JP6088192B2 - Manufacturing method of dust core - Google Patents
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Description
本発明は、軟磁性合金粉末並びにそれを用いた圧粉磁芯及びその製造方法に関する。 The present invention relates to a soft magnetic alloy powder, a dust core using the same, and a method for producing the same.
近年の電気機器や電子機器の小型、軽量、高速化への対応はめざましく、それに伴い電
気機器や電子機器に用いられる磁性材料には、より高い飽和磁束密度と、より高い透磁率
が求められている。そこで、高飽和磁束密度および高透磁率を有する軟磁性合金粉末や、
それを用いた圧粉磁心等を得るために、多様な技術が知られている。
In recent years, electrical devices and electronic devices have been dramatically reduced in size, weight, and speed. Accordingly, magnetic materials used in electrical devices and electronic devices are required to have higher saturation magnetic flux density and higher magnetic permeability. Yes. Therefore, soft magnetic alloy powder having high saturation magnetic flux density and high permeability,
Various techniques are known for obtaining a dust core using the same.
このような技術のうちのひとつとして、特許文献１には、軟磁性粉末に熱処理を施すことによって粉末の表面近傍に非晶質相からなる層を形成し、当該粉末をプレス形成することにより、圧粉磁芯を得る技術が開示されている。 As one of such techniques, Patent Document 1 discloses that a layer made of an amorphous phase is formed in the vicinity of the surface of the powder by heat-treating the soft magnetic powder, and the powder is press-formed, A technique for obtaining a dust core is disclosed.
しかしながら、軟磁性粉末に対して熱処理を施す際には、相変態に伴うエネルギー放出（発熱）が急激に起こり、軟磁性合金粉末の温度が急上昇して結晶粒の粗大化や不純物の生成が引き起こされ、軟磁気特性が劣化することがあり、上記特許文献１に開示されている技術においてはかかる問題に対して何ら考慮がなされていない。また、熱処理に伴う結晶粒の粗大化や不純物の生成を抑制しながらも、十分なα−Ｆｅを析出させるためには複雑な熱処理パターンが必要となる。 However, when heat treatment is performed on the soft magnetic powder, energy release (heat generation) accompanying the phase transformation occurs rapidly, and the temperature of the soft magnetic alloy powder rises rapidly, causing coarsening of crystal grains and generation of impurities. As a result, the soft magnetic characteristics may be deteriorated, and the technique disclosed in Patent Document 1 does not take into consideration such a problem. In addition, a complicated heat treatment pattern is required to precipitate sufficient α-Fe while suppressing the coarsening of crystal grains and the generation of impurities due to the heat treatment.
本発明は、熱処理工程における試料温度の上昇を抑制し且つ複雑な熱処理パターンを行うことなく軟磁気特性を向上させた軟磁性合金粉末を提供し、併せて、当該軟磁性合金粉末を用いた圧粉磁芯及び当該圧粉磁芯の製造方法を提供することを目的とする。 The present invention provides a soft magnetic alloy powder that suppresses an increase in the sample temperature in the heat treatment step and has improved soft magnetic properties without performing a complicated heat treatment pattern. In addition, a pressure using the soft magnetic alloy powder is provided. It aims at providing the manufacturing method of a powder magnetic core and the said powder magnetic core.
本発明によれば、第１の軟磁性合金粉末として、組成式ＦｅａＢｂＳｉｃＰｘＣｙＣｕｚで表わされ、７９≦ａ≦８６ａｔ％、５≦ｂ≦１３ａｔ％、０≦ｃ≦８ａｔ％、１≦ｘ≦１０ａｔ％、０≦ｙ≦５ａｔ％、０．４≦ｚ≦１．４ａｔ％、及び０．０６≦ｚ／ｘ≦１．２０を満たす軟磁性合金粉末であって、
当該軟磁性合金粉末は、結晶相を主相とする結晶相部及び非晶質相を主相とする非晶質相部とを有する軟磁性合金粉末粒を有しており、
当該軟磁性合金粉末粒における前記結晶相部の割合は、５０重量％未満である、
軟磁性合金粉末が得られる。
According to the present invention, as the first soft magnetic alloy powder represented by a composition formula Fe a B b Si c P x C y Cu z, 79 ≦ a ≦ 86at%, 5 ≦ b ≦ 13at%, 0 ≦ Soft magnetic alloy powder satisfying c ≦ 8 at%, 1 ≦ x ≦ 10 at%, 0 ≦ y ≦ 5 at%, 0.4 ≦ z ≦ 1.4 at%, and 0.06 ≦ z / x ≦ 1.20. And
The soft magnetic alloy powder has soft magnetic alloy powder grains having a crystal phase portion having a crystal phase as a main phase and an amorphous phase portion having an amorphous phase as a main phase,
The proportion of the crystal phase part in the soft magnetic alloy powder grains is less than 50% by weight.
A soft magnetic alloy powder is obtained.
また、本発明によれば、第２の軟磁性合金粉末として、第１の軟磁性合金粉末であって、
前記Ｆｅの３ａｔ％以下を、Ｔｉ、Ｖ、Ｚｒ、Ｈｆ、Ｎｂ、Ｔａ、Ｍｏ、Ｗ、Ｃｒ、Ｃｏ、Ｎｉ、Ａｌ、Ｍｎ、Ａｇ、Ａｕ、Ｚｎ、Ｓ、Ｃａ、Ｓｎ、Ａｓ、Ｓｂ、Ｂｉ、Ｎ、Ｏ、Ｍｇ、白金族元素、及び希土類元素のうち、１種類以上の元素で置換してなる、
軟磁性合金粉末が得られる。
According to the present invention, the second soft magnetic alloy powder is the first soft magnetic alloy powder,
Fe, 3 at% or less of Ti, V, Zr, Hf, Nb, Ta, Mo, W, Cr, Co, Ni, Al, Mn, Ag, Au, Zn, S, Ca, Sn, As, Sb, Of Bi, N, O, Mg, platinum group elements, and rare earth elements, substituted with one or more elements,
A soft magnetic alloy powder is obtained.
また、本発明によれば、第３の軟磁性合金粉末として、第１又は第２の軟磁性合金粉末であって、
前記軟磁性合金粉末粒の中心部には、前記結晶相部が位置しており、
前記軟磁性合金粉末粒の外周部には、前記非晶質相部が位置している、
軟磁性合金粉末が得られる。
According to the present invention, the third soft magnetic alloy powder is the first or second soft magnetic alloy powder,
In the central part of the soft magnetic alloy powder grains, the crystal phase part is located,
In the outer peripheral portion of the soft magnetic alloy powder particles, the amorphous phase portion is located,
A soft magnetic alloy powder is obtained.
また、本発明によれば、第４の軟磁性合金粉末として、第３の軟磁性合金粉末であって、
前記非晶質相部の前記軟磁性合金粉末粒における径方向の厚さは２μｍ以上である、
軟磁性合金粉末が得られる。
According to the present invention, the fourth soft magnetic alloy powder is a third soft magnetic alloy powder,
The thickness in the radial direction of the soft magnetic alloy powder grains of the amorphous phase part is 2 μm or more.
A soft magnetic alloy powder is obtained.
また、本発明によれば、第１の圧粉磁芯として、第１乃至第４のいずれかの軟磁性合金粉末と結合剤とを混合した後に加圧成型し、更に熱処理をしてなる圧粉磁芯であって、
当該圧粉磁芯において、前記軟磁性合金粉末粒の前記中心部には粒径６０ｎｍ未満の結晶粒が分散しており、前記軟磁性合金粉末粒の前記外周部には粒径４０ｎｍ未満の結晶粒が分散している、
圧粉磁芯が得られる。
Further, according to the present invention, as the first dust core, the first magnetic core powder is mixed with any one of the first to fourth soft magnetic alloy powders and the binder, and then pressure-molded and further subjected to heat treatment. A powder core,
In the dust core, crystal grains having a particle size of less than 60 nm are dispersed in the central portion of the soft magnetic alloy powder particles, and crystals having a particle size of less than 40 nm are dispersed in the outer peripheral portion of the soft magnetic alloy powder particles. The grains are dispersed,
A dust core is obtained.
また、本発明によれば、第２の圧粉磁芯として、第１の圧粉磁芯であって、
前記中心部における結晶粒の割合及び前記外周部における結晶粒の割合は、夫々３５ｖｏｌ％以上である、
圧粉磁芯が得られる。
Further, according to the present invention, the second dust core is a first dust core,
The proportion of crystal grains in the central portion and the proportion of crystal grains in the outer peripheral portion are each 35 vol% or more.
A dust core is obtained.
また、本発明によれば、第１乃至第４のいずれかの軟磁性合金粉末と結合剤とを混合した後に加圧成型する工程と、成型された前記軟磁性合金粉末を熱処理する工程とを備える、
圧粉磁芯の製造方法が得られる。
Further, according to the present invention, the step of pressure molding after mixing any one of the first to fourth soft magnetic alloy powders and the binder, and the step of heat-treating the molded soft magnetic alloy powders. Prepare
A method for producing a dust core is obtained.
本発明によれば、熱処理前の軟磁性合金粉末において、中心部に結晶相を有し且つ外周部に非晶質層を有する軟磁性合金粉末を用いたことから、熱処理工程における発熱量を減少させることができる。詳しくは、中心部の結晶相の存在により熱容量に対する発熱量が減少し、熱処理時における試料温度の上昇を抑制することができる。これにより、結晶粒の粗大化や不純物の生成が起こらないことから、圧粉磁芯の磁気的特性を向上させることができる。 According to the present invention, since the soft magnetic alloy powder before the heat treatment uses the soft magnetic alloy powder having the crystal phase in the central portion and the amorphous layer in the outer peripheral portion, the calorific value in the heat treatment step is reduced. Can be made. Specifically, the amount of heat generated with respect to the heat capacity is reduced due to the presence of the crystal phase in the center, and the rise in the sample temperature during heat treatment can be suppressed. Thereby, since the coarsening of a crystal grain and the production | generation of an impurity do not occur, the magnetic characteristic of a dust core can be improved.
また、軟磁性合金粉末の最表面に非晶質相が存在していることにより、充填率を低減させることなく圧粉磁心を作製できる。更に、本発明によれば、複雑な熱処理パターンを施すことなく圧粉磁心を作製することができる。 In addition, since the amorphous phase is present on the outermost surface of the soft magnetic alloy powder, a dust core can be produced without reducing the filling rate. Furthermore, according to the present invention, a dust core can be produced without applying a complicated heat treatment pattern.
本発明の実施の形態による圧粉磁心の製造方法は、図１に示されるように、概略、２つの工程：即ち、軟磁性合金粉末（詳しくは後述する）を作製する粉末作製工程と；当該軟磁性合金粉末を用いて圧粉磁心を作製する磁心作製工程とを備えている。磁心作製工程では、混合粉末にシリコーン系などの耐熱性が高く絶縁性が良好な結合材を混合することにより、造粒粉を得る。次いで、金型を用いて造粒粉を加圧成型して圧粉体を得る。その後、圧粉体を熱処理して、ナノ結晶化と結合材の硬化を同時に行い、圧粉磁心を作製する。 As shown in FIG. 1, the method for manufacturing a powder magnetic core according to an embodiment of the present invention is roughly divided into two steps: a powder production step for producing a soft magnetic alloy powder (described later in detail); And a magnetic core manufacturing step of manufacturing a powder magnetic core using soft magnetic alloy powder. In the magnetic core manufacturing process, a granulated powder is obtained by mixing the mixed powder with a binder such as a silicone-based resin having high heat resistance and good insulation. Next, the granulated powder is pressure-molded using a mold to obtain a green compact. Thereafter, the green compact is heat treated to simultaneously perform nanocrystallization and curing of the binder to produce a dust core.
ここで、粉末作製工程の説明の前に本実施の形態による軟磁性合金粉末の組成について説明する。本実施の形態による軟磁性合金粉末の組成式は、ＦｅａＢｂＳｉｃＰｘＣｙＣｕｚで表わされ、７９≦ａ≦８６ａｔ％、５≦ｂ≦１３ａｔ％、０≦ｃ≦８ａｔ％、１≦ｘ≦１０ａｔ％、０≦ｙ≦５ａｔ％、０．４≦ｚ≦１．４ａｔ％、及び０．０６≦ｚ／ｘ≦１．２０を満たしている。 Here, the composition of the soft magnetic alloy powder according to the present embodiment will be described before the description of the powder production process. Composition formula of soft magnetic alloy powder according to the present embodiment is represented by Fe a B b Si c P x C y Cu z, 79 ≦ a ≦ 86at%, 5 ≦ b ≦ 13at%, 0 ≦ c ≦ 8at %, 1 ≦ x ≦ 10 at%, 0 ≦ y ≦ 5 at%, 0.4 ≦ z ≦ 1.4 at%, and 0.06 ≦ z / x ≦ 1.20.
上記軟磁性合金粉末において、Ｆｅは主元素であり、磁性を担う必須元素である。飽和磁束密度の向上及び原料価格の低減のため、Ｆｅの割合が多いことが基本的には好ましい。Ｆｅの割合が７９ａｔ％より少ないと、望ましいＢｓが得られない。Ｆｅの割合が８４ａｔ％より多いと、液体急冷条件下における非晶質相の形成が困難になる。なお、１．６０Ｔ以上の飽和磁束密度を有する圧粉磁芯を得るためには、Ｆｅの割合は、８０ａｔ％以上であることが望ましい。 In the soft magnetic alloy powder, Fe is a main element and an essential element that takes on magnetism. In order to improve the saturation magnetic flux density and reduce the raw material price, it is basically preferable that the ratio of Fe is large. When the proportion of Fe is less than 79 at%, desirable Bs cannot be obtained. When the proportion of Fe is more than 84 at%, it becomes difficult to form an amorphous phase under liquid quenching conditions. In order to obtain a dust core having a saturation magnetic flux density of 1.60 T or more, the ratio of Fe is desirably 80 at% or more.
また、上記軟磁性合金粉末において、Ｂは非晶質相形成を担う必須元素である。Ｂの割合が３ａｔ％より少ないと、液体急冷条件下における非晶質相の形成が困難になる。１３ａｔ％より多いと、ΔＴが減少し、均質なナノ結晶組織を得ることができない。特に、原料を溶湯とする際に融点を低くし量産化を容易にするためには、Ｂの割合は、１０ａｔ％以下であることが望ましい。 In the soft magnetic alloy powder, B is an essential element responsible for forming an amorphous phase. When the proportion of B is less than 3 at%, it becomes difficult to form an amorphous phase under liquid quenching conditions. If it exceeds 13 at%, ΔT decreases and a homogeneous nanocrystalline structure cannot be obtained. In particular, the ratio of B is desirably 10 at% or less in order to lower the melting point and facilitate mass production when the raw material is used as a molten metal.
また、上記軟磁性合金粉末において、Ｓｉは非晶質相形成を担う元素であり、必ずしも含まれなくても良いが、微細結晶化にあたっては微細結晶の安定化に寄与する。Ｓｉの割合が８ａｔ％よりも多いと非晶質形成能が低下する。特に、合金溶湯を急冷する際に容易に非晶質の形成が行われることを考慮すると、Ｓｉの割合は、５ａｔ％以下であることが望ましい。 In the soft magnetic alloy powder, Si is an element responsible for forming an amorphous phase and may not necessarily be contained, but contributes to stabilization of the fine crystal in the fine crystallization. When the proportion of Si is more than 8 at%, the amorphous forming ability is lowered. In particular, it is desirable that the Si ratio be 5 at% or less, considering that the amorphous formation is easily performed when the molten alloy is rapidly cooled.
また、上記軟磁性合金粉末において、Ｐは非晶質相形成を担う必須元素である。Ｐの割合が１ａｔ％より少ないと、液体急冷条件下における非晶質相の形成が困難になる。Ｐの割合が１０ａｔ％より多いと、Ｂｓが低下する。特に、本実施の形態においては、Ｂ、Ｓｉ及びＰの組み合わせを用いることで、いずれか一つしか用いない場合と比較して、非晶質相形成能や微細結晶の安定性を高めることができる。 In the soft magnetic alloy powder, P is an essential element responsible for forming an amorphous phase. When the proportion of P is less than 1 at%, it becomes difficult to form an amorphous phase under liquid quenching conditions. When the proportion of P is more than 10 at%, Bs decreases. In particular, in this embodiment, by using a combination of B, Si, and P, it is possible to improve the amorphous phase forming ability and the stability of the fine crystal as compared with the case where only one of them is used. it can.
また、上記軟磁性合金粉末において、Ｃは非晶質形成を担う元素であり、必ずしも含まれなくても良い。Ｃは安価であるため、Ｃの添加により他の半金属量が低減され、総材料コストが低減される。ただし、Ｃの割合が５ａｔ％を超えると、合金組成物が脆化する。特に、原料の溶湯時におけるＣの蒸発に起因した組成のばらつきを抑えるためには、Ｃの割合は３ａｔ％以下であることが望ましい。また、本実施の形態においては、Ｂ、Ｓｉ、Ｐ、Ｃの組み合わせを用いることで、いずれか一つしか用いない場合と比較して、非晶質相形成能や微細結晶の安定性を高めることができる。 In the soft magnetic alloy powder, C is an element responsible for amorphous formation, and is not necessarily included. Since C is inexpensive, the addition of C reduces the amount of other metalloids and reduces the total material cost. However, when the proportion of C exceeds 5 at%, the alloy composition becomes brittle. In particular, in order to suppress variation in composition due to evaporation of C when the raw material melts, it is desirable that the C ratio be 3 at% or less. Further, in this embodiment, by using a combination of B, Si, P, and C, the amorphous phase forming ability and the stability of the fine crystal are improved as compared with the case where only one of them is used. be able to.
また、上記軟磁性合金粉末において、Ｃｕは微細結晶化に寄与する必須元素である。Ｃｕの割合が０．４ａｔ％より少ないと、ナノ結晶化が困難になる。Ｃｕの割合が１．４ａｔ％より多いと、非晶質相が不均質になり、熱処理によって均質なナノ結晶組織が得られないことに加え、材料コストが嵩む。特に、軟磁性合金粉末の酸化及びナノ結晶への粒成長を考慮すると、Ｃｕの割合は、０．５ａｔ％以上、１．３ａｔ％以下であることが好ましい。 In the soft magnetic alloy powder, Cu is an essential element contributing to fine crystallization. When the ratio of Cu is less than 0.4 at%, nanocrystallization becomes difficult. If the Cu content is higher than 1.4 at%, the amorphous phase becomes inhomogeneous, and a uniform nanocrystal structure cannot be obtained by heat treatment, and the material cost increases. In particular, considering the oxidation of the soft magnetic alloy powder and the grain growth into nanocrystals, the Cu ratio is preferably 0.5 at% or more and 1.3 at% or less.
なお、ＰとＣｕとの間には、強い原子間引力がある。従って、上記軟磁性合金粉末が特定の比率のＰとＣｕとを含んでいると、１０ｎｍ以下のサイズのクラスターが形成され、この微細なクラスターによって微細結晶の形成の際にｂｃｃＦｅ結晶は微細構造を有するようになる。詳しくは、Ｐの割合（ｘ）とＣｕの割合（ｚ）との特定の比率（ｚ／ｘ）は０．０８以上、１．２以下である。特に、軟磁性合金粉末の脆化及び酸化を考慮すると、特定の比率（ｚ／ｘ）は、０．０８以上、０．８以下であることが望ましい。 There is a strong interatomic attractive force between P and Cu. Therefore, if the soft magnetic alloy powder contains a specific ratio of P and Cu, a cluster having a size of 10 nm or less is formed, and the bccFe crystal has a fine structure when the fine crystal is formed by the fine cluster. To have. Specifically, the specific ratio (z / x) of the ratio (x) of P and the ratio (z) of Cu is 0.08 or more and 1.2 or less. In particular, in consideration of embrittlement and oxidation of the soft magnetic alloy powder, the specific ratio (z / x) is preferably 0.08 or more and 0.8 or less.
また、上記軟磁性合金粉末において、Ｆｅの３ａｔ％以下をＴｉ、Ｚｒ、Ｈｆ、Ｎｂ、Ｔａ、Ｍｏ、Ｗ、Ｃｒ、Ｃｏ、Ｎｉ、Ａｌ、Ｍｎ、Ａｇ、Ｚｎ、Ｓ、Ｓｎ、Ａｓ、Ｓｂ、Ｂｉ、Ｙ、Ｎ、Ｏ、Ｍｇ、Ｃａ、Ｖ及び希土類元素のうち１種類以上の元素で置換することにより、ことにより良好な磁気特性が得られる。これらの元素は、基本的に不純物元素であり、製造過程において軟磁性合金粉末に含有される可能性がある。不純物元素を多く含有した場合には、磁気特性が劣化すると考えられるが、Ｆｅ置換が３ａｔ％以下であれば、耐食性の改善や電気抵抗の調整などのため、飽和磁束密度の著しい低下が生じない範囲で置換可能で、良好な磁気特性を維持できる。 In the soft magnetic alloy powder, 3 at% or less of Fe is Ti, Zr, Hf, Nb, Ta, Mo, W, Cr, Co, Ni, Al, Mn, Ag, Zn, S, Sn, As, Sb. By substituting with one or more elements of Bi, Y, N, O, Mg, Ca, V and rare earth elements, good magnetic properties can be obtained. These elements are basically impurity elements and may be contained in the soft magnetic alloy powder in the manufacturing process. When many impurity elements are contained, it is considered that the magnetic characteristics are deteriorated. However, if the Fe substitution is 3 at% or less, the saturation magnetic flux density is not significantly reduced for improving the corrosion resistance and adjusting the electric resistance. It can be replaced within a range, and good magnetic properties can be maintained.
図１を再び参照すると、粉末作製工程においては、例えば、溶湯を細かく粉末化するアトマイズ法を用いて所望とする軟磁性合金粉末を得ることができる。詳しくは、Ｆｅや半金属元素等の原料を秤量した後、溶解して合金溶湯を生成する。この合金溶湯をノズルから排出して出来た合金溶湯の流れに冷却媒体を衝突させて、合金溶湯を微細化すると共に急冷し、軟磁性合金粉末を得る。ここで、冷却媒体についての限定は特にはない。従って、例えば、アルゴンなどの不活性ガスや窒素及び空気などの各種気体を用いるガスアトマイズ法や、高圧の水を用いる水アトマイズ法を採用することができる。加えて、微細化と急冷とに異なる媒体を用いて実施しても良い。 Referring to FIG. 1 again, in the powder preparation step, for example, a desired soft magnetic alloy powder can be obtained by using an atomizing method in which a molten metal is finely powdered. Specifically, after raw materials such as Fe and metalloid elements are weighed, they are melted to form a molten alloy. A cooling medium is made to collide with the flow of the molten alloy produced by discharging the molten alloy from the nozzle, and the molten alloy is refined and rapidly cooled to obtain a soft magnetic alloy powder. Here, there is no particular limitation on the cooling medium. Therefore, for example, a gas atomizing method using an inert gas such as argon or various gases such as nitrogen and air, or a water atomizing method using high-pressure water can be employed. In addition, different media may be used for miniaturization and rapid cooling.
冷却媒体は粉末（溶湯）の外周表面と接触するため、粉末においては粒子の表面近傍の方が中心部よりも急冷速度が速く、非晶質性が良好になる。従って、図２に示されるように、本実施の形態による軟磁性合金粉末においては、粒子の中心部に結晶相を主相とする結晶相部が生じ、粒子の外周部には非晶質相を主相とする非晶質相部が生じている粉末が作製される。なお、冷却媒体の種類や粉末粒径、合金溶湯の出湯温度を変更することで、得られる粉末における結晶相部の粒子全体に占める割合を制御することが可能である。 Since the cooling medium is in contact with the outer peripheral surface of the powder (molten metal), in the powder, the vicinity of the surface of the particles has a faster cooling rate than the central portion, and the amorphousness is improved. Therefore, as shown in FIG. 2, in the soft magnetic alloy powder according to the present embodiment, a crystal phase portion having a crystal phase as a main phase is generated at the center of the particle, and an amorphous phase is formed at the outer periphery of the particle. Thus, a powder in which an amorphous phase portion having a main phase is produced is produced. In addition, it is possible to control the ratio which occupies for the whole particle | grains of the crystal phase part in the obtained powder by changing the kind of cooling medium, a powder particle size, and the tapping temperature of a molten alloy.
図２に示されるように、磁心作製工程において使用される軟磁性合金粉末、即ち熱処理前の軟磁性合金粉末は、非晶質相部の厚みが粉末外表面より２μｍ以上あり、中心部にはｂｃｃＦｅ（αＦｅ，Ｆｅ−Ｓｉ）から成る結晶相部を有している。なお、圧粉磁芯の充填率を維持する効果を十分に得るためには、非晶質相部の厚みが粉末外表面より５μｍ以上あることが望ましい。一方、結晶相部の割合は、粉末全体に対して５０重量％未満である。結晶相部の割合が少ない場合には温度上昇抑制効果が小さくなり、多い場合には大きな結晶粒子の割合が多くなる。よって、後述する熱処理後における圧粉磁心の磁気特性の劣化を考慮すると、結晶相部の割合は、粒子全体に対して１０重量％以上、３０重量％未満であることが望ましい。 As shown in FIG. 2, the soft magnetic alloy powder used in the magnetic core preparation process, that is, the soft magnetic alloy powder before the heat treatment, has an amorphous phase portion thickness of 2 μm or more from the outer surface of the powder, It has a crystal phase portion made of bccFe (αFe, Fe—Si). In order to sufficiently obtain the effect of maintaining the filling rate of the dust core, it is desirable that the thickness of the amorphous phase part is 5 μm or more from the powder outer surface. On the other hand, the ratio of the crystal phase part is less than 50% by weight with respect to the whole powder. When the proportion of the crystal phase portion is small, the temperature rise suppressing effect is small, and when the proportion is large, the proportion of large crystal particles is large. Therefore, considering the deterioration of the magnetic properties of the dust core after heat treatment, which will be described later, the proportion of the crystal phase part is desirably 10% by weight or more and less than 30% by weight with respect to the entire particle.
本発明による軟磁性合金粉末は、図３に示されるように、所定の昇温速度となるように加熱し続けた場合に、発熱ピークを２つ以上有するようなＤＳＣ曲線を得られるようなものであり、結晶相部の割合の測定については、示差走査熱量分析計（ＤＳＣ）によって行われる。詳しくは、結晶相部の割合は、非晶質であることが確認されている同じ合金組成の薄帯における発熱量を基準にして、ｂｃｃＦｅ（αＦｅ，Ｆｅ−Ｓｉ）の析出に伴う単位重量あたりの発熱量が減少した割合として求めることができる（減少分がアトマイズ時に結晶化した割合、すなわち結晶相部の割合を示す）。 As shown in FIG. 3, the soft magnetic alloy powder according to the present invention is such that a DSC curve having two or more exothermic peaks can be obtained when heating is continued at a predetermined rate of temperature increase. The ratio of the crystal phase part is measured by a differential scanning calorimeter (DSC) . Specifically, the ratio of the crystal phase part is based on the calorific value in the ribbon of the same alloy composition that has been confirmed to be amorphous, per unit weight accompanying the precipitation of bccFe (αFe, Fe-Si). The amount of heat generated can be calculated as the rate of reduction (the rate of decrease indicates the rate of crystallization during atomization, that is, the rate of the crystal phase portion).
また、非晶質相部の厚みについては、電子顕微鏡による軟磁性合金粉末断面の組織観察において求めることができる。軟磁性合金粉末断面は、軟磁性合金粉末を冷間樹脂中に埋め込み硬化し、研磨することで作製する。作製した軟磁性合金粉末断面のうち、大きなもの（埋め込んだ粉末のＤ９０程度）を選択することで、粉末のほぼ中心を通る断面の観察が可能である。すなわち、分級等により、粒度分布を調整した軟磁性合金粉末を作製することで、所定の粒径の粉末を観察することができる。非晶質相部の厚みは、粉末作製工程により得られた軟磁性合金粉末における平均粒径Ｄ５０程度の粉末を１０個以上選択し、各粉末あたり３箇所を測定して算出した平均値である。 The thickness of the amorphous phase can be determined by observing the structure of the soft magnetic alloy powder cross section with an electron microscope. The cross section of the soft magnetic alloy powder is prepared by embedding and curing the soft magnetic alloy powder in a cold resin and polishing. By selecting a large one (about D 90 of the embedded powder) among the produced soft magnetic alloy powder cross sections, it is possible to observe a cross section passing through the approximate center of the powder. That is, a powder having a predetermined particle diameter can be observed by preparing a soft magnetic alloy powder having an adjusted particle size distribution by classification or the like. The thickness of the amorphous phase portion, a powder having an average particle size D 50 in the soft magnetic alloy powder obtained by powder manufacturing process selected 10 or more, the average value calculated by measuring the three per each powder is there.
磁心作製工程においては、本発明による軟磁性合金粉末をシリコーン系などの耐熱性が高く絶縁性が良好な結合材と混合・造粒して造粒粉を得る。次いで、金型を用いて造粒粉を加圧成型して圧粉体を得る。その後、圧粉体を熱処理して、ナノ結晶化と結合材の硬化を同時に行い、圧粉磁心を得る。 In the magnetic core preparation process, the soft magnetic alloy powder according to the present invention is mixed and granulated with a binder such as a silicone-based material having high heat resistance and good insulation to obtain granulated powder. Next, the granulated powder is pressure-molded using a mold to obtain a green compact. Thereafter, the green compact is heat treated to simultaneously perform nanocrystallization and curing of the binder to obtain a dust core.
ここで、本実施の形態による熱処理は、軟磁性合金粉末を毎分１０℃以上の昇温速度で加熱し、ナノ結晶を析出させる。その熱量の状況は、ＤＳＣ（Ｄｉｆｆｅｒｅｎｔｉａｌ
ＳｃａｎｎｉｎｇＣａｌｏｒｉｍｅｔｒｙ：示差走査熱量測定、以下ＤＳＣと記す）で、測定することができる。ＤＳＣは、測定試料と基準物質との間の熱量の差を計測することで、縦軸に重量で規格化した熱流、横軸に温度や時間をとった曲線となる。ＤＳＣで測定されるＤＳＣ曲線について説明する。図３は、本発明の実施の形態に係るＤＳＣ曲線の説明図である。ＤＳＣ曲線は、Ｐｔ製試料容器中に投入した試料をＤＳＣ装置内に設置し、不活性雰囲気中において昇温速度４０℃／分で試料を目的の温度まで加熱することで得られる。ここで、熱処理は、図３に示すＤＳＣ曲線において、「第一結晶化開始温度Ｔｘ１−５０℃」以上、「第二結晶化開始温度Ｔｘ２」未満で行われる。「第一結晶化開始温度Ｔｘ１−５０℃」以上、「第二結晶化開始温度Ｔｘ２」未満の適切な温度範囲で熱処理が行われると、平均粒径５ｎｍ以上５０ｎｍ以下のｂｃｃＦｅナノ結晶が析出し、軟磁気特性の向上が図れる。熱処理温度が「第二結晶化開始温度Ｔｘ２」を超えてしまうと、Ｆｅ−ＢやＦｅ−Ｐなどが析出し、軟磁気特性が劣化してしまう。また、図３に示すＤＳＣ曲線において、ベースラインに対する山のピークは発熱反応、谷のピークは吸熱反応として現れる。従って、熱処理工程においては第一結晶化のみを促進するように、熱処理することで、優れた磁気特性を有する圧粉磁心を製造することができる。
Here, in the heat treatment according to the present embodiment, the soft magnetic alloy powder is heated at a temperature rising rate of 10 ° C. or more per minute to precipitate nanocrystals. The amount of heat is determined by DSC (Differential.
Scanning Calorimetry: differential scanning calorimetry (hereinafter referred to as DSC)). DSC is a curve in which the vertical axis represents heat flow normalized by weight and the horizontal axis represents temperature and time by measuring the difference in the amount of heat between the measurement sample and the reference material. The DSC curve measured by DSC will be described. FIG. 3 is an explanatory diagram of a DSC curve according to the embodiment of the present invention. The DSC curve is obtained by placing a sample put in a Pt sample container in a DSC apparatus and heating the sample to a target temperature at a temperature rising rate of 40 ° C./min in an inert atmosphere. Here, the heat treatment is performed at a temperature not less than “first crystallization start temperature Tx 1 −50 ° C.” and less than “second crystallization start temperature Tx 2 ” in the DSC curve shown in FIG. When heat treatment is performed in an appropriate temperature range of “first crystallization start temperature Tx 1 −50 ° C.” or more and less than “second crystallization start temperature Tx 2 ”, bccFe nanocrystals having an average particle size of 5 nm or more and 50 nm or less are formed. Precipitates and can improve soft magnetic properties. If the heat treatment temperature exceeds the “second crystallization start temperature Tx 2 ”, Fe—B, Fe—P and the like are precipitated, and the soft magnetic characteristics are deteriorated. In the DSC curve shown in FIG. 3, the peak of the peak with respect to the baseline appears as an exothermic reaction, and the peak of the valley appears as an endothermic reaction. Therefore, in the heat treatment step, a dust core having excellent magnetic properties can be produced by heat treatment so as to promote only the first crystallization.
以上のようにして得られた圧粉磁心に含まれるＦｅ基ナノ結晶合金粉末は、粉末（粒子）の中心部においては結晶粒径６０ｎｍ以下の結晶粒が非晶質中に体積分率で３５ｖｏｌ％以上分散し、粉末（粒子）の外周部においては結晶粒径４０ｎｍ以下の結晶粒が非晶質中に体積分率３５ｖｏｌ％以上分散した構造を有している。特に、低保磁力化及び良好な磁気特性を得るためには、粉末（粒子）の中心部における結晶粒径は３５ｎｍ未満であることが望ましく、粉末（粒子）の外周部における結晶粒径は３０ｎｍ未満であることが望ましい。また、より高い飽和磁束密度Ｂｓを得るためには、中心部及び外周部の夫々の非晶質中に占める結晶粒の体積分率は、５０ｖｏｌ％以上であることが望ましい。中心部及び外周部の夫々の非晶質中に占める結晶粒の割合（体積分率）が多いほど、高い飽和磁束密度Ｂｓが得られることから、コア等の応用製品の小型化に対して有利となる。詳しくは、上記結晶粒の体積分率が３５ｖｏｌ％以上である場合、１．６０Ｔ以上の飽和磁束密度Ｂｓが得られ、上記結晶粒の体積分率が５０ｖｏｌ％以上である場合、１．７３Ｔ以上の飽和磁束密度Ｂｓが得られる。 The Fe-based nanocrystalline alloy powder contained in the dust core obtained as described above has a volume fraction of 35 vol. In the center of the powder (particles) in which crystal grains having a crystal grain size of 60 nm or less are amorphous. %, And the outer periphery of the powder (particles) has a structure in which crystal grains having a crystal grain size of 40 nm or less are dispersed in an amorphous material with a volume fraction of 35 vol% or more. In particular, in order to obtain a low coercive force and good magnetic properties, it is desirable that the crystal grain size at the center of the powder (particles) is less than 35 nm, and the crystal grain size at the outer periphery of the powder (particles) is 30 nm. It is desirable to be less than. In order to obtain a higher saturation magnetic flux density Bs, it is desirable that the volume fraction of crystal grains in each amorphous portion in the center portion and the outer peripheral portion is 50 vol% or more. A higher saturation magnetic flux density Bs can be obtained as the proportion of crystal grains (volume fraction) in the amorphous material in each of the central portion and the outer peripheral portion is increased, which is advantageous for downsizing of application products such as cores. It becomes. Specifically, when the volume fraction of the crystal grains is 35 vol% or more, a saturation magnetic flux density Bs of 1.60 T or more is obtained, and when the volume fraction of the crystal grains is 50 vol% or more, 1.73 T or more. The saturation magnetic flux density Bs is obtained.
結晶粒径、結晶相部の体積分率については、非晶質相の厚みと同様に、電子顕微鏡による軟磁性合金粉末断面の組織観察において求めることができる。結晶粒径は、軟磁性合金粉末断面の組織写真において、所定位置（外周部／中心部）における結晶粒を３０個以上選択し、各粒子の長径と短径を測定して算出した平均値である。結晶相部の体積分率は、線分法により求めており、組織写真に任意に引いた直線において、その直線の長さのうち、結晶相部を通過している長さの総和が占める割合で表される。 Similar to the thickness of the amorphous phase, the crystal grain size and the volume fraction of the crystal phase part can be obtained by observing the structure of the soft magnetic alloy powder cross section with an electron microscope. The crystal grain size is an average value calculated by selecting 30 or more crystal grains at a predetermined position (outer periphery / center) in the structure photograph of the cross section of the soft magnetic alloy powder, and measuring the major axis and minor axis of each grain. is there. The volume fraction of the crystal phase part is obtained by the line segment method, and in the straight line arbitrarily drawn on the structure photograph, the ratio of the total length passing through the crystal phase part out of the length of the straight line It is represented by
以上より、本発明においては、非晶質性合金粉末が粉末全体に対して５０重量％未満の割合で結晶相部を有し、熱処理工程において急激な発熱を抑制できることから、結晶の粗大化や不要な化合物の生成の抑制されたものであり、また、軟磁性合金粉末において、表面に２μｍ以上の非晶質相部を有することから、発熱を抑制しつつも充填率の低下を防ぐことが可能であり、従って、圧粉磁心も優れた軟磁気特性と高飽和磁束密度を有するものとなる。 As described above, in the present invention, the amorphous alloy powder has a crystal phase part in a proportion of less than 50% by weight with respect to the whole powder, and since rapid heat generation can be suppressed in the heat treatment step, The generation of unnecessary compounds is suppressed, and the soft magnetic alloy powder has an amorphous phase part of 2 μm or more on the surface, so that it is possible to prevent a decrease in filling rate while suppressing heat generation. Therefore, the dust core also has excellent soft magnetic properties and high saturation magnetic flux density.
なお、本実施の形態における軟磁性合金粉末は、粒子全体に非晶質相を有する粉末（即ち、中心部に結晶相を有していない粉末）が混在していても良い。また、上述した実施の形態では軟磁性合金粉末を用いた圧粉磁心について説明しているが、圧粉磁心以外の磁性部品への適用も同様に可能である。 Note that the soft magnetic alloy powder in the present embodiment may include a powder having an amorphous phase throughout the particle (that is, a powder having no crystal phase in the center). In the above-described embodiment, the dust core using the soft magnetic alloy powder has been described. However, application to magnetic parts other than the dust core is also possible.
以下、本発明について実施例および比較例を用いて説明する。 Hereinafter, the present invention will be described using examples and comparative examples.
（実施例１〜３、比較例１及び２）
Ｆｅ、Ｆｅ−Ｓｉ、Ｆｅ−Ｂ、Ｆｅ−Ｐ、Ｃｕからなる原料をＦｅ８１．４Ｓｉ３Ｂ１０Ｐ５Ｃｕ０．６の合金組成になるように秤量し、高周波溶解にて溶解した。溶解した合金溶湯を１３００〜１５５０℃の範囲で保持した後、窒素雰囲気中において水アトマイズ法にて処理し、平均粒径４５μｍ程度で、結晶相部の割合が異なる５種類の合金粉末を作製した。なお、鋳込み温度が高いほど、冷却すべき熱量が多くなり、急冷速度が低下するため、結晶の析出量が多くなる。結晶化に伴う発熱反応は示差走査型熱量分析計（ＤＳＣ）を用いて、毎分４０℃の昇温速度にて評価した。結晶相部の割合、非晶質相部の厚みについては、実施の形態において記述した方法にて求めている。
(Examples 1-3, Comparative Examples 1 and 2)
The raw material consisting of Fe, Fe-Si, Fe-B, Fe-P and Cu was weighed so as to have an alloy composition of Fe 81.4 Si 3 B 10 P 5 Cu 0.6 and dissolved by high-frequency dissolution. After the molten alloy melt was held in the range of 1300 to 1550 ° C., it was processed by a water atomization method in a nitrogen atmosphere, and five types of alloy powders having an average particle size of about 45 μm and different proportions of crystal phase portions were produced. . As the casting temperature is higher, the amount of heat to be cooled increases, and the rapid cooling rate decreases, so that the amount of precipitated crystals increases. The exothermic reaction accompanying crystallization was evaluated using a differential scanning calorimeter (DSC) at a heating rate of 40 ° C. per minute. The ratio of the crystal phase part and the thickness of the amorphous phase part are obtained by the method described in the embodiment.
圧粉磁心の作製については、軟磁性合金粉末と、当該軟磁性合金粉末に対して重量比で２．５％となる熱硬化性バインダを混合し、５００μｍのメッシュを通して造粒した。造粒粉４．５ｇを金型に入れ、油圧式自動プレス機により圧力９８０ＭＰａにて成型し、外径２０ｍｍ−内径１３ｍｍの円筒形状の圧粉体を作製した。赤外線加熱装置を用いて、４５０℃まで毎分４０℃の昇温速度となるように圧粉体を加熱し、４５０℃にて１０分間保持した後、空冷し、圧粉磁心を得た。電磁気特性については、Ｂ−Ｈアナライザを用いて、周波数２０ｋＨｚ−磁束密度１００ｍＴにおけるコアロスＰｃｖを評価した。なお、熱処理後の粉末における結晶粒径および体積分率については、実施の形態において記述した方法にて測定している。表１に、アトマイズ後（熱処理前）の粉末特性および熱処理後の各種評価結果を示す。 For the production of the dust core, a soft magnetic alloy powder and a thermosetting binder having a weight ratio of 2.5% with respect to the soft magnetic alloy powder were mixed and granulated through a 500 μm mesh. 4.5 g of the granulated powder was put into a mold and molded at a pressure of 980 MPa by a hydraulic automatic press machine to produce a cylindrical green compact having an outer diameter of 20 mm and an inner diameter of 13 mm. Using an infrared heating device, the green compact was heated to 450 ° C. at a rate of 40 ° C. per minute, held at 450 ° C. for 10 minutes, and then air-cooled to obtain a dust core. For the electromagnetic characteristics, a core loss Pcv at a frequency of 20 kHz and a magnetic flux density of 100 mT was evaluated using a BH analyzer. Note that the crystal grain size and volume fraction of the heat-treated powder are measured by the method described in the embodiment. Table 1 shows the powder characteristics after atomization (before heat treatment) and various evaluation results after heat treatment.
表１より、実施例１〜３においては、アトマイズ後（熱処理前）の粉末が５０重量％未満の結晶層（結晶相部）を有しており、粉末外表面より２μｍ以上の厚みにて非晶質層（非晶質相を主相とする非晶質相部）を有することから、熱処理における急激な発熱が抑制され、熱処理後には、粉末外周部では４０ｎｍ以下、粉末中心部では６０ｎｍ以下の微細な結晶が析出した組織となり、５００ｋＷ／ｍ３以下の低コアロス特性を有する圧粉磁心を作製できていることがわかる。一方、アトマイズ後の粉末が５０重量％以上の結晶相部を有する比較例１及び比較例２においては、粉末中心部にて結晶粒が粗大化しており、コアロス特性が劣化している。実施例１〜３と、比較例１及び２とを比較すると、アトマイズ後の結晶相（結晶相部）の割合が大きくなるほど、熱処理後における粉末中心部の結晶粒が大きくなっており、粉末外周部の結晶粒は小さくなっている。粉末中心部については、上述した理由により、アトマイズ後の結晶相部の割合が大きい粉末では、急冷速度が低下しているため、アトマイズ時に生成した結晶が粗大化することを反映している。粉末外周部付近の結晶粒は、熱処理工程によって析出したものであるから、アトマイズ後の結晶相部の割合が大きいほど、熱処理工程において急激な発熱反応が抑えられ、微細な組織が形成できることを表している。 From Table 1, in Examples 1 to 3, the powder after atomization (before heat treatment) has a crystal layer (crystal phase part) of less than 50% by weight, and the thickness is 2 μm or more from the outer surface of the powder. Since it has a crystalline layer (amorphous phase part having an amorphous phase as a main phase), rapid heat generation during heat treatment is suppressed, and after the heat treatment, 40 nm or less at the powder outer periphery and 60 nm or less at the powder center part. It can be seen that a dust core having a low core loss characteristic of 500 kW / m 3 or less can be produced. On the other hand, in Comparative Example 1 and Comparative Example 2 in which the powder after atomization has a crystal phase part of 50% by weight or more, the crystal grains are coarsened at the center part of the powder, and the core loss characteristics are deteriorated. Comparing Examples 1 to 3 with Comparative Examples 1 and 2, the larger the ratio of the crystal phase (crystal phase part) after atomization, the larger the crystal grains in the powder center part after heat treatment, The crystal grains in the part are small. For the powder center portion, for the reason described above, the powder having a large proportion of the crystal phase portion after atomization reflects the fact that the crystal generated during atomization becomes coarse because the rapid cooling rate is reduced. Since the crystal grains near the outer periphery of the powder are precipitated by the heat treatment step, the larger the proportion of the crystal phase portion after atomization, the more rapid the exothermic reaction is suppressed in the heat treatment step, and the more the fine structure can be formed. ing.
（実施例４〜６、比較例３〜５）
Ｆｅ、Ｆｅ−Ｓｉ、Ｆｅ−Ｂ、Ｆｅ−Ｐ、Ｃｕからなる原料をＦｅ８１．３Ｓｉ５Ｂ９Ｐ４Ｃｕ０．７の合金組成になるように秤量し、高周波溶解にて溶解した。溶解した合金溶湯を１３００〜１５５０℃の範囲で保持した後、窒素雰囲気中において水アトマイズ法にて処理し、平均粒径１０μｍ程度で、結晶相部の割合が異なる６種類の軟磁性合金粉末を作製した。なお、鋳込み温度が高いほど、冷却すべき熱量が多くなり、急冷速度が低下するため、結晶の析出量が多くなる。結晶化に伴う発熱反応は示差走査型熱量分析計（ＤＳＣ）を用いて、毎分４０℃の昇温速度にて評価した。結晶相部部の割合、非晶質相部の厚みについては、実施の形態において記述した方法にて求めている。
(Examples 4-6, Comparative Examples 3-5)
The raw material consisting of Fe, Fe-Si, Fe-B, Fe-P and Cu was weighed so as to have an alloy composition of Fe 81.3 Si 5 B 9 P 4 Cu 0.7 and dissolved by high-frequency dissolution. After holding the molten alloy in a range of 1300 to 1550 ° C., it is treated by a water atomization method in a nitrogen atmosphere, and six types of soft magnetic alloy powders having an average particle size of about 10 μm and different proportions of crystal phase portions are obtained. Produced. As the casting temperature is higher, the amount of heat to be cooled increases, and the rapid cooling rate decreases, so that the amount of precipitated crystals increases. The exothermic reaction accompanying crystallization was evaluated using a differential scanning calorimeter (DSC) at a heating rate of 40 ° C. per minute. The ratio of the crystal phase portion and the thickness of the amorphous phase portion are obtained by the method described in the embodiment.
圧粉磁心の作製については、軟磁性合金粉末と、当該軟磁性合金粉末に対して重量比で４％となる熱硬化性バインダを混合し、５００μｍのメッシュを通して造粒した。造粒粉２．５ｇを金型に入れ、油圧式自動プレス機により圧力９８０ＭＰａにて成型し、外径１３ｍｍ−内径８ｍｍの円筒形状の圧粉体を作製した。赤外線加熱装置を用いて、４４０℃まで毎分４０℃の昇温速度となるように圧粉体を加熱し、４４０℃にて１０分間保持した後、空冷し、圧粉磁心を得た。電磁気特性については、Ｂ−Ｈアナライザを用いて、周波数３００ｋＨｚ−磁束密度５０ｍＴにおけるコアロスＰｃｖを測定し、評価した。また、振動試料型磁力計（ＶＳＭ）を用いて１５００ｋＡ／ｍの磁場にて測定した飽和磁化より、飽和磁束密度を算出した。なお、熱処理後の粉末における結晶粒径および体積分率については、実施の形態において記述した方法にて測定している。表２に、アトマイズ後（熱処理前）の粉末特性および熱処理後の各種評価結果を示す。 For the production of the dust core, a soft magnetic alloy powder and a thermosetting binder having a weight ratio of 4% with respect to the soft magnetic alloy powder were mixed and granulated through a 500 μm mesh. The granulated powder (2.5 g) was put in a mold and molded by a hydraulic automatic press at a pressure of 980 MPa to prepare a cylindrical green compact having an outer diameter of 13 mm and an inner diameter of 8 mm. Using an infrared heating device, the green compact was heated to 440 ° C. so as to have a temperature rising rate of 40 ° C. per minute, held at 440 ° C. for 10 minutes, and then air-cooled to obtain a dust core. The electromagnetic characteristics were evaluated by measuring the core loss Pcv at a frequency of 300 kHz and a magnetic flux density of 50 mT using a BH analyzer. Further, the saturation magnetic flux density was calculated from the saturation magnetization measured in a magnetic field of 1500 kA / m using a vibrating sample magnetometer (VSM). Note that the crystal grain size and volume fraction of the heat-treated powder are measured by the method described in the embodiment. Table 2 shows the powder characteristics after atomization (before heat treatment) and various evaluation results after heat treatment.
表２より、実施例４〜６及び比較例４、５のいずれにおいても、アトマイズ後（熱処理前）の粉末は５０重量％未満の結晶相（結晶相部）を有しており、熱処理後については、粉末外周部では４０ｎｍ以下、粉末中心部では６０ｎｍ以下の微細な結晶が析出した組織となっている。一方、アトマイズ後の粉末が結晶相部を有していない（即ち、結晶相の割合が０質量％である）比較例３においては、熱処理後において、粉末の外周部及び中心部共に結晶粒径が４０ｎｍ以上となっており、結晶の粗大化が生じている。アトマイズ後における非晶質層（非晶質相部）の厚みが２μｍ以上である実施例４〜６では、２μｍ未満の比較例４及び５に対して、充填率が低下することなく、１５００ｋＷ／ｍ３以下の低コアロス特性を有する圧粉磁心を作製できていることがわかる。これは、軟磁性合金粉末の方がナノ結晶合金に比べてビッカース硬さが小さいために、加圧成形する際に変形しやすく、充填性が高まるためである。なお、前述の実施例１〜３及び比較例１、２と併せて比較すると、非晶質相部の厚みが増加するほど、充填率は高くなる傾向があるが、５μｍ以上の場合にはほぼ一定となることがわかる。 From Table 2, in any of Examples 4 to 6 and Comparative Examples 4 and 5, the powder after atomization (before heat treatment) has a crystal phase (crystal phase part) of less than 50% by weight. Has a structure in which fine crystals of 40 nm or less are precipitated at the outer periphery of the powder and 60 nm or less are precipitated at the center of the powder. On the other hand, in Comparative Example 3 in which the powder after atomization does not have a crystal phase portion (that is, the proportion of the crystal phase is 0% by mass), both the outer peripheral portion and the central portion of the powder after the heat treatment have a crystal grain size. Is 40 nm or more, and the crystal is coarsened. In Examples 4 to 6 in which the thickness of the amorphous layer (amorphous phase portion) after atomization is 2 μm or more, the filling rate does not decrease compared to Comparative Examples 4 and 5 of less than 2 μm, 1500 kW / It can be seen that a dust core having a low core loss characteristic of m 3 or less can be produced. This is because the soft magnetic alloy powder is smaller in Vickers hardness than the nanocrystalline alloy, so that it is easily deformed during pressure forming and the filling property is increased. In addition, when compared with Examples 1 to 3 and Comparative Examples 1 and 2 described above, the filling rate tends to increase as the thickness of the amorphous phase portion increases. It turns out that it becomes constant.
なお、アトマイズ後の結晶相部の割合がそれぞれ１０重量％及び１９重量％である実施例５及び実施例６においては、熱処理後に、粉末外周部付近では３０ｎｍ未満、粉末中心部では３５ｎｍ未満の結晶粒径を有する良好な微細構造が形成され、１２００ｋＷ／ｍ３以下の非常にロスの低い圧粉磁心を作製することができており、アトマイズ時に大きな結晶が生成するのを回避しつつ、急激な発熱を抑制する効果が特に高いことがわかる。 In Examples 5 and 6 in which the proportions of the crystal phase part after atomization are 10% by weight and 19% by weight, respectively, after heat treatment, crystals of less than 30 nm in the vicinity of the powder outer periphery and less than 35 nm in the powder center part. A fine microstructure having a grain size is formed, and a powder core having a very low loss of 1200 kW / m 3 or less can be produced, while avoiding the formation of large crystals during atomization, It can be seen that the effect of suppressing heat generation is particularly high.
（実施例７〜１０）
Ｆｅ、Ｆｅ−Ｓｉ、Ｆｅ−Ｂ、Ｆｅ−Ｐ、Ｃｕからなる原料をＦｅ８０．３Ｓｉ５Ｂ１０Ｐ４Ｃｕ０．７（実施例７）、Ｆｅ８１．４Ｓｉ５Ｂ６Ｐ７Ｃｕ０．６（実施例８）、Ｆｅ８２．４Ｓｉ１Ｂ１１Ｐ５Ｃｕ０．６（実施例９）Ｆｅ８３．３Ｓｉ４Ｂ８Ｐ４Ｃｕ０．７（実施例１０）の夫々の合金組成になるように秤量し、高周波溶解にて溶解した。溶解した合金溶湯を１３００〜１４００℃の範囲で保持した後、窒素雰囲気中において水アトマイズ法にて処理し、平均粒径４５μｍ程度の合金粉末を作製した。結晶化に伴う発熱反応は示差走査型熱量分析計（ＤＳＣ）を用いて、毎分４０℃の昇温速度にて評価した。結晶相部の割合、非晶質相部の厚みについては、実施の形態において記述した方法にて求めている。
(Examples 7 to 10)
Fe 80.3 Si 5 B 10 P 4 Cu 0.7 (Example 7), Fe 81.4 Si 5 B 6 P 7 Cu are raw materials made of Fe, Fe—Si, Fe—B, Fe—P, and Cu. 0.6 (Example 8), Fe 82.4 Si 1 B 11 P 5 Cu 0.6 (Example 9) Fe 83.3 Si 4 B 8 P 4 Cu 0.7 (Example 10) They were weighed so as to have an alloy composition and dissolved by high frequency melting. After the molten alloy melt was held in the range of 1300 to 1400 ° C., it was processed by a water atomization method in a nitrogen atmosphere to produce an alloy powder having an average particle size of about 45 μm. The exothermic reaction accompanying crystallization was evaluated using a differential scanning calorimeter (DSC) at a heating rate of 40 ° C. per minute. The ratio of the crystal phase part and the thickness of the amorphous phase part are obtained by the method described in the embodiment.
圧粉磁心の作製については、軟磁性合金粉末と、軟磁性合金粉末に対して重量比で２．５％となる熱硬化性バインダを混合し、５００μｍのメッシュを通して造粒した。造粒粉４．５ｇを金型に入れ、油圧式自動プレス機により圧力９８０ＭＰａにて成型し、外径２０ｍｍ−内径１３ｍｍの円筒形状の圧粉体を作製した。赤外線加熱装置を用いて、４５０℃まで毎分４０℃の昇温速度となるように圧粉体を加熱し、表３に示した熱処理条件にて熱処理を施した後に、空冷し、圧粉磁心を得た。電磁気特性については、Ｂ−Ｈアナライザを用いて、周波数２０ｋＨｚ−磁束密度１００ｍＴにおけるコアロスＰｃｖを測定し、評価した。また、振動試料型磁力計（ＶＳＭ）を用いて１５００ｋＡ／ｍの磁場にて測定した飽和磁化より、飽和磁束密度を算出した。なお、熱処理後の粉末における結晶粒径および体積分率については、実施の形態において記述した方法にて測定している。表３に、アトマイズ後（熱処理前）の粉末特性および熱処理後の各種評価結果を示す。 For the production of the powder magnetic core, a soft magnetic alloy powder and a thermosetting binder having a weight ratio of 2.5% with respect to the soft magnetic alloy powder were mixed and granulated through a 500 μm mesh. 4.5 g of the granulated powder was put into a mold and molded at a pressure of 980 MPa by a hydraulic automatic press machine to produce a cylindrical green compact having an outer diameter of 20 mm and an inner diameter of 13 mm. Using an infrared heating device, the green compact was heated to 450 ° C. at a rate of 40 ° C. per minute, heat-treated under the heat treatment conditions shown in Table 3, then air-cooled, and the dust core Got. The electromagnetic characteristics were evaluated by measuring the core loss Pcv at a frequency of 20 kHz and a magnetic flux density of 100 mT using a BH analyzer. Further, the saturation magnetic flux density was calculated from the saturation magnetization measured in a magnetic field of 1500 kA / m using a vibrating sample magnetometer (VSM). Note that the crystal grain size and volume fraction of the heat-treated powder are measured by the method described in the embodiment. Table 3 shows the powder characteristics after atomization (before heat treatment) and various evaluation results after heat treatment.
表３より、実施例７〜１０においては、アトマイズ後（熱処理前）の粉末が５０重量％未満の結晶相（結晶相部）を有しており、粉末外表面より５μｍ以上の厚みにて非晶質層（非晶質相部）を有することから、熱処理工程における急激な発熱が抑制され、熱処理後には、粉末外周部では４０ｎｍ以下、粉末中心部では６０ｎｍ以下の微細な結晶が析出した組織となり、５００ｋＷ／ｍ３以下の低コアロス特性を有する圧粉磁心を作製できていることがわかる。特に、アトマイズ後の結晶相部の割合が３０重量％以下であり、結晶化後の粉末外周部の結晶粒径が３０ｎｍ未満、粉末中心部の結晶粒径が３５ｎｍ未満である実施例７〜９においては、２５０ｋＷ／ｍ３以下の非常にロスの低い圧粉磁心を作製することができている。 From Table 3, in Examples 7 to 10, the powder after atomization (before heat treatment) has a crystal phase (crystal phase part) of less than 50% by weight and has a thickness of 5 μm or more from the outer surface of the powder. Since it has a crystalline layer (amorphous phase part), rapid heat generation in the heat treatment process is suppressed, and after heat treatment, a structure in which fine crystals of 40 nm or less in the powder outer peripheral part and 60 nm or less in the powder central part are precipitated. Thus, it can be seen that a dust core having a low core loss characteristic of 500 kW / m 3 or less can be produced. In particular, Examples 7 to 9 in which the ratio of the crystal phase part after atomization is 30% by weight or less, the crystal grain size of the powder outer peripheral part after crystallization is less than 30 nm, and the crystal grain size of the powder center part is less than 35 nm. Can produce a dust core with a very low loss of 250 kW / m 3 or less.
（実施例１１〜１３）
Ｆｅ、Ｆｅ−Ｓｉ、Ｆｅ−Ｂ、Ｆｅ−Ｐ、Ｃｕからなる原料をＦｅ８３．４Ｂ１０Ｐ６Ｃｕ０．６（実施例１１）、Ｆｅ８２．４Ｂ１０Ｐ６Ｃ１Ｃｕ０．６（実施例１２）、Ｆｅ８２．３Ｂ１０Ｓｉ３Ｐ３Ｃ１Ｃｕ０．７（実施例１３）の夫々の合金組成になるように秤量し、高周波溶解にて溶解した。溶解した合金溶湯を１３００〜１４００℃の範囲で保持した後、窒素雰囲気中において水アトマイズ法にて処理し、平均粒径４５μｍ程度の合金粉末を作製した。結晶化に伴う発熱反応は示差走査型熱量分析計（ＤＳＣ）を用いて、毎分４０℃の昇温速度にて評価した。結晶相部の割合、非晶質相部の厚みについては、実施の形態において記述した方法にて求めている。
(Examples 11 to 13)
Fe 83.4 B 10 P 6 Cu 0.6 (Example 11), Fe 82.4 B 10 P 6 C 1 Cu 0. The raw material consisting of Fe, Fe-Si, Fe-B, Fe-P, Cu was used . 6 (Example 12) and Fe 82.3 B 10 Si 3 P 3 C 1 Cu 0.7 (Example 13) were weighed so as to have respective alloy compositions and dissolved by high-frequency dissolution. After the molten alloy melt was held in the range of 1300 to 1400 ° C., it was processed by a water atomization method in a nitrogen atmosphere to produce an alloy powder having an average particle size of about 45 μm. The exothermic reaction accompanying crystallization was evaluated using a differential scanning calorimeter (DSC) at a heating rate of 40 ° C. per minute. The ratio of the crystal phase part and the thickness of the amorphous phase part are obtained by the method described in the embodiment.
圧粉磁心の作製については、軟磁性合金粉末と、当該軟磁性合金粉末に対して重量比で２．５％となる熱硬化性バインダを混合し、５００μｍのメッシュを通して造粒した。造粒粉４．５ｇを金型に入れ、油圧式自動プレス機により圧力９８０ＭＰａにて成型し、外径２０ｍｍ−内径１３ｍｍの円筒形状の圧粉体を作製した。赤外線加熱装置を用いて、４５０℃まで毎分４０℃の昇温速度となるように圧粉体を加熱し、表４に示した熱処理条件にてナノ結晶化熱処理を施した後に、空冷し、圧粉磁心を得た。電磁気特性については、Ｂ−Ｈアナライザを用いて、周波数２０ｋＨｚ−磁束密度１００ｍＴにおけるコアロスＰｃｖを測定し、評価した。なお、熱処理後の粉末における結晶粒径および体積分率については、実施の形態において記述した方法にて測定している。また、振動試料型磁力計（ＶＳＭ）を用いて１５００ｋＡ／ｍの磁場にて測定した飽和磁化より、飽和磁束密度を算出した。表４に、アトマイズ後（熱処理前）の粉末特性および熱処理後の各種評価結果を示す。 For the production of the dust core, a soft magnetic alloy powder and a thermosetting binder having a weight ratio of 2.5% with respect to the soft magnetic alloy powder were mixed and granulated through a 500 μm mesh. 4.5 g of the granulated powder was put into a mold and molded at a pressure of 980 MPa by a hydraulic automatic press machine to produce a cylindrical green compact having an outer diameter of 20 mm and an inner diameter of 13 mm. Using an infrared heating device, the green compact was heated to 450 ° C. at a rate of 40 ° C. per minute, subjected to nanocrystallization heat treatment under the heat treatment conditions shown in Table 4, and then air-cooled. A dust core was obtained. The electromagnetic characteristics were evaluated by measuring the core loss Pcv at a frequency of 20 kHz and a magnetic flux density of 100 mT using a BH analyzer. Note that the crystal grain size and volume fraction of the heat-treated powder are measured by the method described in the embodiment. Further, the saturation magnetic flux density was calculated from the saturation magnetization measured in a magnetic field of 1500 kA / m using a vibrating sample magnetometer (VSM). Table 4 shows the powder characteristics after atomization (before heat treatment) and various evaluation results after heat treatment.
また、実施例１１〜１３に加えて、上述した実施例７〜１０における熱処理後粉に占める結晶層の割合と飽和磁束密度との関係を表５に示す。 Further, in addition to Examples 11 to 13, Table 5 shows the relationship between the ratio of the crystal layer in the powder after heat treatment in Examples 7 to 10 and the saturation magnetic flux density.
表５より、中心部及び外周部の夫々の非晶質中に占める結晶粒の割合（体積分率）が多いほど、高い飽和磁束密度Ｂｓが得られることがわかる。このような高い飽和磁束密度Ｂｓを得ることとすれば、コア等の応用製品の小型化に対して有利となる。具体的には、実施例７〜実施例１３のいずれにおいても、結晶粒の体積分率が３５ｖｏｌ％以上であり、１．６０Ｔ以上の飽和磁束密度Ｂｓが得られている。このうち、中心部及び外周部の少なくともどちらかの結晶粒の体積分率が５０ｖｏｌ％以上である実施例９〜実施例１３においては、１．７０Ｔ以上の飽和磁束密度Ｂｓが得られている。特に、中心部及び外周部いずれの結晶粒の体積分率も５０ｖｏｌ％以上である実施例１０、実施例１１及び実施例１３においては、１．７３Ｔ以上の高い飽和磁束密度Ｂｓが得られている。 From Table 5, it can be seen that the higher the ratio (volume fraction) of the crystal grains in the amorphous material in the central part and the outer peripheral part, the higher the saturation magnetic flux density Bs can be obtained. Obtaining such a high saturation magnetic flux density Bs is advantageous for downsizing of applied products such as cores. Specifically, in any of Examples 7 to 13, the volume fraction of crystal grains is 35 vol% or more, and a saturation magnetic flux density Bs of 1.60 T or more is obtained. Among these, in Examples 9 to 13 in which the volume fraction of crystal grains in at least one of the central part and the outer peripheral part is 50 vol% or more, a saturation magnetic flux density Bs of 1.70 T or more is obtained. Particularly, in Example 10, Example 11 and Example 13 in which the volume fraction of crystal grains in both the central part and the outer peripheral part is 50 vol% or more, a high saturation magnetic flux density Bs of 1.73 T or more is obtained. .
上述した実施の形態では、圧粉磁心およびその作製方法に適用可能であるが、他の磁性部品（磁性シートなど）およびその作製方法に利用することもできる In the above-described embodiment, the present invention can be applied to a dust core and a manufacturing method thereof, but can also be used for other magnetic components (such as a magnetic sheet) and a manufacturing method thereof.
１ アトマイズ後粉末
２ アトマイズ後粉末の外周付近の拡大図
３ 結晶粒（結晶相部）
４ 非晶質相（非晶質相部）
１０ ＤＳＣ曲線
１１ 第１ピーク
１２ 第１立ち上がり部
１５ 第２ピーク
１６ 第２立ち上がり部
２０、２１ ベースライン
３２ 第１上昇接線
４２ 第２上昇接線
1 Powder after
4 Amorphous phase (amorphous phase part)
10 DSC curve 11
Claims (4)
前記軟磁性合金粉末と結合剤とを混合する工程と、
前記結合剤と混合された前記軟磁性合金粉末を加圧成型する工程と、
成型された前記軟磁性合金粉末を熱処理する工程と、を含み、
熱処理工程前の前記軟磁性合金粉末は、結晶相を主相とする結晶相部及び非晶質相を主相とする非晶質相部を有する軟磁性合金粉末粒を有しており、
当該軟磁性合金粉末粒における前記結晶相部の割合は、３重量％以上５０重量％未満であり、
前記軟磁性合金粉末粒の中心部には、前記結晶相部が位置しており、
前記軟磁性合金粉末粒の外周部には、前記非晶質相部が位置しており、
熱処理された前記軟磁性合金粉末粒の前記中心部には粒径６０ｎｍ未満の結晶粒が３５ｖｏｌ％以上分散しており、
熱処理された前記軟磁性合金粉末粒の前記外周部には粒径４０ｎｍ未満の結晶粒が３５ｖｏｌ％以上分散している、
圧粉磁芯の製造方法。 Represented by a composition formula Fe a B b Si c P x C y Cu z, 79 ≦ a ≦ 86at%, 5 ≦ b ≦ 13at%, 0 ≦ c ≦ 8at%, 1 ≦ x ≦ 10at%, 0 ≦ y A step of generating a soft magnetic alloy powder satisfying ≦ 5 at%, 0.4 ≦ z ≦ 1.4 at%, and 0.06 ≦ z / x ≦ 1.20 using an atomizing method;
Mixing the soft magnetic alloy powder and a binder;
Pressure-molding the soft magnetic alloy powder mixed with the binder;
Heat-treating the molded soft magnetic alloy powder,
The soft magnetic alloy powder before the heat treatment step has soft magnetic alloy powder grains having a crystal phase portion having a crystal phase as a main phase and an amorphous phase portion having an amorphous phase as a main phase,
The proportion of the crystalline phase part in the soft magnetic alloy powder grains is 3% by weight or more and less than 50% by weight,
In the central part of the soft magnetic alloy powder grains, the crystal phase part is located,
In the outer peripheral portion of the soft magnetic alloy powder particles, the amorphous phase portion is located,
In the center part of the heat-treated soft magnetic alloy powder particles, crystal grains having a particle size of less than 60 nm are dispersed in an amount of 35 vol% or more,
In the outer peripheral portion of the heat-treated soft magnetic alloy powder particles, crystal grains having a particle size of less than 40 nm are dispersed in an amount of 35 vol% or more.
A method for producing a dust core.
前記軟磁性合金粉末粒における前記結晶相部の割合は、７重量％以上であるThe proportion of the crystal phase part in the soft magnetic alloy powder grains is 7% by weight or more.
圧粉磁芯の製造方法。A method for producing a dust core.
前記Ｆｅの３ａｔ％以下を、Ｔｉ、Ｖ、Ｚｒ、Ｈｆ、Ｎｂ、Ｔａ、Ｍｏ、Ｗ、Ｃｒ、Ｃｏ、Ｎｉ、Ａｌ、Ｍｎ、Ａｇ、Ａｕ、Ｚｎ、Ｓ、Ｃａ、Ｓｎ、Ａｓ、Ｓｂ、Ｂｉ、Ｎ、Ｏ、Ｍｇ、白金族元素、及び希土類元素のうち、１種類以上の元素で置換してなる、
圧粉磁芯の製造方法。 It is a manufacturing method of the dust core according to claim 1 or 2 ,
Fe, 3 at% or less of Ti, V, Zr, Hf, Nb, Ta, Mo, W, Cr, Co, Ni, Al, Mn, Ag, Au, Zn, S, Ca, Sn, As, Sb, Of Bi, N, O, Mg, platinum group elements, and rare earth elements, substituted with one or more elements,
A method for producing a dust core.
前記非晶質相部の前記軟磁性合金粉末粒における径方向の厚さは２μｍ以上である、
圧粉磁芯の製造方法。 It is a manufacturing method of the dust core according to any one of claims 1 to 3 ,
The thickness in the radial direction of the soft magnetic alloy powder grains of the amorphous phase part is 2 μm or more.
A method for producing a dust core.
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