であり、且つ非晶質相のみで構成される非晶質軟磁性合金粉末を得ることができた。 From the above results, the complexing agent used is ammonium chloride, trisodium citrate hydrate, sodium acetate hydrate, citric acid hydrate, potassium citrate hydrate, ammonium iron citrate, ethylene glycol, hydrazine, By using a combination of two complexing agents selected from aqueous ammonia, P composition: 0 wt% or more and 5 wt% or less, B composition: 5 It was possible to obtain amorphous soft magnetic alloy powder that was not less than 10% by weight and not more than 10% by weight and constituted only by an amorphous phase.
また、表4に示した以外の上記錯化剤の組み合わせや、上記錯化剤の3種類以上の組み合わせ、更に上記以外の錯化剤を用いた場合でも、同様な効果を奏するものであれば、それに限定されるものではない。 In addition, combinations of the above complexing agents other than those shown in Table 4, combinations of three or more of the above complexing agents, and even when other complexing agents other than those described above are used, the same effects can be obtained. It is not limited to that.
表5に示されるように、使用するpH調整剤のみを上記pH調整剤に置き換えて試作を行った結果、実施例1及び実施例32で得た粉末の平均粒径は0.9μmから1.0μmの範囲となった。 As shown in Table 5, as a result of trial manufacture by replacing only the pH adjuster to be used with the above pH adjuster, the average particle size of the powders obtained in Example 1 and Example 32 was 0.9 μm to 1. The range was 0 μm.
また、表5に示されるように、使用するpH調整剤のみを上記pH調整剤に置き換えて試作を行った結果、実施例1及び実施例32で得た粉末の結晶構造は全て非晶質単相となった。 Further, as shown in Table 5, as a result of trial manufacture by replacing only the pH adjuster to be used with the above pH adjuster, the crystal structures of the powders obtained in Example 1 and Example 32 were all amorphous. Became a phase.
上記結果より、使用するpH調整剤を水酸化ナトリウム、アンモニア水から選ばれるpH調整剤とすることにより、平均粒径が0.1μm以上5.0μm以下の範囲で、P組成:0重量%以上5重量%以下、B組成:5重量%以上10重量%以下であり、且つ非晶質相のみで構成される、非晶質軟磁性合金粉末を得ることができた。 From the above results, when the pH adjuster to be used is a pH adjuster selected from sodium hydroxide and aqueous ammonia, the average particle size is in the range of 0.1 μm to 5.0 μm, P composition: 0 wt% or more An amorphous soft magnetic alloy powder having 5% by weight or less, B composition: 5% by weight or more and 10% by weight or less and composed only of an amorphous phase could be obtained.
また、表5に示したpH調整剤の2種類以上の組み合わせや、それ以外のpH調整剤を用いた場合でも、同様な効果を奏するものであれば、それに限定されるものではない。 Further, even when two or more combinations of pH adjusting agents shown in Table 5 or other pH adjusting agents are used, the same effects are not limited thereto.
表6に示されるように、使用する還元剤のみを上記還元剤から選ばれる2種類の物質に置き換えて試作を行った結果、実施例1、実施例33から実施例39で得た粉末の平均粒径は0.8μmから1.5μmの範囲となった。 As shown in Table 6, as a result of trial manufacture by replacing only the reducing agent to be used with two kinds of substances selected from the above reducing agents, the average of the powders obtained in Example 1, Example 33 to Example 39 The particle size ranged from 0.8 μm to 1.5 μm.
また、表6に示されるように、使用する還元剤のみを上記還元剤から選ばれる2種類の物質に置き換えて試作を行った結果、実施例1、実施例33から実施例39で得た粉末の結晶構造は全て非晶質単相となった。 Further, as shown in Table 6, as a result of trial manufacture by replacing only the reducing agent to be used with two kinds of substances selected from the above reducing agents, the powders obtained in Example 1, Example 33 to Example 39 were obtained. The crystal structure of all became an amorphous single phase.
一方、使用する還元剤を次亜リン酸ナトリウムとヒドラジンの組み合わせとして作製した比較例4の場合、平均粒径0.5μmの粉末が得られたが、いずれの還元剤にもBは含まれていないため、得られた粉末のB組成は5重量%以上10重量%以下を満たしておらず、更にその結晶構造も結晶質と非晶質の混相であった。 On the other hand, in the case of Comparative Example 4 in which the reducing agent used was a combination of sodium hypophosphite and hydrazine, a powder having an average particle size of 0.5 μm was obtained, but B was included in any reducing agent. Therefore, the B composition of the obtained powder did not satisfy 5% by weight or more and 10% by weight or less, and the crystal structure was a mixed phase of crystalline and amorphous.
上記結果より、使用する還元剤として次亜リン酸ナトリウム水和物、次亜リン酸、次亜リン酸アンモニウム、次亜リン酸カルシウム、亜リン酸から選ばれる1種類のP系還元剤と水素化ホウ素ナトリウム、水素化ホウ素カリウム、ジメチルアミンボランから選ばれる1種類のB系還元剤との組み合わせ、もしくは上述したB系還元剤から選ばれる1種類の還元剤とヒドラジンの組み合わせとすることにより、平均粒径が0.1μm以上5.0μm以下の範囲で、P組成:0重量%以上5重量%以下、B組成:5重量%以上10重量%以下であり、且つ非晶質相のみで構成される、非晶質軟磁性合金粉末を得ることができた。 From the above results, one reducing agent selected from sodium hypophosphite hydrate, hypophosphorous acid, ammonium hypophosphite, calcium hypophosphite and phosphorous acid as a reducing agent to be used and borohydride By using a combination of one type B reducing agent selected from sodium, potassium borohydride, and dimethylamine borane, or a combination of one type of reducing agent selected from the aforementioned B type reducing agent and hydrazine, the average particle size In the range of 0.1 μm to 5.0 μm in diameter, P composition: 0% to 5% by weight, B composition: 5% to 10% by weight, and composed only of an amorphous phase An amorphous soft magnetic alloy powder could be obtained.
また、表6に示した還元剤の2種類以上の組み合わせや、それ以外の還元剤を用いた場合でも、同様な効果を奏するものであれば、それに限定されるものではない。 In addition, even when two or more combinations of reducing agents shown in Table 6 or other reducing agents are used, the same is not limited thereto as long as the same effect is obtained.
続いて、本発明の実施例1、2により得られた非晶質軟磁性合金粉末を熱硬化性樹脂からなる結合材と混合し、圧縮成型して作製したインダクタ用圧粉磁心の実施例について説明する。 Subsequently, examples of the powder magnetic cores for inductors produced by mixing the amorphous soft magnetic alloy powders obtained in Examples 1 and 2 of the present invention with a binder made of a thermosetting resin and compression molding them. explain.
上述の実施例1、2にて作製した非晶質軟磁性合金粉末に対して樹脂成分で3.0重量%の割合となるようにフェノール樹脂を加えて混合した後、その混合物を金型に充填し、面圧:10ton/cm2の圧力で圧縮成型することで、外形13mm、内径8mm、高さ5mmのリング状の圧粉磁心を製造し、樹脂硬化熱処理を行い、インダクタ用圧粉磁心を得た。 After adding and mixing a phenol resin so that it may become a ratio of 3.0 weight% with a resin component with respect to the amorphous soft magnetic alloy powder produced in the above-mentioned Example 1, 2, the mixture was made into a metal mold. Filled and compression molded at a pressure of 10 ton / cm 2 to produce a ring-shaped dust core having an outer diameter of 13 mm, an inner diameter of 8 mm, and a height of 5 mm, followed by resin curing heat treatment, and a dust core for inductors Got.
(比較例5)
比較例5として、カルボニル鉄粉(平均粒径=6μm)に対して樹脂成分で3.0重量%の割合となるようにフェノール樹脂を加えて混合した後、その混合物を金型に充填し、面圧:10ton/cm2の圧力で圧縮成型することで、外形13mm、内径8mm、高さ5mmのリング状の圧粉磁心を製造し、樹脂硬化熱処理を行い、インダクタ用圧粉磁心を得た。
(Comparative Example 5)
As Comparative Example 5, a phenol resin was added and mixed so that the proportion of the resin component was 3.0% by weight with respect to carbonyl iron powder (average particle size = 6 μm), and then the mixture was filled in a mold. Surface pressure: By compression molding at a pressure of 10 ton / cm 2 , a ring-shaped dust core having an outer shape of 13 mm, an inner diameter of 8 mm, and a height of 5 mm was manufactured, and resin curing heat treatment was performed to obtain a dust core for inductors. .
次に、実施例1、2の非晶質軟磁性合金粉末により作製したインダクタ用圧粉磁心、比較例5のインダクタ用圧粉磁心に対して、それぞれ銅線を用いて10ターンの巻線を施したものについて、インピーダンスアナライザーを用いて1kHz以上40MHz以下の周波数範囲におけるQ値を測定し、その測定結果を図3に示した。 Next, a 10-turn winding was made using a copper wire for the dust core for inductor made of the amorphous soft magnetic alloy powder of Examples 1 and 2 and the dust core for inductor of Comparative Example 5 respectively. About what gave, Q value in the frequency range of 1 kHz or more and 40 MHz or less was measured using the impedance analyzer, and the measurement result was shown in FIG.
尚、本発明において取り扱うQ値は、インダクタの特性である共振の鋭さを表し、値が高いほど損失が少ないことを示すものである。 The Q value handled in the present invention represents the sharpness of resonance, which is a characteristic of the inductor, and the higher the value, the smaller the loss.
図3に示されるように実施例1の非晶質軟磁性合金粉末により作製したインダクタ用圧粉磁心の場合、そのQ値は100kHz未満の周波数範囲においては比較例5のQ値とほぼ同等だったが、100kHz以上の周波数範囲では比較例5のQ値に比べて顕著に大きくなった。また、Q値のピークはより高い周波数側に移動し、Q値の最大値も大きくなった。 As shown in FIG. 3, in the case of the inductor dust core made of the amorphous soft magnetic alloy powder of Example 1, the Q value is almost equal to the Q value of Comparative Example 5 in the frequency range below 100 kHz. However, in the frequency range of 100 kHz or more, it was significantly larger than the Q value of Comparative Example 5. Further, the peak of the Q value moved to a higher frequency side, and the maximum value of the Q value also increased.
また、図3に示されるように実施例2の非晶質軟磁性合金粉末により作製したインダクタ用圧粉磁心の場合、そのQ値は100kHz未満の周波数範囲で比較例5のQ値とほぼ同等だったが、100kHz以上の周波数範囲では比較例5のQ値に比べ顕著に大きくなった。また、Q値のピークはより高い周波数側に移動し、Q値の最大値も大きくなった。 As shown in FIG. 3, in the case of the dust core for inductor made of the amorphous soft magnetic alloy powder of Example 2, the Q value is almost equal to the Q value of Comparative Example 5 in a frequency range of less than 100 kHz. However, in the frequency range of 100 kHz or more, it was significantly larger than the Q value of Comparative Example 5. Further, the peak of the Q value moved to a higher frequency side, and the maximum value of the Q value also increased.
また、図3に示されるように、実施例2の非晶質軟磁性合金粉末により作製したインダクタ用圧粉磁心のQ値は、実施例1の非晶質軟磁性合金粉末により作製したインダクタ用圧粉磁心のQ値と比べて、5MHz未満の周波数範囲ではわずかに小さいが、5MHzを超えたところで同程度となり、20MHzを超えるとQ値は完全に上回った。 Further, as shown in FIG. 3, the Q value of the powder magnetic core for the inductor produced from the amorphous soft magnetic alloy powder of Example 2 is the same as that for the inductor produced from the amorphous soft magnetic alloy powder of Example 1. Compared with the Q value of the dust core, it is slightly smaller in the frequency range below 5 MHz, but it is almost the same when the frequency exceeds 5 MHz, and the Q value is completely above 20 MHz.
上記結果より、本発明の製造方法に従い作製した非晶質軟磁性合金粉末を用いることによって、従来のカルボニル鉄粉を用いたインダクタ用圧粉磁心に比べ、高い周波数範囲においてQ値が大きく低損失なインダクタ用圧粉磁心を得ることができた。 From the above results, by using the amorphous soft magnetic alloy powder produced according to the manufacturing method of the present invention, the Q value is large and the loss is low in a high frequency range as compared with the conventional dust core for inductors using carbonyl iron powder. A dust core for inductors was obtained.
よって、上述の通り、本発明の非晶質軟磁性合金粉末の製造方法によれば、従来技術のカルボニル鉄粉より粒径が小さく、且つ高い飽和磁束密度(Bs)の非晶質軟磁性合金粉末を製造することができた。 Therefore, as described above, according to the method for producing the amorphous soft magnetic alloy powder of the present invention, the amorphous soft magnetic alloy having a smaller particle size and higher saturation magnetic flux density (Bs) than the carbonyl iron powder of the prior art. A powder could be produced.
また、本発明の非晶質軟磁性合金粉末と結合材を混合して本発明のインダクタ用圧粉磁心を製造することにより、従来技術で作製したカルボニル鉄粉を用いて製造したインダクタ用圧粉磁心より、高い周波数において低損失なインダクタ用圧粉磁心を製造することができた。 Also, the powder for inductor produced by using the carbonyl iron powder produced by the prior art by producing the powder magnetic core for inductor of the present invention by mixing the amorphous soft magnetic alloy powder of the present invention and the binder. It was possible to manufacture a dust core for inductors with lower loss at a higher frequency than the magnetic core.
以上、図面を用いて本発明の実施例を説明したが、本発明はこの実施例に限られるものでなく、本発明の趣旨を逸脱しない範囲で部材や構成の変更があっても、本発明に含まれる。すなわち、当事者であれば、当然なしうるであろう各種変形、修正もまた本発明に含まれることは勿論である。 The embodiment of the present invention has been described above with reference to the drawings. However, the present invention is not limited to this embodiment, and the present invention can be applied even if there are changes in members and configurations without departing from the spirit of the present invention. include. That is, it goes without saying that the present invention also includes various modifications and corrections that can naturally be made by those skilled in the art.
本発明により得られる非晶質軟磁性合金粉末は、従来技術により得られる軟磁性粉末に比べて粒径が小さく、更にその粉末は微細粒子あるいは微細粒子集合体粒子により構成されており、且つ高い飽和磁束密度(Bs)を有することから、高周波域での軟磁気特性に優れている。 The amorphous soft magnetic alloy powder obtained by the present invention has a smaller particle size compared to the soft magnetic powder obtained by the prior art, and the powder is composed of fine particles or fine particle aggregate particles and is high. Since it has a saturation magnetic flux density (Bs), it has excellent soft magnetic characteristics in a high frequency range.
よって、本発明により得られる非晶質軟磁性合金粉末は大電流化・高周波化への対応を必要とされている、電子機器の電源部品用インダクタとしての適用が好適である。 Therefore, the amorphous soft magnetic alloy powder obtained by the present invention is suitable for use as an inductor for power supply components of electronic equipment, which is required to cope with large current and high frequency.
Claims (4)
製造された粉末全体の平均粒径が0.1μm以上5.0μm以下であり、
5重量%≦B≦10重量%、0.06重量%≦P≦5重量%で残部はFeからなることを特徴とする非晶質軟磁性合金粉末。 An amorphous soft magnetic alloy powder comprising particles formed from an aggregate of two or more fine particles having a particle size of 0.01 μm or more and 1.0 μm or less and single particles formed of only one particle. And
Ri Der average particle diameter of the total produced powder is 0.1μm or more 5.0μm or less,
An amorphous soft magnetic alloy powder characterized in that 5% by weight ≦ B ≦ 10% by weight, 0.06% by weight ≦ P ≦ 5% by weight, and the balance is Fe .
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