JP7418194B2 - Manufacturing method of powder magnetic core - Google Patents
Manufacturing method of powder magnetic core Download PDFInfo
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- JP7418194B2 JP7418194B2 JP2019221685A JP2019221685A JP7418194B2 JP 7418194 B2 JP7418194 B2 JP 7418194B2 JP 2019221685 A JP2019221685 A JP 2019221685A JP 2019221685 A JP2019221685 A JP 2019221685A JP 7418194 B2 JP7418194 B2 JP 7418194B2
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Description
本発明は、圧粉磁心の製造方法に関する。 The present invention relates to a method for manufacturing a powder magnetic core.
圧粉磁心は、インダクタ及びリアクトルとも呼ばれるコイルのコアに用いられる磁性体である。圧粉磁心は軟磁性粉末により成る。軟磁性粉末としては、鉄を主成分とするパーマロイ（Ｆｅ－Ｎｉ合金）、Ｓｉ含有鉄合金（Ｆｅ－Ｓｉ合金）、センダスト合金（Ｆｅ－Ｓｉ－Ａｌ合金）、アモルファス合金、純鉄粉等が挙げられる。この軟磁性粉末は、粉砕法、水アトマイズ法、ガスアトマイズ法、水ガスアトマイズ法等の手法によって作製される。近年では、水アトマイズ法は、もっとも入手性が良く低コストであり、ガスアトマイズ法は、ヒステリシス損失を効果的に低減でき、特に多用されている。 A powder magnetic core is a magnetic material used in the core of a coil, also called an inductor or reactor. The powder magnetic core is made of soft magnetic powder. Examples of soft magnetic powders include permalloy whose main component is iron (Fe-Ni alloy), Si-containing iron alloy (Fe-Si alloy), sendust alloy (Fe-Si-Al alloy), amorphous alloy, pure iron powder, etc. Can be mentioned. This soft magnetic powder is produced by a method such as a pulverization method, a water atomization method, a gas atomization method, a water gas atomization method, or the like. In recent years, the water atomization method is the most readily available and low cost, and the gas atomization method is particularly widely used because it can effectively reduce hysteresis loss.
リアクトルやインダクタ等のコイルは、用途に応じて求められる磁気的特性が異なる。例えば、商用電源用途等、低周波数領域での使用が想定される場合、コイルには高いインダクタンス値が求められることがあり、その場合、コイルに用いる圧粉磁心の初透磁率を向上させることが望ましい。 Required magnetic properties of coils such as reactors and inductors differ depending on the application. For example, if the coil is expected to be used in a low frequency range, such as in commercial power supply applications, a high inductance value may be required for the coil. desirable.
圧粉磁心の初透磁率を向上させるため、より低損失で、初透磁率が高く、安価なＦｅＳｉＡｌ合金粉末がよく用いられている。しかしながら、近年では、更に高い初透磁率を有する圧粉磁心が要望されるところである。本発明は、上記のような課題を解決するために提案されたものであり、本発明の目的は、初透磁率の高い圧粉磁心の製造方法を提供することにある。 In order to improve the initial permeability of powder magnetic cores, FeSiAl alloy powder, which has lower loss, higher initial permeability, and is inexpensive, is often used. However, in recent years, there has been a demand for powder magnetic cores with even higher initial permeability. The present invention was proposed to solve the above problems, and an object of the present invention is to provide a method for manufacturing a powder magnetic core with high initial permeability.
上記の目的を達成するため、本発明の実施形態に係る圧粉磁心の製造方法は、メジアン径で粒径６０μｍ以上のＦｅＳｉＡｌ合金の粉砕粉を、絶縁樹脂で被覆する絶縁処理工程と、前記絶縁処理工程前に、前記ＦｅＳｉＡｌ合金の粉砕粉に対して０．２ｗｔ％以上の割合で潤滑剤を混合する被覆前混合工程と、前記絶縁樹脂で被覆された前記ＦｅＳｉＡｌ合金の粉砕粉を所定形状の成形体に加圧成形する成形工程と、前記成形体を焼鈍する熱処理工程と、を含むこと、を特徴とする。 In order to achieve the above object, a method for manufacturing a powder magnetic core according to an embodiment of the present invention includes an insulation treatment step of coating pulverized FeSiAl alloy powder having a median particle size of 60 μm or more with an insulating resin; Before the treatment step, a pre-coating mixing step includes mixing a lubricant at a ratio of 0.2 wt% or more to the FeSiAl alloy pulverized powder, and a pre-coating mixing step in which the FeSiAl alloy pulverized powder coated with the insulating resin is shaped into a predetermined shape. The method is characterized in that it includes a forming step of press-molding the molded object, and a heat treatment step of annealing the molded object.
前記絶縁処理工程は、加熱による乾燥工程を含み、前記被覆前混合工程では、遅くとも前記乾燥工程の前までに潤滑剤を混合するようにしてもよい。 The insulation treatment step may include a drying step by heating, and in the pre-coating mixing step, a lubricant may be mixed at the latest before the drying step.
前記被覆前混合工程は、潤滑剤を前記ＦｅＳｉＡｌ合金の粉砕粉に対して０．３以上０．７ｗｔ％以下の割合で混合するようにしてもよい。 In the pre-coating mixing step, the lubricant may be mixed with the pulverized powder of the FeSiAl alloy at a ratio of 0.3 to 0.7 wt%.
前記被覆前混合工程は、潤滑剤を前記ＦｅＳｉＡｌ合金の粉砕粉に対して０．４以上０．７ｗｔ％以下の割合で混合するようにしてもよい。 In the pre-coating mixing step, the lubricant may be mixed with the pulverized powder of the FeSiAl alloy at a ratio of 0.4 to 0.7 wt%.
前記絶縁処理工程の後、及び前記加圧成形工程の前に、前記絶縁樹脂で被覆された前記ＦｅＳｉＡｌ合金の粉砕粉に更に潤滑剤を混合する被覆後混合工程を含むようにしてもよい。 After the insulation treatment step and before the pressure molding step, a post-coating mixing step may be included in which a lubricant is further mixed into the pulverized powder of the FeSiAl alloy coated with the insulating resin.
前記被覆前混合工程では、前記被覆後混合工程より多くの潤滑剤を混合するようにしてもよい。 In the pre-coating mixing step, more lubricant may be mixed than in the post-coating mixing step.
前記被覆後混合工程は、潤滑剤を前記ＦｅＳｉＡｌ合金の粉砕粉に対して０．１以上０．３ｗｔ％以下の割合で混合するようにしてもよい。 In the post-coating mixing step, a lubricant may be mixed with the pulverized powder of the FeSiAl alloy at a ratio of 0.1 to 0.3 wt%.
粉砕法により、メジアン径で粒径６０μｍ以上のＦｅＳｉＡｌ合金の粉砕粉を作製する粉末作製工程を含むようにしてもよい。 The method may include a powder production step of producing pulverized FeSiAl alloy powder having a median particle size of 60 μm or more using a pulverization method.
圧粉磁心の初透磁率を１４４以上にするようにしてもよい。 The powder magnetic core may have an initial permeability of 144 or more.
本発明によれば、圧粉磁心の初透磁率を高めることができる。 According to the present invention, the initial permeability of a powder magnetic core can be increased.
以下、本実施形態に係る圧粉磁心の製造方法について詳細に説明する。なお、本発明は、以下に説明する実施形態に限定されるものでない。 Hereinafter, a method for manufacturing a powder magnetic core according to this embodiment will be described in detail. Note that the present invention is not limited to the embodiments described below.
（概略製法）
圧粉磁心は、インダクタ及びリアクトルとも呼ばれるコイルのコアに用いられる磁性体である。圧粉磁心は、絶縁被覆された軟磁性粉末により成る。この圧粉磁心は、図１に示すように、軟磁性粉末を作製する粉末作製工程（ステップＳ０１）、軟磁性粉末と潤滑剤を混合する被覆前混合工程（ステップＳ０２）、結着性絶縁樹脂で軟磁性粉末を被覆する絶縁処理工程（ステップＳ０３）、更に潤滑剤を混合する被覆後混合工程（ステップＳ０４）、加圧成形する成型工程（ステップＳ０５）、及び焼鈍する熱処理工程（ステップＳ０６）を経て作製される。
(General manufacturing method)
A powder magnetic core is a magnetic material used in the core of a coil, also called an inductor or reactor. A powder magnetic core is made of soft magnetic powder coated with insulation. As shown in FIG. 1, this powder magnetic core is manufactured through a powder production process (step S01) for producing soft magnetic powder, a pre-coating mixing process (step S02) for mixing soft magnetic powder and lubricant, and a binding insulating resin. An insulation treatment step of coating the soft magnetic powder with (step S03), a post-coating mixing step of further mixing a lubricant (step S04), a molding step of pressure molding (step S05), and a heat treatment step of annealing (step S06) It is produced through the process.
（粉末作製工程）
軟磁性粉末は、センダスト（登録商標）等のＦｅＳｉＡｌ合金である。この軟磁性粉末は、平均粒径Ｄ５０とも呼ばれるメジアン径で６０μｍ以上の粒径を有する。そして、この軟磁性粉末は粉砕粉である。即ち、この軟磁性粉末は粉砕法によって作製される。粉砕法では、ＦｅＳｉＡｌ合金の金属塊をゾークラッシャー、ハンマーミル、アトリションミル、スタンプミル又はボールミル加工等によって機械的に粉砕し、振動櫛等により平均粒径Ｄ５０で６０μｍ以上の粒径となるように、ふるい分ける。
(Powder production process)
The soft magnetic powder is a FeSiAl alloy such as Sendust (registered trademark). This soft magnetic powder has a median particle size, also called average particle size D50, of 60 μm or more. This soft magnetic powder is a pulverized powder. That is, this soft magnetic powder is produced by a pulverization method. In the pulverization method, a metal lump of FeSiAl alloy is mechanically pulverized by a zoe crusher, hammer mill, attrition mill, stamp mill, or ball mill, etc., and then crushed using a vibrating comb or the like to obtain a particle size of 60 μm or more with an average particle size D50. Then, sieve.
ＦｅＳｉＡｌ合金は、元来、高い透磁率を有するが、メジアン径で粒径６０μｍ以上及び粉砕粉の条件が加わると、圧粉磁心の初透磁率を飛躍的に向上させる。尚、初透磁率は、直流印加磁界を限りなくゼロに近づけた状態における透磁率である。 FeSiAl alloy originally has high magnetic permeability, but when conditions such as a median particle size of 60 μm or more and pulverized powder are added, the initial magnetic permeability of the dust core is dramatically improved. Note that the initial magnetic permeability is the magnetic permeability in a state where the DC applied magnetic field is brought as close to zero as possible.
この理由は、推測であり、これに限られないが、粒径６０μｍ以上とすることによって、粉末内に発生する反磁界が良好に低減していると考えられる。反磁界とは磁性体の内部に、磁性体が発生する磁界とは逆方向の磁界が発生する現象であり、反磁界は、磁性体内部に発生する磁界の一部を打ち消してしまう。そのため、反磁界の低減によって、必要な磁束密度Ｂを発生させるための磁場Ｈが小さくて済み、磁場Ｈに反比例する透磁率が上昇したものと考えられる。 Although the reason for this is speculation and is not limited to this, it is thought that by setting the particle size to 60 μm or more, the demagnetizing field generated within the powder is reduced favorably. A diamagnetic field is a phenomenon in which a magnetic field is generated inside a magnetic material in a direction opposite to the magnetic field generated by the magnetic material, and the diamagnetic field cancels out a portion of the magnetic field generated inside the magnetic material. Therefore, it is considered that by reducing the demagnetizing field, the magnetic field H required to generate the necessary magnetic flux density B is small, and the magnetic permeability, which is inversely proportional to the magnetic field H, increases.
また、この理由についても推測であり、これに限られないが、ＦｅＳｉＡｌ合金は粉砕粉とすることで扁平形状を採る。扁平方向に対して粉砕粉は大きくなることで反磁場を低減することができる。そして、その扁平方向に磁束が流れるようにプレス成形するため、磁束の流れに対して透磁率が大きくなるものと考えられる。 Further, although the reason for this is speculation and is not limited to this, the FeSiAl alloy takes on a flat shape when it is pulverized. The demagnetizing field can be reduced by making the crushed powder larger in the flat direction. Since the press molding is performed so that the magnetic flux flows in the flat direction, it is thought that the magnetic permeability increases with respect to the flow of the magnetic flux.
（被覆前混合工程）
被覆前混合工程は、結着性絶縁樹脂で軟磁性粉末を被覆する前に実行される。後述のように絶縁処理工程では、結着性絶縁樹脂の混合工程と、加熱による乾燥工程を経るが、詳細には、乾燥工程前に潤滑剤が混合されればよい。先に潤滑剤を混合し、後に結着性絶縁樹脂を混合してもよいし、潤滑剤と結着性絶縁樹脂を同時に混合してもよい。
(Pre-coating mixing process)
The pre-coating mixing step is performed before coating the soft magnetic powder with the binding insulating resin. As will be described later, in the insulation treatment step, a binding insulating resin mixing step and a drying step by heating are performed, but in detail, a lubricant may be mixed before the drying step. The lubricant may be mixed first and the binding insulating resin may be mixed later, or the lubricant and the binding insulating resin may be mixed at the same time.
潤滑剤としては、ステアリン酸、ステアリン酸塩、ステアリン酸石鹸、エチレンビスステアラマイド、エチレンビスステアレートアミドなどのワックスを使用できる。潤滑剤の添加量は、軟磁性合金粉末に対して０．２以上０．７ｗｔ％以下とする。 As a lubricant, waxes such as stearic acid, stearate, stearic acid soap, ethylene bis stearamide, ethylene bis stearate amide, etc. can be used. The amount of lubricant added is 0.2 or more and 0.7 wt% or less based on the soft magnetic alloy powder.
潤滑剤の混合量を０．２ｗｔ％以上とすると、更に初透磁率が向上する。好ましくは、潤滑剤の混合量は０．３ｗｔ％以上であり、更に初透磁率は向上する。特に好ましくは、潤滑剤の混合量は０．４ｗｔ％以上であり、初透磁率はピークに達する。粉砕粉同士の滑りが向上するので、軟磁性粉末の密度が向上し、成形密度が高くなると考えられる。 When the amount of lubricant mixed is 0.2 wt% or more, the initial magnetic permeability is further improved. Preferably, the mixing amount of the lubricant is 0.3 wt% or more, and the initial magnetic permeability is further improved. Particularly preferably, the amount of lubricant mixed is 0.4 wt% or more, and the initial magnetic permeability reaches its peak. It is thought that since the sliding between the pulverized powders is improved, the density of the soft magnetic powder is improved and the compacted density is increased.
但し、潤滑剤の混合量を０．７ｗｔ％超とすると、良好な初透磁率は得られるが、初透磁率のピークから降下し始める。その理由は、潤滑剤が結着性絶縁樹脂に入り込むこともあり、潤滑剤が圧粉磁心に残留してしまい、圧粉磁心に占める軟磁性粉末の割合を寧ろ低下させるためと考えられる。 However, if the mixing amount of the lubricant exceeds 0.7 wt%, a good initial magnetic permeability can be obtained, but the initial magnetic permeability starts to drop from its peak. The reason for this is thought to be that the lubricant sometimes enters the binding insulating resin and remains in the powder magnetic core, which actually reduces the proportion of soft magnetic powder in the powder magnetic core.
（絶縁処理工程）
結着性絶縁樹脂は、絶縁性を有し、軟磁性粉末の粒子間の電気的絶縁性を確保し、圧粉磁心の渦電流損失を低下させる。この結着性絶縁樹脂は、バインダー作用も兼ね備えて、成形時の保形性を高め、更には焼鈍後の成形体の強度をより強固なものとする。また、この結着性絶縁樹脂は、バインダー作用を兼ねる備えることで、軟磁性粉末の密度を向上させ、圧粉磁心の透磁率を上げる。
(Insulation treatment process)
The binding insulating resin has insulating properties, ensures electrical insulation between particles of the soft magnetic powder, and reduces eddy current loss in the dust core. This binding insulating resin also has a binder function, improves shape retention during molding, and further strengthens the strength of the molded product after annealing. In addition, this binding insulating resin also has a binder function, thereby improving the density of the soft magnetic powder and increasing the magnetic permeability of the dust core.
結着性絶縁樹脂としては、シリコーンレジンを使用することができる。シリコーンレジンは、シロキサン結合（Ｓｉ－Ｏ―Ｓｉ）を主骨格に持つ樹脂であり、可撓性に優れた絶縁層を形成することができる。シリコーンレジンとしては、典型的には、メチル系、メチルフェニル系、プロピルフェニル系、エポキシ樹脂変性系、アルキッド樹脂変性系、ポリエステル樹脂変性系、ゴム系等を用いることができる。 Silicone resin can be used as the binding insulating resin. Silicone resin is a resin having a siloxane bond (Si--O--Si) as its main skeleton, and can form an insulating layer with excellent flexibility. As the silicone resin, typically, a methyl type, methylphenyl type, propylphenyl type, epoxy resin modified type, alkyd resin modified type, polyester resin modified type, rubber type, etc. can be used.
この中でも特に、メチルフェニル系のシリコーンレジンを用いた場合、加熱減量が少なく、耐熱性に優れた絶縁層を形成することができる。メチルフェニル系シリコーン樹脂は、Ｓｉ上の官能基が、メチル基またはフェニル基となっている。メチルフェニル系シリコーン樹脂は、３５０℃程度でＳｉ基に直結しているメチル基が熱分解し、その後、シリカ（ＳｉＯ２）層として軟磁性粉末の表面に残り、緻密で強固なバインダーとなるため、圧環強度に優れている。また、形成されたシリカ層は絶縁膜であるため絶縁性にも優れており、渦電流損を低減させることができ、磁気特性が向上する。なお、ガラス粉末等を使用しないので、製造コストが極端に高騰することはない。 Among these, in particular, when a methylphenyl silicone resin is used, it is possible to form an insulating layer with little heat loss and excellent heat resistance. In the methylphenyl silicone resin, the functional group on Si is a methyl group or a phenyl group. In methylphenyl-based silicone resin, the methyl group directly connected to the Si group thermally decomposes at around 350°C, and then remains on the surface of the soft magnetic powder as a silica (SiO2) layer, forming a dense and strong binder. Excellent radial crushing strength. Further, since the formed silica layer is an insulating film, it has excellent insulation properties, can reduce eddy current loss, and improve magnetic properties. Furthermore, since no glass powder or the like is used, the manufacturing cost will not rise significantly.
絶縁処理工程では、まず、この結着性絶縁樹脂と軟磁性粉末との混合工程を経る。結着性絶縁樹脂は、軟磁性合金粉末に対して１．０以上３．０ｗｔ％以下の割合で混合する。１．０ｗｔ％未満であると絶縁性に劣り、軟磁性粉末に適度な電気抵抗を付与することができない。また、３．０ｗｔ％超であると、密度低下による最大磁束密度及び透磁率の低下、ヒステリシス損失の増加による磁気特性が低下する問題が発生する。 In the insulation treatment step, first, the binding insulating resin and soft magnetic powder are mixed together. The binding insulating resin is mixed with the soft magnetic alloy powder at a ratio of 1.0 to 3.0 wt%. If it is less than 1.0 wt%, the insulation properties will be poor and it will not be possible to impart appropriate electrical resistance to the soft magnetic powder. Moreover, if it exceeds 3.0 wt%, there will occur problems such as a decrease in maximum magnetic flux density and magnetic permeability due to a decrease in density, and a decrease in magnetic properties due to an increase in hysteresis loss.
絶縁処理工程では、混合工程の後、加熱による乾燥工程を有する。乾燥工程では、特に限定はされないが７０以上３００℃以下の温度環境下に２時間程度晒しておくとよい。尚、被覆前混合工程での潤滑剤の混合は、遅くとも、この乾燥工程の前までに実行しておく。 The insulation treatment process includes a drying process by heating after the mixing process. In the drying step, although not particularly limited, it is preferable to expose the material to a temperature environment of 70° C. or more and 300° C. or less for about 2 hours. Note that the mixing of the lubricant in the pre-coating mixing step is performed at the latest before this drying step.
その他の結着性絶縁樹脂としてはシリコーンオリゴマーが挙げられる。また、結着性絶縁樹脂としてシリコーンレジンとシリコーンオリゴマーの混合が用いられてもよい。シリコーンオリゴマーとしては、アルコキシシリル基を有し、反応性官能基を有さないメチル系、メチルフェニル系のものや、アルコキシシリル基及び反応性官能基を有するエポキシ系、エポキシメチル系、メルカプト系、メルカプトメチル系、アクリルメチル系、メタクリルメチル系、ビニルフェニル系、又はアルコキシシリル基ではなく、反応性官能基を有する脂環式エポキシ系等を用いることができる。特に、メチル系またはメチルフェニル系のシリコーンオリゴマーを用いることで厚く硬い絶縁層を形成することができる。また、シリコーンオリゴマー層の形成のしやすさを考慮して、粘度の比較的低いメチル系、メチルフェニル系を用いてもよい。シリコーンオリゴマーの添加量は、軟磁性粉末に対して０．２５以上２．０ｗｔ％以下が望ましく、乾燥工程での温度は２５以上３００℃以下で２時間程度の熱処理を行うことが望ましい。 Other binding insulating resins include silicone oligomers. Further, a mixture of silicone resin and silicone oligomer may be used as the binding insulating resin. Examples of silicone oligomers include methyl-based and methylphenyl-based ones that have an alkoxysilyl group and no reactive functional group; epoxy-based, epoxymethyl-based, and mercapto-based ones that have an alkoxysilyl group and a reactive functional group; Instead of mercaptomethyl, acrylicmethyl, methacrylmethyl, vinylphenyl, or alkoxysilyl groups, an alicyclic epoxy having a reactive functional group or the like can be used. In particular, a thick and hard insulating layer can be formed by using a methyl-based or methylphenyl-based silicone oligomer. Furthermore, in consideration of ease of forming a silicone oligomer layer, a methyl type or methyl phenyl type having a relatively low viscosity may be used. The amount of silicone oligomer added is desirably 0.25 or more and 2.0 wt % or less based on the soft magnetic powder, and the temperature in the drying step is preferably 25 or more and 300° C. or less for about 2 hours.
更に絶縁処理工程では、結着性絶縁樹脂と共に絶縁材料を軟磁性粉末に混合してもよい。絶縁材料としてはシランカップリング剤が挙げられる。シランカップリング剤としては、アミノシラン系、エポキシシラン系、イソシアヌレート系のシランカップリング剤を使用することができ、特に、３－アミノプロピルトリエトキシシラン、３－グリシドキシプロピルトリメトキシシラン、トリス－（３－トリメトキシシリルプロピル）イソシアヌレートが好ましい。シランカップリング剤の添加量は０．２５以上１．０ｗｔ％以下が望ましく、乾燥工程での温度は２５以上２００℃以下で２時間程度の熱処理を行うことが望ましい。 Furthermore, in the insulation treatment step, an insulating material may be mixed with the soft magnetic powder together with the binding insulating resin. Examples of the insulating material include silane coupling agents. As the silane coupling agent, aminosilane-based, epoxysilane-based, and isocyanurate-based silane coupling agents can be used, and in particular, 3-aminopropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, tris -(3-trimethoxysilylpropyl)isocyanurate is preferred. The amount of the silane coupling agent added is preferably 0.25 or more and 1.0 wt% or less, and the temperature in the drying step is preferably 25 or more and 200° C. or less for about 2 hours.
複数種類の結着性絶縁樹脂、１種類以上の結着性絶縁樹脂と絶縁材料、又は複数種類の結着性絶縁樹脂と絶縁材料を軟磁性粉末に混合する場合、軟磁性粉末の外側に単一層として付着させてもよいし、種類毎に各層に分かれて軟磁性粉末の外側に積層されてもよい。また、軟磁性粉末に積層される各層のうちの一部の層は、複数種類の結着性絶縁樹脂の混合層や、１種類以上の結着性絶縁樹脂と絶縁材料の混合層となっていてもよい。例えば、シランカップリング剤とシリコーンレジンが単一層を形成し、軟磁性合金粉末の外側に付着していてもよいし、シランカップリング剤とシリコーンレジンが別々の層を形成し、軟磁性合金粉末の外側に積層されて付着していてもよい。シリコーンオリゴマーとシリコーンレジンが単一層を形成し、軟磁性合金粉末の外側に付着していてもよいし、シリコーンオリゴマーとシリコーンレジンが別々の層を形成し、軟磁性合金粉末の外側に積層されて付着していてもよい。 When mixing multiple types of binding insulating resins, one or more types of binding insulating resins and insulating materials, or multiple types of binding insulating resins and insulating materials into soft magnetic powder, a single layer is added to the outside of the soft magnetic powder. It may be deposited as a single layer, or it may be divided into layers for each type and laminated on the outside of the soft magnetic powder. In addition, some of the layers laminated on the soft magnetic powder are a mixed layer of multiple types of binding insulating resin, or a mixed layer of one or more types of binding insulating resin and an insulating material. You can. For example, the silane coupling agent and silicone resin may form a single layer and adhere to the outside of the soft magnetic alloy powder, or the silane coupling agent and silicone resin may form separate layers and adhere to the outside of the soft magnetic alloy powder. It may be laminated and attached to the outside of the . The silicone oligomer and silicone resin may form a single layer and adhere to the outside of the soft magnetic alloy powder, or the silicone oligomer and silicone resin may form separate layers and are laminated on the outside of the soft magnetic alloy powder. It may be attached.
（被覆後混合工程）
被覆後混合工程は、絶縁処理工程の後、成形工程前に実行される。潤滑剤は、被覆前混合工程と同種でも異種でもよい。この被覆後混合工程で潤滑剤を追加することで、圧粉磁心の初透磁率は更に向上する。
(Mixing process after coating)
The post-coating mixing step is performed after the insulation treatment step and before the molding step. The lubricant may be the same or different from the pre-coating mixing step. By adding a lubricant in this post-coating mixing step, the initial permeability of the powder magnetic core is further improved.
尚、メジアン径で粒径６０μｍ以上のＦｅＳｉＡｌ合金の粉砕粉を圧粉磁心の軟磁性粉末とすることによって得られる初透磁率の向上、及び被覆前混合工程によって得られる初透磁率の向上と比べると、被覆後混合工程による初透磁率の向上効果は限られるため、目的とする初透磁率に応じて、被覆後混合工程を省いてもよい。但し、被覆後混合工程を経て潤滑剤を追加することで、成形時の上パンチを離型させる際の抜き圧が低減する。潤滑剤の混合量は、軟磁性粉末に対して０．１以上０．３ｗｔ％程度が好ましい。被覆前混合工程に加えて、０．３ｗｔ％の潤滑剤を追加することで抜き圧をほぼゼロにすることができる。 In addition, compared with the improvement in initial magnetic permeability obtained by using pulverized powder of FeSiAl alloy with a median particle size of 60 μm or more as the soft magnetic powder of the powder magnetic core, and the improvement in initial magnetic permeability obtained by the pre-coating mixing process. Since the effect of improving the initial magnetic permeability by the post-coating mixing step is limited, the post-coating mixing step may be omitted depending on the desired initial magnetic permeability. However, by adding a lubricant through the mixing process after coating, the removal pressure when releasing the upper punch during molding is reduced. The mixing amount of the lubricant is preferably about 0.1 to 0.3 wt% based on the soft magnetic powder. In addition to the pre-coating mixing step, the addition of 0.3 wt% lubricant can reduce the extraction pressure to nearly zero.
ここで、被覆後混合工程では、被覆前混合工程よりも少ない量の潤滑剤を混合する。換言すると、被覆後混合工程は省かれるか、又は被覆前混合工程では、被覆後混合工程よりも多くの潤滑剤を混合する。 Here, in the post-coating mixing step, a smaller amount of lubricant is mixed than in the pre-coating mixing step. In other words, the post-coating mixing step is either omitted or more lubricant is mixed in the pre-coating mixing step than in the post-coating mixing step.
その理由は、被覆前混合工程の潤滑剤と被覆後混合工程の潤滑剤の用途の違いによる。被覆前混合工程の潤滑材は、結着性絶縁被膜内に混在することにより、成形工程時の粉砕粉間の滑り性を向上させて軟磁性粉末を高密度化し、透磁率を向上させる。一方、被覆後混合工程の潤滑材は、金型側面の滑り性を更に良くするものであり、また金型への焼き付き防止と軟磁性粉末の滑りを良くするために用いられる。従って、透磁率の向上に必須の被覆前混合工程の潤滑剤は、相対的に必須ではない被覆後混合工程の潤滑剤よりも多くする必要がある。 The reason for this is the difference in the usage of the lubricant used in the pre-coating mixing process and the lubricant used in the post-coating mixing process. The lubricant used in the pre-coating mixing step is mixed in the binding insulating coating, thereby improving the slipperiness between the pulverized powder during the molding step, increasing the density of the soft magnetic powder, and improving the magnetic permeability. On the other hand, the lubricant used in the post-coating mixing step is used to further improve the slipperiness of the side surface of the mold, and is also used to prevent seizure of the mold and to improve the slippage of the soft magnetic powder. Therefore, it is necessary to use more lubricant in the pre-coating mixing step, which is essential for improving magnetic permeability, than in the post-coating mixing step, which is relatively indispensable.
（成型工程）
成形工程では、絶縁被覆された軟磁性粉末を加圧成形することにより、成形体を形成する。成形時の圧力は１０～２０ｔｏｎ／ｃｍ２であり、平均で１２～１５ｔｏｎ／ｃｍ２程度が好ましい。被覆後混合工程を経ていると、成形時の上パンチを離型させる際の抜き圧が低減し、軟磁性粉末が金型への焼き付きくことも防止され、成形体の品質が向上する。
(molding process)
In the molding step, a molded body is formed by pressure molding the insulatingly coated soft magnetic powder. The pressure during molding is 10 to 20 ton/cm 2 , preferably about 12 to 15 ton/cm 2 on average. If the mixing step is carried out after coating, the ejection pressure when releasing the upper punch during molding is reduced, the soft magnetic powder is prevented from sticking to the mold, and the quality of the molded product is improved.
（熱処理工程）
熱処理工程では、成型体を焼鈍して歪を除去する。加熱環境の温度帯としては、６５０℃以上８５０℃以下が好ましい。６５０℃未満であると、歪除去の効果が限定的となる。８５０℃超であると、結着性絶縁樹脂の被覆層が破壊され、渦電流損失の低減効果が減殺される。
(Heat treatment process)
In the heat treatment step, the molded body is annealed to remove strain. The temperature range of the heating environment is preferably 650°C or higher and 850°C or lower. If the temperature is less than 650°C, the effect of strain removal will be limited. If the temperature exceeds 850° C., the coating layer of the binding insulating resin is destroyed, and the effect of reducing eddy current loss is diminished.
熱処理工程は、大気中などの酸素雰囲気中で行っても良い。大気中などの酸化雰囲気中で熱処理が行われると、Ｓｉ基に直結しているメチル基が熱分解する。その後、シリカ（ＳｉＯ２）層として、軟磁性粉末表面に残り、これが強固なバインダーかつ絶縁膜となる。また、緻密で強固なシリカ層となるため、高温で熱処理をおこなっても絶縁性が劣化しないで、酸化などによるヒステリシス損失の増加が起きない。また、大気中で熱処理を行うことにより、熱分解してメチル基が炭素として残ることがないので、機械的強度が改善出来る。 The heat treatment step may be performed in an oxygen atmosphere such as in the air. When heat treatment is performed in an oxidizing atmosphere such as in the air, the methyl groups directly bonded to the Si groups are thermally decomposed. Thereafter, a silica (SiO2) layer remains on the surface of the soft magnetic powder, and this becomes a strong binder and insulating film. Furthermore, since the silica layer is dense and strong, the insulation properties do not deteriorate even when heat-treated at high temperatures, and hysteresis loss does not increase due to oxidation or the like. Furthermore, by performing heat treatment in the atmosphere, mechanical strength can be improved because methyl groups do not remain as carbon due to thermal decomposition.
但し、熱処理工程は、不活性雰囲気中又は還元雰囲気中で行ってもよい。不活性雰囲気及び還元雰囲気中は、反応性ガスが低量であり、不活性ガス又は中性ガスで満たされた雰囲気である。反応性ガスは、酸素、水蒸気又は炭素ガス等である。不活性ガスは、アルゴンやヘリウム等である。中性ガスは、窒素やアンモニア等である。不活性雰囲気中で熱処理工程を行っても、圧粉磁心は良好な初透磁率を得られる。 However, the heat treatment step may be performed in an inert atmosphere or a reducing atmosphere. Inert and reducing atmospheres are atmospheres with low amounts of reactive gases and filled with inert or neutral gases. The reactive gas is oxygen, water vapor, carbon gas, or the like. The inert gas is argon, helium, or the like. Neutral gases include nitrogen and ammonia. Even if the heat treatment process is performed in an inert atmosphere, the powder magnetic core can obtain a good initial permeability.
以下、実施例に基づいて本発明をさらに詳細に説明する。なお、本発明は下記実施例に限定されるものではない。 Hereinafter, the present invention will be explained in more detail based on Examples. Note that the present invention is not limited to the following examples.
（実施例１乃至８）
軟磁性粉末として、粉砕法により得られたＦｅＳｉＡｌ合金の粉砕粉を用いた。この粉砕粉は、目開き１２０μｍの櫛でふるい分けされることにより、平均粒子経Ｄ５０が９１．２μｍであった。尚、この粉砕粉は、平均粒径Ｄ１０では３２．４μｍ、平均粒径Ｄ９０では１２７．７μｍであった。
(Examples 1 to 8)
As the soft magnetic powder, pulverized FeSiAl alloy powder obtained by a pulverization method was used. This pulverized powder was sieved with a comb with an opening of 120 μm, and had an average particle size D50 of 91.2 μm. Note that this pulverized powder had an average particle size D10 of 32.4 μm and an average particle size D90 of 127.7 μm.
この軟磁性粉末を用いて下表１に示す条件により、実施例１乃至８及び比較例１の圧粉磁心を作製した。尚、表中、雰囲気の項目の「Ａｉｒ」は大気雰囲気を示す。
（表１）
(Table 1)
表１に示すように、被覆前混合工程では、軟磁性粉末に対して実施例１乃至８及び比較例１に応じた混合量で潤滑剤を添加し、潤滑剤と軟磁性粉末とを混合した。潤滑剤としては、実施例１乃至８及び比較例１において、エチレンビスステアラマイド（Ａｃｒａｗａｘ（登録商標））を用いた。 As shown in Table 1, in the pre-coating mixing step, a lubricant was added to the soft magnetic powder in a mixing amount according to Examples 1 to 8 and Comparative Example 1, and the lubricant and the soft magnetic powder were mixed. . As the lubricant, ethylene bisstearamide (Acrawax (registered trademark)) was used in Examples 1 to 8 and Comparative Example 1.
被覆前混合工程での潤滑剤の混合を経て、絶縁処理工程に移り、実施例１乃至８及び比較例１に共通の結着性絶縁樹脂を混合し、加熱乾燥した。即ち、実施例１乃至８及び比較例１とも、軟磁性粉末に対して１．２ｗｔ％の割合でシリコーンレジンを添加し、混合した。そして、１５０℃の温度雰囲気中に２時間晒した。 After mixing the lubricant in the pre-coating mixing step, the insulating treatment step was carried out, where the binding insulating resin common to Examples 1 to 8 and Comparative Example 1 was mixed and dried by heating. That is, in both Examples 1 to 8 and Comparative Example 1, silicone resin was added and mixed at a ratio of 1.2 wt% to the soft magnetic powder. Then, it was exposed to an atmosphere at a temperature of 150° C. for 2 hours.
被覆前混合工程を経た後、乾燥後の混合物を目開き２５０μｍの篩に通した。そして、被覆後混合工程に移り、潤滑剤としてエチレンビスステアラマイド（Ａｃｒａｗａｘ）を添加して混合した。実施例１乃至８及び比較例１とも、潤滑剤は、軟磁性粉末に対して０．３ｗｔ％の割合で添加した。 After the pre-coating mixing step, the dried mixture was passed through a sieve with an opening of 250 μm. Then, after coating, a mixing step was carried out, and ethylene bisstearamide (Acrawax) was added as a lubricant and mixed. In both Examples 1 to 8 and Comparative Example 1, the lubricant was added at a ratio of 0.3 wt% to the soft magnetic powder.
成形工程に移り、実施例１乃至８及び比較例１とも、金型を用いて、室温状況下において１５ｔｏｎ／ｃｍ２で加圧成形した。最後に、熱処理工程に移った。成形体を大気雰囲気の加熱環境に置き、６時間かけて７００℃まで昇温し、７００℃を２時間保つ温度プロファイルを用いて加熱した。最終的に、外径１６．５ｍｍ、内径１１．０ｍｍ及び高さ５ｍｍのトロイダル状の圧粉磁心が得られた。 Moving on to the molding process, both Examples 1 to 8 and Comparative Example 1 were pressure molded at 15 ton/cm 2 at room temperature using a mold. Finally, we moved on to the heat treatment process. The molded body was placed in an atmospheric heating environment, and heated using a temperature profile in which the temperature was raised to 700° C. over 6 hours and the temperature was maintained at 700° C. for 2 hours. Finally, a toroidal powder magnetic core having an outer diameter of 16.5 mm, an inner diameter of 11.0 mm, and a height of 5 mm was obtained.
実施例１乃至８及び比較例１の圧粉磁心の密度（ｇ／ｃｃ）、成形工程における離型時の抜き圧（ｔｏｎ）、鉄損Ｐｃｖ、ヒステリシス損失Ｐｈｖ、渦電流損失Ｐｅｖ、初透磁率μ（０ｋＡ／ｍ）、及び直流を重畳させて磁界の強さが５ｋＡ／ｍの時の透磁率μ（５ｋＡ／ｍ）を測定した。 Density (g/cc) of powder magnetic cores of Examples 1 to 8 and Comparative Example 1, ejection pressure (ton) during mold release in the molding process, iron loss Pcv, hysteresis loss Phv, eddy current loss Pev, initial magnetic permeability μ (0 kA/m), and the magnetic permeability μ (5 kA/m) when the magnetic field strength was 5 kA/m by superimposing direct current.
密度（ｇ／ｃｃ）は、見かけ密度である。圧粉磁心の外径、内径、及び高さを測り、これらの値から各圧粉成形体の体積（ｃｍ３）を、π×（外径２－内径２）×高さに基づき算出した。そして、圧粉磁心の重量を測定し、測定した重量を算出した体積で除して密度を算出した。抜き圧（ｔｏｎ）は、圧粉磁心を金型から抜き出す際の荷重を測定した。 Density (g/cc) is apparent density. The outer diameter, inner diameter, and height of the powder magnetic core were measured, and from these values, the volume (cm 3 ) of each powder compact was calculated based on π×(outer diameter 2 − inner diameter 2 )×height. Then, the weight of the dust core was measured, and the density was calculated by dividing the measured weight by the calculated volume. The ejection pressure (ton) was measured by the load when ejecting the dust core from the mold.
透磁率μの測定に際し、圧粉磁心にφ０．５ｍｍの銅線を１７ターン巻回した。損失の測定に際しては、圧粉磁心にφ０．５ｍｍの銅線を１次巻線として１７ターン巻回し、また２次巻線として１７ターン巻回した。そして、ＬＣＲメータ（アジレントテクノロジー：４２８４Ａ）を使用することで、１０ｋＨｚ、１．０Ｖにおける各磁界の強さのインダクタンスから透磁率μ（０ｋＡ／ｍ）及び透磁率μ（５ｋＡ／ｍ）を算出した。また、磁気計測機器であるＢＨアナライザ（岩通計測株式会社：ＳＹ－８２１９）を用いて、周波数が１００ｋＨｚ及び最大磁束密度Ｂｍが１００ｍＴの測定条件にて鉄損Ｐｃｖ（ｋｗ／ｍ３）の測定を行った。 When measuring the magnetic permeability μ, a copper wire with a diameter of 0.5 mm was wound 17 turns around the powder magnetic core. When measuring the loss, a powder magnetic core was wound with 17 turns of a copper wire having a diameter of 0.5 mm as a primary winding, and 17 turns as a secondary winding. Then, by using an LCR meter (Agilent Technologies: 4284A), magnetic permeability μ (0 kA/m) and magnetic permeability μ (5 kA/m) were calculated from the inductance of each magnetic field strength at 10 kHz and 1.0 V. . In addition, iron loss Pcv (kw/m 3 ) was measured using a BH analyzer (Iwatsu Keizoku Co., Ltd.: SY-8219), which is a magnetic measuring instrument, under measurement conditions of a frequency of 100 kHz and a maximum magnetic flux density Bm of 100 mT. I did it.
更に、鉄損Ｐｃｖの測定結果からヒステリシス損失Ｐｈｖ（ｋｗ／ｍ３）と渦電流損失Ｐｅ（ｋｗ／ｍ３）とを算出した。ヒステリシス損失Ｐｈｖ（ｋｗ／ｍ３）と渦電流損失Ｐｅ（ｋｗ／ｍ３）は、鉄損Ｐｃｖの周波数曲線を次の（１）～（３）式で最小２乗法により、ヒステリシス損失係数（Ｋｈ）、渦電流損失係数（Ｋｅ）を算出することで行った。
Ｐｃｖ ＝Ｋｈ×ｆ＋Ｋｅ×ｆ２・・（１）
Ｐｈｖ ＝Ｋｈ×ｆ・・（２）
Ｐｅｖ ＝Ｋｅ×ｆ２・・（３）
Ｐｃｖ：鉄損
Ｋｈ ：ヒステリシス損失係数
Ｋｅ ：渦電流損失係数
ｆ ：周波数
Ｐｈｖ ：ヒステリシス損失
Ｐｅｖ ：渦電流損失
Furthermore, hysteresis loss Phv (kw/m 3 ) and eddy current loss Pe (kw/m 3 ) were calculated from the measurement results of iron loss Pcv. The hysteresis loss Phv (kw/m 3 ) and the eddy current loss Pe (kw/m 3 ) are determined by calculating the hysteresis loss coefficient (Kh ), and calculated the eddy current loss coefficient (Ke).
Pcv =Kh×f+Ke×f 2 ...(1)
Phv=Kh×f...(2)
Pev = Ke×f 2 ...(3)
Pcv: Iron loss Kh: Hysteresis loss coefficient Ke: Eddy current loss coefficient f: Frequency Phv: Hysteresis loss Pev: Eddy current loss
比較例１並びに実施例１乃至８の密度（ｇ／ｃｃ）、抜き圧（ｔｏｎ）、鉄損Ｐｃｖ、ヒステリシス損失Ｐｈｖ、渦電流損失Ｐｅｖ及び透磁率μの測定結果を下表２に示す。
（表２）
(Table 2)
また、上表２に従って、図２及び図３のグラフを作成した。図２は、被覆前混合工程における潤滑剤の混合量と初透磁率との関係を示すグラフである。図３は、被覆前混合工程における潤滑剤の混合量と鉄損との関係を示すグラフである。 In addition, the graphs in FIGS. 2 and 3 were created according to Table 2 above. FIG. 2 is a graph showing the relationship between the amount of lubricant mixed in the pre-coating mixing step and the initial magnetic permeability. FIG. 3 is a graph showing the relationship between the amount of lubricant mixed in the pre-coating mixing step and iron loss.
表２及び図２に示すように、実施例１乃至８の圧粉磁心は、比較例１の圧粉磁心と比べて初透磁率が向上し、１３０以上になっていることが確認された。即ち、軟磁性粉末をメジアン径で粒径６０μｍ以上である９１．２μｍのＦｅＳｉＡｌ合金の粉砕粉とし、当該粉砕粉を絶縁樹脂で被覆する前に０．２ｗｔ％以上の割合で潤滑剤を混合すると、初透磁率が向上することが確認された。 As shown in Table 2 and FIG. 2, it was confirmed that the powder magnetic cores of Examples 1 to 8 had improved initial permeability compared to the powder magnetic core of Comparative Example 1, reaching 130 or more. That is, if the soft magnetic powder is a 91.2 μm FeSiAl alloy pulverized powder with a median particle size of 60 μm or more, and a lubricant is mixed at a ratio of 0.2 wt% or more before coating the pulverized powder with an insulating resin. It was confirmed that the initial magnetic permeability was improved.
また、表２及び図２に示すように、実施例２乃至６の圧粉磁心は、実施例１、７及び８の圧粉磁心と比べて初透磁率が向上し、１４０以上になっていることが確認された。即ち、絶縁処理工程前に０．３ｗｔ％以上０．７ｗｔ％以下の割合で潤滑剤を混合すると、初透磁率が更に向上することが確認された。 Moreover, as shown in Table 2 and FIG. 2, the powder magnetic cores of Examples 2 to 6 have improved initial permeability compared to the powder magnetic cores of Examples 1, 7, and 8, and are 140 or more. This was confirmed. That is, it was confirmed that the initial magnetic permeability was further improved when a lubricant was mixed at a ratio of 0.3 wt% or more and 0.7 wt% or less before the insulation treatment step.
また、表２及び図２に示すように、実施例３乃至５の圧粉磁心は、実施例１、２、６、７及び８の圧粉磁心と比べて初透磁率が向上し、１５０以上になっていることが確認された。即ち、絶縁処理工程前に０．４以上０．７ｗｔ％以下の割合で潤滑剤を混合すると、初透磁率が更に向上することが確認された。 Moreover, as shown in Table 2 and FIG. 2, the powder magnetic cores of Examples 3 to 5 have improved initial permeability compared to the powder magnetic cores of Examples 1, 2, 6, 7, and 8, and are 150 or more. It was confirmed that . That is, it was confirmed that the initial magnetic permeability was further improved when a lubricant was mixed at a ratio of 0.4 to 0.7 wt% before the insulation treatment step.
尚、表２及び図３に示すように、比較例１に対して実施例１乃至８を比べるとわかるように、絶縁処理工程前に潤滑剤を軟磁性粉末と混合しても鉄損Ｐｃｖに大きな変化はない。従って、軟磁性粉末をメジアン径で粒径６０μｍ以上のＦｅＳｉＡｌ合金の粉砕粉とし、当該粉砕粉を絶縁樹脂で被覆する前に０．２ｗｔ％以上の割合で潤滑剤を混合しても、磁気特性に悪影響なく初透磁率を向上させることが確認された。 As shown in Table 2 and FIG. 3, when comparing Examples 1 to 8 with Comparative Example 1, it can be seen that even if the lubricant is mixed with the soft magnetic powder before the insulation treatment process, the iron loss Pcv does not change. There are no major changes. Therefore, even if the soft magnetic powder is a pulverized FeSiAl alloy powder with a median particle size of 60 μm or more, and a lubricant is mixed at a ratio of 0.2 wt% or more before coating the pulverized powder with an insulating resin, the magnetic properties It was confirmed that the initial magnetic permeability was improved without any negative effects.
（実施例９乃至１３）
次に、下表３の条件に従って実施例９乃至１３の圧粉磁心を作製した。
（表３）
Next, powder magnetic cores of Examples 9 to 13 were produced according to the conditions shown in Table 3 below.
(Table 3)
表３に示すように、実施例９乃至１３の圧粉磁心は、被覆前混合工程において、潤滑剤の混合量を軟磁性粉末に対して０．６ｗｔ％に統一して添加し、潤滑剤と軟磁性粉末とを混合した。一方、実施例９乃至１３の圧粉磁心は、被覆後混合工程において混合される潤滑剤の混合量を変化させた。その他の作製方法及び条件は実施例１乃至８と同一である。 As shown in Table 3, in the powder magnetic cores of Examples 9 to 13, in the pre-coating mixing step, the amount of lubricant was uniformly added to the soft magnetic powder at 0.6 wt%. and soft magnetic powder. On the other hand, in the powder magnetic cores of Examples 9 to 13, the amount of lubricant mixed in the post-coating mixing step was varied. Other manufacturing methods and conditions are the same as Examples 1 to 8.
実施例９乃至１３の圧粉磁心について、密度（ｇ／ｃｃ）、成形工程中の離型時の抜き圧（ｔｏｎ）、鉄損Ｐｃｖ、ヒステリシス損失Ｐｈｖ、渦電流損失Ｐｅｖ、初透磁率μ（０ｋＡ／ｍ）、及び透磁率μ（５ｋＡ／ｍ）を測定した。その結果を下表４に示す。
（表４）
(Table 4)
また、上表４に従って、図４及び図５のグラフを作成した。図４は、被覆後混合工程における潤滑剤の混合量と初透磁率との関係を示すグラフである。図５は、被覆後混合工程における潤滑剤の混合量と抜き圧との関係を示すグラフである。 In addition, the graphs shown in FIGS. 4 and 5 were created according to Table 4 above. FIG. 4 is a graph showing the relationship between the amount of lubricant mixed in the post-coating mixing step and the initial magnetic permeability. FIG. 5 is a graph showing the relationship between the amount of lubricant mixed and the extraction pressure in the post-coating mixing step.
表４に示すように、実施例９乃至１３は、被覆後混合工程における潤滑剤の混合量がゼロから０．３０ｗｔ％以下で変更されている。そして、表４及び図４に示すように、被覆後混合工程の有無に関わらず、被覆前混合工程の経ることで初透磁率は向上していることが確認された。 As shown in Table 4, in Examples 9 to 13, the amount of lubricant mixed in the post-coating mixing step was changed from zero to 0.30 wt% or less. As shown in Table 4 and FIG. 4, it was confirmed that the initial magnetic permeability was improved by the pre-coating mixing process, regardless of the presence or absence of the post-coating mixing process.
また、表４及び図５に示すように、実施例９乃至１３を比較するとわかるように、被覆後混合工程において潤滑剤を０．１ｗｔ％以上混合すると、抜き圧が低下することが確認された。そして、被覆後混合工程での潤滑剤の混合量を増やすと抜き圧が低下していくことが確認された。また、表２の実施例３乃至８に示すように、被覆後混合工程での潤滑剤の混合量を軟磁性粉末に対して０．３０ｗｔ％とし、且つ被覆前混合工程での潤滑剤の混合量を、被覆後混合工程の潤滑剤よりも多く、軟磁性粉末に対して０．４ｗｔ％以上にすると、抜き圧をゼロにできることが確認された。 Furthermore, as shown in Table 4 and Figure 5, when comparing Examples 9 to 13, it was confirmed that when 0.1 wt% or more of lubricant was mixed in the post-coating mixing process, the evacuation pressure decreased. . It was also confirmed that when the amount of lubricant mixed in the post-coating mixing step was increased, the extraction pressure decreased. In addition, as shown in Examples 3 to 8 in Table 2, the amount of lubricant mixed in the post-coating mixing step was 0.30 wt% with respect to the soft magnetic powder, and the lubricant was mixed in the pre-coating mixing step. It was confirmed that if the amount of the lubricant was larger than that of the lubricant used in the post-coating mixing process, and was 0.4 wt % or more based on the soft magnetic powder, the extraction pressure could be reduced to zero.
（実施例１４乃至２０）
次に、実施例１４乃至２０の圧粉磁心を作製した。実施例１４乃至２０の製造条件を下表５に示す。下表５に示すように、実施例１４乃至２０の圧粉磁心は、主に、ＦｅＳｉＡｌ合金の粉砕粉の粒径が異なる。尚、表中、「Ｎ２」は窒素雰囲気を示す。
（表５）
Next, powder magnetic cores of Examples 14 to 20 were produced. The manufacturing conditions of Examples 14 to 20 are shown in Table 5 below. As shown in Table 5 below, the dust cores of Examples 14 to 20 differ mainly in the particle size of the crushed FeSiAl alloy powder. In addition, in the table, "N2" indicates a nitrogen atmosphere.
(Table 5)
ここで、目開き２５０μｍ、目開き１６８μｍ、目開き１５０μｍ及び目開き１２０μｍの櫛によって得られた粉砕粉において、平均粒径Ｄ５０、平均粒径Ｄ１０及び平均粒径は、下表６の通りであった。
（表６）
(Table 6)
この実施例１４乃至２０の圧粉磁心の密度（ｇ／ｃｃ）、成形工程中の離型時の抜き圧（ｔｏｎ）、鉄損Ｐｃｖ、ヒステリシス損失Ｐｈｖ、渦電流損失Ｐｅｖ、初透磁率μ（０ｋＡ／ｍ）、及び透磁率μ（５ｋＡ／ｍ）を測定した。その結果を下表７に示す。
（表７）
(Table 7)
また、上表７に従って、図６のグラフを作成した。図６は、軟磁性粉末をふるい分ける櫛の目開きと初透磁率μ（０ｋＡ／ｍ）との関係を示すグラフである。 In addition, the graph in FIG. 6 was created according to Table 7 above. FIG. 6 is a graph showing the relationship between the opening of the comb that sieves the soft magnetic powder and the initial magnetic permeability μ (0 kA/m).
表７及び図６に示すように、実施例１４乃至２０の初透磁率に大きな変化はない。即ち、ＦｅＳｉＡｌ合金の粉砕粉の粒径をメジアン径（平均粒径Ｄ５０）で６０μｍ以上とすれば、大きな初透磁率を獲得できることが確認された。また、実施例１４乃至１７と実施例１８乃至２０との比較によりわかるように、熱処理工程の雰囲気に初透磁率が影響されないことも確認された。 As shown in Table 7 and FIG. 6, there is no significant change in the initial magnetic permeability of Examples 14 to 20. That is, it was confirmed that a large initial magnetic permeability can be obtained by setting the median particle size (average particle size D50) of the pulverized powder of FeSiAl alloy to 60 μm or more. Further, as can be seen from the comparison between Examples 14 to 17 and Examples 18 to 20, it was confirmed that the initial magnetic permeability was not affected by the atmosphere of the heat treatment process.
特に、実施例１乃至２０の全てについて比べて見ると、ＦｅＳｉＡｌ合金の粉砕粉の粒径をメジアン径（平均粒径Ｄ５０）で６０μｍ以上とし、被覆前混合工程において、潤滑剤の混合量を軟磁性粉末に対して０．４以上０．７ｗｔ％以下とすると、透磁率は１４０を超えて、少なくとも１４４以上となることが確認された。初透磁率が１４０以上の圧粉磁心をリアクトルやインダクタ等のコイルに用いることで、これらコイルは低電流及び低周波数領域で高いインダクタンスを得ることができる。 In particular, when comparing all of Examples 1 to 20, the particle size of the FeSiAl alloy pulverized powder was set to be 60 μm or more in median diameter (average particle size D50), and the amount of lubricant mixed was softened in the pre-coating mixing process. It was confirmed that when the amount is 0.4 or more and 0.7 wt% or less based on the magnetic powder, the magnetic permeability exceeds 140 and becomes at least 144 or more. By using a powder magnetic core with an initial magnetic permeability of 140 or more for coils such as reactors and inductors, these coils can obtain high inductance in low current and low frequency regions.
（他の実施形態）
以上、本発明の実施形態及び実施例は例として提示したものであって、上記実施形態及び実施例に限定されるものではない。上記実施形態及び実施例は、その他の様々な形態で実施されることが可能であり、発明の範囲を逸脱しない範囲で、種々の省略や置き換え、変更を行うことができる。そして、実施形態、実施例及びその変形は本発明の範囲に含まれるものである。
(Other embodiments)
The embodiments and examples of the present invention have been presented as examples, and the present invention is not limited to the above embodiments and examples. The embodiments and examples described above can be implemented in various other forms, and various omissions, substitutions, and changes can be made without departing from the scope of the invention. The embodiments, examples, and modifications thereof are included within the scope of the present invention.
Claims (4)
前記絶縁処理工程前に、前記ＦｅＳｉＡｌ合金の粉砕粉に対して０．４ｗｔ％以上０．６ｗｔ％以下の割合で潤滑剤を混合する被覆前混合工程と、
前記絶縁樹脂で被覆された前記ＦｅＳｉＡｌ合金の粉砕粉を所定形状の成形体に加圧成形する成形工程と、
前記成形体を大気雰囲気下で焼鈍する熱処理工程と、
前記絶縁処理工程の後、及び前記成形工程の前に、前記絶縁樹脂で被覆された前記ＦｅＳｉＡｌ合金の粉砕粉に更に潤滑剤を混合する被覆後混合工程と、
を含み、
前記被覆前混合工程では、前記被覆後混合工程より多くの潤滑剤を混合すること、
を特徴とする圧粉磁心の製造方法。 An insulation treatment step of coating pulverized FeSiAl alloy powder with a median particle size of 87.2 μm or more and 91.2 μm or less with an insulating resin;
Before the insulation treatment step, a pre-coating mixing step of mixing a lubricant in a proportion of 0.4 wt% or more and 0.6 wt% or less with respect to the pulverized powder of the FeSiAl alloy;
a molding step of press-molding the pulverized powder of the FeSiAl alloy coated with the insulating resin into a molded body of a predetermined shape;
a heat treatment step of annealing the molded body in an atmospheric atmosphere ;
After the insulation treatment step and before the molding step, a post-coating mixing step of further mixing a lubricant into the pulverized powder of the FeSiAl alloy coated with the insulating resin;
including;
mixing more lubricant in the pre-coating mixing step than in the post-coating mixing step;
A method for producing a dust core characterized by:
前記被覆前混合工程では、遅くとも前記乾燥工程の前までに潤滑剤を混合すること、
を特徴とする請求項１記載の圧粉磁心の製造方法。 The insulation treatment step includes a drying step by heating,
In the pre-coating mixing step, mixing a lubricant at least before the drying step;
The method for manufacturing a powder magnetic core according to claim 1, characterized in that:
を特徴とする請求項１又は２記載の圧粉磁心の製造方法。 In the post-coating mixing step, a lubricant is mixed with the pulverized powder of the FeSiAl alloy at a ratio of 0.1 to 0.3 wt%;
The method for manufacturing a powder magnetic core according to claim 1 or 2, characterized in that:
を特徴とする請求項１記載の圧粉磁心の製造方法。 Making the initial permeability of the powder magnetic core 150 or more ,
The method for manufacturing a powder magnetic core according to claim 1 , characterized in that:
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